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reference is made now in detail to a specific embodiment of the present invention , which illustrates the best mode presently contemplated by the inventor for practicing the invention . alternative embodiments are also briefly described as applicable . referring to fig1 a programmable array logic ( pal ) device 10 includes a programmable logic array 12 , a register pair 14 , a multiplexer 16 , input logic 18 , an observability buffer 20 , and a dual clock buffer 22 . associated with logic array 12 are a number of input buffers such as buffers 24 and 26 , a number of output buffers such as buffers 28 and 30 , and a number of data sense amplifiers such as those shown at 32 and 34 . external inputs and outputs to logic device 10 include pins 1 , 2 , 5 , and 11 as well as input pin 36 and i / 0 pins 38 and 40 . logic array 12 is preferably a fuse programmable and array and a fixed or array having a plurality of array inputs such as inputs 42a / b and 44a / b , a plurality of control inputs such as control input 46 , and a plurality of array outputs such as outputs 48 , 50 , 52 , 54 , and 56 . alternatively or additionally , logic array 12 can include a fuse programmable or array . the manufacture and use of a logic array 12 is well known to those skilled in the art , and will not be discussed here in detail . a good reference describing pal architecture is the programmable array logic handbook published by advanced micro devices , inc . of sunnyvale , calif . input buffer 24 couples input pin 36 to array input lines 42a and 42b . more specifically , input pin 36 is coupled to the input of a first inverter 58 , the output of which is coupled to array input 42b and to the input of a second inverter 60 which has an output coupled to array input 42a . thus , a signal applied to pin 36 is developed on input 42a , and its inverse is developed on input 42b . in an analogous manner , a signal applied to pin 38 develops a signal on input 44a , and an inverse signal on input 44b . array outputs 48 and 50 are inverted by inverters 28 and 30 , respectively , to produce a synchronous preset ( sp ) signal on a line 62 , and an asynchronous reset ( ar ) signal on a line 64 . data sense amplifier 32 includes a first inverter 66 and a second inverter 68 which produce a data ( d ) signal on a line 70 and an inverse data signal ( id ) on a line 72 . similarly , data sense amplifier 34 produces a data signal ( d ) on a line 74 and an inverse data signal ( id ) on a line 76 . the register pair 14 includes a buried register 78 and an output register 80 . both buried register 78 and output register 80 include a preload enable ( p ) input , an inverse data input ( id ), a data input ( d ), an asynchronous reset input ( ar ), a synchronous preset input ( sp ), a preload data input ( pd ), and a clock input ( ci ). buried register 78 has a data output qb , and output register 80 has a data output q . buried register 78 has its id and d inputs coupled to lines 76 and 74 , respectively , and its ar and sp inputs coupled to lines 64 and 62 , respectively . output register 80 has its id and d inputs coupled to lines 72 and 70 , respectively , and its ar and sp inputs coupled to lines 64 and 62 , respectively . the p inputs of buried register 78 and output register 80 are both coupled to a line 82 , and their pd inputs are coupled to i / 0 pin 40 by a line 84 . multiplexer 16 has a q input which is coupled to the q output of output register 80 , and a qb input which is coupled to the qb output of buried registers 78 . multiplexer 16 also has an iobs select input coupled to a line 86 , and an obs select input coupled to a line 88 . the iobs and obs select inputs determine which of data inputs q and qb is multiplexed to line 84 and thus to i / 0 in 40 . input logic 18 includes a zenered buffer 90 , a zenered inverter 92 , a zenered nor gate 94 , a zenered or gate 96 , a zenered inverter 98 , and a pair of nand gates 100 and 102 . zenered gates 90 - 98 are tri - level logic devices having input logic levels lo , hi , and zhi . in ttl implementations of the present device , a lo input is no more than 0 . 8 volts , a hi input is no less than 2 . 0 volts , and a zhi input is nominally 11 volts . while the - outputs of zenered gates 90 - 98 have internal logic levels that are either lo or hi , only zhi is recognized as a logical high input to the zenered gates . thus , applying zhi to the input of zenered buffer 90 produces an internal logic level hi on line 82 , and applying a lo or hi to the input of zenered buffer 90 produces an internal logic level lo on line 82 . the rest of the gates of logic device 10 are not zenered , and thus are responsive to and generate only lo and hi logic signals . pin 2 is coupled to a line 104 which is connected to inputs of zenered buffer 90 , zenered inverter 92 , and zenered nor gate 94 . zenered buffer 90 develops a preload enable signal ( preload ) on line 82 , zenered invertor 92 develops an inverted preload enable signal ( ipreen ) on a line 105 , and zenered nor gate 94 develops an observability disable ( obsd ) signal on a line 106 . pin 1 is connected to a line 108 which is coupled to dual clock buffer 22 , zenered nor gate 94 , and zenered or gate 96 . except during the program mode of the present device , pin 1 is used as an external clock input pin , and develops a clock signal on line 108 . the clock signal on line 108 can generally be considered to be the master clock for the device 10 . pin 11 is coupled by a line 110 to an input of zenered nor gate 94 and to an input of zenered or gate 96 . zenered or gate 96 develops a programming and verification ( pvcc ) signal on line 46 which is input to logic array 12 and to nand gates 100 and 102 . pin 5 is coupled to a line 112 which is input into zenered inverter 98 and to nand gate 100 . the output of nand gate 100 on a line 114 is input to nand gate 102 as the signal i5 . zenered inverter 98 develops an observe during preload signal ( iobspre ) on a line 116 , and nand gate 102 develops an observe during verify ( iobsver ) signal on a line 118 . the observability buffer 20 includes an and gate 120 and an or gate 122 . and gate 120 is coupled to line 56 of logic array 12 and to line 106 of input logic 18 . the output of and gate 120 is developed on a line 124 which is a non - inverted input to or gate 122 . or gate 122 has a pair of inverted inputs which are coupled to lines 116 and 118 of input logic 18 , and an inverted output on line 86 and a non - inverted output on a line 88 . the signal on line 88 is the observation signal ( obs ), and the signal on line 86 is the inverse observation signal ( iobs ). clock buffer 22 includes a pair of and gates 126 and 128 , and a pair of or gates 130 and 132 . inverted inputs of and gates 126 and 128 are coupled to line 105 , and non - inverted inputs to and gates 126 and 128 are coupled to lines 86 and 88 , respectively . the outputs of and gates 126 and 128 on lines 134 and 136 , respectively , are input to or gates 130 and 132 , respectively . inverted inputs to or gates 130 and 132 are coupled to line 108 . or gate 130 develops a buried register clock signal ( cpb ) on a line 138 , and or gate 132 develops a output register clock signal ( cpo ) on a line 140 . line 138 is coupled to the clock input of buried register 78 , and line 140 is coupled to the clock input of output register 80 . as mentioned previously , logic device 10 operates on three input logic levels , namely lo , hi , and zhi . the logic device 10 has four modes of operation , namely the logic mode , the preload mode , the verify mode , and the program mode . of these four modes , the first three are associated with observing the contents of register pair 14 , and the program mode is used to program the logic array 12 . the four modes of operation will be discussed one at a time , commencing with the observability modes , and finishing with the programming mode . the logic mode of operation of logic device 10 will be discussed with reference to fig1 a , and 2b . fig2 a is a truth table for the various input , output , ard internal signals found in logic device 10 , and fig2 b is the legend for fig2 a . the encircled letters a - p in fig1 correspond to the encircled letters a - p of fig2 a . when in the logic mode , data of either output register 80 or of buried state register 78 can be observed under user control by producing an obspt signal on line 56 . to observe the data of output register 80 , the obspt signal on line 56 must be lo , and to observe the data of the buried state register 78 the obspt on line 56 must be hi . the obspt is produced within logic array 12 from the various inputs 36 and 38 . when in the logic mode , none of pins 1 , 2 , 5 , or 11 are zenered . thus , the preload signal on line 82 is lo , the ipreen signal on line 105 is hi , the obsd signal on line 106 is hi , the iobspre signal d on line 116 is hi , and the iobsver signal on line 118 is hi . since the preload enable inputs of buried register 78 and output register 80 are not enabled by the preload signal , register pair 14 operate as standard set / reset ( sr ) or d - type registers . since the ipreen signal on line 105 is hi , the output signals at l and m of and gates 126 and 128 , respectively , are lo . therefore , the clock signal on line 108 is inverted by or gates 130 and 132 and are output on lines 138 and 140 , respectively , as clock signals cpb and cpo . it should be noted that when in the logic mode , clock signals cpb and cpo are synchronized , and are essentially an inverted image of the clock signal . therefore , buried registers 78 and output register 80 are clocked together during the logic mode , and the device 10 operates as if it only had a single clock . every clock cycle the buried register 78 and the output register 80 clock in data from the outputs of data sense amplifier 34 and 32 , respectively . the data being clocked into registers 78 and 80 will , after a short internal delay , show up at outputs qb and q , respectively . multiplexer 16 couples either the q output of output register 80 or the qb output of buried register 78 to line 84 under the control of the iobs and the obs signals on lines 86 and 88 , respectively . since the obsd signal on line 106 , the iobspre signal on line 116 , and the iobsver signal on line 118 are all hi , the obs signal on line 88 is essentially the same as the obspt signal on line 56 . when obs on line 88 is hi and iobs on line 86 is lo , qb is multiplexed to line 84 , and in the inverse case q is multiplexed to line 84 . thus , when in the logic mode , a logical hi signal on line 56 allows the observation of the contents of buried register 78 , while a logical lo signal on line 56 allows the observation of output register 80 . still referring to fig1 a , and 2b to preload the buried register 78 and output register 80 the pin 2 is raised to a zhi logic level , which causes the preload signal on line 82 to go hi , the ipreen signal on line 105 to go lo . and the obsd signal on line 106 to go lo . the hi on line 82 enables the preload inputs of buried register 78 and output register 80 . the hi on line 82 furthermore disables multiplexer 16 , causing its output on line 84 to be tri - stated via an inverted enable input en . the lo logic level ipreen signal on line 105 enables and gates 126 and 128 , and the lo logic level obsd signal on line 106 disables and gate 120 , causing the signal level on line 124 to go lo . if the input signal on pin 5 is lo or hi , the signal iobspre on line 116 will be hi , as will be the iobsver signal on line 118 . since the signal level on line 124 is lo , and the signals on lines 116 and 118 are hi , the obs signal on line 88 will be lo , and the iobs signal on line 86 will be hi . furthermore , since line 86 and 88 are also inputs to the clock buffer 22 , a hi signal for iobs and a lo signal for obs enables and gate 126 and disables and gate 128 . since the ipreen signal on line 105 is lo , the output of and gate 126 is hi and the output of and gate 128 on line 136 is lo . thus , the cpb signal on line 138 must always be hi , while the signal cpo on line 140 will be the inverse of the clock signal on line 108 . in consequence , only output register 80 will be clocked when pin 2 is at a zhi level and pin 5 is at a lo or hi level , and only output register 80 will be preloaded via a line 84 . if pin 5 is raised to zhi while pin 2 is still at a zhi level , iobspre on line 116 is forced lo which , in turn , forces obs on line 88 hi and iobs on line 86 lo . as mentioned previously , multiplexer 16 is disabled and its output on line 84 is tri - stated during the preload cycle . furthermore , the obs and iobs signals on lines 88 and 86 , respectively , disable and gate 126 and enable and gate 128 . thus , when obs is hi and iobs is lo , cpo on line 140 is hi while cpb on line 138 is essentially an inversion of the clock signal on line 108 . in consequence , only buried register 78 is clocked and thus only buried register 78 preloads data from line 84 . it is important to note that clock buffer 22 operates differently in the preload mode than it did in the logic mode . as mentioned previously , in the logic mode cpb and cpo were essentially the same clock signals . however , in the preload mode only one of the clock signals cpb and cpo is activated at a time under the control of the input signal applied to pin 5 . the preload waveforms will be discussed with reference to fig3 . time delays or periods are indicated by td , and are not necessarily to scale . during a first period 300 , pin 5 is raised to zhi if the buried state registers are to be preloaded , and is hi or lo if the output registers are to be loaded . during period 302 , pin 2 is raised to zhi to preload enable the buried register 78 and the output register 80 . after a time delay in period 304 , the preload data is clocked into the selected register during a period 306 . after time delay periods 308 and 310 the zhi logic level on pin 2 is removed and the preload cycle is completed . the verification mode can be used to verify product terms stored within logic array 12 . since all of the product terms are associated either with a buried register 78 or an output register 80 , it is necessary to clock the desired product term into a register and then observe the contents of that register . to enter the verification mode , pin 11 is forced to a zhi level which , in turn , forces obsd on line 106 to a lo , and pvcc on line 46 to a hi . the hi logic level pvcc signal on line 46 is input to logic array 12 to enable appropriate gates within the logic array so that individually selected product terms are developed on the array outputs 52 and 54 . the hi logic level pvcc signal is also input into nand gates 100 and 102 . as before , the lo logic level obsd signal on line 106 forces and gate 120 to output a lo logic level signal on line 124 . pin 5 is used to select either the output qb of buried register 78 or the output q of register 80 for observation . when pin 5 is lo , signal i5 on line 114 is hi and signal iobsver on line 118 is lo . this , in turn , forces obs on line 88 to go hi and iobs on line 86 to go lo . since ipreen on line 105 is hi , cpb on line 138 and cpo on line 140 are essentially inversions of the clock signal on line 108 . thus , individually selected product terms from logic array 12 are being loaded into buried register 78 and output register 80 on a clock pulse . with obs on line 88 hi , multiplexer 16 selects input qb for output on line 84 . when pin 5 is hi , signal i5 on line 114 is forced l0 and iobsver on line 118 is forced hi . since the signal on line 124 is lo , iobspre on line 116 is hi , and iobsver on line 118 is hi , the or gate 122 forces the obs signal on line 88 to a lo level and iobs on line 86 to a hi level . again , individually selected product terms from logic array are clocked into buried register 78 and output register 80 on a clock pulse . however , multiplexer 16 is caused to select input q for output on line 84 when pin 5 is forced hi . referring now to fig4 the verification waveforms will be discussed . as before , td represents a time delay or period , and is not necessarily to scale in the drawings . starting in period 410 , pin 11 is at the zhi level to force device 10 into its verification mode . after a time delay in period 410 , a clock signal is applied to pin 1 to permit individually selected product terms from logic array 12 to be clocked into buried register 78 and output register 80 . the data output at pin 40 is stable after the end of period 412 . referring now to fig1 and 4 , to enter the programming mode the clock signal , if present , is removed from pin 1 and a zhi signal is applied to pin 1 . the zhi level signal on line 108 forces obsd on line 106 to go lo , causing signal on line 124 to also go lo and the pvcc signal on line 46 to go hi . control logic within logic array 12 is activated by the hi level pvcc signal on line 46 to permit individually selected product terms within logic array 12 to be programmed . referring more particularly to the waveforms of fig4 after a settling period 400 , pin 1 is raised to zhi during period 402 . column addresses are applied to various input pins , and a programming voltage vop is applied to the device 10 during a period 404 . during period 406 , pin 11 is raised to zhi to blow the appropriate fuse of the individually selected product term . in the present implementation of device 10 , a blown fuse is a logical lo as verified on an appropriate output pin . with reference to fig5 an observability buffer 20 &# 39 ; includes a number of bipolar npn transistors 510 , 512 , 514 , 516 , 518 , 520 , and 522 ; a number of diodes ( rectifiers ) 524 , 526 , 528 , 530 , and 532 ; and a number of resistors 534 , 536 , 538 , 540 , 542 , 544 , 546 , and 548 . a fuse 550 is provided to balance a fuse within logic array 12 ( not shown ). when in the logic mode , obsd , iobspre , and iobsver are all hi , and the obspt signal on line 56 controls the outputs of observability buffer 20 &# 39 ;. when obspt is lo , the base of transistor 510 will be lo , causing the transistor to turn off . this will force the base of transistor 512 hi , causing it to conduct and thereby turning off transistor 514 and turning on transistor 516 . this , in turn , causes the obs signal on line 88 to go lo , turns off transistor 518 , turns on transistor 520 , and turns off transistor 522 to raise the iobs signal on line 86 to hi . when in the logic mode and when obspt is hi , transistor 510 is turned on , forcing the base of transistor 512 to a lo signal level . this causes transistor 512 to turn off , transistor 514 to turn on , and transistor 516 to turn off , causing the obs signal on line 88 to go hi . the base of transistor 518 is coupled to line 88 by diode 530 and will therefore also be at a hi logic level , turning on transistor 518 and 522 , with the result that the iobs signal on line 86 will go lo . in the preload mode , the obsd signal on line 106 is lo , which pulls the base of transistor 510 down to a lo logic level , shutting it off . in consequence , the obspt signal on line 56 is disabled . since , in the preload mode , the iobsver signal on line 118 is always hi , the iobspre signal on 116 will control the outputs of observability buffer 20 &# 39 ;. when the iobspre signal on line 116 is hi , transistor 512 is turned on , shutting off transistor 514 and turning on transistor 516 . the obs signal on line 88 will therefore be lo when the iobspre signal 116 is hi . the iobs signal on line 86 will be the inversion of the obs signal on line 88 ( i . e . hi ) because transistors 518 and 522 will be off , and transistor 520 will be on . when the iobspre signal on line 116 is lo , the base of transistor 512 is pulled lo , shutting off transistor 512 . this , in turn , turns on transistor 514 and turns off transistor 516 , causing the obs signal on line 88 to go hi and the iobs signal on line 86 to go lo . in the verify mode , the obsd signal on line 106 is lo which ensures that transistor 510 is off and that the cbspt signal on line 56 is disabled . since the iobspre signal on line 116 is always hi , the iobsver signal on line 118 controls the outputs of the observability buffer 20 &# 39 ;. the iobsver signal on line 118 controls the observability buffer 20 &# 39 ; during the verify mode in the same manner that the iobspre signal on line 116 controls the observability buffer 20 &# 39 ; during the preload mode . the observability buffer 20 &# 39 ; can be thought of as being comprised of three stages , namely an input stage 552 , a first inversion stage 554 , and a second inversion stage 556 . the input stage 552 is responsive to a first input signal obspt , a second input signal obsd , a third input signal iobspre , and a fourth input signal iobsver , and is operative to develop an intermediate signal on a line 558 . in effect , transistor 510 and diodes 524 and 526 cooperate to perform the logical nand operation on the obspt and obsd signals , and line 558 serves as a hard - wired and for the signal on the collector of transistor 510 and for the iobspre and iobsver signals . the first inversion stage 554 and the second inversion stage 556 are substantially identical , and are coupled together by diode 530 . it should be noted that the logic gates of observability buffer 20 of fig1 are slightly different than the logic embodied in the three stages of observability buffer 20 &# 39 ; of fig5 . this serves as an example that there are many possible logic gate combinations for the observability buffer which can produce the results shown in the truth table of fig2 a . the foregoing description of the preferred embodiment of the present invention has been presented for purposes of illustration and description . it is not intended to be exhaustive or to limit the invention to the precise form disclosed . obviously , many modifications and variations will be apparent to practitioners skilled in this art . it is possible that the invention may be practiced in many fabrication technologies in mos or bipolar processes . similarly , any process steps described might be interchangeable with other steps in order to achieve the same result . the embodiment was chosen and described in order to best explain the principles of the invention and its practical application , thereby enabling others skilled in the art to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated . it is intended that the scope of the invention be defined by the claims appended hereto and their equivalents . | 6 |
with reference to fig1 there is shown a preferred embodiment of the present invention , a duplex electrical connector 20 that is an assembly of a two - piece die cast connector body 22 including a front connector body 24 and a rear connector body 26 . the front connector body 24 and rear connector body 26 are slideably connectable to one another along lines 27 as shown in fig1 . the front connector body 24 includes a nose portion 28 and a leading end 30 and a trailing end 32 . a fastening arrangement 34 is included on the leading end of the front connector body 22 for fastening the duplex electrical connector 20 to an electrical panel or junction box ( not shown ). the fastening arrangement 34 includes a seat 36 on the nose portion 28 and a snap ring 38 that is shown exploded away from the leading end 30 of the front connector body 24 . the rear connector body 26 includes a leading end 40 , a trailing end 42 with two bores 44 therein , and a cable retaining ring 46 inserted in each trailing bore 44 . a throat insert 48 is inserted the nose portion 28 of the front connector body 26 and a fastener 50 secures the front connector body 24 and rear connector body 26 together . referring to fig2 - 4 , the front connector body 24 includes a top side 52 , a bottom side 54 , and a lip 56 extending from the top side 52 of the front connector body 24 at the trailing end 32 . a tab 58 extends from the lip 56 at the top side 52 of the front connector body 24 as shown in fig3 and includes an aperture 60 therein . the front connector body 24 further includes a leading flange 62 and an intermediate flange 64 surrounding the seat 36 . a trailing flange 65 extends along the bottom periphery of the trailing end 32 . the front connector body further includes rounded shoulders 66 . two viewports 68 are included on both the top side 52 and bottom side 54 of the front connector body 24 . with reference to fig5 - 7 , the front connector body 24 includes a wide bore 70 at the trailing end 32 narrowing to a narrower leading bore 72 . the interior walls 74 that form the transition from the wide bore 70 to the leading bore 72 are smooth , gradually arcuate , and devoid of sharp edges to enable easy passage of wire conductors from the wide bore 70 to the leading bore 72 . each viewport 68 on the top side 52 is axially aligned with a viewport on the bottom side 54 of the front connector body 24 as shown by axis 76 in fig7 . referring to fig8 - 10 , the rear connector body 26 includes a top side 78 , a bottom side 80 , and a front extension 82 extending from the leading end 40 . the front extension 82 extends from the lower half of the rear connector body and includes an open channel 84 therein . a boss 86 is included on the top side 78 of the rear connector body 26 and includes an aperture 88 therein . two semi - circular notches 90 are included in the front extension 82 . openings 92 a and 92 b are included in the rear connector body 26 , with each opening in communication with one of the trailing bores 44 . as shown in fig1 , the front extension 82 may include outer portions 82 a and an inner portion 82 b separated by the semi - circular notches 90 . as shown in fig1 and 15 , a rim 91 extends from the outer periphery 93 of the rear connector body 26 at the leading end 40 . with reference to fig1 and 17 , the duplex electrical connector 20 is assembled by securing front connector body 24 and rear connector body 26 together with fastener 50 to form a two - piece die cast connector body 22 . snap ring 38 , which is preferably a split ring formed of a resilient metal and in its unbiased state includes a diameter smaller than the diameter of the seat 36 , is slightly expanded to slip over the leading flange 62 and is then secured onto the seat 36 on the nose portion 28 of front connector body 24 . the snap ring 38 includes locking tangs 94 thereon . the locking tangs 94 will function to secure the leading end 30 of the duplex electrical connector 20 to an electrical box or panel . leading flange 62 and intermediate flange 64 surround the seat 36 and hold snap ring 38 in place on the connector . a cable retaining ring 46 , which is preferably a split ring formed of a resilient metal and in its unbiased state includes a diameter larger than the diameter of each of the trailing bores 44 , is slightly compressed and then slipped into each of the trailing bores 44 . locking tangs 96 on the cable retaining rings 46 snap into openings 92 a and 92 b in rear connector body 26 and hold the cable retaining rings securely within the trailing bores 44 . throat insert 48 , preferably constructed of plastic , is pressed into the leading bore 72 ( see fig6 ) of front connector body 24 and held therein by a friction fit . throat insert 48 , optional for use on the duplex electrical connector 20 , acts to shield wire conductors from the interior of the leading bore in order to minimize fraying or abrasion of the outer sheath of the conductors ( not shown ). with reference to fig1 and 19 , each cable retaining ring 46 includes three cable retaining tangs 98 extending inward of the cable retaining ring , including a center tang 98 a and two outer tangs 98 b . center tang 98 a includes a flat end 101 that is perpendicular to the sides 103 of the center tang . outer tangs 98 b include ends 105 that are angled with respect to the sides 107 of the outer tangs . the orientation of the tangs 98 a and 98 b with respect to the duplex connector are set by the arrangement of the openings 92 a and 92 b ( see fig1 ) in the rear connector body 26 . outer tangs 92 b are positioned such that the short sides 107 are oriented toward the center 109 of the duplex connector and toward opposing quadrants . as shown in fig1 , when an electrical cable is inserted within the left trailing bore 44 a , the tangs 98 a and 98 b in the left trailing bore push the cable toward the center of the connector and toward the right lower quadrant of the bore 44 a , or in the direction of arrow 111 in fig1 . when an electrical cable is inserted within the right trailing bore 44 b , the tangs 98 a and 98 b in the right trailing bore push the cable toward the center of the connector and toward left upper quadrant of the bore 44 b , or in the direction of arrow 113 in fig1 . the orientation of the tangs 98 a and 98 b therefore advantageously maintain separation of the electrical cables and direct them toward the center of the leading bore ( see fig6 ). referring to fig2 - 22 , to secure the two connector body portions 24 and 26 together , front connector body 24 is slid sideways with respect to rear connector body 26 in the direction of arrow 115 until trailing flange 65 of front connector body latches into open channel 84 on front extension 82 of rear connector body 26 . fastener 50 is then secured through aperture 60 in tab 58 of front connector body 24 into aperture 88 in rear connector body 26 . with reference to fig2 and 24 , the duplex electrical connector 20 includes a leading end 117 and a trailing end 119 . the connector is used to secure one or two electrical cables ( not shown ) to a panel or an electrical box . to operate the invention , leading end 117 is simply pressed into the knockout of an electrical box . locking tangs 94 on snap ring 38 , being constructed of resilient metal such as spring steel , deflect inward when in contact with the walls of the knockout and then spring outward to their unbiased position after clearing the wall . the leading end is then securely locked into the knockout in the electrical box . one or two electrical cables ( not shown ) are then inserted into the bores 44 on the trailing end 119 of the duplex connector 20 . the three cable retaining tangs 98 a and 98 b ( see fig1 ), then direct each electrical cable to the center of the connector and the proper quadrant , after which the electrical cables are locked securely to the duplex connector 20 . the types of electrical cables and conduits that can be connector to an electrical box with the duplex electrical connector 20 include mc / hcf steel or aluminum cable , ac / hcf steel or aluminum cable , flexible metal conduit steel and aluminum , including both regular and reduced wall thickness , and mc cable continuous corrugated aluminum . with reference to fig1 , the present invention provides a method for securing an electrical cable to an electrical box , the method including : a . providing a duplex fitting 20 including a front connector body 24 having a leading end 30 , a trailing end 32 including a lip 56 and a trailing flange 65 , and a tab 58 with an aperture 68 therein ; b . providing a rear connector body 26 having a leading end 40 including a front extension 82 , an open channel 84 , and a rim 91 , and a boss 86 with a bore 88 therein ; c . pressing the trailing end 32 of the front connector body 24 against the leading end 40 of the rear connector body 26 ; d . sliding the trailing end 32 of the front connector body 24 along the leading end 40 of the rear connector body 26 until the trailing flange 65 of the front connector body 24 engages the open channel 84 in the rear connector body 26 and the lip 56 of the front connector body 24 engages the rim of the rear connector body 26 ; and e . threading a screw 50 through the aperture 68 in the tab 58 of said front connector body 24 and into the bore 88 of the boss 86 of the rear connector body 26 . preferably , the front connector body 24 and rear connector body 26 are each die - cast in one - piece of zinc alloy . the snap ring 38 and cable retaining rings 46 are preferably constructed of spring steel . the throat insert 48 is preferably constructed of plastic . although the description above contains many specific descriptions , materials , and dimensions , these should not be construed as limiting the scope of the invention but as merely providing illustrations of some of the presently preferred embodiments of this invention . thus the scope of the invention should be determined by the appended claims and their legal equivalents , rather than by the examples given . | 7 |
reference will now be made in detail to the subject matter disclosed , which is illustrated in the accompanying drawings . the scope of the invention is limited only by the claims ; numerous alternatives , modifications and equivalents are encompassed . for the purpose of clarity , technical material that is known in the technical fields related to the embodiments has not been described in detail to avoid unnecessarily obscuring the description . referring to fig1 , a block diagram of a system for displaying data having multiple security levels is shown . the system may include a processor 100 . the processor may be connected to a mls display 102 . the mls display 102 may render one or more entities 112 , 114 , 116 ; and each of the one or more entities 112 , 114 , 116 may be associated with a different security level . for example , a first entity 112 may be associated with a security level such as “ unclassified ” while a second entity 114 and a third entity 116 may be associated with a security level such as “ secret .” entities 112 , 114 , 116 may include data received via communication channels , representations of physical objects identified by radar , or any other data subject to graphical representation . the processor 100 may also be connected to one or more input devices 118 and a memory 120 . an input device 118 may include any device capable of receiving a user input to select a security level , or an entity having a security level , such as a touch screen , keyboard or voice input . the memory 120 may comprise a data structure to associate entities 112 , 114 , 116 with a security level . the system may also include one or more data communication devices 106 , 108 , 110 . data communication devices 106 , 108 , 110 may include navigation equipment , identification equipment , communication equipment , or any other device capable of sending , receiving or producing data for representation on a display such as the mls display 102 . each of the one or more data communication devices 106 , 108 , 110 may produce or communicate data at varying levels of security . the processor 100 may receive data , and an associated indicator of a security level for such data , from each of the one or more data communication devices 106 , 108 , 110 . alternatively , a security level for particular data may be inferred based on the nature of the data communication device 106 , 108 , 110 from which the data was received . the processor 100 and the mls display 102 may render data from each of the one or more communication device 106 , 108 , 110 as one or more entities 112 , 114 , 116 . the security level associated with each entity 112 , 114 , 116 may correspond to the security level associated with the data used to render the entity 112 , 114 , 116 . referring to fig2 , a block diagram of a system displaying de - emphasized entities is shown . in a system such as the system shown in fig1 , having a processor 100 connected to a mls display 102 , the processor 100 and mls display 102 may render entities 212 , 214 , 216 having more than one associated security levels . the entities 212 , 214 , 216 may be rendered based on data and a security level associated with the data . such data and associated security level may be stored in a data structure in a memory 120 connected to the processor 100 . a user may select a particular security level associated with one or more entities 212 , 214 , 216 through an input device 118 . the processor 100 and mls display 102 may render entities 212 , 214 , 216 in such a way as to emphasize entities 212 , 214 , 216 associated with the selected security level and de - emphasize entities 212 , 214 , 216 associated with a different security level . for example , a first entity 212 may be associated with a security level such as “ unclassified ” while a second entity 214 and a third entity 216 may be associated with a security level such as “ secret .” a user may select “ unclassified ” using the input device 118 . the processor may reference a data structure in the memory 120 to determine which entities 212 , 214 , 216 are associated with an “ unclassified ” security level . the processor 100 and mls display 102 may then render the second entity 214 and third entity 216 in such a way as to de - emphasize those entities 214 , 216 . de - emphasizing may include dimming , removing or otherwise visually distinguishing the de - emphasized entities 214 , 216 so as to make the entities 212 associated with the selected security level relatively more pronounced . additionally or alternatively , the processor 100 may emphasize entities 212 associated with the selected security level . alternatively , a user may select an entity 212 , 214 , 216 via an input device capable of allowing direct selection of entities 212 , 214 , 216 . the processor 100 may reference one or more data structures associating the selected entity 212 , 214 , 216 with a security level . the processor 100 and mls display 102 may then render entities 212 , 214 , 216 in such a way as to emphasize entities 212 , 214 , 216 associated with the security level corresponding to the elected entity 212 , 214 , 216 and de - emphasize entities 212 , 214 , 216 associated with a different security level . de - emphasized entities 214 , 216 may continue to be selectable via the input device 118 . the processor 100 may designate de - emphasized entities 214 , 216 as non - selectable to further enhance de - cluttering and segregation of entities 212 , 214 , 216 on the mls display 102 . a system according to this embodiment may allow a user to easily distinguish entities 212 , 214 , 216 based on the security level of each entity 212 , 214 , 216 and thereby help the user limit disclosure of information to data and entities 212 , 214 , 216 within a particular security classification . the processor 100 and mls display 102 may also render a visual indication of the security level associated any emphasized entities 212 . security levels may be hierarchical such that an authorization to receive data at a particular security level may include an authorization to receive data at all inferior security levels . where security levels are hierarchical , the processor 100 may de - emphasize entities 212 , 214 , 216 having superior security levels as compared to a security level selected via an input device 118 , but not de - emphasize entities 212 , 214 , 216 having inferior security levels . a user may also select , via the input device 118 , to return to a default rendering on the mls display 102 . the processor 100 may then re - render all entities 212 , 214 , 216 normally . referring to fig3 , a flowchart for a method of de - cluttering an mls display is shown . a user may select a desired security level through an input device connected to a processor . the processor may receive 300 the security level selection from the user and identify 302 one or more entities associated with the selected security level . entities may be associated with a selected security level in a data structure , or data used to render entities may be associated with a security level . entities associated with a selected security level may include entities associated with an inferior security level in a system where security levels are hierarchical . the processor may then de - emphasize 304 entities having a security level other than the selected security level such that the entities may be rendered in a visually distinct way . de - emphasis may include dimming the de - emphasized entities or prohibiting the de - emphasized entities from being drawn . the processor may also designate 306 one or more of the de - emphasized entities as non - selectable . “ security levels ” according to the present invention may be relative or absolute . while the foregoing discussion has specifically referenced “ unclassified ” and “ secret ” as examples of security levels , security levels may include any appropriate designation . furthermore , definitions of security levels may not be consistent between systems or networks . a system according to the present invention may interpret security levels as necessary to conform to entities and associated security levels already rendered in the system . it is believed that the present invention and many of its attendant advantages will be understood by the foregoing description , and it will be apparent that various changes may be made in the form , construction , and arrangement of the components thereof without departing from the scope and spirit of the invention or without sacrificing all of its material advantages . the form herein before described being merely an explanatory embodiment thereof , it is the intention of the following claims to encompass and include such changes . | 6 |
in the following detailed description , reference is made to the accompanying drawings which form a part hereof wherein like numerals designate like parts throughout , and in which are shown , by way of illustration , specific embodiments in which the disclosure may be practiced . it is to be understood that other embodiments may be utilized and structural or logical changes may be made without departing from the scope of the present disclosure . therefore , the following detailed description is not to be taken in a limiting sense , and the scope of a portion of the present disclosure is defined by the appended drawings and their equivalents . throughout the specification and drawings , the following terms take at least the meanings explicitly associated herein , unless the context clearly dictates otherwise . the meanings identified below are not intended to limit the terms , but merely provide illustrative examples for use of the terms . the meaning of “ a ,” “ an ,” and “ the ” may include reference to both the singular and the plural . reference in the specification to “ one embodiment ” or “ an embodiment ” means that a particular feature , structure , or characteristic described in connection with the embodiment is included in at least one embodiment of the disclosure . the meaning of “ in ” may include “ in ” and “ on .” the appearances of the phrases “ in one embodiment ” or “ in an embodiment ” in various places in the specification do not necessarily all refer to the same embodiment , but it may . the term “ connected ” or “ coupled ” can mean a direct connection between items , an indirect connection through one or more intermediaries , or communication between items in a manner that may not constitute a direct mechanical , systematic , physical , or other connection between the items connected . for example , in various embodiments component devices may be connected via a wireless connection that may allow for the exchange of data and / or information between the participating devices . the terms “ consumer ”, “ customer ” and “ user ” may or may not be used interchangeably . the various embodiments of performance evaluation systems in this disclosure are designed to collect multiple types of logs from a wireless device to determine the performance of the device or an application on the device . in one embodiment , the system performance evaluation uses a data collection tool to collect logs in multiple ways . for example , radio logs for voice & amp ; data may be collected . these are wireless protocol layer logs that relate to the radio interface . os / application layer logs may also be collected . these are logs related to various services . these logs are generally captured by the client on the mobile device . context aware connectivity logs may also be collected from the device or an external tool , which currently include logs for bt , nfc , wi - fi and may also include any new connectivity technology as needed . device information logs may also be collected and include battery , memory , processor , process , and other component device logs . once the contextual and device logs are collected at the device , in one embodiment , each individual set of collected logs may be uploaded , collectively or individually , to the database module via a parser using a wireless network , lan connectivity or wi - fi . the parser processes all logs and combines related events . the business logic modules may be custom designed per the customer requirements and processes the parsed data . an embodiment of custom logic for business module may include data for understanding the data throughput of a device or network in comparison with other networks . another embodiment of a custom logic may include data processing logic to determine the performance of a device under test and provide a comparative report including results from other devices . alternatively in a third embodiment of custom business logic the data and logs are parsed to understand the performance characteristics of a particular family of devices using a common component such as a specific chipset . in a fourth example of embodiment the business logic may be developed with the logs collected to calculate the relationship of connectivity logs with performance to determine the area of performance for a particular network . for example if at a range of − 65 dbm to − 95 dbm the throughput is better than 12 mbps then from the network design information it is possible to calculate the total area which has a throughput performance of above 12 mbps . other embodiments can manipulate the test data to analyze device , network or application performance and are considered within the scope of this disclosure . analysis of processed data may be available to create reports . report generation may be accomplished locally or remotely . in one embodiment , the web service may include report presentation , necessary data performance ratings and custom recommendations as needed for the specific customer . in another embodiment the results of the tests may be represented in an active geographical map with logs and data displayed on the maps in different ways . a third embodiment may report the analysis and the results in a combination of maps , graphs and other forms of data representation . other embodiments can manipulate the test data to analyze device , network or application performance and are considered within the scope of this disclosure . referring now to fig1 , various components of a performance evaluation system of services and applications on devices in live wireless environments are shown in a suitable operating environment in accordance with various embodiments of the present disclosure . fig1 is a high level system diagram , which shows components of the performance evaluation system including a device under test ( 100 ), test client ( 200 ), an external computing device ( 300 ), and a backend system ( 400 ) that includes a database server and a web service . the wireless test client 200 may be installed and runs on multiple platforms including on device ( 100 ), laptop ( 300 ), back end system server 400 , etc . so that it may be used by the tester . in one embodiment , the mobile test client 200 includes operational control logic on a receiving client . the back end system 400 includes , among other components , a database module and tools including : business logic modules that include reporting tools and a web service module that includes endpoints . other configurations may include other components or a subset of the above described components to enable a collaborative environment for wireless product or a group of products testing . referring now to fig4 , a flow diagram view of a performance evaluation system of services and applications on devices in live wireless environments is shown in accordance with at least one embodiment . more particularly , fig4 is a system flow chart of a sample scenario . in the illustrated scenario the test application and the custom configuration file is downloaded on the device under test ( 100 ) via an over the air methodology or via the external computing device . the test is run and the associated logs and device information are either sent to the back end server ( 400 ) directly over the air or through the external computing device ( 300 ). if it is connected to the device under test . the back end system completes the parsing and analysis of the data using the custom business logic and creates the reports . the customer may see these reports via a web service . in one embodiment , the test client 200 or client application on an external computing device , such as a laptop or another wireless device , interfaces or connects with the device under test . this client is capable of configuring the test allowing for user input . this variable configuration file can be made available to a user at the site of testing or a remote user . the collected device logs are then transmitted to a remote database via a wired or wireless interface . the client application may also have a user interface that may convey the status of the test to the user and may also allow for certain remedial action ( such as restarting the test ). the back end system database server 400 receives the combined logs from the client application or directly from the device under test . the parser formats the received logs and deposits the data into the relational database . business logic server / application , in one embodiment , has the logic to generate reports and ratings . this node in the system may have a predetermined logic as well as a customized logic that the user can generate via the web service . the web service may provide the interface to the licensed user . in one embodiment , the web service may have an interface that allows the user to provide certain customizations to the test and may also allow the user to generate custom reports . in another embodiment the web service has the logic to manage permissions and authentication for the user and / or a group of users . the performance evaluation system may also include user experience modules that include user authentication , certificate based transactions and user interface presentation . other embodiments can manipulate the test data to analyze or troubleshoot device , network or application performance and are considered within the scope of this disclosure . referring now to fig2 , various test clients and components of the test client are shown configured in accordance with at least one embodiment . fig2 shows a test client ( s ) ( 200 ). the full client / application may reside on the external computing device ( 300 ) which when connected to the device under test ( 100 ) controls , manages and monitors the test . the external computing client receives the logs and device information related to the test and transmits this to the backend . the device under test may have a light client that can be downloaded over the air . this client will be capable of running the test and transmitting the logs and device information back to the server over the air or at a later time to the external computing device when it is connected . in one embodiment , the front end of this test client tool is a software client application on the mobile operating system ( e . g ., android ; apple ios or windows phone ) that may include the ability to : 1 . load a test configuration file , where a user customizable test scripts can be run . the user customizable test scripts are run sequentially or in parallel and can target various applications or services that are already available on the mobile device . 2 . run a debugger / logger of the events and protocol messages related to each service / application that are run from the above and store the results in separate log files . this would include also capturing radio level protocol logs . in one embodiment , the test client may use laptop usb connectivity to a mobile device to run a configuration app and to upload log files to an external storage location . as previously shown , the test client 200 can be installed on the device under test [ 100 ] and on an external computing device . the test client 200 can also be updated by the back end system server . at least two variations of the test client 200 may exist . in one embodiment , the light client may be present on the device [ 300 ] and this may communicate with the full client on the external computing device [ 200 ]. the configuration files and the test scripts related to a specific routine as identified by the customer and uploaded on to the device under test [ 300 ] via the external computing device [ 200 ]. the tests are then run and logs collected . these logs are then packaged and sent to the back end system [ 400 ] via a communication channel from the external computing device [ 200 ]. in another embodiment , the device under test [ 100 ] may act independently and run the test as directed by the user . the collected logs may be packaged and sent directly via a communication channel to the back end system server [ 400 ] thus not requiring an external computing device [ 200 ]. in one embodiment , the test client on the device consists of at least two applications that are mutually exclusive . the first application is a test configuration client . one sample process block diagram of the test configuration client is shown and described in fig2 . the test configuration client collects device information from the device as follows [ 201 ]: device name , device software version , device hardware version , device firmware version , and test date / time . in one embodiment , the collected information is put in a folder “ device info ” for later access . the test configuration client may also load user customizable ui script that loads a test script ui that the user can use to select the tests that needs to be run . the selected tests can be run in sequence or simultaneously . the running of the selected test scripts enable the event logging trace [ 202 ] on the debugger tool ( internal os tool ) to log information . for example , the following table provides some available tests that may be selected . the logging and filtering of the event logs [ 203 ] by the test configuration client is also shown . the event logging captures designated events that are running on the mobile device under test . these include not only the events related to the test being run but also other useful information like radio signal information ( signal strength , signal quality ), data state , phone manager state , location info etc . next the system is shown parsing and saving of logs into folders [ 204 ]. in one embodiment , different captured logs may be collected in combined logs . to run the correct metrics from the captured logs , the combined logs must be parsed . in one embodiment of the client , the initial parsing of the combined logs can be done in the device under test ( dut ). this initial parsing of the combined logs is to separate the combined logs pertaining to an event into separate folders that can be easily uploaded to the back end system server where the business analysis can be done . in another embodiment , the combined logs are captured by the external computing device attached to the mobile device under test and parsed into their separate folders . next , the system uploads log folders to the back end system , which may include a database server [ 205 ]. in one embodiment of the process , the log folders can be uploaded using wi - fi to the back end system server . in another embodiment the cellular communication channel itself can be used to upload the combined logs . referring now to fig6 , radio logs collected during a voice call test are shown in accordance with at least one embodiment . the chart depicts activities and events associated with a particular call . these may vary depending on the network and device technology and hence will be unique to the test . the logs may also include other information , for example location etc . as per the design of the test and the custom test configuration . in this particular example , the different protocol states of the radio call control ( cc ) may be observed . as seen from the combined logs , the time to connect the call is the time difference between the connection request [ 14 : 10 : 13 : 318 ] and the cc / connect [ 14 : 10 : 24 : 518 ] which is approximately 11 seconds . referring now to fig7 , operating system ( os )/ application logs collected during a voice call test are represented . more specifically , fig5 depicts activities and events associated with a particular call . these may vary depending on the network and device technology and hence will be unique to the test . these logs may also include other information , for example location , etc . as per the design of the test and the custom test configuration . in the example shown in fig7 , we can see the different event states related to a voice call . various performance information can be gleaned from the logs . for example , as seen from the combined logs , the duration of the call is the time difference between the connection [ 14 : 10 : 24 : 613 ] and the disconnection [ 14 : 10 : 38 . 758 ] which is approximately 14 secs . referring now to fig5 , a flowchart of a test client process 200 is shown in accordance with at least one embodiment . the user can use the default test configuration or customize the configuration ( 201 ) that is used in the test . logging is enabled ( 202 ) and the captured logs ( 203 ) are parsed , packaged and saved ( 204 ). the test client then sends these logs and device information to the back end system ( 205 ) that stores this information in the database , analyses and creates reports . these reports are then made available to the licensed user . device testing : application ( s ) may be on the wireless device that runs the test process . this app can be an independent on device application or a larger application that is controlled by an external device . the test application can be used to test and determine the performance of multiple software and hardware components ( e . g . chipset ) of the device . in addition certain pre - determined consumer and enterprise applications can also be tested . collecting logs : the test client applications 200 collect data and logs from the operating system as well as the lower layers of the device ( such as chipsets and other hardware ) from the device and store it in a predetermined file on the device . when the device is connected to an external computing device ( via usb for example ) the combined logs can be downloaded or streamed to that device . this may be accomplished by collecting device logs that pertain to the entire stack ( operating system as well as the silicon and radio ) and combining the combined logs of various layers of the device and network communication protocol for devices in which the various logs need to be collected separately . in one embodiment , controlling the test process including methods for initiating , controlling , managing and termination of the tests or operation on the device from a local or remote location . also installation of the configurable device client software may originate from a local or remote location . controlling the test process may also include methods for transferring the combined logs either in real time or at a delayed time to a computing device ( memory card , laptop or server ). in one embodiment , the test process may also include methods to auto - detect the device based on custom set of variables . in one embodiment , the test process includes methods for auto configuration of the test / operation and device based on a custom set of variables , which may or may not have been provided by the test requestor . the test process may allow configuring of the test from a local and / or remote location . in one embodiment , encryption may be used to secure the combined logs : encryption may occur during collection of the logs and / or during the process of combining the logs so that the resulting combined logs would be encrypted . for example , one may use custom logic to encrypt the device logs and data prior to transmitting them . decryption of the encrypted combined logs may start with an authentication process on the backend system . this process may safeguard the data to improve veracity of the results . the performance evaluation system may monitor a variety of locations and devices within the target test system . in particular , the system may be monitored at various points including wireless device , computing nodes , and reports . the monitoring allows for local or remote control of the system . referring now to fig3 , the architecture of a device loaded with a test client application in accordance with at least one embodiment . more particularly , a view of the various architecture , abstract , and sw layers of a typical wireless device is shown . the actual implementation may vary by device . the test client will be loaded on to the application layer as an application . in one embodiment , the device under test can be any wireless device . a wireless device can be a mobile device or a fixed wireless device . the system described in this invention consists of test applications that can be run independently on the device under test or can be controlled by a client application on an external computing system . the communication method between the device under test and the external computing device can utilize any standard technology such as a usb connection or a bluetooth ( bt ) connection . this system can auto - detect the identification of the device under test by collecting device specific and software specific information . in one embodiment , the device under test and the client on the external computing device can collect device logs ( including os , baseband and hardware ) and package this before transmitting . fig2 and fig2 , illustrates a screen shot of an external tool for specific voice and data tests being integrated into the performance system in accordance with one embodiment the system can consider a variety of metrics including voice and audio services / apps , such as cs voice - mo and / or cs voice - mt . a . normal conditions b . voice and data ( background ) conditions c . lte packet data conditions d . supporting radio logs other system services / apps that can be evaluated include conference calls - lync , voip ( wi - fi calling / volte ) using metrics as outlined above , music streaming ( pandora ) performance , voicemail performance , combinations of the above , and location based services and voice / music . referring now to fig9 and fig2 , various components of a backend system are shown in accordance with at least one embodiment . the backend system ( 400 ) at a minimum includes a web service server ( 401 ), relational database ( 402 ), business logic unit ( 403 ) and a web service ui module ( 404 ). the web service server ( 401 ) receives the logs and device information from the device under test ( 100 ) or the external computing device ( 300 ). these logs are decrypted , parsed and stored in the relational database ( 402 ) as per the database schema . the business logic server ( 403 ) custom logic associated with the particular test or user is applied to the data to create reports and analysis that this made available to the user ( may be licensed ) via the web service ui ( 404 ). the back end system processing portion of the system includes a relational database ( 402 ), a business logic unit ( 403 ) and a web service ( 401 ). the web service ( 401 ) includes a user interface ( 404 ) that enables the licensed user to generate the reports and provide customization . this back end system may receive the combined logs via the client application or directly from the device via a wireless network . in one embodiment , the backend system 400 may use one or more of the following methods and processes : encryption / decryption : the data and logs may be encrypted and decrypted data storage : the data is eventually sent ( via tethered means or the cloud ) and stored on a relational database . data parsing : data is parsed using accustom logic that allows for various reports to be generated that are pivoted on custom requirements generating reports : the reports are generated using custom logic and are made available to licensed users . the data from testing may be crowd sourced and utilized to provide a performance rating to the device or application under test . providing web service : an interactive web service may be provided to licensed users that may allow these users to customize their reports and test process based on their license agreement . in various embodiments , the network may include at least one of a wireless network , the internet or an intranet . accordingly , a participating telephony device may be any wireless device . referring now to fig1 , a flow diagram view of a test routine analysis and process is shown in accordance with at least one embodiment . the flow diagram depicts one embodiment of a test routine analysis and process as per the description in fig1 . in one embodiment , collecting the performance of an application utilizing a wireless device may include one or more of the following methods and processes . collecting device logs that pertain to the entire stack ( operating system as well as the silicon ). combining the logs of various layers of the device . originating , initiating , controlling , managing and terminating of the tests / operation on the wireless device . transferring the combined logs either in real time or at a delayed time to a computing device ( memory card , laptop or server ). auto detection of the application / device based on custom set of variables . auto configuration of the test / operation and application based on a custom set of variables . configuring the test / operation from a local or remote location . scheduling the test / process from a local or remote location . monitoring the operation on wireless device may include at least one of the methods of log analysis or custom test probes to gain an understanding of the status of the tests including the status of normal progression , abnormal progression or an unexpected state . this information may be utilized along with human understanding of the environment to determine the next steps . for example one step might include taking remedial action to ensure that the tests are completed . another step is to validate that the complete logs have been collected . in one embodiment the status of the tests is transmitted to a local or remote location . initiating remedial action to be done from the local or remote location . the log files and metadata of the test procedure may be packaged , encrypted and transmitted in a secure environment . decryption of the packages may utilize custom authentication methods including but not limited to use of certificates , parity checks and other authentication methodology . the test results and the combined logs may be analyzed using a procedure and logic that includes information from the device under test , network and any associated back end system servers . the analysis procedure may have a custom logic to meet the customer requirements . for example in one embodiment the call performance may be analyzed from the combined logs of the device and from network traces provided by the mobile operator to highlight dropped calls due to inter radio technology handovers . in another embodiment the device oem might want to use logic to determine if the device fails to set up a data call in a particular application and radio technology . in this scenario logs are taken from the device and can be analyzed with additional information from the application server that might be provided . thus the analysis logic can be customized as per the customer needs , request or other criteria . other examples of reports are shown in fig the test results , logs and reports may be made available to the customer via a web service . referring now to fig1 , a communication flow diagram associated with a user request for a default ( pre - defined ) test and report coupled with a request for a new test report using the same logs and data is shown in accordance with at least one embodiment . in this example the business logic associated with the new report is applied to the same logs and data to create this new report . sample communications flow for a pre - determined report combined with new user report using the same set of data and logs is referred to fig1 . for example the user might have asked for a report of dropped calls and on seeing this report now wants a new report indicating the number of background data calls that happened during the same test . this supplemental report request can be analyzed using custom logic . referring now to fig1 , a communication flow diagram associated with a user request for a new test and report is shown in accordance with at least one embodiment . the sample communication flow associated with the user request for a new test and report . the user might now design a new test request for the next test run and the sample communication flow is shown in fig1 . this requires a new configuration file that is sent to the device under test ( 100 ) or to the external computing device ( 300 ) so that the test client ( 200 ) can manage and run the customized test . this also shows the user requesting new test report using the same logs and data . in this example the business logic associated with the new report is applied to the same logs and data to create this new report . turning now to the web service user interface , in one embodiment , the web service may include : 1 . allow the customer to get custom reports that can be pivoted on various pieces of data utilizing data from a single test or multiple tests . 2 . present ratings based on predetermined or custom logic 3 . provide a custom user interface based on the rights and privileges accorded to the end customer the method may be enhanced with data or tools external to the test procedure including but not limited to network logs , network design information and application information . this system can by utilized by various entities to determine the performance of a device or application and develop an understanding of the cause of this performance this system can by utilized by wireless operators this system can by utilized by wireless device application creators this system can by utilized by enterprise entities this system can by utilized by device manufacturers this system can by utilized by end consumers g . login to move onto custom screen based on user permission referring now to fig1 , a test request page including possibilities for customization of a test and a report as per user requests is shown in accordance with at least one embodiment . this shows one embodiment of a web service ui test request page : while this is a functional depiction of a possible test request page made available to the licensed user , it is understood that other components may be added or removed from the request page . the sample set of features shown here indicate the possibilities for customization of the test as per the user . referring now to fig1 , a report page for a voice call made available to the licensed user is shown in accordance with at least one embodiment . the shown web service ui provides a sample report page : this is also a functional depiction of a possible test report page for a voice call made available to the licensed user , but other configurations may be made that add or remove illustrated components . the illustrated sample page includes information on the device ( 100 ), report information , observations , and a map of the area that was tested . in this sample the details of the logs associated with a particular location are shows . another way to pivot the report may be based on time ( vs . location ). referring now to fig1 , a report page for a data call made available to the licensed user is shown in accordance with at least one embodiment . the illustrated web service ui shows a sample report page . this report is a functional depiction of a possible test report page for a data call made available to the licensed user . other reports may include additional information and / or remove portions of the illustrated report . the sample page includes information on the device ( 100 ), report information , performance comparisons , observations , performance graphs and a map of the area that was tested . in this sample the details of the logs associated with a particular location are shows . another way to pivot the report may be based on time ( vs . location ). referring now to fig8 , a flow diagram view of a client application on an external computing device ( such as a laptop or another wireless device ) that interfaces with the device under test is shown in accordance with various embodiments . in one embodiment , the client application is resident on an external computing device ( such as a laptop or another wireless device ) and interfaces with the device under test . this client is capable of configuring the test allowing for user input . this variable configuration file can be made available to a user at the site of testing or a remote user . the collected device logs are then transmitted to a remote database via a wired or wireless interface . the client application may also have a user interface that may convey the status of the test to the user and may also allow for certain remedial action ( such as restarting the test ). referring now to fig2 illustrates the various key performance indicators rating indexes otherwise also referred to as the health index and sample formulae that is used to develop the indexes in accordance with various embodiments referring now to fig1 , 20 , and 21 , screenshots illustrate features and functionality for the on device client interface is shown in accordance with various embodiments . more specifically fig1 shows a screenshot of a mobile device client landing page in accordance with various embodiments . fig2 depicts a screen shot of a mobile device client for manual test configuration in accordance with various embodiments . fig2 shows a screen shot of a mobile device client for specific test configuration in accordance with various embodiments . additionally , although specific embodiments have been illustrated and described herein , it will be appreciated by those of ordinary skill in the art and others , that a wide variety of alternate and / or equivalent implementations may be substituted for the specific embodiments shown and described without departing from the scope of the embodiments described herein . this application is intended to cover any adaptations or variations of the embodiments discussed herein . while various embodiments have been illustrated and described , as noted above , many changes can be made without departing from the spirit and scope of the embodiments described herein . | 7 |
fig1 illustrates a board 10 illustrated as squares having a series of playing squares 11 located close to the edge , along each side of the board 10 . many of playing squares 11 are feature squares 11a which indicate a trait or interest associated with a particular personality type . feature squares are colour coded so that , for example , the feature squares coded with the colour purple will indicate interests appropriate for the same personality trait . ______________________________________jigsaw puzzle bluecrossword puzzle greensales clerk brownrace horse silverteddy bear redromantic evening redlaw vegas silverresearch study yellowtheatre tickets yellowhouse pet orangepension plan purplelogical argument blueincome taxes greensports fan brownlong walk orangepleasure trip silverlove letters redcomputer technology yellowsingle apartment orangeold coins purplepublic figure brownstock market greenlegal ppers bluesavings bond purplequiet spot orangescience fiction yellowdozen roses redlottery ticket silverreal estate purpleactual proof bluemoney order greenstand - up comic brown______________________________________ the playing squares also include direction squares 11b which in fig1 are labelled &# 34 ; what &# 39 ; s my type ?&# 34 ;. a player landing on a direction square will draw a card from the stack 12 marked &# 34 ; what &# 39 ; s my type ?&# 34 ;. fig2 illustrates typical directions found on turning over card 12 . the playing squares also include at the corners a start square 13 , a visit the analyst square 14 , a free draw square 15 and a return to the analyst square 16 . the significance of these can most conveniently be explained in connection with the rules . board markers 17 and 17a shown in fig1 and fig3 a are typical board markers colour coded and bearing insignia 18 and 18a to indicate a category of interests or traits associated with personality types . the colour codes match those on the feature squares . when board markers such as 17 and 17a are turned over , they reveal one of several notations that correspond to the feature squares which they represent , as well as indicating an appropriate interest or trait as illustrated by fig3 a . board markers are turned down and distributed at random on squares 19 which are preferably located interiorly of the playing squares . the board markers act as tokens and correspond to each feature square . as illustrated in fig4 playing piece 20 may be of conventional design including base 21 and upper portion 21a that can easily be grasped . preferably , as illustrated by fig5 and 5a there are feature square cards 22 which act as tokens and provide written information about the feature squares . the game could be played using board markers 17 or feature square square cards 22 as tokens , but it is best to use both . the backs of the feature square cards correspond to the feature squares as exemplified by fig5 a . fig1 also indicates four stacks of choice cards 23 , 24 , 25 , 26 . choice cards 23 each include a question as to personality having two possible answers , with one of the answers showing an aspect of personality opposite to that shown by the other answer . choice cards such as those in stack 23 indicate a choice between &# 34 ; lucky strikes &# 34 ; coded silver and indicating a gambling nature ; and &# 34 ; clear cuts &# 34 ; coded purple suggesting a more cautious aspect of personality . similarly , choice cards 24 contrast &# 34 ; sweet dreams &# 34 ; coded yellow and &# 34 ; sure things &# 34 ; coded green . choice cards 25 contrast &# 34 ; social charms &# 34 ; coded brown and &# 34 ; private lives &# 34 ; coded orange , and choice cards 26 contrast &# 34 ; hard truths &# 34 ; coded blue and &# 34 ; warm fuzzies &# 34 ; coded red . fig6 , 8 and 9 illustrate typical questions from choice cards 25 , 24 , 26 and 23 respectively , each answer is colour coded by means of a coloured stripe and appropriate insignia such as brown stripe 27 and orange stripe 28 . the game could be played using cards with coloured designations or insignia only , but it is better if both methods of identification are used . fig1 illustrates a personality type tabulator 30 which includes aligned rows 31 , 32 , 33 and 34 each indicating an opposite pair of feature styles that correspond to the colour coding which matches the colour stripes and insignia such as 27 and 28 on the choice cards . in the centre of each row there is a neutral position 35 . each row including the neutral position has holes 36 to receive pegs such as 37 . if the choice card in fig6 is , for example , answered &# 34 ; outgoing and energetic &# 34 ;, peg 37 will be advanced from the neutral position to the first hole 38 in the brown &# 34 ; social charms &# 34 ; section . depending on the player &# 39 ; s next answer to a question from stack 25 , the peg will either be returned to the neutral position or advanced to the second hole in the brown &# 34 ; social charms &# 34 ; category . as will be explained in connection with the rules , it is necessary to qualify under each feature style by advancing the appropriate peg from the neutral position at least one and preferably two holes to qualify to obtain tokens , namely , board markers 17 and feature cards 22 . in other words , such tokens are obtained only if the player has qualified to obtain them both by having landed on the appropriate playing square , and also by having advanced the corresponding peg at least two holes in the direction matching the insignia and description on the token . the player must correctly locate the appropriate board marker , which will involve memory if it has been previously turned over and turned back . once a board marker has been claimed it is then located and conveniently stored in recesses 40 on the personality type tabulator . as colours cannot be illustrated on fig1 a colour key is included at the bottom to identify the various colours used to designate the letters . as will be explained in the rules , the game ends when a player has a token , such as a board marker in each of the four categories illustrated by the rows in fig1 . there are 16 possible combinations e . g . social charms , plus sure things , plus hard truths , plus lucky strikes is one combination . the method of declaring a winner is most conveniently explained in connection with the rules . a personality type profile card 38 as illustrated in fig1 may then be provided from a selection of 16 to indicate the personality of the declared winner as indicated by the colour coded feature style combination on the personality type tabulator , being the same as at 41 on fig1 . we will now present the preferred playing directions and rules from which variations may be made within the scope of the appended claims . how to play what &# 39 ; s my type ? ( what &# 39 ; s my type ? is a proposed trademark ). the aim of what &# 39 ; s my type ? is to answer questions which enable you to learn more about your personality type . the game is played by 2 to 6 people throwing dice and moving playing pieces around the board in a clockwise direction . when a playing piece lands on a feature square , the player answers a corresponding choice card . two answers are provided on the choice card and the player picks whichever one is closer to his or her usual way of doing things . the answers to these questions correspond to various features styles which typify how people ordinarily look at things and make decisions . the personality type tabulators are used to keep track of each player &# 39 ; s responses to the choice cards . there are four pairs of opposite feature styles portrayed along the game board . a player &# 39 ; s personality type consists of the feature styles that are indicated by the personality type tabulator . a player who lands on a feature square which matches any one of the preferred feature styles in his or her personality type has a chance to claim the feature square . the object of what &# 39 ; s my type ? is to be the first player who claims one feature square for each of the four feature styles in his or her personality type . what &# 39 ; s my type ? cards add some rather interesting moments to the game and there is always the unexpected opportunity to visit the analyst . there are no right or wrong answers to any of the questions on the choice cards . none of the players are ever eliminated from the game and no personality type has any particular advantage over the rest . the equipment consists of the game board , a pair of dice , six playing pieces , six personality type tabulators ; twenty - four feature style point pegs , thirty - two feature square cards , 32 board markers ; four sets of choice cards , sixteen what &# 39 ; s my type ? profile cards , and a deck of what &# 39 ; s my type ? cards . shuffle each deck of cards separately and place them face down on the game board in their marked spots . randomly place the thirty - two board markers face down along the inner squares on the game board . no player should know the position of any board marker before the start of the game . each of the players selects a playing piece to represent his or her position on the game board and receives a personality type tabulator along with four feature style point pegs . the remaining equipment is looked after by a player who is selected to be the analyst . the personality type tabulators are used to keep a running total of each player &# 39 ; s responses to the questions from the choice cards . each of the four horizontal columns on the personality type tabulator contains a pair of opposite feature styles ( example : private lives and social charms ). when a player answers a question , the corresponding feature style point peg is moved one hole ( along the horizontal column ) in the direction of the feature style identified on the choice card . the feature style point pegs may be moved in either direction and from one feature style to the other . the positions of the four feature style point pegs identify the preferred feature styles in a player &# 39 ; s personality type . the middle holes are the starting positions for the feature style point pegs and are referred to as neutral positions . when a player correctly draws a matching board marker and claims a feature square -- the board marker is then positioned in the correct holder on the personality type tabulator . every player selects a playing piece and positions it on the start square . the players roll the dice to determine who will start first . the player with the highest roll begins the game . he or she rolls the dice and moves his or her playing piece according to the number shown on both dice . playing pieces always move in a clockwise direction around the outer squares on the game board . upon completion , the turn passes to the player on the left . playing pieces remain in their location until the player &# 39 ; s next turn -- unless another player lands on the same square . only one playing piece may occupy the same square on the board at one time ( except visit the analyst ). when a player lands on a square already occupied , the first playing piece to land there goes to visit the analyst . each time a playing piece lands on a game board square there are several possible options ; a player may be eligible to draw , answer a choice card , take a what &# 39 ; s my type ? card , earn a free draw , receive an extra turn , or return to visit the analyst . when a player rolls doubles three times in a row , the playing piece goes immediately to visit the analyst -- unless the player happens to land on start . a player receives an extra turn for landing on start . landing on start also cancels the number of doubles that a player may have rolled to reach the square . the feature squares portray the various feature styles which combine to identify a player &# 39 ; s personality type . descriptions for each feature style are printed on the feature square cards . whenever a player lands on a feature square , he or she must first answer a choice card question . the players may decide who will ask each question . a player is not entitled to ask himself or herself a choice card question . feature squares remain unclaimed until a player who is eligible to draw lands there and correctly draws the matching board marker . a draw consists of turning a board marker completely face up for all to see . to be eligible for a draw , a player must have a minimum of two feature style points ( as shown by the coloured portion on the personality type tabulator ) for the style portrayed on the feature square . for example : a player with two or more feature style points for lucky strikes who lands on race horse , las vegas , pleasure trip , or lottery ticket is eligible to draw . after a player draws a board marker it is either returned face down to its original position or placed in the personality type tabulator -- if it matches the feature square . a player may claim only one feature square at a time from any feature style pairing . at all times , the board markers in the personality type tabulator must correspond to the feature styles indicated by the positions of the feature style point pegs . if one of the player &# 39 ; s feature style preferences becomes neutral , he or she must remove the board marker from the personality type tabulator and return it along with the feature square card to the analyst . there is no penalty for landing on another player &# 39 ; s feature square . however , in place of the draw , a player ( who is eligible to draw ) may challenge the owner for the right to claim the square . when this happens , the two players must throw the dice to see who will keep the feature square and board marker . if the owner rolls doubles he or she wins , otherwise , the player who rolls the higher number keeps the square . a tie goes to the owner . the one who loses the challenge must return to visit the analyst . when a playing piece lands on what &# 39 ; s my type ? the player takes the top card from the deck and upon completing the directions , returns the card face down to the bottom of the deck . the card marked &# 34 ; excused from visiting the analyst &# 34 ; may be kept by the player until needed . after it is used it must be returned to the bottom of the deck . cards which require the player to answer a choice card entitle the player to select the category of the card . &# 34 ; return to visit the analyst &# 34 ; is the only card which causes a player to lose his or her next turn . a player who lands on free draw must draw from any available board marker and proceed directly to the feature square , position the board marker in his or her personality type tabulator , and then receive a choice card question . if the player is not eligible to draw a board marker , when he or she lands on free draw , then his or her playing piece remains on the square and his or her turn ends . if a playing piece lands on or is sent to visit the analyst , the player is required to remain on the square until he or she rolls an even number with the dice . there is no other means of leaving the square except by using a what &# 39 ; s my type ? &# 34 ; exemption &# 34 ; card before rolling the dice . if a player throws doubles and lands on visit the analyst , he or she is not entitled to roll again and the turn passes to the next player . at the start of play , a player is selected to be the analyst for the entire game . the analyst acts as the controller for the feature square cards , board markers , and what &# 39 ; s my type ? profile cards . when a feature card is claimed , the analyst issues the player with the feature square card . when a player forfeits a feature square , he or she returns the feature square card and board marker to the analyst . next , the analyst takes all of the corresponding board markers that are unclaimed ( including the one being returned ) and randomly repositions them so that no player knows their new locations . the game is over when the first player has claimed one feature square for each feature style in his or her personality type . at this point the player immediately returns his or her playing piece to visit the analyst . the player is then asked one question from each of the four choice card decks to confirm the player &# 39 ; s personality type . the player is not entitled to learn either the category of the choice card being answered or the feature style represented by his or her response -- until all four answers have been given . the player must forfeit to the analyst any feature square which did not match the response given to the corresponding choice card and play continues . the player who successfully defends his or her personality type in this manner receives the appropriate what &# 39 ; s my type ? profile card from the analyst , after it has been read aloud to all of the players . the corresponding what &# 39 ; s my type ? profile card is easily identified by matching the colours on the card with those on the board markers in the personality type tabulator . | 0 |
fig3 shows a rough construction of the saturable reactor in accordance with the present invention . a pair of dual drum cores 14 , 15 are arranged in parallel with a certain specified clearance and common permanent magnets 21 , 22 are arranged closely to each other with the same polarities , for example , n polarities opposed at both ends of these dual drum cores . the dual drum core herein used is a core which is made of a material with high magnetic permeability such as , for example , ferrite and provided with disk - shaped flanges 141 , 142 , 143 , 151 , 152 and 153 at both ends and the center of the bar type magnetic core and with winding portions 14a , 14b , 15a , and 15b around the coils are to be wound between these flanges . common impedance coil 17 is wound around the winding portions 14a , 15a of the drum cores 14 , 15 and another common impedance coil 16 is wound around the winding portions 14b , 15b . the control coil 18 wound around the coil bobbin not shown is arranged around a pair of dual drum cores 14 , 15 . said impedance coils 16 , 17 and the control coil 18 are connected to the horizontal deflection coil and the vertical deflection coil of the deflection yoke . fig4 shows the electrical circuit of the deflection yoke and the saturable reactor is shown inside the one - dotted broken line 10 . one - side ends of impedance coils 16 , 17 are directly connected to the terminals 20a of the horizontal deflection circuit 20 and the other ends are respectively connected to one - side ends of the horizontal deflection coils 11 , 12 and the other end of the horizontal deflection coil is connected to the terminal 20b of the horizontal deflection coil 20 . in other words , the series circuit of the horizontal deflection coil and the impedance coil is connected in parallel to the horizontal deflection circuit 20 . on the other hand , the control coil 18 is connected to the terminal 19a of the vertical deflection circuit 19 through the vertical deflection coils 13 , 13 &# 39 ;, which are connected in series , and the other end of the coil 18 is connected to the terminal 19b of the circuit 19 . the following describes the operation of the saturable reactor . when the vertical deflection current i v from the vertical deflection circuit 19 is supplied to the control coil 18 and the horizontal deflection current i h supplied from the horizontal deflection circuit 20 flows through the the impedance coils 16 , 17 , a magnetic flux is generated in the direction as shown with the arrowhead in fig3 . in other words , a control flux φ v in the arrowhead direction shown with a one - dotted broken line is generated by the control coil 18 in the winding portions 14a , 14b , 15a and 15b of the drum cores 14 , 15 and the magnetic fluxes φh1 , φh2 from the impedance coils 16 , 17 are generated as shown with the solid arrowhead so that the directions of magnetic flux φh2 passing through the winding portions 14a , 15a and magnetic flux φh1 passing through the winding portions 14b , 15b are reversed . these magnetic fluxes φh1 , φh2 pass through the closed magnetic path formed by the flanges 141 - 143 , 151 - 153 and the winding portions 14a , 15a , 14b and 15b of the drum core . magnets 21 , 22 add the biased magnetic fluxes φm1 , φm2 shown with reversed arrowheads to the winding portions 14a , 14b , 15a , 15b as shown with a broken line and return to the magnets from the flanges 143 , 153 through the space magnetic path . the directions of magnetic fluxes φv , φh1 , φh2 shown in fig3 only indicate the timing when deflection currents i v , i h exist . in fact , these directions vary at every half cycle of deflection currents i v , i h supplied to impedance coils 16 , 17 and the control coil 18 . as known from fig3 since the magnetism of the winding portions 14a , 15b of the drum cores are biased to φv + φm2 , it becomes equivalent to the reduction of magnetic permeabilities of the drum cores whereby the inductance of the impedance coil 17 also reduces . in other words , the impedance of the impedance coil 17 reduces and the amount of current of the horizontal deflection current i h flowing through the horizontal deflection coil 12 slightly increases or does not nearly increase . this is because the cores are magnetically biased up to a point near the saturation point of the b - h curve which depends on the material of the drum cores . on the other hand , since the winding portions 14b , 15b are magnetically biased to φv - φm1 , such bias becomes equivalent to an increase of the magnetic permeability , the impedance of the impedance coil 16 increases and the horizontal deflection current flowing through the horizontal deflection coil 11 reduces . the above - mentioned operation is carried out in a cycle of the vertical deflection current and the horizontal deflection current flowing through the horizontal deflection coils 11 , 12 is differentially varied in a cycle of the vertical deflection current . if such deflection current is supplied to the deflection yoke , the cross misconvergence as shown in fig2 is corrected and the amount of misconvergence is within the tolerance . the magnetitude of misconvergence can be adjusted by varying the magnetic flux density of magnetic fluxes φm1 , φm2 supplied from magnets 21 , 22 . for example , the balance of magnetic bias against the drum cores 14 , 15 can be changed by biasing one or both of magnets 21 , 22 to the right or left on the figure . the densities of magnetic fluxes can be varied by reducing the sizes or thickness of the magnets . fig5 to 8 respectively show the structures of embodiments of the saturable reactor in accordance with the present invention . the coil bobbin 23 which is made of a plastic material and formed in an oval profile has the cylindrical part 231 and the enlarged cylindrical parts 232 , 233 which are formed at both ends of said cylindrical part 231 around which the control coil 18 is wound . inside the cylindrical part 231 of the coil bobbin 23 , two tubular tunnels 24 , 25 are provided which communicate each other through the space 26 as expressly shown by the cross sectional view in fig7 . in two tunnels 24 , 25 are inserted the dual drum cores 14 , 15 around which impedance coils 16 , 17 are wound as shown in fig5 and 6 . in other words , cores 14 , 15 are supported by the disk - shaped flanges 141 - 143 , 151 - 153 from the inside wall of the coil bobbin 23 . in this case , the closest parts of flanges 141 - 143 and 151 - 153 are separated as much as the width of the partition s so that the fluctuation of the reluctance of the closed magnetic circuit formed by two drum cores 14 , 15 is reduced . projection members 232a , 233a , 233b which control the positions of magnets 21 , 22 are provided in the enlarged cylindrical parts 232 , 233 formed at both ends of the coil bobbin 23 , as shown in fig5 and fig6 and oval - shaped plate magnets 21 , 22 are inserted into the section surrounded by these projection members as shown with the one - dotted broken line . the magnets are magnetized in the direction of thickness . in addition , the enlarged cylindrical parts 232 , 233 are protected with the covers 27 , 28 made of a plastic material as shown in fig5 . covers 27 , 28 are composed of the oval cylindrical member 271 and the plate member 272 as shown in fig8 . the engaging hole 29 is provided at the shorter diameter part of the oval cylindrical member 271 and the stepped stopper 30 is provided at both ends of the plate member 272 in the longer diameter direction . the engaging hole 29 engages with the engaging claws ( not shown ) provided on the outside of the enlarged cylindrical parts 232 , 233 and the stopper 30 hits against the projection members 232a , 233a inside the enlarged cylindrical parts in order to fix the covers 27 , 28 to the enlarged cylindrical parts 232 , 233 . lugs 31 are provided on the plate number 272 of the covers 27 , 28 in the direction of the longer diameter . these lugs 31 are formed by providing the u - shaped holes 31a in the plate member 272 . the lugs 31 are provided with projections 32 , which are projected inside the covers 27 , 28 , at their tip ends to depress the magnets 21 , 22 against the flanges 141 , 142 , 151 , 152 of the drum cores as shown in fig5 . various variations of the embodiment can be made within the range of the objects of the present invention . for example , the permanent magnets can be small - sized to be slidable inside the enlarged cylindrical member and can also be formed in a rectangular or circular shape . the shape of the coil bobbin and the cover can also be changed in the stage of design . | 7 |
an exemplary embodiment of the invention is illustrated in fig1 to 3 , and various possible solutions are illustrated in fig4 and 5 in terms of two driving situations . in fig1 the front wheels of a motor vehicle are designated by 1 and 2 , and its rear wheels by 3 and 4 . an engine 5 is normally connected through a drive shaft 10 with a differential 6 through which the rear wheels 3 and 4 are driven . in the vehicle shown in fig1 provision is made for shifting to four - wheel drive , to which end a longitudinal differential 7 can be switched so that in addition to the shaft 10 for the rear - wheel drive a shaft 8 is driven , through which and through a further differential 9 the front wheels are driven . the shafts 8 and 10 can be rigidly coupled to the engine through a central lock contained in the differential 7 . the differentials 6 and 9 may also have differential locks that can be engaged . the assumption is here made that the shifting to four - wheel drive and the engagement of the locks are brought about automatically by means of a control circuit 11 to which signals corresponding to the speeds of the wheels 1 to 4 are fed . ( this is indicated in fig1 only by the wheel speed sensors 2a and 4a for the wheels 2 and 4 , respectively . corresponding wheel speed sensors 1a and 3a are also connected to the control circuit 11 .) on the basis of the wheel - speed differences ascertained , a shifting to four - wheel drive and / or an engaging of the differential locks occurs , triggered by means of lines 13 . a brake light switch signal is fed to the terminal 12 for releasing the locks and disengaging the four - wheel drive . shown in fig2 is the associated anti - lock braking system , consisting of the four wheel - speed sensors 1a to 4a , an evaluation circuit 20 , brake - pressure control units 21 and 22 for the two front wheels 1 and 2 , and a single brake - pressure control unit 23 for the rear wheels 3 and 4 . also shown in fig2 is the control circuit 11 from fig1 to which the signals of the sensors 1a to 4a are fed , and which delivers the switching signals for the four - wheel drive and the differential locks by way of the terminals 24 to 27 . the switching signals at the terminals 26 ( for four - wheel drive shifting ) and 27 ( for the central lock ) are also fed to the evaluation circuit to enter into the formation of the reference value . fig3 is a basic diagram showing the formation of slip in the evaluation circuit 20 of fig2 . the wheel - speed signal of one of the sensors 1a to 4a is fed to a terminal 30 and then to a reference - value former 31 and a comparator 32 . switching signals for the four - wheel drive ( terminal 34 ) and for engagement of the central lock ( terminal 35 ) are further fed to the reference - value former 31 . the reference value produced by the latter is compared in the comparator 32 with the wheel - signal , and a broke pressure - reduction signal is generated at a terminal 33 when the wheel - speed signal falls below the reference - speed signal . the diagram of fig4 illustrates the mode of operation of the reference - value former 31 of fig3 for the driving situation in which the vehicle starts to climb a hill with the wheels spinning . curve 40 shows the wheel speed , curve 41 the vehicle speed , and curves 42a , 42b and 42c different ( alternative ) reference values . the driving situation starts at t o . at t 1 , shifting to four - wheel drive occurs automatically since the wheels are spinning ( the vehicle speed 41 remains practically zero ). this illustrates the case where the gradient of the reference speed 42 is limited and of the same magnitude ( e . g ., 0 . 2 grade ) whether the four - wheel drive is engaged or not . since the wheels continue to spin , the central lock is engaged at t 2 . now the reference value is either held constant ( curve 42a ) or then increased just slightly and continuously ( not illustrated ), reduced with a constant gradient ( curve 42b ), or set at a minimal speed ( curve 42c ; here approximately equal to the vehicle speed ). this state persists until the brakes are applied at t 3 ( see brake light switch signal bls ) and the wheel speed is consequently reduced . at t 3 the central lock is released and the four - wheel drive is also disengaged . the reference value now can rise with a given gradient of about 0 . 2 to 0 . 4 gr ( course 42 &# 39 ; in curve 42a ; course 42 &# 34 ; in curves 42 b and 42c ). at t 4 , the wheel - speed signal ( 40 ) drops below the reference value ( 42 &# 39 ;), and a brake pressure - reduction signal ( av ) is now generated at the terminal 33 . at the same time the reference value is reduced with a given negative gradient of about 0 . 3 to 0 . 4 gr . the brake pressure reduction here brought about actually occurs only rarely or , when it does , only momentarily . this would not be the case if the reference value were allowed to rise further , as in the range from t o to t 2 , which would result in a temporarily depressurized brake . in the case of the reduction proposed according to curve 42b and 42 &# 34 ;, the advantage described in enhanced , and in the case of curve 42c and 42 &# 34 ; it is even less likely that the brake pressure will be reduced . in the case of the last - mentioned curve , but also in the case of curve 42b with an appropriate negative gradient , the reference speed cannot exceed the vehicle speed even when the vehicle decelerates , with the central lock engaged . the vehicle speed will not be appreciably exceeded by the reference speed even with the central lock momentarily released ( for example , to check whether engaging the lock is still appropriate ). in the case of curve 42b and 42 &# 34 ;, even spurious signals indicating an engaged central lock will not appreciably distort the reference . in fig4 the assumption is made that the gradient is the same with and without four - wheel drive . actually , the reference value could be allowed to rise with a steeper gradient during the period from t o to t 1 ( as is usually the case with abs ). however , there is then the risk that if the shifting to four - wheel drive is not recognized , the reference signal will increase too much and a long - lasting pressure - reduction phase will also result . fig5 is based on the assumption that the vehicle is about to climb a hill , with the wheels at first spinning but then reaching ground with a higher coefficient of friction ( μ ). the wheel - speed curve is denoted by 50 , and the reference - speed curve ( or the corresponding signal curve ) by 52 ( with the different characteristics 52a to 52c and 52 &# 39 ; and 52 &# 34 ;, respectively ). the vehicle is to start moving at t o , but since the wheels are spinning the vehicle speed 51 remains practically zero . at t 1 , shifting to four - wheel drive occurs ; however , in this example also , the gradient of the reference speed is not changed . only at time t 2 , when the central lock is engaged , does one of the optional reference curves 52a or 42c of fig4 provided as alternatives , become effective . at time t 3 , the wheel reaches high - μ ground and is at first decelerated until the slip ceases ( at t 4 ). here the vehicle speed has caught up with the wheel speed , and both speeds increase in unison until the brake is applied at t 5 ( bls signal ). between t 2 and t 5 , the reference speed has taken a selected course according to the curves 52a to 52c . from t 5 onward , the reference speed increases according to curves 52 &# 39 ;,/ 52 &# 34 ; with a given positive gradient ( about 0 . 2 to 0 . 4 gr ). at the same time , the four - wheel drive and the locks were here disengaged . from t 5 onward , pressure - reduction signals av are generated by the wheel - speed oscillations due to the deceleration until ( at t 6 ) pressure - reduction signals are generated also by the slip . in the case of fig5 the curve 52a and 52 &# 34 ;, or the case of the slight increase in the reference , not shown here , is preferred since the reference catches up with the wheel speed sooner . the increase in the reference after the application of the brakes is advantageous in the case of fig5 but a drawback in the case of fig4 . as a compromise , a small gradient ( e . g ., 0 . 3 to 0 . 4 gr ) is preferably selected . there has thus been shown a novel anti - lock braking system which fulfills all the objects and advantages sought therefor . many changes , modifications , variations and other uses and applications of the subject invention will , however , become apparent to those skilled in the art after considering this specification and the accompanying drawings which disclose the preferred embodiments thereof . all such changes , modifications , variations and other uses and applications which do not depart from the spirit and scope of the invention are deemed to be covered by the invention which is limited only by the claims which follow . | 8 |
hereinafter , the present invention will be further illustrated with reference to the following examples . however , these examples are only provided for illustration purposes , and are not to limit the scope of the present invention . all of the modifications made based on the above disclosures will fall into the scope of the present invention . r 1 represents — h , — c m h ( 2m + 1 ) , c 3 - c 2 cycloalkyl , — c m h ( 2m + 1 ) substituted by c 3 - c 2 cycloalkyl , c 3 - c 2 cycloalkyl substituted by — c m h ( 2m + 1 ) , heterocyclyl containing 3 - 8 carbon atoms , amino substituted by heterocyclyl containing 3 - 8 carbon atoms , aryl containing 6 - 8 carbon atoms , or heteroaryl containing 6 - 8 carbon atoms ; said heterocyclyl contains 1 - 3 heteroatoms selected from n , o and s ; said heteroaryl contains 1 - 3 heteroatoms selected from n , o and s ; r 2 represents — h , — nh 2 , — oh , — f , — cl , — br , — cf 3 , — c m h ( 2m + 1 ) , — oc m h ( 2m + 1 ) , — nhc m h ( 2m + 1 ) , aryloxy containing 6 - 12 carbon atoms , or arylamino containing 6 - 12 carbon atoms ; r 3 represents c 3 - c 2 cycloalkyl , c 3 - c 2 cycloalkyl substituted by — c m h ( 2m + 1 ) , aryl containing 6 - 80 carbon atoms , or heteroaryl containing 6 - 80 carbon atoms ; said heteroaryl contains 1 - 15 heteroatoms selected from n , o and s ; r 4 - r 8 respectively represent — h , — f , — cl , — br , — cf 3 , — ocf 3 , — oc m h ( 2m + 1 ) , aqueous ammonia ( 8 . 0 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 10 . 0 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 1 hour . the precipitate was filtered off . the filter cake was recrystallized to obtain a yellow solid ( 8 . 1 g ) in a yield of 90 . 1 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 20 ( s , 1h ), 9 . 02 ( s , 1h ), 8 . 60 ( s , 1h ) ppm . a solution of methyl amine - ethanol ( 7 . 6 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 10 . 0 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for half an hour . purification was conducted by a column chromatography to obtain a yellow solid ( 8 . 3 g ) in a yield of 85 . 4 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 05 ( s , 1h ), 8 . 41 ( s , 1h ), 3 . 22 ( s , 3h ) ppm . isopropylamine ( 4 . 5 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 10 . 0 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for half an hour . purification was conducted by a column chromatography to obtain a bright - yellow solid ( 10 . 1 g ) in a yield of 90 . 4 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 03 ( s , 1h ), 8 . 24 ( s , 1h ), 4 . 53 ( m , 1h ), 1 . 34 ( d , j = 6 . 8 hz , 6h ) ppm . cyclopropylamine ( 1 . 8 ml ) and n , n - diisopropylethylamine ( 6 . 6 ml ) were dissolved into 75 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 5 . 0 g ) in dichloromethane ( 15 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 40 min . purification was conducted by a column chromatography to obtain a bright - yellow solid ( 2 . 6 g ) in a yield of 47 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 84 ( s , 1h ), 7 . 35 ( s , 1h ), 3 . 84 ( m , 1h ), 1 . 36 ( m , 4h ) ppm . cyclopentylamine ( 5 . 17 ml ) and n , n - diisopropylethylamine ( 12 . 4 ml ) were dissolved into 125 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 9 . 7 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 80 min . purification was conducted by a column chromatography to obtain a bright - yellow solid ( 7 . 9 g ) in a yield of 65 . 13 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 03 ( s , 1h ), 8 . 38 ( s , 1h ), 4 . 59 ( m , 1h ), 2 . 13 - 2 . 21 ( m , 2h ), 1 . 72 - 1 . 85 ( m , 4h ), 1 . 53 - 1 . 71 ( m , 2h ) ppm . cyclopentylamine ( 5 . 2 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitro - 6 - methylpyrimidine ( 10 . 7 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 1 hour . purification was conducted by a column chromatography to obtain a bright - yellow solid ( 11 . 2 g ) in a yield of 84 . 8 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 44 ( s , 2h ), 4 . 41 ( m , 1h ), 2 . 64 ( s , 3h ), 2 . 01 - 2 . 15 ( m , 2h ), 1 . 61 - 1 . 76 ( m , 4h ), 1 . 45 - 1 . 63 ( m , 2h ) ppm . isopropylamine ( 4 . 5 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitro - 6 - methoxypyrimidine ( 11 . 5 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 45 min . purification was conducted by a column chromatography to obtain a yellow solid ( 10 . 9 g ) in a yield of 86 . 1 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 25 ( s , 1h ), 4 . 42 ( m , 1h ), 4 . 01 ( s , 3h ), 1 . 23 ( d , j = 6 . 8 hz , 6h ) ppm . isopropylamine ( 4 . 5 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitro - 6 - methylaminopyrimidine ( 11 . 5 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for half an hour . purification was conducted by a column chromatography to obtain a yellow solid ( 10 . 4 g ) in a yield of 82 . 1 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ8 . 17 ( s , 1h ), 4 . 48 ( m , 1h ), 2 . 78 ( s , 3h ), 1 . 31 ( d , j = 6 . 8 hz , 6h ) ppm . isopropylamine ( 4 . 5 ml ) and n , n - diisopropylethylamine ( 13 . 2 ml ) were dissolved into 150 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitro - 6 - methylpyrimidine ( 10 . 7 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for half an hour . purification was conducted by a column chromatography to obtain a bright - yellow solid ( 10 . 2 g ) in a yield of 86 . 8 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 01 ( s , 1h ), 4 . 48 ( m , j = 4 . 1 , 1h ), 2 . 72 ( s , 3h ), 1 . 32 ( d , j = 6 . 8 hz , 6h ) ppm . cyclohexylamine ( 5 . 72 ml ) and n , n - diisopropylethylamine ( 12 . 4 ml ) were dissolved into 125 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 9 . 7 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 80 min . purification was conducted by a column chromatography to obtain a bright - yellow solid ( 9 . 1 g ) in a yield of 71 . 2 %. esi - ms ( m / z , %) 258 ( m − h ) + ; 1 h nmr ( 400 mhz , cdcl 3 ): δ9 . 04 ( s , 1h ), 8 . 35 ( s , 1h ), 4 . 34 ( m , 1h ), 2 . 03 ( m , 2h ), 1 . 79 ( m , 2h ), 1 . 53 - 1 . 25 ( m , 6h ). cyclohexylmethylamine ( 3 . 11 g ) and n , n - diisopropylethylamine ( 6 . 2 ml ) were dissolved into 45 ml dichloromethane . the mixture was added dropwise to a solution of 2 , 4 - dichloro - 5 - nitropyrimidine ( 4 . 85 g ) in dichloromethane ( 30 ml ) at 0 ° c . after the completion of the dropwise addition , the mixture was kept at the same temperature to react for 20 min . purification was conducted by a column chromatography to obtain a bright - yellow sheet - like solid ( 1 . 73 g ) in a yield of 26 %. esi - ms ( m / z , %) 272 ( m − h ) + . 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 03 ( s , 1h ), 8 . 48 ( s , 1h ), 3 . 52 ( m , 2h ), 1 . 78 - 1 . 64 ( m , 7h ), 1 . 33 - 1 . 14 ( m , 4h ), 1 . 08 - 1 . 00 ( m , 2h ). 4 - amino - n -( 4 - methylpiperazin - 1 - yl ) benzamide ( 4 . 7 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 5 . 9 g ) in a yield of 71 . 2 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 01 ( s , 1h ), 9 . 32 ( s , 1h ), 8 . 78 ( s , 1h ), 8 . 21 ( m , 2h ), 7 . 84 ( s , 1h ), 7 . 63 ( m , 2h ), 4 . 31 ( m , 1h ), 2 . 75 ( t , j = 4 . 8 hz , 4h ), 2 . 38 ( br , 4h ), 2 . 13 ( s , 3h ), 1 . 19 ( d , j = 6 . 8 hz , 6h ) ppm . 4 - amino - 3 - fluoro - n -( 4 - methylpiperazin - 1 - yl ) benzamide ( 5 . 0 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 6 . 5 g ) in a yield of 75 . 7 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 11 ( s , 1h ), 9 . 47 ( s , 1h ), 8 . 99 ( s , 1h ), 8 . 38 ( d , j = 7 . 6 hz , 1h ), 7 . 86 ( m , 1h ), 7 . 65 ( m , 2h ), 4 . 27 ( m , 1h ), 2 . 89 ( t , j = 4 . 8 hz , 4h ), 2 . 42 ( br , 4h ), 2 . 19 ( s , 3h ), 1 . 23 ( d , j = 6 . 4 hz , 6h ) ppm . 4 - amino - 3 - methoxy - n -( 4 - methylpiperazin - 1 - yl ) benzamide ( 5 . 3 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 6 . 8 g ) in a yield of 77 . 1 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 13 ( s , 1h ), 8 . 38 ( d , j = 6 . 8 hz , 1h ), 7 . 93 ( m , 1h ), 7 . 63 ( d , j = 8 . 0 hz , 1h ), 7 . 46 ( m , 1h ), 7 . 08 ( m , 1h ), 7 . 01 ( m , 1h ), 4 . 31 ( m , 1h ), 3 . 86 ( s , 3h ), 3 . 55 ( br , 4h ), 2 . 52 ( br , 4h ), 2 . 32 ( s , 3h ), 1 . 24 ( d , j = 6 . 4 hz , 6h ) ppm . 4 - amino - n -( 4 - methylpiperidin - 1 - yl ) benzamide ( 4 . 6 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 5 . 7 g ) in a yield of 70 . 0 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 58 ( s , 1h ), 9 . 02 ( s , 1h ), 8 . 48 ( d , j = 5 . 6 hz , 1h ), 8 . 20 ( d , j = 6 . 8 hz , 1h ), 7 . 86 ( m , 4h ), 4 . 45 ( m , 1h ), 3 . 80 ( m , 1h ), 2 . 94 ( br , 4h ), 2 . 32 ( s , 3h ), 1 . 62 - 1 . 83 ( m , 4h ), 1 . 33 ( d , j = 6 . 4 hz , 6h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 1 ( 3 . 5 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 5 . 2 g ) in a yield of 79 . 5 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 07 ( s , 1h ), 8 . 52 ( s , 2h ), 8 . 40 ( s , 1h ), 7 . 57 ( s , 1h ), 7 . 51 ( s , 1h ), 7 . 10 ( m , 2h ), 3 . 31 ( t , j = 4 . 8 hz , 4h ), 2 . 81 ( t , j = 4 . 8 hz , 4h ), 2 . 30 ( s , 3h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 2 ( 3 . 8 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 5 . 1 g ) in a yield of 74 . 8 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 11 ( s , 1h ), 8 . 34 ( s , 1h ), 7 . 59 ( s , 1h ), 7 . 51 ( m , 2h ), 7 . 23 ( m , 2h ), 4 . 21 ( s , 3h ), 3 . 15 ( t , j = 4 . 8 hz , 4h ), 2 . 87 ( t , j = 4 . 8 hz , 4h ), 2 . 48 ( s , 3h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 2 g ) in a yield of 84 . 1 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 02 ( s , 1h ), 8 . 42 ( s , 1h ), 7 . 63 ( s , 1h ), 7 . 51 ( s , 2h ), 6 . 95 ( m , 2h ), 4 . 41 ( m , 1h ), 3 . 22 ( t , j = 4 . 8 hz , 4h ), 2 . 61 ( t , j = 4 . 8 hz , 4h ), 2 . 37 ( s , 3h ), 1 . 33 ( d , j = 6 . 4 hz , 6h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 4 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 4 g ) in a yield of 87 . 2 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 08 ( s , 1h ), 8 . 39 ( s , 1h ), 7 . 90 ( s , 1h ), 7 . 58 ( m , 2h ), 6 . 94 ( m , 2h ), 4 . 32 ( m , 1h ), 3 . 05 ( t , j = 4 . 8 hz , 4h ), 2 . 90 ( t , j = 4 . 8 hz , 4h ), 2 . 67 ( s , 3h ), 1 . 39 ( m , 4h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 5 ( 4 . 8 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 0 g ) in a yield of 76 . 0 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 9 . 03 ( s , 1h ), 8 . 47 ( s , 1h ), 7 . 69 ( s , 1h ), 7 . 51 ( m , 2h ), 7 . 11 ( m , 2h ), 4 . 43 ( m , 1h ), 3 . 28 ( t , j = 4 . 8 hz , 4h ), 2 . 67 ( t , j = 4 . 8 hz , 4h ), 2 . 45 ( s , 3h ), 2 . 15 - 2 . 23 ( m , 2h ), 1 . 74 - 1 . 86 ( m , 4h ), 1 . 50 - 1 . 72 ( m , 2h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 6 ( 5 . 1 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 5 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 4 g ) in a yield of 78 . 3 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 42 ( s , 1h ), 7 . 62 ( s , 1h ), 7 . 41 ( s , 2h ), 6 . 98 ( m , 2h ), 4 . 21 ( m , 1h ), 3 . 14 ( t , j = 4 . 8 hz , 4h ), 2 . 56 ( t , j = 4 . 8 hz , 4h ), 2 . 51 ( s , 3h ), 2 . 34 ( s , 3h ), 1 . 47 - 1 . 85 ( m , 8h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 7 ( 4 . 9 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 5 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a reddish - brown solid ( 6 . 5 g ) in a yield of 81 . 5 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 51 ( s , 1h ), 7 . 86 ( s , 1h ), 7 . 43 ( s , 2h ), 7 . 01 ( m , 2h ), 4 . 32 ( m , 1h ), 3 . 94 ( s , 3h ), 3 . 08 ( t , j = 4 . 8 hz , 4h ), 2 . 64 ( t , j = 4 . 8 hz , 4h ), 2 . 53 ( s , 3h ), 1 . 43 ( d , j = 6 . 4 hz , 6h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 8 ( 4 . 9 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 6 hours , cooled to room temperature , filtered , washed and dried to obtain a reddish - brown solid ( 6 . 0 g ) in a yield of 75 . 4 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 8 . 58 ( s , 1h ), 7 . 81 ( s , 1h ), 7 . 47 ( s , 2h ), 7 . 08 ( m , 2h ), 4 . 45 ( m , 1h ), 3 . 14 ( t , j = 4 . 8 hz , 4h ), 2 . 79 ( s , 3h ), 2 . 54 ( t , j = 4 . 8 hz , 4h ), 2 . 42 ( s , 3h ), 1 . 45 ( d , j = 6 . 4 hz , 6h ) ppm . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 9 ( 4 . 6 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 3 g ) in a yield of 82 . 3 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 11 . 01 ( s , 1h ), 10 . 15 ( s , 1h ), 7 . 66 ( d , j = 8 . 4 , 2h ), 6 . 99 ( d , j = 9 . 2 , 2h ), 4 . 35 ( s , 1h ), 3 . 76 ( d , j = 11 . 2 , 2h ), 3 . 46 ( d , j = 10 . 8 , 2h ), 3 . 11 ( m , j = 13 . 6 , 4h ), 2 . 79 ( s , 3h ), 2 . 60 ( s , 3h ), 1 . 27 ( d , j = 6 . 4 , 6h ) ppm . 4 - amino - n -( 4 - methylpiperazin - 1 - yl ) benzamide ( 4 . 85 g ) was added to a solution of compound 2 - 5 ( 4 . 7 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 6 . 4 g ) in a yield of 72 . 6 %. ms m / z ( esi ): 441 [ m + h ] + . 4 - amino - 3 - fluoro - n -( 4 - methylpiperidin - 1 - yl ) benzamide ( 5 . 0 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 6 . 3 g ) in a yield of 72 . 8 %. ms m / z ( esi ): 432 [ m + h ] + . n -( 3 - aminophenyl ) acrylamide ( 3 . 2 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 0 g ) in a yield of 88 . 3 %. ms m / z ( esi ): 344 [ m + h ] + . 4 -( 2 - morpholinoethoxy ) phenylamine ( 4 . 4 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 . 5 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 4 g ) in a yield of 80 . 0 %. ms m / z ( esi ): 403 [ m + h ] + . 4 -( 3 -( 4 - methylpiperazin - 1 - yl ) propylamino ) phenylamine ( 4 . 9 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 8 g ) in a yield of 79 . 9 %. ms m / z ( esi ): 429 [ m + h ] + . 4 - morpholinophenylamine ( 3 . 6 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 5 . 3 g ) in a yield of 74 . 7 %. ms m / z ( esi ): 359 [ m + h ] + . 4 - morpholinomethylphenylamine ( 3 . 8 g ) was added to a solution of compound 2 - 5 ( 4 . 8 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow solid ( 6 . 3 g ) in a yield of 80 . 6 %. ms m / z ( esi ): 399 [ m + h ] + . 4 -( 4 - methylpiperazinyl ) phenylamine ( 3 . 1 g ) was added to a solution of compound 2 - 10 ( 2 . 3 g ) in n - butanol ( 40 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 4 . 13 g ) in a yield of 83 . 8 %. ms m / z ( esi ): 412 [ m + h ] + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 71 ( s , 1h ), 10 . 35 ( s , 1h ), 8 . 96 ( s , 1h ), 8 . 48 ( d , j = 6 . 8 hz , 1h ), 7 . 71 ( d , j = 8 . 8 hz , 1h ), 6 . 99 ( d , j = 9 . 2 hz , 2h ), 4 . 04 ( m , 1h ), 3 . 78 ( m , 2h ), 3 . 46 ( m , 2h ), 3 . 15 ( m , 2h ), 3 . 04 ( m , 2h ), 2 . 83 ( s , 1h ), 1 . 98 ( m , 2h ), 1 . 65 ( m , 1h ), 1 . 43 ( m , 4h ), 1 . 26 ( m , 1h ) ppm . 4 -( 2 - methoxyethoxy ) phenylamine ( 2 . 7 g ) was added to a solution of compound 2 - 5 ( 3 . 7 g ) in n - butanol ( 80 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain a yellow floc - like solid ( 4 . 53 g ) in a yield of 80 . 9 %. ms m / z ( esi ): 374 [ m + h ] + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ10 . 34 ( s , 1h ), 8 . 95 ( s , 1h ), 8 . 50 ( s , 1h ), 7 . 70 ( d , j = 6 . 0 hz , 2h ), 6 . 93 ( d , j = 8 . 8 hz , 2h ), 4 . 43 ( m , 1h ), 4 . 07 ( m , 2h ), 3 . 64 ( m , 2h ), 3 . 30 ( s , 3h ), 2 . 03 ( m , 2h ), 1 . 72 ( m , 2h ), 1 . 61 ( m , 4h ) ppm . 4 -(( 4 - ethylpiperazin - 1 - yl ) methyl ) phenylamine ( 3 . 6 g ) was added to a solution of compound 2 - 5 ( 6 . 0 g ) in n - butanol ( 130 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid in a yield of 81 . 8 %. ms m / z ( esi ): 426 [ m + h ] + . 4 -(( 4 - methylpiperazin - 1 - yl ) methyl ) phenylamine ( 4 . 7 g ) was added to a solution of compound 2 - 5 ( 5 . 28 g ) in n - butanol ( 130 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid in a yield of 85 . 7 %. ms m / z ( esi ): 412 [ m + h ] + . 4 -( 4 - methylpiperazinyl ) phenylamine ( 1 . 13 g ) was added to a solution of compound 2 - 11 ( 1 . 6 g ) in n - butanol ( 25 ml ). the mixture was reacted at 90 ° c . for 4 . 0 hours , cooled to room temperature , filtered , washed and dried to obtain an orange - red solid ( 4 . 13 g ) in a yield of 87 . 6 %. ms m / z ( esi ): 426 [ m + h ] + . a solution of rongalite ( sodium dithionite ) ( 9 . 6 g ) in water ( 30 ml ) was added to a solution of 4 - 1 ( 2 . 1 g ) in tetrahydrofuran ( 25 ml ). the mixture was stirred at room temperature for 6 - 12 hours , adjusted to a ph of 7 - 8 by adding a saturated potassium carbonate solution , and then extracted with dichloromethane ( 5 × 20 ml ). the organic phase was dried over anhydrous sodium sulfate , and rotary evaporated to dryness to obtain a jade - green solid ( 1 . 2 g ) in a yield of 63 . 2 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 01 ( s , 1h ), 9 . 32 ( s , 1h ), 8 . 78 ( s , 1h ), 8 . 01 ( m , 2h ), 7 . 83 ( s , 1h ), 7 . 72 ( m , 2h ), 4 . 29 ( m , 1h ), 4 . 08 ( s , 2h ), 2 . 87 ( t , j = 4 . 8 hz , 4h ), 2 . 47 ( br , 4h ), 2 . 24 ( s , 3h ), 1 . 22 ( d , j = 6 . 8 hz , 6h ) ppm . a solution of rongalite ( 9 . 6 g ) in water ( 30 ml ) was added to a solution of 4 - 2 ( 2 . 2 g ) in tetrahydrofuran ( 25 ml ). the mixture was stirred at room temperature for 6 - 12 hours , adjusted to a ph of 7 - 8 by adding a saturated potassium carbonate solution , and then extracted with dichloromethane ( 5 × 20 ml ). the organic phase was dried over anhydrous sodium sulfate , and rotary evaporated to dryness to obtain a jade - green solid ( 1 . 4 g ) in a yield of 68 . 4 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 26 ( s , 1h ), 8 . 44 ( m , 1h ), 7 . 81 ( s , 1h ), 7 . 56 ( d , j = 10 . 8 hz , 2h ), 7 . 40 ( s , 1h ), 6 . 24 ( d , j = 7 . 2 hz , 1h ), 4 . 31 ( s , 2h ), 4 . 22 ( m , 1h ), 2 . 86 ( t , j = 4 . 8 hz , 4h ), 2 . 41 ( br , 4h ), 2 . 18 ( s , 3h ), 1 . 22 ( d , j = 6 . 4 hz , 6h ) ppm . in a 500 ml round - bottom flask , compound 4 - 3 ( 4 . 0 g ) was dissolved into 150 ml ethanol , and then 40 ml water and 5 . 0 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 7 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 8 g ) in a yield of 75 . 0 %. ms m / z ( esi ): 415 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 4 ( 4 . 0 g ) was dissolved into 150 ml ethanol , and then 40 ml water and 5 . 0 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 7 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 4 . 2 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 6 g ) in a yield of 70 . 8 %. ms m / z ( esi ): 384 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 5 ( 6 . 6 g ) was dissolved into 160 ml ethanol , and then 40 ml water and 5 . 35 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 6 . 6 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 4 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and recrystallized to obtain a bluish - black solid in a yield of 71 . 0 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 8 . 18 ( s , 1h ), 7 . 56 ( d , j = 9 . 2 hz , 2h ), 6 . 79 ( d , j = 8 . 8 hz , 2h ), 6 . 00 ( d , j = 7 . 6 hz , 1h ), 4 . 24 ( m , 1h ), 4 . 01 ( s , 2h ), 2 . 99 ( t , j = 4 . 4 hz , 4h ), 2 . 43 ( t , j = 4 . 8 hz , 4h ), 2 . 21 ( s , 3h ), 1 . 21 ( d , j = 6 . 4 hz , 6h ) ppm . in a 100 ml round - bottom flask , compound 4 - 6 ( 1 . 0 g ) was dissolved into 60 ml ethanol , and then 15 ml water and 0 . 8 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 0 . 84 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 1 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 0 . 7 g ) in a yield of 70 . 2 %. ms m / z ( esi ): 314 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 7 ( 3 . 7 g ) was dissolved into 200 ml ethanol , and then 50 ml water and 2 . 7 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 8 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 4 g ) in a yield of 70 . 6 %. 1 h nmr ( 400 mhz , dmso - d 6 ): δ 8 . 18 ( s , 1h ), 7 . 56 ( d , j = 9 . 2 hz , 2h ), 6 . 79 ( d , j = 8 . 8 hz , 2h ), 6 . 00 ( d , j = 7 . 6 hz , 1h ), 4 . 24 ( m , 1h ), 4 . 01 ( s , 2h ), 2 . 99 ( t , j = 4 . 4 hz , 4h ), 2 . 43 ( t , j = 4 . 8 hz , 4h ), 2 . 21 ( s , 3h ), 1 . 21 ( d , j = 6 . 4 hz , 6h ) ppm . in a 100 ml round - bottom flask , compound 4 - 8 ( 1 . 1 g ) was dissolved into 60 ml ethanol , and then 15 ml water and 0 . 8 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 0 . 84 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 1 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a column chromatography to obtain bluish - black solid ( 0 . 8 g ) in a yield of 79 . 2 %. ms m / z ( esi ): 340 [ m + h ] + . in a 250 ml round - bottom flask , compound 4 - 9 ( 2 . 0 g ) was dissolved into 100 ml ethanol , and then 25 ml water and 1 . 4 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 1 . 4 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 2 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and recrystallized to obtain a bluish - black solid ( 1 . 1 g ) in a yield of 59 . 3 %. ms m / z ( esi ): 368 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 10 ( 3 . 7 g ) was dissolved into 200 ml ethanol , and then 50 ml water and 2 . 7 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 8 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 6 g ) in a yield of 75 . 7 %. ms m / z ( esi ): 382 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 11 ( 3 . 9 g ) was dissolved into 200 ml ethanol , and then 50 ml water and 2 . 7 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 8 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 5 g ) in a yield of 70 . 0 %. ms m / z ( esi ): 372 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 12 ( 3 . 8 g ) was dissolved into 200 ml ethanol , and then 50 ml water and 2 . 7 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 8 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 4 g ) in a yield of 67 . 3 %. ms m / z ( esi ): 371 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 13 ( 3 . 7 g ) was dissolved into 200 ml ethanol , and then 50 ml water and 2 . 7 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 8 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid ( 2 . 5 g ) in a yield of 73 . 3 %. 1 h nmr ( 400 mhz , cdcl 3 ): δ 7 . 51 ( d , j = 8 . 8 , 2h ), 6 . 89 ( d , j = 8 . 8 , 2h ), 6 . 59 ( s , 1h ), 5 . 17 ( d , j = 7 . 2 , 1h ), 4 . 63 ( s , 2h ), 4 . 22 ( m , j = 6 . 72 , 1h ), 3 . 14 ( t , j = 5 . 0 , 4h ), 2 . 59 ( t , j = 4 . 8 , 4h ), 2 . 35 ( s , 3h ), 2 . 25 ( s , 3h ), 1 . 26 ( d , j = 6 . 4 , 6h ) ppm . in a 500 ml round - bottom flask , compound 4 - 14 ( 4 . 4 g ) was dissolved into 150 ml ethanol , and then 40 ml water and 5 . 0 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 7 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and recrystallized to obtain a bluish - black solid ( 3 . 2 g ) in a yield of 77 . 9 %. ms m / z ( esi ): 411 [ m + h ] + . a solution of rongalite ( 9 . 6 g ) in water ( 30 ml ) was added to a solution of 4 - 15 ( 2 . 2 g ) in tetrahydrofuran ( 25 ml ). the mixture was stirred at room temperature for 6 - 12 hours , adjusted to a ph of 7 - 8 by adding a saturated potassium carbonate solution , and then extracted with dichloromethane ( 5 × 20 ml ). the organic phase was dried over anhydrous sodium sulfate , and rotary evaporated to dryness to obtain a jade - green solid ( 1 . 5 g ) in a yield of 69 . 6 %. ms m / z ( esi ): 402 [ m + h ] + . n -( 3 - aminophenyl ) acrylamide ( 3 . 2 g ) was added to a solution of compound 2 - 3 ( 4 . 3 g ) in n - butanol ( 150 ml ). the mixture was reacted at 90 ° c . for 3 hours , cooled to room temperature , filtered , washed and dried to obtain a red solid ( 6 . 0 g ) in a yield of 88 . 3 %. ms m / z ( esi ): 344 [ m + h ] + . in a 100 ml round - bottom flask , compound 4 - 17 ( 1 . 21 g ) was dissolved into 60 ml ethanol , and then 15 ml water and 0 . 8 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 0 . 84 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 1 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid in a yield of 75 . 2 %. ms m / z ( esi ): 373 [ m + h ] + . in a 100 ml round - bottom flask , compound 4 - 18 ( 1 . 3 g ) was dissolved into 60 ml ethanol , and then 15 ml water and 0 . 8 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 0 . 84 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 1 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid in a yield of 78 . 9 %. ms m / z ( esi ): 399 [ m + h ] + . in a 100 ml round - bottom flask , compound 4 - 19 ( 1 . 1 g ) was dissolved into 60 ml ethanol , and then 15 ml water and 0 . 8 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 0 . 84 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 2 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid in a yield of 74 . 1 %. ms m / z ( esi ): 329 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 20 ( 3 . 85 g ) was dissolved into 150 ml ethanol , and then 40 ml water and 5 . 0 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 7 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 . 5 hours . the mixture was filtered while hot , rotary evaporated to dryness , and subjected to a column chromatography to obtain a bluish - black solid in a yield of 74 . 5 %. ms m / z ( esi ): 369 [ m + h ] + . in a 100 ml round - bottom flask , compound 4 - 21 ( 1 . 03 g ) was dissolved into 40 ml ethanol , and then 10 ml water and 0 . 67 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 0 . 7 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 3 . 7 hours . the mixture was filtered while hot , and rotary - evaporated to dryness to obtain a crude product in a yield of 78 . 9 %. ms m / z ( esi ): 382 [ m + h ] + . in a 250 ml round - bottom flask , compound 4 - 22 ( 3 . 73 g ) was dissolved into 120 ml ethanol , and then 30 ml water and 2 . 67 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 2 . 8 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 4 hours . the mixture was filtered while hot , and rotary - evaporated to dryness to obtain a crude product in a yield of 84 . 6 %. ms m / z ( esi ): 344 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 23 ( 10 g ) was dissolved into 240 ml ethanol , and then 60 ml water and 2 . 67 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 6 . 6 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 4 hours . the mixture was filtered while hot , and rotary - evaporated to dryness to obtain a crude product in a yield of 82 . 7 %. ms m / z ( esi ): 396 [ m + h ] + . in a 500 ml round - bottom flask , compound 4 - 24 ( 9 . 42 g ) was dissolved into 240 ml ethanol , and then 60 ml water and 1 . 92 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 6 . 85 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the reaction time was 4 hours . the mixture was filtered while hot , and rotary - evaporated to dryness to obtain a crude product in a yield of 80 . 6 %. ms m / z ( esi ): 382 [ m + h ] + . in a 100 ml round - bottom flask , compound 4 - 23 ( 2 . 0 g ) was dissolved into 30 ml ethanol , and then 10 ml water and 0 . 62 g nh 4 cl were added thereto . the mixture was stirred at room temperature for 10 minutes , and warmed to 90 ° c . 1 . 29 g fe powder was added to the mixture in three portions . tlc detection indicated the completion of the reaction of the starting material . the mixture was filtered while hot , and rotary - evaporated to dryness to obtain a crude product in a yield of 81 . 4 %. ms m / z ( esi ): 396 [ m + h ] + . compound 5 - 1 ( 2 . 3 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 1 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 64 . 3 %. esi - ms ( m / z , %) 484 . 29 ( m − h ) − ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 63 ( s , 1h ), 9 . 21 ( s , 1h ), 9 . 11 ( s , 1h ), 7 . 85 ( m , 4h ), 7 . 73 ( d , j = 8 . 4 hz , 2h ), 7 . 34 ( m , 2h ), 7 . 00 ( m , 1h ), 4 . 94 ( m , 1h ), 2 . 88 ( t , j = 4 . 4 hz , 4h ), 2 . 42 ( br , 4h ), 2 . 19 ( s , 3h ), 1 . 70 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 1 ( 2 . 3 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - chloro - 4 - fluorophenyl isothiocyanate ( 1 . 35 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 1 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 62 . 9 %. esi - ms ( m / z , %) 536 . 27 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 65 ( s , 1h ), 9 . 31 ( s , 1h ), 9 . 20 ( s , 1h ), 8 . 51 ( s , 1h ), 8 . 23 ( m , 1h ), 7 . 86 ( d , j = 8 . 8 hz , 2h ), 7 . 78 ( m , 1h ), 7 . 75 ( t , j = 6 . 6 hz , 2h ), 7 . 41 ( t , j = 9 . 2 hz , 1h ), 4 . 90 ( s , 1h ), 2 . 88 ( d , j = 4 hz , 4h ), 2 . 43 ( m , 4h ), 2 . 20 ( s , 3h ), 1 . 70 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 2 ( 2 . 4 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and meta - acetamidophenyl isothiocyanate ( 1 . 4 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 2 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 1 %. esi - ms ( m / z , %) 561 . 18 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 00 ( s , 1h ), 9 . 52 ( s , 1h ), 9 . 20 ( s , 1h ), 8 . 88 ( s , 1h ), 8 . 42 ( s , 1h ), 8 . 26 ( m , 1h ), 8 . 08 ( s , 1h ), 7 . 66 ( d , j = 10 . 0 hz , 2h ), 7 . 57 ( d , j = 7 . 2 hz , 1h ), 7 . 21 ( m , 2h ), 4 . 94 ( m , 1h ), 2 . 90 ( s , 4h ), 2 . 68 ( br , 4h ), 2 . 06 ( s , 3h ), 1 . 64 ( d , j = 6 . 0 hz , 6h ) ppm . compound 5 - 2 ( 2 . 4 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 2 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 64 . 8 %. esi - ms ( m / z , %) 502 . 17 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 37 ( s , 1h ), 9 . 10 ( s , 1h ), 8 . 88 ( s , 1h ), 8 . 43 ( s , 1h ), 8 . 25 ( m , 1h ), 7 . 84 ( d , j = 8 . 4 hz , 2h ), 7 . 64 ( d , j = 10 . 4 hz , 2h ), 7 . 00 ( m , 2h ), 4 . 90 ( m , 1h ), 2 . 89 ( s , 4h ), 2 . 42 ( br , 4h ), 2 . 19 ( s , 3h ), 1 . 65 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 2 ( 2 . 4 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - chloro - 4 - fluorophenyl isothiocyanate ( 1 . 35 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 2 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 68 . 8 %. esi - ms ( m / z , %) 554 . 30 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ9 . 21 ( s , 1h ), 9 . 04 ( s , 1h ), 8 . 41 ( s , 1h ), 8 . 22 ( d , j = 5 . 2 hz , 1h ), 7 . 74 ( m , 1h ), 7 . 62 ( d , j = 8 . 8 hz , 1h ), 7 . 57 ( d , j = 8 . 8 hz , 1h ), 7 . 39 ( m , 1h ), 6 . 87 ( d , j = 8 . 4 hz , 2h ), 4 . 84 ( m , 1h ), 3 . 05 ( s , 4h ), 2 . 45 ( br , 4h ), 2 . 22 ( s , 3h ), 1 . 66 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 15 ( 2 . 4 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 15 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 67 . 6 %. esi - ms ( m / z , %) 502 . 22 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 22 ( s , 1h ), 8 . 87 ( s , 1h ), 8 . 49 ( s , 1h ), 8 . 44 ( s , 1h ), 8 . 29 ( t , j = 8 . 4 , 1h ), 7 . 86 ( d , j = 8 . 0 , 2h ), 7 . 78 ( d , j = 8 . 8 , 2h ), 7 . 34 ( t , j = 7 . 6 , 2h ), 7 . 01 ( t , j = 7 . 2 , 1h ), 4 . 97 ( m , 1h ), 4 . 04 ( m , 1h ), 3 . 38 ( m , 2h ), 3 . 09 ( m , 2h ), 2 . 72 ( s , 3h ), 1 . 99 ( m , 4h ), 1 . 65 ( d , j = 6 . 8 , 6h ) ppm . compound 5 - 3 ( 2 . 5 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 3 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 66 . 5 %. esi - ms ( m / z , %) 514 . 21 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 98 ( s , 1h ), 9 . 65 ( s , 1h ), 8 . 90 ( s , 1h ), 8 . 50 ( s , 1h ), 8 . 27 ( d , j = 7 . 6 hz , 1h ), 7 . 83 ( d , j = 7 . 6 hz , 2h ), 7 . 39 ( t , j = 8 hz , 2h ), 7 . 18 - 7 . 08 ( m , 3h ), 5 . 026 ( m , 1h ), 3 . 94 ( s , 4h ), 3 . 42 ( d , j = 7 . 6 hz , 2h ), 3 . 09 ( d , j = 12 hz , 2h ), 2 . 79 ( d , j = 7 . 2 hz , 3h ), 1 . 66 ( d , j = 6 . 4 hz , 6h ) ppm . to a solution of compound 5 - 4 ( 2 . 0 g ) and methyl 3 - ethynylphenylcarbamodithioate ( 1 . 3 g ) in n , n - dimethylformamide ( 30 ml ) were added copper oxide ( 0 . 08 g ) and potassium carbonate ( 1 . 4 g ). the mixture was heated to 60 ° c . and reacted for 2 - 6 hours . the reaction solution was cooled to room temperature and filtered . the filtrate was washed with ethyl acetate , a saturated saline solution and water . the organic layer was dried over anhydrous sodium sulfate and concentrated . purification was conducted by a column chromatography to obtain an off - white solid in a yield of 64 . 1 %. esi - ms ( m / z , %) 507 . 22 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 9 . 51 ( s , 1h ), 9 . 04 ( s , 1h ), 8 . 91 ( s , 1h ), 7 . 88 ( m , 4h ), 7 . 65 ( d , 2h ), 7 . 41 ( m , 2h ), 7 . 12 ( m , 1h ), 4 . 80 ( m , 1h ), 4 . 14 ( s , 1h ), 3 . 71 ( m , 1h ), 2 . 80 ( m , 4h ), 2 . 39 ( br , 4h ), 2 . 21 ( s , 3h ), 1 . 62 ( d , 6h ) ppm . compound 5 - 4 ( 2 . 3 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 4 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 67 . 9 %. esi - ms ( m / z , %) 483 . 25 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 72 ( s , 1h ), 9 . 63 ( s , 1h ), 9 . 11 ( s , 1h ), 8 . 45 ( s , 1h ), 8 . 28 ( s , 1h ), 7 . 89 - 7 . 81 ( m , 5h ), 7 . 34 ( t , j = 7 . 8 hz , 2h ), 7 . 00 ( t , j = 7 . 2 hz , 1h ), 4 . 95 ( m , 1h ), 4 . 02 ( s , 1h ), 3 . 44 ( d , j = 10 . 8 hz , 2h ), 3 . 08 ( s , 2h ), 2 . 75 ( s , 3h ), 1 . 99 ( s , 2h ), 1 . 82 ( d , j = 11 . 2 hz , 2h ), 1 . 70 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 67 . 5 %. esi - ms ( m / z , %) 441 . 29 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 9 . 09 ( d , j = 6 . 8 hz , 2h ), 8 . 36 ( s , 1h ), 7 . 83 ( d , j = 8 . 0 hz , 2h ), 7 . 69 ( d , j = 9 . 2 hz , 2h ), 7 . 33 ( m , 2h ), 6 . 97 ( m , 3h ), 4 . 92 ( m , 1h ), 3 . 44 ( br , 4h ), 3 . 17 ( br , 4h ), 2 . 81 ( s , 3h ), 1 . 67 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and meta - bromophenyl isothiocyanate ( 1 . 5 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 57 . 4 %. esi - ms ( m / z , %) 519 . 19 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 47 ( s , 1h ), 9 . 09 ( s , 1h ), 8 . 42 ( s , 1h ), 8 . 25 ( s , 1h ), 7 . 85 ( d , j = 8 . 0 hz , 1h ), 7 . 67 ( d , j = 8 . 8 hz , 2h ), 7 . 28 ( t , j = 8 . 4 hz , 1h ), 7 . 14 ( d , j = 8 . 0 hz , 1h ), 6 . 93 ( d , j = 8 . 8 hz , 2h ), 4 . 99 ( m , 1h ), 3 . 51 - 3 . 40 ( m , 2h ), 3 . 25 ( s , 2h ), 3 . 07 ( s , 4h ), 2 . 64 ( s , 3h ), 1 . 66 ( d , j = 6 . 8 ; h , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and meta - ethynylphenyl isothiocyanate ( 1 . 1 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 53 . 9 %. esi - ms ( m / z , %) 465 . 23 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 10 ( s , 1h ), 9 . 02 ( s , 1h ), 8 . 41 ( s , 1h ), 8 . 07 ( s , 1h ), 7 . 81 ( d , j = 8 . 4 hz , 1h ), 7 . 64 ( d , j = 9 . 2 hz , 2h ), 7 . 34 ( t , j = 8 . 0 , 1h ), 7 . 08 ( d , j = 7 . 2 hz , 1h ), 6 . 88 ( d , j = 9 . 2 hz , 2h ), 4 . 85 ( m , 1h ), 4 . 18 ( s , 1h ), 3 . 05 ( s , 4h ), 2 . 47 ( t , j = 9 . 0 , 4h ), 2 . 22 ( s , 3h ), 1 . 67 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - chloro - 4 - fluorophenyl isothiocyanate ( 1 . 35 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 60 . 8 %. esi - ms ( m / z , %) 493 . 16 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 9 . 21 ( s , 1h ), 9 . 04 ( s , 1h ), 8 . 41 ( s , 1h ), 8 . 22 ( d , j = 5 . 2 hz , 1h ), 7 . 74 ( m , 1h ), 7 . 62 ( d , j = 8 . 8 hz , 1h ), 7 . 57 ( d , j = 8 . 8 hz , 1h ), 7 . 39 ( m , 1h ), 6 . 87 ( d , j = 8 . 4 hz , 2h ), 4 . 84 ( m , 1h ), 3 . 05 ( br , 4h ), 2 . 45 ( br , 4h ), 2 . 22 ( s , 3h ), 1 . 66 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 8 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and meta - bromophenyl isothiocyanate ( 1 . 5 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 8 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 58 . 2 %. esi - ms ( m / z , %) 517 . 21 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 9 . 78 ( s , 1h ), 9 . 32 ( s , 1h ), 8 . 45 ( s , 1h ), 7 . 79 ( m , 2h ), 7 . 61 ( m , 2h ), 7 . 49 ( m , 2h ), 7 . 36 ( m , 1h ), 4 . 15 ( m , 1h ), 2 . 94 ( tr , 4h ), 2 . 63 ( br , 4h ), 2 . 19 ( s , 3h ), 1 . 26 ( m , 4h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and para - bromophenyl isothiocyanate ( 1 . 5 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 53 . 4 %. esi - ms ( m / z , %) 519 . 22 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 25 ( s , 1h ), 9 . 11 ( s , 1h ), 8 . 39 ( s , 1h ), 7 . 85 ( d , j = 8 . 8 hz , 2h ), 7 . 69 ( d , j = 9 . 2 hz , 2h ), 7 . 50 ( d , j = 8 . 8 hz , 2h ), 6 . 95 ( d , j = 9 . 2 hz , 2h ), 4 . 91 ( m , 1h ), 3 . 69 ( s , 1h ), 3 . 45 ( s , 1h ), 3 . 17 ( s , 1h ), 3 . 00 ( s , 1h ), 2 . 82 ( s , 3h ), 1 . 66 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and meta - trifluoromethylphenyl isothiocyanate ( 1 . 4 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 55 . 8 %. esi - ms ( m / z , %) 509 . 24 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 80 ( s , 1h ), 10 . 03 ( s , 1h ), 8 . 50 ( s , 1h ), 8 . 32 ( s , 1h ), 8 . 19 ( d , j = 8 . 0 , 1h ), 7 . 62 ( t , j = 7 . 8 , 1h ), 7 . 55 ( d , j = 8 . 8 , 2h ), 7 . 40 ( d , j = 7 . 6 , 1h ), 7 . 04 ( d , j = 9 . 2 , 2h ), 5 . 05 ( m , 1h ), 3 . 78 ( d , j = 12 . 4 , 4h ), 3 . 04 - 3 . 20 ( m , 4h ), 2 . 82 ( d , j = 4 . 0 , 3h ), 1 . 64 ( d , j = 6 . 4 , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and meta - methoxyphenyl isothiocyanate ( 1 . 2 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 58 . 8 %. esi - ms ( m / z , %) 471 . 28 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 06 ( d , j = 16 . 8 , 2h ), 8 . 37 ( s , 1h ), 7 . 69 ( d , j = 8 . 8 , 2h ), 7 . 52 ( s , 1h ), 7 . 42 ( d , j = 4 . 0 , 1h ), 7 . 22 ( t , j = 8 . 2 , 1h ), 6 . 95 ( d , j = 9 . 2 , 2h ), 6 . 56 ( m , 1h ), 4 . 91 ( m , 1h ), 3 . 76 ( s , 1h ), 2 . 81 ( s , 1h ), 1 . 66 ( d , j = 6 . 8 , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and para - methoxyphenyl isothiocyanate ( 1 . 2 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 59 . 8 %. esi - ms ( m / z , %) 471 . 28 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 04 ( s , 1h ), 8 . 93 ( s , 1h ), 8 . 30 ( s , 1h ), 7 . 71 ( m , j = 8 . 9 , 4h ), 6 . 94 ( t , j = 9 . 4 , 4h ), 4 . 90 ( m , 1h ), 3 . 75 ( s , 3h ), 3 . 46 - 3 . 43 ( m , 4h ), 3 . 17 - 3 . 06 ( m , 4h ), 2 . 81 ( s , 3h ), 1 . 67 ( d , j = 6 . 8 , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - chloro - 4 -( 3 - fluorobenzyloxy ) phenyl isothiocyanate ( 2 . 1 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 7 %. esi - ms ( m / z , %) 599 . 22 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 02 ( d , j = 4 . 8 hz , 2h ), 8 . 36 ( s , 1h ), 8 . 08 ( d , j = 2 . 4 hz , 1h ), 7 . 67 ( m , 3h ), 7 . 46 ( m , 1h ), 7 . 31 ( t , j = 7 . 6 hz , 2h ), 7 . 20 ( m , 2h ), 6 . 91 ( d , j = 8 . 8 hz , 2h ), 5 . 21 ( s , 2h ), 4 . 83 ( m , 1h ), 3 . 15 ( s , 4h ), 2 . 81 ( s , 3h ), 2 . 48 ( s , 2h ), 2 . 30 ( s , 2h ), 1 . 66 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and ( 3 - chloro - 4 -( pyridin - 2 - yl ) methoxy ) phenyl isothiocyanate ( 2 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 9 %. esi - ms ( m / z , %) 582 . 31 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 9 . 13 ( s , 1h ), 8 . 60 ( d , 1h ), 8 . 30 ( s , 1h ), 7 . 85 ( m , 3h ), 7 . 69 ( m , 1h ), 7 . 60 ( d , 2h ), 7 . 30 - 7 . 15 ( m , 4h ), 7 . 05 ( d , 1h ), 4 . 88 ( m , 1h ), 3 . 48 ( br , 4h ), 2 . 97 ( br , 4h ), 2 . 78 ( s , 3h ), 1 . 59 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 -( 3 -( 3 - chloro - 4 - fluorophenyl ) ureido ) phenyl isothiocyanate ( 2 . 3 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 62 . 5 %. esi - ms ( m / z , %) 627 . 21 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 8 . 99 ( d , j = 9 . 6 hz , 2h ), 8 . 88 ( s , 1h ), 8 . 80 ( s , 1h ), 8 . 34 ( s , 1h ), 7 . 94 ( s , 1h ), 7 . 84 ( m , 1h ), 7 . 63 ( d , j = 9 . 2 hz , 2h ), 7 . 47 ( d , j = 8 hz , 1h ), 7 . 37 - 7 . 28 ( m , 2h ), 7 . 22 ( t , j = 8 hz , 1h ), 7 . 11 ( d , j = 8 hz , 1h ), 6 . 88 ( d , j = 9 . 2 hz , 2h ), 4 . 90 ( m , 1h ), 3 . 06 ( t , j = 4 . 8 hz , 3h ), 2 . 51 ( m , 4h ), 2 . 48 ( d , j = 4 . 4 hz , 2h ), 2 . 26 ( d , j = 19 . 6 hz , 2h ), 1 . 67 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 4 -( 3 - fluorophenylcarbamoyl ) phenyl isothiocyanate ( 2 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 54 . 6 %. esi - ms ( m / z , %) 578 . 22 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 30 ( s , 1h ), 9 . 44 ( s , 1h ), 9 . 12 ( s , 1h ), 8 . 44 ( s , 1h ), 7 . 98 ( s , 3h ), 7 . 78 ( d , j = 11 . 6 hz , 1h ), 7 . 68 ( d , j = 8 . 8 hz , 2h ), 7 . 59 ( d , j = 7 . 2 hz , 2h ), 7 . 38 ( m , 1h ), 6 . 91 ( m , 3h ), 4 . 94 ( m , 1h ), 3 . 27 ( s , 4h ), 2 . 96 ( d , j = 8 hz , 2h ), 2 . 73 ( s , 3h ), 2 . 55 ( s , 2h ), 1 . 69 ( d , j = 6 . 4 hz , 6h ) ppm ; compound 5 - 8 ( 2 . 0 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 86 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 8 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 58 . 3 %. esi - ms ( m / z , %) 439 . 23 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 14 ( s , 1h ), 9 . 64 ( s , 1h ), 8 . 39 ( s , 1h ), 7 . 851 ( d , j = 8 hz , 2h ), 7 . 60 ( d , j = 8 . 8 hz , 2h ), 7 . 41 ( t , j = 8 hz , 2h ), 7 . 13 ( t , j = 7 . 2 hz , 1h ), 7 . 05 ( d , j = 9 . 2 hz , 2h ), 3 . 43 - 3 . 50 ( m , 4h ), 3 . 20 - 3 . 24 ( m , 4h ), 2 . 82 ( d , j = 3 . 2 hz , 3h ), 1 . 19 - 1 . 30 ( m , 4h ) ppm . compound 5 - 6 ( 1 . 9 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 86 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 6 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 51 . 1 %. esi - ms ( m / z , %) 413 . 24 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 57 ( s , 1h ), 9 . 52 ( s , 1h ), 8 . 37 ( s , 1h ), 7 . 88 ( d , j = 7 . 6 hz , 2h ), 7 . 656 ( d , j = 8 . 4 hz , 2h ), 7 . 37 ( t , j = 8 hz , 2h ), 7 . 05 ( t , j = 7 . 2 hz , 1h ), 6 . 99 ( d , j = 8 . 8 hz , 2h ), 3 . 69 ( s , 3h ), 3 . 381 ( s , 4h ), 3 . 16 ( d , j = 8 . 8 hz , 2h ), 3 . 03 ( d , j = 12 hz , 2h ), 2 . 82 ( s , 3h ) ppm . compound 5 - 5 ( 2 . 4 g ) was dissolved into dichloromethane ( 120 ml ). to the mixture were successively added edci ( 3 . 1 g ), n , n - diisopropylethylamine ( 6 . 6 ml ), and para - trifluoromethylphenyl isothiocyanate ( 1 . 1 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 5 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 57 . 3 %. esi - ms ( m / z , %) 399 . 27 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 89 ( s , 1h ), 9 . 93 ( s , 1h ), 8 . 77 ( s , 1h ), 8 . 20 ( s , 1h ), 7 . 30 ( d , j = 7 . 2 hz , 2h ), 7 . 63 ( d , j = 8 . 4 hz , 2h ), 7 . 34 ( t , j = 6 . 8 hz , 2h ), 7 . 00 ( s , 1h ), 6 . 87 ( d , j = 8 . 8 hz , 2h ), 3 . 04 ( t , j = 4 . 4 hz , 4h ), 2 . 46 ( t , j = 4 . 4 hz , 4h ), 2 . 23 ( s , 3h ) ppm . compound 5 - 9 ( 1 . 6 g ) was dissolved into dichloromethane ( 65 ml ). to the mixture were successively added edci ( 1 . 7 g ), n , n - diisopropylethylamine ( 3 . 7 ml ), and phenyl isothiocyanate ( 0 . 6 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 52 . 1 %. esi - ms ( m / z , %) 467 . 26 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 18 ( s , 1h ), 9 . 08 ( s , 1h ), 8 . 36 ( s , 1h ), 7 . 85 ( d , j = 7 . 6 hz , 2h ), 7 . 67 ( d , j = 8 . 4 hz , 2h ), 7 . 32 ( t , j = 3 . 6 hz , 2h ), 6 . 93 - 7 . 00 ( m , 3h ), 5 . 04 ( t , j = 8 hz , 1h ), 3 . 36 ( s , 8h ), 2 . 79 ( s , 3h ), 2 . 46 ( s , 2h ), 2 . 05 ( s , 4h ), 1 . 70 ( s , 2h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and para - trifluoromethylphenyl isothiocyanate ( 1 . 4 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 55 . 4 %. esi - ms ( m / z , %) 509 . 25 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 46 ( s , 1h ), 9 . 09 ( s , 1h ), 8 . 44 ( s , 1h ), 8 . 03 ( d , j = 8 . 4 hz , 2h ), 7 . 67 ( m , j = 8 . 8 hz , 4h ), 6 . 90 ( d , j = 8 . 8 hz , 2h ), 4 . 90 ( m , 1h ), 3 . 10 ( s , 4h ), 2 . 59 ( s , 4h ), 2 . 32 ( s , 3h ), 1 . 68 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - acrylylaminophenyl isothiocyanate ( 1 . 5 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 58 . 9 %. esi - ms ( m / z , %) 510 . 25 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 51 ( s , 1h ), 9 . 07 ( s , 1h ), 8 . 52 ( s , 1h ), 8 . 09 ( d , j = 8 . 4 hz , 2h ), 7 . 61 ( m , 4h ), 6 . 92 ( d , j = 8 . 8 hz , 2h ), 6 . 54 ( s , 1h ), 6 . 05 ( s , 1h ), 5 . 59 ( s , 1h ), 4 . 79 ( m , 1h ), 2 . 93 ( s , 4h ), 2 . 62 ( br , 4h ), 2 . 38 ( s , 3h ), 1 . 61 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - pyridinyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 7 %. esi - ms ( m / z , %) 442 . 26 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 38 ( s , 1h ), 9 . 13 ( s , 1h ), 8 . 99 ( s , 1h ), 8 . 40 ( s , 1h ), 8 . 36 ( d , j = 8 . 4 hz , 1h ), 8 . 20 ( d , j = 4 . 4 hz , 1h ), 7 . 70 ( d , j = 8 . 8 hz , 2h ), 7 . 37 ( m , 1h ), 6 . 96 ( d , j = 8 . 8 hz , 2h ), 4 . 97 - 4 . 92 ( m , 1h ), 3 . 35 ( s , 6h ), 2 . 80 ( s , 3h ), 2 . 53 ( s , 2h ), 1 . 69 ( s , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and cyclohexyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 67 . 8 %. esi - ms ( m / z , %) 447 . 28 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 89 ( s , 1h ), 9 . 26 ( s , 1h ), 8 . 23 ( s , 1h ), 7 . 62 ( d , j = 9 . 2 , 2h ), 6 . 95 ( d , j = 8 . 8 , 2h ), 4 . 72 ( m , 1h ), 4 . 03 ( m , j = 7 . 1 , 1h ), 3 . 69 ( s , 4h ), 3 . 13 - 3 . 09 ( m , 4h ), 2 . 80 ( s , 3h ), 1 . 98 ( d , j = 5 . 6 , 2h ), 1 . 76 ( d , j = 9 . 6 , 2h ), 1 . 57 ( d , j = 6 . 8 , 6h ), 1 . 37 - 1 . 26 ( m , 6h ) ppm . compound 5 - 10 ( 2 . 3 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 mlg ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 10 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 61 . 1 %. esi - ms ( m / z , %) 481 . 27 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 12 ( s , 1h ), 8 . 39 ( s , 1h ), 7 . 75 ( m , 2h ), 7 . 59 ( m , 2h ), 7 . 46 ( m , 2h ), 7 . 10 m , 3h ), 4 . 62 ( m , 1h ), 3 . 38 ( s , 6h ), 2 . 75 ( s , 3h ), 2 . 68 ( s , 3h ), 2 . 42 ( br , 2h ), 2 . 15 ( s , 4h ), 1 . 76 ( m , 4h ) ppm . compound 5 - 11 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 mlg ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 11 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 63 . 5 %. esi - ms ( m / z , %) 471 . 28 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 8 . 56 ( s , 1h ), 7 . 82 ( d , j = 8 . 0 hz , 2h ), 7 . 61 ( d , j = 8 . 4 hz , 2h ), 7 . 39 ( m , 2h ), 7 . 26 ( m , 2h ), 7 . 02 ( m , 2h ), 4 . 92 ( m , 1h ), 4 . 06 ( s , 3h ), 3 . 49 ( br , 4h ), 3 . 27 ( br , 4h ), 2 . 83 ( s , 3h ), 1 . 61 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 12 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 mlg ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 12 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 4 %. esi - ms ( m / z , %) 470 . 25 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d6 ): δ 8 . 61 ( s , 1h ), 7 . 83 ( d , j = 8 . 0 hz , 2h ), 7 . 69 ( m , 2h ), 7 . 37 ( m , 2h ), 7 . 25 ( m , 1h ), 7 . 04 ( m , 3h ), 4 . 71 ( m , 1h ), 3 . 49 ( br , 4h ), 3 . 27 ( br , 4h ), 2 . 86 ( s , 3h ), 1 . 65 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 13 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 13 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 66 . 7 %. esi - ms ( m / z , %) 455 . 28 ( m − h ) − ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 08 ( s , 1h ), 9 . 01 ( s , 1h ), 7 . 84 ( d , j = 8 . 0 , 2h ), 7 . 71 ( d , j = 8 . 8 , 2h ), 7 . 32 ( t , j = 7 . 8 , 2h ), 6 . 96 ( t , j = 8 . 4 , 3h ), 4 . 91 ( m , j = 6 . 6 , 1h ), 3 . 67 ( s , 4h ), 3 . 27 ( s , 4h ), 2 . 80 ( s , 3h ), 2 . 49 ( s , 3h ), 1 . 66 ( d , j = 6 . 8 , 6h ) ppm . compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - chloro - 4 - fluorophenyl isothiocyanate ( 1 . 35 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 67 . 6 %. esi - ms ( m / z , %) 519 . 20 ( m − h ) − ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 41 ( s , 1h ), 9 . 10 ( s , 1h ), 8 . 42 ( s , 1h ), 8 . 23 ( m , j = 3 . 07 , 1h ), 7 . 80 ( m , 1h ), 7 . 66 ( d , j = 8 . 8 , 2h ), 7 . 39 ( t , j = 9 . 2 , 1h ), 6 . 94 ( d , j = 9 . 2 , 2h ), 5 . 01 ( m , 1h ), 3 . 41 ( s , 4h ), 2 . 81 ( s , 3h ), 2 . 54 ( s , 4h ), 2 . 46 ( s , 2h ), 2 . 05 ( s , 4h ), 1 . 70 ( d , j = 4 . 4 , 2h ) ppm . compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - pyridinyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 64 . 3 %. esi - ms ( m / z ,%) 468 . 23 ( m − h ) − ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 40 ( s , 1h ), 9 . 11 ( s , 1h ), 8 . 97 ( d , j = 2 . 0 , 1h ), 8 . 40 ( s , 1h ), 8 . 35 ( d , j = 8 . 4 , 1h ), 8 . 20 ( d , j = 4 . 4 , 1h ), 7 . 66 ( d , j = 8 . 8 , 2h ), 7 . 36 ( m , j = 6 . 6 , 1h ), 6 . 93 ( d , j = 8 . 8 , 2h ), 5 . 02 ( m , 1h ), 3 . 20 ( s , 4h ), 2 . 73 ( s , 3h ), 2 . 47 ( s , 4h ), 2 . 06 ( s , 4h ), 1 . 71 ( s , 2h ), 1 . 23 ( s , 2h ) ppm . compound 5 - 14 ( 2 . 46 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - pyridinyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 14 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 70 . 3 %. esi - ms ( m / z , %) 511 . 23 ( m − h ) − ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 66 ( d , j = 11 . 2 , 2h ), 9 . 48 ( s , 1h ), 8 . 99 ( d , j = 2 . 0 , 1h ), 8 . 49 ( s , 1h ), 8 . 36 ( d , j = 7 . 6 , 1h ), 8 . 22 ( d , j = 4 . 0 , 1h ), 7 . 86 ( d , j = 8 . 8 , 2h ), 7 . 75 ( d , j = 8 . 4 , 2h ), 7 . 39 ( m , j = 4 . 3 , 1h ), 5 . 06 ( m , 1h ), 3 . 21 ( s , 4h ), 2 . 78 ( s , 3h ), 2 . 51 ( s , 4h ), 2 . 10 ( s , 4h ), 1 . 76 ( s , 2h ), 1 . 24 ( s , 2h ) ppm . compound 5 - 16 ( 1 . 87 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 16 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 5 %. esi - ms ( m / z , %) 414 . 23 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ 10 . 05 ( s , 1h ), 9 . 29 ( s , 1h ), 9 . 02 ( s , 1h ), 8 . 40 ( s , 1h ), 8 . 02 ( s , 1h ), 7 . 84 ( d , j = 8 . 0 , 2h ), 7 . 57 ( d , j = 6 . 8 , 1h ), 7 . 34 ( t , j = 7 . 2 , 2h ), 7 . 20 ( t , j = 7 . 4 , 2h ), 7 . 00 ( t , j = 7 . 2 , 1h ), 6 . 49 ( m , j = 9 . 1 , 1h ), 6 . 26 ( d , j = 16 . 8 , 1h ), 5 . 74 ( d , j = 10 . 0 , 1h ), 4 . 90 ( m , 1h ), 1 . 68 ( d , j = 6 . 8 , 6h ) ppm . compound 5 - 17 ( 2 . 23 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 17 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 70 . 5 %. esi - ms ( m / z , %) 474 . 26 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 08 ( s , 1h ), 8 . 30 ( s , 1h ), 8 . 01 ( s , 1h ), 7 . 88 ( d , j = 8 . 0 hz , 2h ), 7 . 71 ( d , j = 9 . 2 hz , 2h ), 7 . 30 ( m , 2h ), 7 . 17 ( m , 3h ), 4 . 84 ( m , 1h ), 4 . 04 ( m , 2h ), 3 . 84 ( m , 4h ), 3 . 24 ( br , 4h ), 2 . 81 ( m , 2h ), 1 . 63 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 18 ( 2 . 39 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 18 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 1 %. esi - ms ( m / z , %) 500 . 29 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 09 ( s , 1h ), 8 . 56 ( s , 1h ), 7 . 83 ( s , 1h ), 7 . 69 ( s , 1h ), 7 . 53 ( m , 2h ), 7 . 36 ( m , 4h ), 6 . 96 ( m , 3h ), 4 . 95 ( m , 1h ), 3 . 44 ( m , 2h ), 3 . 11 ( m , 2h ), 2 . 95 ( m , 8h ), 2 . 41 ( s , 3h ), 1 . 68 ( m , 2h ), 1 . 62 ( d , j = 6 . 8 hz , 6h ) ppm . compound 5 - 7 ( 2 . 05 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 2 - chloro - 5 - pyridinyl isothiocyanate ( 1 . 3 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 7 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 8 %. esi - ms ( m / z , %) 476 . 29 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 65 ( s , 1h ), 9 . 21 ( s , 1h ), 8 . 85 ( s , 1h ), 8 . 44 ( d , j = 6 . 8 hz , 2h ), 7 . 68 ( d , j = 8 . 0 hz , 2h ), 7 . 49 ( d , j = 8 . 8 hz , 1h ), 6 . 96 ( d , j = 8 . 0 hz , 2h ), 4 . 96 ( m , 1h ), 3 . 71 ( m , 2h ), 3 . 47 ( m , 2h ), 3 . 15 ( br , 2h ), 3 . 03 ( m , 2h ), 2 . 82 ( s , 2h ), 1 . 67 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 19 ( 1 . 97 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 0 . 9 ml ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 19 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale yellow solid in a yield of 70 . 6 %. esi - ms ( m / z , %) 586 . 27 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ 9 . 01 ( d , j = 7 . 2 hz , 2h ), 8 . 37 ( s , 1h ), 8 . 08 ( d , j = 2 . 4 hz , 1h ), 7 . 67 ( m , 3h ), 7 . 46 ( m , 1h ), 7 . 31 ( m , 2h ), 7 . 20 ( m , 2h ), 6 . 91 ( d , j = 9 . 2 hz , 2h ), 5 . 21 ( s , 2h ), 4 . 83 ( m , 1h ), 3 . 74 ( m , 4h ), 3 . 03 ( m , 4h ), 1 . 67 ( d , j = 6 . 4 hz , 6h ) ppm . compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 4 - bromophenyl isothiocyanate ( 1 . 65 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 66 . 7 %. esi - ms ( m / z , %) 548 . 18 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 22 ( s , 1h ), 9 . 09 ( s , 1h ), 8 . 39 ( s , 1h ), 7 . 83 ( d , j = 9 . 2 hz , 2h ), 7 . 65 ( d , j = 7 . 0 hz , 2h ), 7 . 50 ( d , j = 9 . 2 hz , 2h ), 6 . 93 ( d , j = 8 . 8 hz , 2h ), 4 . 95 ( m , 1h ), 3 . 27 - 3 . 02 ( m , 4h ), 2 . 75 ( m , 4h ), 2 . 45 ( s , 3h ), 2 . 05 ( m , 4h ), 1 . 68 ( m , 2h ), 1 . 23 ( m , 2h ). compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - nitrophenyl isothiocyanate ( 1 . 50 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 4 %. esi - ms ( m / z , %) 514 . 23 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 75 ( s , 1h ), 9 . 23 ( s , 1h ), 8 . 87 ( s , 1h ), 8 . 45 ( s , 1h ), 8 . 32 ( d , j = 7 . 6 hz , 1h ), 7 . 84 ( d , j = 7 . 2 hz , 1h ), 7 . 65 ( m , 3h ), 6 . 95 ( d , j = 8 . 8 hz , 2h ), 5 . 04 ( m , 1h ), 3 . 72 ( m , 2h ), 3 . 49 ( m , 2h ), 3 . 16 ( m , 2h ), 2 . 99 ( m , 2h ), 2 . 83 ( s , 3h ), 2 . 45 ( m , 2h ), 2 . 06 ( m , 4h ), 1 . 71 ( m , 2h ). compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and benzyl isothiocyanate ( 1 . 45 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 63 . 9 %. esi - ms ( m / z , %) 483 . 26 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ8 . 97 ( s , 1h ), 8 . 15 ( s , 1h ), 7 . 63 ( m , 3h ), 7 . 35 ( m , 4h ), 7 . 25 ( m , 1h ), 6 . 91 ( d , j = 9 . 2 hz , 2h ), 4 . 75 ( m , 1h ), 4 . 56 ( d , j = 8 . 0 hz , 2h ), 3 . 67 ( m , 2h ), 3 . 44 ( m , 2h ), 3 . 16 ( m , 2h ), 2 . 97 ( m , 2h ), 2 . 82 ( s , 3h ), 2 . 38 ( m , 2h ), 1 . 99 ( m , 4h ), 1 . 65 ( m , 2h ). compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - ethynylphenyl isothiocyanate ( 1 . 34 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 5 %. esi - ms ( m / z , %) 493 . 28 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 26 ( s , 1h ), 9 . 13 ( s , 1h ), 8 . 43 ( s , 1h ), 8 . 09 ( s , 1h ), 7 . 84 ( d , j = 8 . 0 hz , 1h ), 7 . 67 ( d , j = 8 . 4 hz , 2h ), 7 . 34 ( m , 1h ), 7 . 09 ( d , j = 7 . 2 hz , 1h ), 6 . 94 ( d , j = 10 . 8 hz , 2h ), 5 . 00 ( m , 1h ), 4 . 20 ( s , 1h ), 3 . 67 ( m , 2h ), 3 . 47 ( m , 2h ), 3 . 17 ( m , 2h ), 3 . 00 ( m , 2h ), 2 . 78 ( s , 3h ), 2 . 46 ( m , 2h ), 2 . 05 ( m , 4h ), 1 . 71 ( m , 2h ). compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 2 - fluoro - 4 - bromophenyl isothiocyanate ( 1 . 60 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 7 %. esi - ms ( m / z , %) 565 . 20 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 06 ( s , 1h ), 8 . 93 ( s , 1h ), 8 . 35 ( s , 1h ), 7 . 85 ( m , 1h ), 7 . 61 ( m , 3h ), 7 . 40 ( d , j = 8 . 4 hz , 1h ), 8 . 67 ( d , j = 9 . 2 hz , 2h ), 4 . 88 ( m , 1h ), 3 . 10 ( m , 4h ), 2 . 62 ( m , 4h ), 2 . 43 ( m , 2h ), 2 . 34 ( s , 3h ), 2 . 03 ( m , 4h ), 1 . 68 ( m , 2h ). compound 5 - 20 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and phenyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 9 %. esi - ms ( m / z , %) 470 . 27 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 57 ( s , 1h ), 9 . 16 ( s , 1h ), 8 . 45 ( s , 1h ), 7 . 91 ( s , 1h ), 7 . 86 ( d , j = 8 . 0 hz , 2h ), 7 . 76 ( s , 1h ), 7 . 47 ( s , 1h ), 7 . 38 ( m , 2h ), 7 . 22 ( s , 1h ), 7 . 03 ( m , 1h ), 5 . 04 ( m , 1h ), 4 . 10 ( m , 2h ), 3 . 70 ( m , 4h ), 3 . 15 ( m , 2h ), 2 . 37 ( m , 2h ), 2 . 05 ( m , 4h ), 1 . 75 ( m , 2h ), 1 . 29 ( m , 2h ). compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 4 . 9 ml ), and 3 - fluorophenyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 67 . 4 %. esi - ms ( m / z , %) 487 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 42 ( s , 1h ), 9 . 13 ( s , 1h ), 8 . 42 ( s , 1h ), 7 . 92 ( d , j = 12 . 0 hz , 1h ), 7 . 67 ( d , j = 9 . 2 hz , 2h ), 7 . 59 ( d , j = 8 . 0 hz , 1h ), 7 . 35 ( m , 1h ), 6 . 94 ( d , j = 8 . 8 hz , 2h ), 6 . 79 ( m , 1h ), 5 . 02 ( m , 1h ), 3 . 68 ( m , 2h ), 3 . 44 ( m , 2h ), 3 . 18 ( m , 2h ), 3 . 01 ( m , 2h ), 2 . 81 ( s , 3h ), 2 . 44 ( m , 2h ), 2 . 05 ( m , 4h ), 1 . 70 ( m , 2h ). compound 5 - 21 ( 1 . 53 g ) was dissolved into dichloromethane ( 35 ml ). to the mixture were successively added edci ( 1 . 54 g ), n , n - diisopropylethylamine ( 3 . 31 ml ), and phenyl isothiocyanate ( 0 . 56 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 21 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 69 . 4 %. esi - ms ( m / z , %) 483 . 25 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 04 ( s , 1h ), 8 . 99 ( s , 1h ), 8 . 34 ( s , 1h ), 7 . 80 ( d , j = 8 . 4 hz , 2h ), 7 . 67 ( d , j = 8 . 8 hz , 2h ), 7 . 33 ( m , 2h ), 6 . 98 ( m , 1h ), 6 . 87 ( d , j = 8 . 4 hz , 2h ), 4 . 74 ( m , 1h ), 3 . 05 ( m , 4h ), 2 . 61 ( m , 2h ), 5 . 47 ( m , 4h ), 2 . 23 ( s , 3h ), 1 . 91 ( m , 2h ), 1 . 81 ( m , 3h ), 1 . 44 ( m , 2h ), 1 . 34 ( m , 1h ). compound 5 - 9 ( 2 . 1 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine - 2 . 1 ml ), and 3 - hydroxyphenyl isothiocyanate ( 1 . 05 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 70 . 4 %. esi - ms ( m / z , %) 485 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 36 ( s , 1h ), 9 . 07 ( s , 1h ), 8 . 93 ( s , 1h ), 8 . 35 ( s , 1h ), 7 . 67 ( d , j = 9 . 2 hz , 2h ), 7 . 38 ( s , 1h ), 7 . 16 ( d , j = 9 . 2 hz , 1h ), 7 . 08 ( m , 1h ), 6 . 93 ( d , j = 9 . 2 hz , 2h ), 6 . 39 ( s , 1h ), 4 . 96 ( m , 1h ), 3 . 43 ( m , 2h ), 3 . 34 ( m , 2h ), 3 . 16 ( m , 4h ), 2 . 75 ( s , 1h ), 2 . 46 ( m , 2h ), 2 . 04 ( m , 4h ), 1 . 69 ( m , 2h ). compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 70 ml ). to the mixture were successively added edci ( 2 . 7 g ), n , n - diisopropylethylamine ( 2 . 5 ml ), and 3 - chlorophenyl isothiocyanate ( 1 . 42 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 71 . 7 %. esi - ms ( m / z , %) 503 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 38 ( s , 1h ), 9 . 13 ( s , 1h ), 8 . 44 ( s , 1h ), 8 . 11 ( s , 1h ), 7 . 75 ( d , j = 8 . 0 hz , 1h ), 7 . 65 ( d , j = 8 . 4 hz , 2h ), 7 . 35 ( m , 1h ), 7 . 02 ( m , 1h ), 6 . 94 ( d , j = 8 . 8 hz , 2h ), 5 . 01 ( m , 1h ), 3 . 43 ( m , 4h ), 3 . 10 ( m , 4h ), 2 . 82 ( s , 3h ), 2 . 45 ( m , 2h ), 2 . 05 ( m , 4h ), 1 . 70 ( m , 2h ) ppm . compound 5 - 9 ( 2 . 1 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine 2 . 1 ml ), and 3 - methylphenyl isothiocyanate ( 1 . 0 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 72 . 7 %. esi - ms ( m / z , %) 483 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 08 ( s , 1h ), 9 . 02 ( s , 1h ), 8 . 37 ( s , 1h ), 7 . 68 - 7 . 62 ( m , 4h ), 7 . 22 ( m , 1h ), 6 . 93 ( d , j = 8 . 8 hz , 2h ), 6 . 80 ( d , j = 7 . 6 hz , 1h ), 4 . 99 ( m , 1h ), 3 . 67 ( m , 2h ), 3 . 44 ( m , 2h ), 3 . 03 ( m , 4h ), 2 . 81 ( s , 3h ), 2 . 45 ( m , 2h ), 2 . 31 ( s , 3h ), 2 . 04 ( m , 4h ), 1 . 69 ( m , 2h ) ppm . compound 5 - 9 ( 2 . 55 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 2 . 67 g ), n , n - diisopropylethylamine 2 . 7 ml ), and 3 , 5 - dichlorophenyl isothiocyanate ( 1 . 7 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 73 . 7 %. esi - ms ( m / z , %) 537 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 40 ( s , 1h ), 9 . 08 ( s , 1h ), 8 . 48 ( s , 1h ), 7 . 97 ( s , 1h ), 7 . 60 ( d , j = 8 . 8 hz , 2h ), 7 . 21 ( m , 2h ), 6 . 99 ( m , 2h ), 4 . 90 ( m , 1h ), 3 . 12 ( m , 2h ), 3 . 04 ( m , 2h ), 2 . 54 ( m , 4h ), 2 . 21 ( m , 4h ), 2 . 04 ( s , 3h ), 1 . 67 ( m , 2h ), 1 . 19 ( m , 2h ) ppm . compound 5 - 9 ( 2 . 7 g ) was dissolved into dichloromethane ( 100 ml ). to the mixture were successively added edci ( 2 . 8 g ), n , n - diisopropylethylamine ( 3 ml ), and 2 , 5 - difluorophenyl isothiocyanate ( 1 . 5 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 70 . 6 %. esi - ms ( m / z , %) 505 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 16 ( s , 1h ), 9 . 06 ( s , 1h ), 8 . 43 ( s , 1h ), 7 . 91 ( m , 1h ), 7 . 56 ( m , 2h ), 7 . 32 ( m , 1h ), 6 . 91 ( m , 3h ), 4 . 92 ( m , 1h ), 3 . 45 ( m , 4h ), 3 . 23 - 3 . 03 ( m , 4h ), 2 . 80 ( s , 3h ), 2 . 42 ( m , 2h ), 2 . 03 ( m , 4h ), 1 . 68 ( m , 2h ) ppm . compound 5 - 22 ( 3 . 2 g ) was dissolved into dichloromethane ( 90 ml ). to the mixture were successively added edci ( 3 . 6 g ), n , n - diisopropylethylamine 3 . 3 ml ), and phenyl isothiocyanate ( 1 . 52 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 75 . 3 %. esi - ms ( m / z , %) 443 . 25 ( m − h ) − . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 20 ( s , 1h ), 9 . 06 ( s , 1h ), 8 . 36 ( s , 1h ), 7 . 86 ( d , j = 9 . 6 hz , 2h ), 7 . 65 ( d , j = 8 . 0 hz , 2h ), 7 . 34 ( m , 2h ), 6 . 97 ( m , 1h ), 6 . 85 ( d , j = 8 . 0 hz , 2h ), 5 . 05 ( m , 1h ), 4 . 04 ( m , 2h ), 3 . 64 ( m , 2h ), 3 . 31 ( s , 3h ), 2 . 43 ( m , 2h ), 2 . 03 ( m , 4h ), 1 . 68 ( m , 2h ) ppm . compound 5 - 9 ( 2 . 1 g ) was dissolved into dichloromethane ( 60 ml ). to the mixture were successively added edci ( 2 . 15 g ), n , n - diisopropylethylamine ( 2 ml ), and 2 , 4 , 5 - trichlorophenyl isothiocyanate ( 1 . 6 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . after cooling the mixture , a solid was separated out and purified by recrystallization to obtain a pale yellow solid in a yield of 74 . 3 %. esi - ms ( m / z , %) 571 . 25 ( m − h ) + ; 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 09 ( s , 1h ), 9 . 01 ( s , 1h ), 8 . 27 ( s , 1h ), 7 . 64 ( m , 2h ), 7 . 12 ( m , 1h ), 6 . 89 ( d , j = 8 . 4 hz , 2h ), 6 . 78 ( d , j = 7 . 2 hz , 1h ), 4 . 93 ( m , 1h ), 3 . 64 ( m , 2h ), 3 . 41 ( m , 2h ), 3 . 13 ( m , 4h ), 2 . 75 ( s , 3h ), 2 . 43 ( m , 2h ), 2 . 14 ( m , 4h ), 1 . 65 ( m , 2h ) ppm . compound 5 - 23 ( 4 . 6 g ) was dissolved into dichloromethane ( 100 ml ). to the mixture were successively added edci ( 1 . 67 g ), n , n - diisopropylethylamine 1 . 2 ml ), and phenyl isothiocyanate ( 0 . 79 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 25 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 65 . 1 %. esi - ms ( m / z , %) 497 . 25 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 25 ( s , 1h ), 9 . 06 ( s , 1h ), 8 . 40 ( s , 1h ), 7 . 82 ( d , j = 8 . 0 hz , 2h ), 7 . 71 ( d , j = 8 . 4 hz , 2h ), 7 . 34 ( m , 2h ), 7 . 15 ( d , j = 8 . 4 hz , 2h ), 6 . 99 ( m , 1h ), 4 . 97 ( m , 1h ), 3 . 38 ( s , 2h ), 2 . 47 - 2 . 29 ( m , 12h ), 2 . 05 ( m , 2h ), 1 . 71 ( m , 2h ), 0 . 97 ( m , 3h ) ppm . compound 5 - 25 ( 4 . 6 g ) was dissolved into dichloromethane ( 100 ml ). to the mixture were successively added edci ( 1 . 74 g ), n , n - diisopropylethylamine 1 . 2 ml ), and phenyl isothiocyanate ( 0 . 82 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 25 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 71 . 8 %. esi - ms ( m / z , %) 483 . 25 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 25 ( s , 1h ), 9 . 05 ( s , 1h ), 8 . 39 ( s , 1h ), 7 . 82 ( d , j = 8 . 0 hz , 2h ), 7 . 70 ( d , j = 8 . 0 hz , 2h ), 7 . 33 ( m , 2h ), 7 . 15 ( d , j = 8 . 0 hz , 2h ), 6 . 99 ( m , 1h ), 4 . 97 ( m , 2h ), 3 . 38 ( m , 4h ), 2 . 50 ( m , 4h ), 2 . 33 ( m , 4h ), 2 . 14 ( s , 3h ), 2 . 05 ( m , 4h ), 1 . 71 ( m , 2h ) ppm . compound 5 - 9 ( 1 . 3 g ) was dissolved into dichloromethane ( 60 ml ). to the mixture were successively added edci ( 0 . 8 g ), n , n - diisopropylethylamine ( 2 ml ), and 2 , 5 - dichlorophenyl isothiocyanate ( 0 . 72 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 16 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . purification was conducted by a column chromatography to obtain a pale yellow solid in a yield of 64 . 3 %. esi - ms ( m / z , %) 537 . 23 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 02 ( s , 1h ), 8 . 62 ( s , 1h ), 8 . 37 ( s , 1h ), 7 . 91 ( s , 1h ), 7 . 59 ( d , j = 8 . 4 hz , 2h ), 7 . 49 ( d , j = 7 . 6 hz , 1h ), 7 . 10 ( m , 1h ), 6 . 86 ( d , j = 9 . 2 hz , 2h ), 4 . 91 ( m , 1h ), 3 . 04 ( m , 4h ), 2 . 45 ( m , 4h ), 2 . 22 ( s , 3h ), 2 . 00 ( m , 4h ), 1 . 67 ( m , 2h ) ppm . compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 40 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 5 ml ), and 2 , 4 - dichlorophenyl isothiocyanate ( 1 . 5 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 12 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . purification was conducted by a column chromatography to obtain a pale yellow solid in a yield of 67 . 4 %. esi - ms ( m / z , %) 537 . 22 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 01 ( s , 1h ), 8 . 70 ( s , 1h ), 8 . 26 ( s , 1h ), 7 . 59 ( d , j = 8 . 4 hz , 4h ), 7 . 39 ( s , 1h ), 6 . 86 ( d , j = 8 . 8 hz , 2h ), 4 . 90 ( m , 1h ), 3 . 04 ( m , 4h ), 2 . 45 ( m , 6h ), 2 . 22 ( s , 3h ), 2 . 00 ( m , 4h ), 1 . 67 ( m , 2h ) ppm . compound 5 - 9 ( 2 . 2 g ) was dissolved into dichloromethane ( 40 ml ). to the mixture were successively added edci ( 2 . 3 g ), n , n - diisopropylethylamine ( 5 ml ), and 3 - bromophenyl isothiocyanate ( 1 . 54 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 12 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 9 . purification was conducted by a column chromatography to obtain a pale yellow solid in a yield of 69 . 5 %. esi - ms ( m / z , %) 547 . 12 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 34 ( s , 1h ), 9 . 13 ( s , 1h ), 8 . 44 ( s , 1h ), 8 . 22 ( s , 1h ), 7 . 83 ( d , j = 8 . 4 hz , 1h ), 7 . 67 ( d , j = 8 . 8 hz , 2h ), 7 . 29 ( m , 1h ), 7 . 15 ( d , j = 8 . 0 hz , 1h ), 6 . 94 ( d , j = 9 . 2 hz , 2h ), 5 . 01 ( m , 1h ), 3 . 65 ( m , 4h ), 3 . 28 ( m , 4h ), 2 . 81 ( s , 3h ), 2 . 45 ( m , 2h ), 2 . 05 ( m , 4h ), 1 . 70 ( m , 2h ) ppm . compound 5 - 23 ( 2 . 0 g ) was dissolved into dichloromethane ( 25 ml ). to the mixture were successively added edci ( 1 . 92 g ), n , n - diisopropylethylamine ( 2 . 25 ml ), and phenyl isothiocyanate ( 0 . 82 g ). the mixture was stirred at room temperature for half an hour , and refluxed for 10 hours . tlc detection indicated the completion of the reaction of the starting material 5 - 23 . after cooling the mixture , purification was conducted by a column chromatography to obtain a pale red solid in a yield of 66 . 2 %. esi - ms ( m / z , %) 497 . 26 ( m − h ) + . 1 h nmr ( 400 mhz , dmso - d 6 ): δ9 . 04 ( s , 1h ), 8 . 59 ( s , 1h ), 8 . 30 ( s , 1h ), 7 . 81 ( d , j = 8 . 4 hz , 2h ), 7 . 65 ( d , j = 8 . 8 hz , 2h ), 7 . 31 ( m , 2h ), 6 . 88 ( m , 1h ), 6 . 75 ( d , j = 8 . 4 hz , 2h ), 3 . 78 ( m , 2h ), 3 . 05 ( m , 4h ), 1 . 82 - 1 . 54 ( m , 7h ), 1 . 36 - 1 . 18 ( m , 4h ), 1 . 12 - 1 . 00 ( m , 2h ). assay 1 : the test of the arylamino purine derivatives for the kinase inhibitory activity the object of this assay was to test the inventive compounds for the kinase inhibitory activity in vitro . in this assay , an isotopic labeling method was used to label the γ phosphate group on atp . egfr ( including wild type , l858r mutant type and l858r / t790m double mutant type ), vegfr2 , alk , btk , c - kit , c - src , met , pdgfrα and flt3 kinases were tested in vitro for the activity inhibition . staurosporine was used as a reference molecule ( or referred to as a positive control ). the kinase inhibitory activities of the tested compounds were expressed in the ic 50 value ( half inhibition concentration ) or the kinase activity inhibitory rate by the tested compounds at 10 μm . the ic 50 value can be obtained by the calculation of the inhibitory rates at a series of different concentrations of the tested compounds . 0 . 1 mg / ml glutamic acid / tyrosine ( 4 : 1 ) polymerized polypeptide ( poly ( glu , tyr ) 4 : 1 ) ( the substrate for wild type and l858r mono mutant type egfrs , c - kit and pdgfrα ); 250 μm polypeptide ggmediyfefmggkkk ( the substrate for l858r / t790m double mutant type egfr ); 250 μm polypeptide kvekigegty gvvyk ( the substrate for btk and c - src ); 10 mm a solution of magnesium acetate and γ - 33 p - atp ; egfrs ( including wild type , l858r mono mutant type and l858r / t790m double mutant type egfrs ), vegfr2 , alk , btk , c - kit , c - src , met , pdgfrα , flt3 kinase , and the tested compounds . to a reaction tube were successively added the buffer solution ( 8 mm mops , ph 7 . 0 , 0 . 2 mm edta , 10 mm mncl 2 ), the kinase to be tested ( 5 - 10 mu ) ( egfr / alk / btk / c - kit / c - src / met / pdgfrα / vegfr2 ), the substrate for the kinase to be tested ( a reference material ), 10 mm of the solution of magnesium acetate and γ - 33 p - atp , and different concentrations of the tested compounds . the reaction was started by adding mgatp ( the final concentration of atp is the km value of the corresponding kinase , i . e ., 10 μm for egfrwild type , 200 μm for egfr l858r , 45 μm for egfr l858r / t790m , 200 μm for alk , 200 μm for btk , 200 μm for c - kit , 90 μm for vegfr2 , 200 μm for c - src , 45 μm for met , 120 μm for pdgfrα , and 200 μm for flt3 ), and incubated at room temperature for 40 minutes . the reaction was terminated with 54 of the 3 % phosphate buffer solution . 10 μl of the reaction liquid was titrated on the filtermat a membrane . the membrane was washed with 75 mm of the phosphate solution thrice ( 5 minutes each time ), and then with methanol once , and finally dried . the membrane was subjected to a scintillation counting . the value of the scintillation counting reflected the phosphorylation level of the substrate and therefore could characterize the inhibition of the kinase activity . through the above procedures , the inhibitory activities of the present compounds were tested for the kinases egfrs ( comprising wild type , l858r mutant type and l858r / t790m double mutant type ), vegfr2 , alk , btk , c - kit , c - src , met , pdgfrα , and flt3 . the kinase inhibitory activities ( ic 50 values ) of the tested compounds for egfrs ( comprising wild type , l858r mutant type and l858r / t790m double mutant type ) and vegfr2 are shown in table 1 . the activity inhibition ratio (%) of the tested compounds at 10 μm for the kinases alk , btk , c - kit , c - src , met , pdgfrα , and flt3 are shown in table 2 . the results indicated that the tested compounds had strong inhibitory activities on the wild type , l858r mutant type and l858r / t790m double mutant type egfrs , and some of the tested compounds also had good inhibitory activities on vegfr2 , alk , btk , c - kit , c - src , met , pdgfrα , flt3 kinases . the object of this assay was to test the inventive compounds for the inhibitory activity of in - vitro tumor cell proliferation . the mtt ( tetreamethyl - azo - zole - salt ) colorimetric method was used in this assay . rpmi - 1640 , fetal bovine serum , pancreatin and the like were purchased from gibco brl company ( invitrogen corporation , usa ). the imdm culture medium was purchased from atcc ( american type culture collection ). tetreamethyl - azo - zole - salt ( mtt ) and dimethylsulfoxide ( dmso ) were the products available from sigma company ( usa ). the arylamino purine derivatives were synthesized by the present inventors . in this in - vitro assay , 100 % dmso was formulated into a 10 mm stocking solution and preserved in a freezer at − 20 ° c . and in dark place for use . the stocking solution was diluted with a complete culture solution to a desired concentration immediately before use . human non - small cell lung carcinoma cell strains hcc827 , pc - 9 , h1975 ( egfr l858r / t790m mutation ) and h292 ( egfr wt ), and other tumor type cell strains , including human acute myelogenous leukemia cell strain mv4 - 11 , human chronic granulocytic leukemia cell strain k562 , human squamous cell carcinoma cell strain a431 , human breast carcinoma cell strains mda - mb - 468 and bt 474 , human colon cancer cell strains sw480 , hct116 and sw620 , human liver cancer cell strain hep g2 , human gastric cancer cell strain mk - 45 , and human malignant melanoma cell strain a375 used in this assay were all purchased from atcc company , usa and kept in the laboratory . all of the above - mentioned non - small cell lung carcinoma cell strains and the breast carcinoma cell strain bt 474 were cultured with a rpmi - 1640 complete culture medium containing 10 % fetal bovine serum , 100 u / ml penicillin and 100 μg / ml streptomycin under 5 % co2 and at 37 ° c . the other cell strains were cultured with a dmem complete culture medium containing 10 % fetal bovine serum ( having a mv4 - 11 cell content of 20 %), 100 u / ml penicillin and 100 μg / ml streptomycin under 5 % co2 and 37 ° c . a cell suspension having a cell concentration of 1 - 2 × 10 4 cells / ml was treated with a complete cell culture solution to adjust the cell concentration , wherein the cell concentrations for hcc827 and mv4 - 11 were adjusted to 6 × 10 4 cells / ml and 1 × 10 5 cells / ml respectively . the cell suspension was inoculated in a 96 - well plate with 200 μl cell suspension / well and cultured overnight . next day , the supernatant was drawn off and discarded . then , the cells were treated with the tested compounds in a gradient concentration respectively . in the meanwhile , a negative control group free of the drug substance and an isovolumetric solvent control group ( having a dmso concentration of 1 %) were used . the triplicate wells were used for each of dose groups . the culturing was conducted at 37 ° c . under 5 % co2 . after 72 hours , 200 mtt agent having a concentration of 5 mg / ml was added to each of wells . the culturing was further conducted for 2 - 4 hours . the supernatant was discarded . then 1504 dmso was added to each of wells . the contents in the well were mixed homogenously by oscillation for 15 minutes . the absorbance ( a ) value was measured with a microplate reader at λ = 570 nm ( the a value is in the direct proportion to the number of living cells ) and averaged . the relative cell proliferation inhibitory rate is ( a 570 control - group − a 570 dose - group )/ a 570 control - group × 100 %. the assay was repeated for at least three times . the data was expressed as number average . the statistical data were analyzed using t - test . p & lt ; 0 . 05 was considered significant . the cell proliferation inhibition of the following compounds was expressed as ic50 or inhibitory rate . according to the above - mentioned procedure , human non - small cell lung carcinoma cell strains hcc827 , pc - 9 ( egfr dele746 - a750 deletion mutation ), h1975 ( egfr l858r / t790m mutation ) and h292 ( egfr wt ), and other tumor type cell strains , including human acute myelogenous leukemia cell strain mv4 - 11 , human chronic granulocytic leukemia cell strain k562 , human squamous cell carcinoma cell strain a431 , human breast carcinoma cell strains mda - mb - 468 and bt 474 , human colon cancer cell strains sw480 , hct116 and sw620 , human liver cancer cell strain hep g2 , human gastric cancer cell strain mk - 45 , and human malignant melanoma cell strain a375 were subjected to the proliferation inhibition activity test . the proliferation inhibitory activities ( ic 50 ) of the tested compounds for human non - small cell lung carcinoma cell strains hcc827 , pc - 9 and h1975 are shown in the table 3 . the proliferation inhibitory activities ( ic 50 ) of the tested compounds for human tumor cell strains mv4 - 11 , k562 , a431 , mda - mb - 468 , bt474 , sw480 , hct116 , hepg2 , sw620 , mk - 45 , h292 and a375 are shown in the tables 4 and 5 . the results indicated that the tested compounds had strong inhibitory activities on the cell strains hcc827 and pc - 9 which were sensitive to gefitinib ; some of the tested compounds also had a good inhibitory activity on the cell strain h1975 which was resistant to gefitinib ; and in addition , some of the tested compounds also had good inhibitory activities on the other tumor cell strains including human mv4 - 11 , k562 , a431 , mda - mb - 468 , bt474 , sw480 , hct116 , hepg2 , sw620 , mk - 45 , h292 , a375 and the like . the object of this assay was to determine the in - vivo anti - tumor effect of the present compound . in this assay , a nude mouse subcutaneously transplanted non - small cell lung carcinoma model was used to test the present compound 8 - 10 for the in - vivo anti - tumor activity . the used cell strain was human non - small cell lung carcinoma cell strain hcc827 . rpmi - 1640 , fetal bovine serum , pancreatin and the like were purchased from gibco brl company ( invitrogen corporation , usa ); rpmi 1640 culture medium was purchased from atcc ( american type culture collection ); human non - small cell lung carcinoma cell strain hcc827 was purchased from atcc company , usa ; and balb / c nude mice were purchased from institute of zoology , chinese academy of sciences . balb / c nude mice , aged 6 - 8 weeks , were inoculated with hcc827 cell subcutaneously at the posterior segment of rib in a concentration of about 5 × 10 6 cells / 0 . 1 ml per mouse . upon the growth of the tumor up to 200 - 300 mm 3 ( about 20 days ), mice were grouped ( n = 6 ) and administrated intragastrically . ( each of drug groups was dissolved in 5 % dmso + 1 % tween80 + 94 % water ). observation indices : the mice were measured every three days for the weight , and the length and width of tumor , and the tumor volume was calculated as length × width 2 × 0 . 52 . the mice were observed for the reactions such as diarrhea , convulsion , exanthema , and substantial weight reduction . the measured tumor growth curves for each of the groups are shown in fig1 . the photograph of tumors obtained by dissection after the assay is shown in fig2 . the results indicated that the tested compound 8 - 10 had a substantial in - vivo growth inhibition for the egfr dele746 - a750 mutated human non - small cell lung carcinoma cell strain hcc827 . upon administrating in 2 mg / kg q . d . or higher , the tumor growth could be substantially inhibited , or even the tumor could be eliminated . in the course of administration , the nude mice did not show the untoward reactions such as weight reduction , exanthema , and diarrhea , which indicated that under the test doses , the tested compound 8 - 10 had a low toxicity in the dose range of administration . the object of this assay was to determine the in - vivo anti - tumor effect of the present compound . in this assay , a nod - scid mouse subcutaneously transplanted human leukemic solid tumor model was used to test the present compound 8 - 29 for the in - vivo anti - tumor activity . the used cell strain was human acute myelogenous leukemia cell strain mv4 - 11 . imdm , fetal bovine serum , pancreatin and the like were purchased from gibco brl company ( invitrogen corporation , usa ); imdm culture medium was purchased from atcc ( american type culture collection ), human leukemia cell strain mv4 - 11 was purchased from atcc company , usa ; and the nod - scid mice were purchased from laboratory animal center , peking union medical college , china . nod - scid mice , aged 6 - 8 weeks , were inoculated with mv4 - 11 cell subcutaneously at the posterior segment of rib in a concentration of about 1 × 10 7 cells / 0 . 1 ml per mouse . upon the growth of the tumor up to 400 - 500 mm 3 ( about 20 days ), mice were grouped ( n = 6 ) and administrated intragastrically . ( each of drug groups was dissolved in 5 % dmso + 25 % peg400 + 70 % water ) observation indices : the mice were measured every three days for the weight , and the length and width of tumor , and the tumor volume was calculated as length × width 2 × 0 . 52 . the mice were observed for the reactions such as diarrhea , convulsion , exanthema , and substantial weight reduction . the measured tumor growth curves for each of the groups are shown in fig3 . the results indicated that the tested compound 8 - 29 had a substantial in - vivo growth inhibition for the flt3 - itd mutated human acute myelogenous leukemia cell strain mv4 - 11 . upon administrating in 5 mg / kg q . d . or higher , the tumor growth could be substantially inhibited , or even the tumor could be eliminated . in the course of administration , the mice did not show the untoward reactions such as weight reduction , exanthema , and diarrhea , which indicated that under the test doses , the tested compound 8 - 29 had a low toxicity in the dose range of administration . | 2 |
the following detailed description is presented to enable any person skilled in the art to make and use the invention . for purposes of explanation , specific details are set forth to provide a thorough understanding of the present invention . however , it will be apparent to one skilled in the art that these specific details are not required to practice the invention . descriptions of specific applications are provided only as representative examples . various modifications to the preferred embodiments will be readily apparent to one skilled in the art , and the general principles defined herein may be applied to other embodiments and applications without departing from the scope of the invention . the present invention is not intended to be limited to the embodiments shown , but is to be accorded the widest possible scope consistent with the principles and features disclosed herein . the electric roof access hatch unlocking and opening system consists of a locking mechanism , an opening mechanism , and a control panel , each more fully described below . through its electronic circuitry , the control panel controls the actions of the locking mechanism and the opening mechanism . the locking mechanism is a device , as depicted in fig4 , fig9 , and fig1 , which engages a lock on the roof access hatch . it is controlled by the control panel 1 ( as depicted in fig1 and fig2 ) and may either lock or unlock upon application of a current . in the present embodiment , when current is applied , solenoid 4 retracts , pulling latch 19 into a recessed state . the locking system is preferably solenoid driven , as depicted in fig9 . however , other electrically - operated locking mechanisms may be used , including , but not limited to , magnetic locks , motor - operated locks , and electric strikes . the locking mechanism optionally includes a manual key override 3 , as depicted in fig9 a , that allows the locking system to be unlocked in the event of emergency if the control panel circuitry or opening mechanism cannot function properly due to extended power outages or damage to any component . lever 24 is operatively coupled to the manual key override . inserting and turning a key in the manual key override 3 causes lever 24 to push against a protrusion 25 on the latch 19 , forcing the latch 19 into a recessed state , allowing access hatch 8 to be opened . opening mechanism 5 is depicted in fig3 and in fig5 . in the preferred embodiment , the opening mechanism is driven by a linear thrust actuator 6 . linear thrust actuator 6 is coupled to access hatch 8 at a pivot point 7 on angled access hatch mounting bracket 27 . angled access hatch mounting bracket 27 is configured such that pivot point 7 is located at a distance from the hinge side of the roof access hatch . when the control panel circuitry applies power to opening mechanism 5 , the thrust rod of linear thrust actuator 6 extends . as the linear thrust actuator 6 extends , it applies a force to pivot point 7 . the force of the linear thrust actuator 6 at pivot point 7 causes access hatch 8 to rotate about the axis of the roof access hatch hinge , causing the hatch to lift open from the side opposite the hinges . other mechanisms for opening the roof access hatch may be used and include electric motors or pneumatic cylinders . the opening mechanism 5 may be adjustable to accommodate different angles and mounting positions and varying thicknesses of insulation . as can be seen from fig1 , the roof - mounted mounting bracket 12 may be coupled to linear thrust actuator 6 by use of adjustable bracket 14 . in the preferred embodiment , the bracket consists of a bar with equally spaced holes along its length . the linear thrust actuator 6 is affixed to the upper end of the adjustable bracket using bracket pin 13 . the lower end of adjustable bracket 14 is connected to the roof - mounted mounting bracket 12 . the roof - mounted mounting bracket 12 is further securely attached to the underside of the roof decking 16 . to accommodate for varying thicknesses of installations or lowered mounting positions , bracket pin 13 can be inserted into any of the equally spaced holes situated along the length of the bar on the adjustable bracket . bracket pin 13 can also be removed to disengage the roof access hatch 8 from the opening mechanism 5 . circuitry in the control panel 1 activates the locking mechanism 2 and the opening mechanism 5 . although various methods of providing power to the locking and opening mechanisms are known and may be used , a simple circuit is disclosed herein . an example of such a circuit can be seen in fig6 , fig7 , and fig8 . control panel 1 can be placed into different modes of operation as the operator desires . in the open mode , the control panel circuitry directs the roof access hatch to open . in the closed mode , the control panel circuitry directs the roof access hatch to close . the off position is the default position to be used when the roof access hatch is not being utilized . in the preferred embodiment , the various modes are selected by use of a key switch 26 . as seen in fig1 , status lights 10 on the front of the control panel 1 , may indicate the current mode of operation of the roof access hatch 8 . when control panel 1 is placed in open mode , power is applied to open relay 28 that sends power to the opening mechanism 5 and to a lock relay 29 for limited duration sufficient to unlock the locking mechanism 2 . the lock relay 29 transmits power to the locking mechanism 2 , causing it to unlock . in the current embodiment , this is a delay - on - break relay . this lock relay 29 keeps the latch 19 recessed until the hatch access 8 begins to open . open relay 28 is set to output power to the linear thrust actuator 6 at a time after the lock relay 29 has unlocked the roof access hatch 8 , but before the flow of current to the locking mechanism 2 is terminated . in the preferred embodiment , the open relay 28 is a delay - on - make relay . when the open relay 28 permits current to flow , power is transmitted to the linear thrust actuator 6 in the opening mechanism 5 , causing the opening mechanism to lift open the roof access hatch 8 . the open relay 28 stops transmitting power after a duration sufficient for the linear thrust actuator 6 to fully open the roof access hatch 8 . the duration will vary based on the size and weight of the roof access hatch . limit switches may be used on the roof access hatch to prevent the opening mechanism from forcing the roof access hatch beyond the fully open position . when control panel 1 is placed in close mode , power is applied to the close relay 34 . the close relay 34 transmits current to the linear thrust actuator 6 with the polarity reversed such that the linear thrust actuator 6 returns to a retracted state , pulling the roof access hatch 8 closed . the close relay 34 transmits power only for a duration sufficient to close the roof access hatch . the spring loaded latch 19 on the locking mechanism 2 secures the roof access hatch 8 in a locked position when the roof access hatch 8 is in a fully closed position . the control panel 1 is placed into either the open mode , close mode , or off mode by use of a switch . in the preferred embodiment , a key switch 26 is used to place the control panel into one of the three modes , allowing the operator to remove the key for security purposes . other known access control devices may be used to place the control panel into its various modes , including , but not limited to , pushbutton operation , biometric means , or computer - based access control . indicator lights 10 on the front of the control panel 1 may be used to indicate the status of the electrically - operated access hatch 8 , such as whether the roof access hatch 8 is opening or closing and whether the lock is engaged . current is supplied to control panel 1 from an exterior source , such as a standard power outlet . the control panel 1 may optionally house a surge protector 30 , as seem in fig2 , to protect the circuitry of the control panel 1 from electrical spikes . the current is transmitted to a dc transformer 31 that converts incoming power to a dc current . in the preferred embodiment , the transformer outputs 12v dc . however , any voltage may be adapted for use in the system . the control panel optionally includes a battery charger 32 and battery 33 . the battery 33 provides emergency back - up power if the external power source fails . this allows the operator to use the roof access hatch 8 as an emergency egress if there is a power failure . backup power relay 36 switches the source of power from the dc transformer 31 to the battery 33 in the event of a power outage . the opening mechanism 5 optionally has an emergency release that allows the roof access hatch 8 to be separated from the opening mechanism 5 in the event that manual operation is required in an emergency . in the preferred embodiment , the emergency release is bracket pin 13 that may be removed from adjustable bracket 14 causing the linear thrust actuator 6 to disconnect from roof - mounted mounting bracket 12 . in the event of an emergency , such as a malfunction or damage to the claimed device , or when the emergency battery 33 is depleted of reserve power during extended power outages , the roof access hatch can be manually opened . to open the roof access hatch 8 , the manual override key 3 is turned to unlock locking mechanism 2 , and bracket pin 13 is removed from adjustable bracket 14 . the roof access hatch 8 can then freely open . to close the roof access hatch 8 in the event of an emergency , the roof access hatch 8 can be pulled closed manually . to do so , linear thrust actuator 6 must be disengaged from adjustable bracket 14 by removal of bracket pin 13 . the roof access hatch 8 can then be pulled shut using handle 17 which is preferably affixed to the outside of locking mechanism 2 . however , the handle 17 can be located anywhere on the roof access hatch 8 . as the roof access hatch 8 is pulled closed , the latch 19 on the locking mechanism is pushed inward toward the roof access hatch hinge . the latch 19 is springloaded by means of spring 18 so that latch 19 returns to its fully extended state once access hatch 8 is in the fully closed position . under normal operating conditions , the linear thrust actuator 6 maintains access hatch 8 in the open position while the operator is on the roof . the roof access hatch will not blow closed in gusty winds while the linear thrust actuator is in the open position . however , when the roof access hatch is opened manually by removal of bracket pin 13 , a prop bar similar to that used to keep the hood of a vehicle open can be used to keep the roof access hatch open . this prop bar will prevent the operator from being trapped on the roof by preventing the closure of the roof access hatch . the electrically - operated access hatch 8 may also optionally include safety features to prevent accidental closure of the roof access hatch while a person is accessing the hatch . sensors may be mounted to detect the presence of a person near the opening mechanism of the roof access hatch . in the preferred embodiment , a retro reflective photoelectric beam sensor is employed to ensure that a person is not injured by a closing roof access hatch . the retro reflective photoelectric beam sensor is mounted on the wall near the hinge side of the roof access hatch 8 . a reflector placed on the wall near the ladder 22 reflects emitted light back to the light sensor of the retro reflective photoelectric beam sensor . a person or object near the roof access hatch would prevent emitted light from reflecting back to the retro reflective photoelectric beam sensor . the retro reflective photoelectric beam sensor is configured to cause the control panel 1 to interrupt power to the linear thrust actuator 6 whenever light is not reflected back , indicating the presence of a person or object near the roof access hatch 8 . this is handled by the safety relay 35 in control panel 1 that directs power to the open relay 28 if the light is not reflected back to the retro reflective photoelectric beam sensor . the roof access hatch will cease closing and will enter open mode . the circuitry disclosed in this application is one possible embodiment of the invention . however , it is evident to a person of ordinary skill in the art that the circuitry can be designed in many variations to operate the opening and locking mechanisms of the roof access hatch . specifically , a computer board or digital circuitry may be used that performs the same functions as the circuitry disclosed . the electric roof access hatch unlocking and opening system can be mounted to a roof access hatch 8 that is already installed in a building . alternatively , the electric roof access hatch unlocking and opening system may be part of a kit that includes the roof access hatch 8 and any accessories such as a ladder 22 . it should be understood that features of any of these embodiments may be used with another in a way that will now be understood in view of the foregoing disclosure . although the present invention has been described and illustrated with respect to at least one preferred embodiment and use therefor , it is not to be so limited since modifications and changes can be made therein which are within the fully intended scope of the invention . | 4 |
in accordance with some embodiments , circuits and methods for wireless transmitters are provided . turning to fig1 , an example 100 of a digital polar phased array transmitter in accordance with some embodiments is shown . in some embodiments , any suitable number of transmitters 100 can be used in a transmitter application . for example , in some embodiments , one transmitter ( having four ( for example ) elements ( described below )) can be used . in another embodiment , four transmitters ( each having four ( for example ) elements ( described below )) can be used , for example . in some embodiments , any suitable modulation technique can be used with transmitter ( s ) 100 . for example , in some embodiments , qam64 modulation can be used . as illustrated , transmitter 100 includes a local oscillator reference input 102 , a frequency multiplier 104 , a quadrature hybrid 106 , a resistor 108 , a phase modulator 110 , a digital interface 112 , an array driver 114 , digital polar transmitter elements 116 , 118 , 120 , and 122 , transmitter outputs 124 , 126 , 128 , and 130 , serial digital inputs 132 , a global biasing circuit 170 , and an esd circuit 172 . a local oscillator reference signal is received by transmitter 100 at input 102 . any suitable local oscillator reference signal having any suitable frequency can be used . for example , in some embodiments , local oscillator reference signal can have a frequency of 30 ghz . the local oscillator reference signal is received by frequency multiplier 104 and multiplied to a higher frequency . any suitable frequency multiplier can be used ( e . g ., a frequency multiplier as described below in connection with fig2 can be used ), and the local oscillator reference signal can be multiplied by any suitable amount . for example , in some embodiments , the frequency multiplier can multiply the local oscillator reference signal by two . the output of frequency multiplier 104 can be received by quadrature hybrid 106 . the quadrature hybrid can be any suitable quadrature hybrid in accordance with some embodiments . as illustrated , resistor 108 can be connected from one of the inputs of the quadrature hybrid to ground to provide a reference impedance . any suitable resistor can be used in some embodiments . for example , a 50 ohm resistor can be used . in - phase and quadrature components of the multiplied local oscillator reference signal can be output by hybrid 106 to phase modulator 110 . the phase modulator can be any suitable phase modulator , such as the phase modulator / shifter described below in connection with fig3 and 4 . the phase modulator can be controlled by phase control outputs [ p 0 , i - p 7 , i ] and [ p 0 , q - p 7 , q ] of digital interface 112 . array driver 114 can receive the output of phase modulator 110 and provide a drive signal to digital polar transmitter elements 116 , 118 , 120 , and 122 that is split evenly among the digital polar transmitter elements . any suitable array driver can be used in some embodiments . for example , in some embodiments , the array driver described below in connection with fig5 can be used . digital polar transmitter elements 116 , 118 , 120 , and 122 can drive transmitter outputs 124 , 126 , 128 , and 130 in response to the drive signal from array driver 114 and amplitude control outputs [ a 0 - a 7 ] of digital interface 112 . each of transmitter outputs 124 , 126 , 128 , and 130 can be connected to a suitable antenna . for example , in some embodiments , the antenna ( s ) can be phased array antennas , on - printed - circuit - board antennas , and / or any other suitable type of antenna . any suitable number of digital polar transmitter elements can be used in some embodiments . for example , in some embodiments , four digital polar transmitter elements can be used to drive a 2 × 2 array of four antennas . as further shown in fig1 , digital polar transmitter elements 116 , 118 , 120 , and 122 can each include a resistor 140 , a quadrature hybrid 142 , a phase shifter 144 , a limiting amplifier 146 , and a hybrid power digital amplitude converter ( dac ) 148 . the drive signal from array driver 114 can be provided to quadrature hybrid 142 . the quadrature hybrid can be any suitable quadrature hybrid in accordance with some embodiments . as illustrated , resistor 140 can be connected from one of the inputs of the quadrature hybrid to ground to provide a reference impedance . any suitable resistor can be used in some embodiments . for example , a 50 ohm resistor can be used . in - phase and quadrature components of the drive signal from array driver 114 can be output by hybrid 142 to phase shifter 144 . the phase shifter can be any suitable phase shifter , such as the phase modulator / shifter described below in connection with fig3 and 4 . the phase shifter can be controlled by control signals φ 1 , φ 2 , φ 3 , and φ 4 from a controller 174 . these control signals can be used to control the phase of the signal to be transmitted by the digital polar transmitter element for any suitable purpose , such as for beamforming . controller can include any suitable hardware processor ( e . g ., a microprocessor , microcontroller , dedicated control logic , a digital signal processor , etc . ), a scan chain , registers , memory , interfaces , inputs , outputs , etc . and can perform any suitable functions , such as controlling phase shifters 144 , controlling bias functions , performing specialized processing for phased arrays , compensating for various implementation non - idealities that result in beam pointing error , etc . the outputs of phase shifter 144 can be provided to limiting amplifier 146 . the limiting amplifier can be any suitable limiting amplifier , such as the limiting amplifier described below in connection with fig6 . the output of limiting amplifier 146 can be provided to hybrid power dac 148 . hybrid power dac 148 can be any suitable hybrid power dac in some embodiments . for example , hybrid power dac 148 can be implemented using the hybrid power dac described below in connection with fig7 . as shown in fig1 , digital interface 112 can include variable gain amplifiers ( vgas ) 158 , continuous time linear equalizers ( ctles ) 160 , and demultiplexers 162 , 164 , and 166 . digital interface can receive digital serial inputs 132 . more particularly , inputs 132 can include i phase control inputs , q phase control inputs , amplitude control inputs , and a clock at inputs 150 , 154 , 152 , and 156 , respectively . based on the inputs received at 132 , the digital interface can generate phase control outputs [ p 0 , i - p 7 , i ] and [ p 0 , q - p 7 , q ] and amplitude control outputs [ a 0 - a 7 ] from demultiplexers 162 , 166 , and 164 , respectively . global biasing circuitry 170 can be provided , as known in the art , to generate biasing voltages in circuit 100 in accordance with some embodiments . esd circuitry 172 can be provided , as known in the art , to protect circuit 100 from electrostatic discharge and over - voltage conditions in accordance with some embodiments . fig2 shows an example 200 of a frequency multiplier that can be used to implement frequency multiplier 104 of fig1 in some embodiments . as shown , a local oscillator reference signal can be received at node 202 , the signal multiplied by two , and then the resulting signal output at node 204 . in some embodiments , match blocks 206 and 208 can include any suitable components for matching the impedance of the points on the left and right of each match block . for example , in some embodiments , match blocks 206 and 208 can include inductors , spirals , transmission lines , and / or capacitors . turning to fig3 , an example 300 of a phase modulator / shifter that can be used as phase modulator 110 and / or phase shifter 144 of fig1 in some embodiments . as shown , phase modulator / shifter 300 includes mixers 302 and 304 . any suitable mixers can be used as mixers 302 and 304 . for example , in some embodiments , example mixer 400 described below in connection with fig4 can be used as mixers 302 and / or 304 . as shown in fig4 , mixer 400 includes eight switching transistors represented in this figure by transistors 402 , 404 , 406 , and 408 . the transistors other than transistor 408 ( the most significant bit ( msb ) transistor ) are binary weighted with weights of w , 2w , . . . , 2 6 w , where w represents a given combination of finger width and number of fingers in a transistor . any suitable combination of finger width and number of fingers can be used in the transistors for w , such as a finger width of 0 . 152 micron and one finger , in some embodiments . the gates of these transistors are connected to inputs b 0 , b 1 , b 2 , . . . , b 7 . these bits can be provided by phase control bits [ p 0 , i - p 7 , i ], [ p 0 , q - p 7 , q ], φ 1 , φ 2 , φ 3 , or φ 4 shown in fig1 in some embodiments . the binary value that is provided to the inputs , determines the amount of modulation or shift of the input signal such that a higher value turns on a higher total weighting of switches , resulting in a higher current flow through the switches . although eight transistors and inputs are shown , any suitable number of inputs and transistors can be used in some embodiments . a bias voltage , v b , can also be provided to calibrate the shifter to account for variations in process , voltage , and temperature . turning to fig5 , an example 500 of an array driver that can be used to implement array driver 114 of fig1 is shown in accordance with some embodiments . as shown , an input signal can be presented at inputs 502 of driver 500 , the signal will be amplified , and the resulting signal will be provided at node 504 . turning to fig6 , an example 600 of a limiting amplifier that can be used to implement limiting amplifier 146 of fig1 is shown in accordance with some embodiments . as shown , an input signal can be presented at node 602 of limiting amplifier 600 , the signal will be amplified , and the resulting signal will be provided at node 504 . fig7 shows an example 700 of a hybrid power dac that can be used to implement hybrid power dac 148 of fig1 in accordance with some embodiments . as shown , in some embodiments , hybrid power dac 700 can be implemented as a differential class - e power amplifier with four stacked transistors that is augmented with trail transistors ( at the common source node ) and a supply inverter ( connected to the differential dc - feed spiral of the four - stack class e power amplifier ) to incorporate amplitude modulation capability . in some embodiments , hybrid power dac 700 includes inputs 702 and 704 , outputs 706 and 708 , inverters 710 , switching transistors 712 , 714 , and 716 , stacked transistors 717 , 718 , 720 , and 722 , dc feed inductors ( implemented as transmission lines ) 724 , gate bias inputs 726 , 728 , 730 , and 732 , two - stack drivers 734 , and match blocks 736 . as shown in fig7 , hybrid power dac 700 includes two inverters 710 and n − 1 switching transistors , represented in this figure by transistors 712 , 714 , and 716 . the n − 1 switching transistors ( represented by transistors 712 , 714 , and 716 ) are binary weighted with weights of w 1 , 2w 1 , . . . , 2 n - 1 w 1 , where w 1 represents a given combination of finger width and number of fingers in a transistor . any suitable combination of finger width and number of fingers can be used in the transistors for w 1 , such as a finger width of 2 . 793 micron and two fingers , in some embodiments . the gates of the transistors are connected to inputs b 0 , b 1 , b 2 , . . . , b n - 1 and the input to the inverter is connected to input b n ( the most significant bit ( msb )). as suggested by the use of n in fig7 , any suitable number of switching transistors , and hence inputs b 0 . . . b n - 1 can be used in some embodiments . the binary value that is provided to inputs b 0 , b 1 , b 2 , . . . , b n determines the amount of amplification provided by the hybrid power dac . these bits can be provided by amplitude control bits [ a 0 - a 7 ] shown in fig1 in some embodiments . more particularly , a higher value at inputs b 0 , b 1 , b 2 , . . . , b n - 1 turns on a higher total weighting of the switching transistors , resulting in a higher current flow through the switching transistors , and the value of input b n at the input to inverter 710 determines the supply voltage v dd , pa supplied to the stack of transistors including stacked transistors 717 , 718 , 720 , and 722 and the switching transistors . the manner in which this amplification is achieved is further illustrated in connection with fig1 . as shown , for a given input at the gate of transistor m 1 1002 , a voltage between ground and 2v dd ( represented by voltage 1010 ) ( where , v dd here represents the nominal voltage supply in the technology used , for example , 1 . 2v nominally in 45 nm soi cmos ) is produced at the source of transistor m 2 1004 . this results in a voltage between v on and 2v dd being present at the gate of transistor m 2 1004 through capacitance cgs between the source and the gate of transistor m 2 1004 ( which capacitance is inherently present in transistor m 2 1004 ), resulting in a voltage between ground and 4v dd ( represented by voltage 1012 ) being produced at the source of transistor m 3 1006 . this results in a voltage between v on and 4v dd being present at the gate of transistor m 3 1006 through capacitance cgs between the source and the gate of transistor m 3 1006 , resulting in a voltage between ground and 6v dd ( represented by voltage 1014 ) being produced at the source of the transistor above transistor m 3 1006 . this process is repeated for the transistors going upward along the stack represented by transistors 1002 , 1004 , 1006 , and 1008 until a voltage of between v on and 2 ( n − 1 ) v dd ( represented by voltage 1016 ) is produced at the gate of transistor m n 1008 , which results in a voltage between ground and 2nv dd being produced at the drain of transistor m n 1008 and the output of the stack . as stated above , whether the output of the stack is at ground or 2nv dd depends on the input at the gate of transistor m 1 1002 . referring back to fig7 , the corresponding inputs in the hybrid power dac are at the gates of transistors m 1 717 . as shown , these input are controlled by the outputs of two - stack drivers 734 , which are driven by inputs 702 and 704 . an example 800 of a two - stack driver that can be used for two - stack driver 734 in accordance with some embodiments is shown in fig8 . as shown , the input to the two - stack driver is provided at node 802 and the output is produced at node 804 . as shown in fig7 , the outputs of two - stack drivers 734 are connected to the gates of transistors m 1 717 by match blocks 736 . in some embodiments , match blocks 736 can include any suitable components for matching the impedance of the points on the left and right of each match block . for example , in some embodiments , match blocks 736 can include inductors , spirals , transmission lines , and / or capacitors . as also shown in fig7 , the gates of transistors m 1 717 , m 2 718 , m 3 720 , and m 4 722 are biased by bias voltages v g1 , v g2 , v g3 , and v g4 . these bias voltages can be produced in any suitable manner . for example , in some embodiments , for each hybrid power dac 700 , an adaptive bias circuit , such as adaptive bias circuit 900 shown in fig9 , can be provided . as illustrated in fig9 , circuit 900 includes a voltage divider 902 formed from four resistors r 1 . these resistors can have any suitable value . the voltage divider is powered by v dd , pa , which as described in fig7 is variable and controlled by the output of inverters 710 . voltages v 1 , v 2 , and v 3 shown in fig9 are provided to transistors 904 , 906 , and 908 , respectively . the bias voltages are then produced at the nodes labelled v g1 , v g2 , v g3 , and v g4 . resistors r big can have any suitable values sufficiently large compared to the gate impedance ( of the gates connected to the corresponding bias voltage ) to have suitable performance but not too large so as to affect modulation speed . in some embodiments , r big can be a 1 kω resistor . in some embodiments , transistor 910 can be implemented as a bank of parallel binary weighted transistors ( e . g ., like the binary weighted transistors described above in connection with fig4 and 7 ) so that the bias voltages produced by circuit 900 can be controlled by controller 174 of fig1 . in some of these embodiments , any suitable number of parallel binary weighted transistors can be provided , and each of the transistors can have any suitable weighting ( s ). when such control is not needed , transistor 910 can be a single transistor . although specific components having specific properties ( e . g ., resistances , capacitance , sizes , relative sizes , voltages , etc .) are shown in fig1 - 10 , one or more of the components in any one or more of these figures can be omitted or substituted with one or more alternate components having one or more different properties , in some embodiments . the provision of the examples described herein ( as well as clauses phrased as “ such as ,” “ e . g .,” “ including ,” and the like ) should not be interpreted as limiting the claimed subject matter to the specific examples ; rather , the examples are intended to illustrate only some of many possible aspects . although the invention has been described and illustrated in the foregoing illustrative embodiments , it is understood that the present disclosure has been made only by way of example , and the numerous changes in the details of implementation of the invention can be made without departing from the spirit and scope of the invention , which is only limited by the claims which follow . features of the disclosed embodiments can be combined and rearranged in various ways . | 7 |
the novel features of the invention are set forth with particularity in the appended claims . a better understanding of the features and advantages of the present invention will be obtained by reference to the following detailed description that sets forth illustrative embodiments , in which the principles of the invention are utilized . while preferred embodiments of the present invention have been shown and described herein such embodiments are provided by way of example only . it should be understood that various alternatives to the embodiments of the invention described herein may be employed in practicing the invention . those ordinary skilled in the art will appreciate that numerous variations , changes , and substitutions are possible without departing from the invention . it is intended that the following claims define the scope of aspects of the invention and that methods and structures within the scope of these claims and their equivalents be covered thereby . the section headings used herein are for organizational purposes only and are not to be construed as limiting the subject matter described . all documents , or portions of documents , cited in the application including , without limitation , patents , patent applications , articles , books , manuals , and treatises are hereby expressly incorporated by reference in their entirety for any purpose . unless defined otherwise , all technical and scientific terms used herein have the same meaning as is commonly understood by one of skill in the art to which the claimed subject matter belongs . all patents , patent applications , published materials referred to throughout the entire disclosure herein , unless noted otherwise , are incorporated by reference in their entirety . in the event that there is a plurality of definitions for terms herein , those in this section prevail . where reference is made to a url or other such identifier or address , it is understood that such identifiers can change and particular information on the internet can come and go , but equivalent information can be found by searching the internet or other appropriate reference source . reference thereto evidences the availability and public dissemination of such information . it is to be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of any subject matter claimed . in this application , the use of the singular includes the plural unless specifically stated otherwise . it must be noted that , as used in the specification and the appended claims , the singular forms “ a ”, “ an ” and “ the ” include plural referents unless the context clearly dictates otherwise . it should also be noted that use of “ or ” means “ and / or ” unless stated otherwise . furthermore , use of the term “ including ” as well as other forms , such as “ include ”, “ includes ”, and “ included ” is not limiting . likewise , use of the term “ comprising ” as well as other forms , such as “ comprise ”, “ comprises ”, and “ comprised ” is not limiting . definition of standard chemistry terms may be found in reference works , including carey and sundberg “ advanced organic chemistry 4 ed .” vols . a ( 2000 ) and b ( 2001 ), plenum press , new york . unless otherwise indicated , conventional methods of mass spectroscopy , nmr , hplc , ir and uv / vis spectroscopy and pharmacology , within the skill of the art are employed . unless specific definitions are provided , the nomenclature employed in connection with , and the laboratory procedures and techniques of , analytical chemistry , synthetic organic chemistry , and medicinal and pharmaceutical chemistry described herein are those known in the art . standard techniques can be used for chemical syntheses , chemical analyses , pharmaceutical preparation , formulation , and delivery , and treatment of patients . reactions and purification techniques can be performed e . g ., using kits of manufacturer &# 39 ; s specifications or as commonly accomplished in the art or as described herein . the foregoing techniques and procedures can be generally performed of conventional methods well known in the art and as described in various general and more specific references that are cited and discussed throughout the present specification . throughout the specification , groups and substituents thereof can be chosen by one skilled in the field to provide stable moieties and compounds . where substituent groups are specified by their conventional chemical formulas , written from left to right , they equally encompass the chemically identical substituents that would result from writing the structure from right to left . as a non - limiting example , ch 2 o is equivalent to och 2 . unless otherwise noted , the use of general chemical terms , such as though not limited to “ alkyl ,” “ amine ,” “ aryl ,” are equivalent to their optionally substituted forms . for example , “ alkyl ,” as used herein , includes optionally substituted alkyl . the compounds presented herein may possess one or more stereocenters and each center may exist in the r or s configuration , or combinations thereof . likewise , the compounds presented herein may possess one or more double bonds and each may exist in the e ( trans ) or z ( cis ) configuration , or combinations thereof . presentation of one particular stereoisomer , regioisomer , diastereomer , enantiomer or epimer should be understood to include all possible stereoisomers , regioisomers , diastereomers , enantiomers or epimers and mixtures thereof . thus , the compounds presented herein include all separate configurational stereoisomeric , regioisomeric , diastereomeric , enantiomeric , and epimeric forms as well as the corresponding mixtures thereof . techniques for inverting or leaving unchanged a particular stereocenter , and those for resolving mixtures of stereoisomers are well known in the art and it is well within the ability of one of skill in the art to choose an appropriate method for a particular situation . see , for example , fumiss et al . ( eds . ), vogel &# 39 ; s encyclopedia of practical organic chemistry 5 . sup . th ed ., longman scientific and technical ltd ., essex , 1991 , 809 - 816 ; and heller , acc . chem . res . 1990 , 23 , 128 . the term “ bond ” or “ single bond ” refers to a chemical bond between two atoms , or two moieties when the atoms joined by the bond are considered to be part of larger substructure . the term “ optional ” or “ optionally ” means that the subsequently described event or circumstance may or may not occur , and that the description includes instances where said event or circumstance occurs and instances in which it does not . for example , “ optionally substituted alkyl ” means either “ alkyl ” or “ substituted alkyl ” as defined below . further , an optionally substituted group may be un - substituted ( e . g ., ch 2 ch 3 ), fully substituted ( e . g ., cf 2 cf 3 ), mono - substituted ( e . g ., ch 2 ch 2 f ) or substituted at a level anywhere in - between fully substituted and mono - substituted ( e . g ., ch 2 chf 2 , cf 2 ch 3 , cfhchf 2 , etc ). it will be understood by those skilled in the art with respect to any group containing one or more substituents that such groups are not intended to introduce any substitution or substitution patterns ( e . g ., substituted alkyl includes optionally substituted cycloalkyl groups , which in turn are defined as including optionally substituted alkyl groups , potentially ad infinitum ) that are sterically impractical and / or synthetically non - feasible . thus , any substituents described should generally be understood as having a maximum molecular weight of about 1 , 000 daltons , and more typically , up to about 500 daltons ( except in those instances where macromolecular substituents are clearly intended , e . g ., polypeptides , polysaccharides , polyethylene glycols , dna , rna and the like ). as used herein , c 1 - cn , includes c 1 - c 2 , c 1 - c 3 , . . . c 1 - cn . by way of example only , a group designated as “ c 1 - c 4 ” indicates that there are one to four carbon atoms in the moiety , i . e . groups containing 1 carbon atom , 2 carbon atoms , 3 carbon atoms or 4 carbon atoms , as well as the ranges c 1 - c 2 and c 1 - c 3 . thus , by way of example only , “ c 1 - c 4 alkyl ” indicates that there are one to four carbon atoms in the alkyl group , i . e ., the alkyl group is selected from among methyl , ethyl , propyl , iso - propyl , n - butyl , isobutyl , sec - butyl , and t - butyl . whenever it appears herein , a numerical range such as “ 1 to 10 ” refers to each integer in the given range ; e . g ., “ 1 to 10 carbon atoms ” means that the group may have 1 carbon atom , 2 carbon atoms , 3 carbon atoms , 4 carbon atoms , 5 carbon atoms , 6 carbon atoms , 7 carbon atoms , 8 carbon atoms , 9 carbon atoms , or 10 carbon atoms . the terms “ heteroatom ” or “ hetero ” as used herein , alone or in combination , refer to an atom other than carbon and hydrogen . heteroatoms are independently selected from among oxygen , nitrogen , sulfur , phosphorous , silicon , selenium and tin but are not limited to these atoms . in embodiments in which two or more heteroatoms are present , the two or more heteroatoms can be the same as each another , or some or all of the two or more heteroatoms can each be different from the others . the term “ alkyl ” as used herein , alone or in combination , refers to an optionally substituted straight - chain , or optionally substituted branched - chain saturated hydrocarbon monoradical having from one to about ten carbon atoms , more preferably one to six carbon atoms . examples include , but are not limited to methyl , ethyl , n - propyl , isopropyl , 2 - methyl - 1 - propyl , 2 - methyl - 2 - propyl , 2 - methyl - 1 - butyl , 3 - methyl - 1 - butyl , 2 - methyl - 3 - butyl , 2 , 2 - dimethyl - 1 - propyl , 2 - methyl - 1 - pentyl , 3 - methyl - 1 - pentyl , 4 - methyl - 1 - pentyl , 2 - methyl - 2 - pentyl , 3 - methyl - 2 - pentyl , 4 - methyl - 2 - pentyl , 2 , 2 - dimethyl - 1 - butyl , 3 , 3 - dimethyl - 1 - butyl , 2 - ethyl - 1 - butyl , n - butyl , isobutyl , sec - butyl , t - butyl , n - pentyl , isopentyl , neopentyl , tert - amyl and hexyl , and longer alkyl groups , such as heptyl , octyl and the like . whenever it appears herein , a numerical range such as “ c 1 - c 6 alkyl ” or “ c 1 — 6 alkyl ”, means that the alkyl group may consist of 1 carbon atom , 2 carbon atoms , 3 carbon atoms , 4 carbon atoms , 5 carbon atoms or 6 carbon atoms , although the present definition also covers the occurrence of the term “ alkyl ” where no numerical range is designated . the term “ alkylene ” as used herein , alone or in combination , refers to a diradical derived from the above - defined monoradical , alkyl . examples include , but are not limited to methylene (— ch 2 ), ethylene (— ch 2 ch 2 ), propylene (— ch 2 ch 2 ch 2 ), isopropylene (— ch ( ch 3 ) ch 2 ) and the like . the term “ alkenyl ” as used herein , alone or in combination , refers to an optionally substituted straight - chain , or optionally substituted branched - chain hydrocarbon monoradical having one or more carbon - carbon double - bonds and having from two to about ten carbon atoms , more preferably two to about six carbon atoms . the group may be in either the cis or trans conformation about the double bond ( s ), and should be understood to include both isomers . examples include , but are not limited to ethenyl ( ch ═ ch 2 ), 1 - propenyl ( ch 2 ch ═ ch 2 ), isopropenyl [ c ( ch 3 )═ ch 2 ], butenyl , 1 , 3 - butadienyl and the like . whenever it appears herein , a numerical range such as “ c 2 - c 6 alkenyl ” or “ c 2 — 6 alkenyl ”, means that the alkenyl group may consist of 2 carbon atoms , 3 carbon atoms , 4 carbon atoms , 5 carbon atoms or 6 carbon atoms , although the present definition also covers the occurrence of the term “ alkenyl ” where no numerical range is designated . the term “ alkynyl ” as used herein , alone or in combination , refers to an optionally substituted straight - chain or optionally substituted branched - chain hydrocarbon monoradical having one or more carbon - carbon triple - bonds and having from two to about ten carbon atoms , more preferably from two to about six carbon atoms . examples include , but are not limited to ethynyl , 2 - propynyl , 2 - butynyl , 1 , 3 - butadiynyl and the like . whenever it appears herein , a numerical range such as “ c 2 - c 6 alkynyl ” or “ c 2 — 6 alkynyl ”, means that the alkynyl group may consist of 2 carbon atoms , 3 carbon atoms , 4 carbon atoms , 5 carbon atoms or 6 carbon atoms , although the present definition also covers the occurrence of the term “ alkynyl ” where no numerical range is designated . the term “ aliphatic ” as used herein , alone or in combination , refers to an optionally substituted , straight - chain or branched - chain , non - cyclic , saturated , partially unsaturated , or fully unsaturated nonaromatic hydrocarbon . thus , the term collectively includes alkyl , alkenyl and alkynyl groups . the terms “ heteroalkyl ”, “ heteroalkenyl ” and “ heteroalkynyl ” as used herein , alone or in combination , refer to optionally substituted alkyl , alkenyl and alkynyl structures respectively , as described above , in which one or more of the skeletal chain carbon atoms ( and any associated hydrogen atoms , as appropriate ) are each independently replaced with a heteroatom ( i . e . an atom other than carbon , such as though not limited to oxygen , nitrogen , sulfur , silicon , phosphorous , tin or combinations thereof . the terms “ halo alkyl ”, “ halo alkenyl ” and “ haloalkynyl ” as used herein , alone or in combination , refer to optionally substituted alkyl , alkenyl and alkynyl groups respectively , as defined above , in which one or more hydrogen atoms is replaced by fluorine , chlorine , bromine or iodine atoms , or combinations thereof . in some embodiments two or more hydrogen atoms may be replaced with halogen atoms that are the same as each another ( e . g . difluoromethyl ); in other embodiments two or more hydrogen atoms may be replaced with halogen atoms that are not all the same as each other ( e . g . 1 - chloro - 1 - fluoro - 1 - iodoethyl ). non - limiting examples of haloalkyl groups are fluoromethyl and bromoethyl . a non - limiting example of a haloalkenyl group is bromoethenyl . a non - limiting example of a haloalkynyl group is chloroethynyl . the terms “ cycle ”, “ cyclic ”, “ ring ” and “ membered ring ” as used herein , alone or in combination , refer to any covalently closed structure , including alicyclic , heterocyclic , aromatic , heteroaromatic and polycyclic fused or non - fused ring systems as described herein . rings can be optionally substituted . rings can form part of a fused ring system . the term “ membered ” is meant to denote the number of skeletal atoms that constitute the ring . thus , by way of example only , cyclohexane , pyridine , pyran and pyrimidine are six - membered rings and cyclopentane , pyrrole , tetrahydrofuran and thiophene are five - membered rings . the term “ fused ” as used herein , alone or in combination , refers to cyclic structures in which two or more rings share one or more bonds . the term “ cycloalkyl ” as used herein , alone or in combination , refers to an optionally substituted , saturated , hydrocarbon monoradical ring , containing from three to about fifteen ring carbon atoms or from three to about ten ring carbon atoms , though may include additional , non - ring carbon atoms as substituents ( e . g . methylcyclopropyl ). a non - limiting example of “ cycloalkyl ” includes azinyl , azetidinyl , oxetanyl , thietanyl , homopiperidinyl , oxepanyl , thiepanyl , oxazepinyl , diazepinyl , thiazepinyl , 1 , 2 , 3 , 6 - tetrahydropyridinyl , 2 - pyrrolinyl , 3 - pyrrolinyl , indolinyl , 2h - pyranyl , 4h - pyranyl , dioxanyl , 1 , 3 - dioxolanyl , pyrazolinyl , dithianyl , dithiolanyl , dihydropyranyl , dihydrothienyl , dihydrofuranyl , pyrazolidinyl , imidazolinyl , imidazolidinyl , 3 - azabicyclo [ 3 . 1 . 0 ] hexyl , 3 - azabicyclo [ 4 . 1 . 0 ] heptyl , 3h - indolyl and quinolizinyl and the like . the terms also include all ring forms of the carbohydrates , including but not limited to the monosaccharides , the disaccharides and the oligosaccharides . the term “ aromatic ” as used herein , refers to a planar , cyclic or polycyclic , ring moiety having a delocalized at - electron system containing 4n + 2 n electrons , where n is an integer . aromatic rings can be formed by five , six , seven , eight , nine , or more than nine atoms . aromatics can be optionally substituted and can be monocyclic or fused - ring polycyclic . the term aromatic encompasses both all carbon containing rings ( e . g ., phenyl ) and those rings containing one or more heteroatoms ( e . g ., pyridine ). the term “ aryl ” as used herein , alone or in combination , refers to an optionally substituted aromatic hydrocarbon radical of six to about twenty ring carbon atoms , and includes fused and non - fused aryl rings . a fused aryl ring radical contains from two to four fused rings where the ring of attachment is an aryl ring , and the other individual rings may be alicyclic , heterocyclic , aromatic , heteroaromatic or any combination thereof . further , the term aryl includes fused and non - fused rings containing from six to about twelve ring carbon atoms , as well as those containing from six to about ten ring carbon atoms . a non - limiting example of a single ring aryl group includes phenyl ; a fused ring aryl group includes naphthyl , phenanthrenyl , anthracenyl , azulenyl ; and a non - fused bi - aryl group includes biphenyl . the term “ heteroaryl ” as used herein , alone or in combination , refers to optionally substituted aromatic mono - radicals containing from about five to about twenty skeletal ring atoms , where one or more of the ring atoms is a heteroatom independently selected from among oxygen , nitrogen , sulfur , phosphorous , silicon , selenium and tin but not limited to these atoms and with the proviso that the ring of said group does not contain two adjacent o or s atoms . in embodiments in which two or more heteroatoms are present in the ring , the two or more heteroatoms can be the same as each another , or some or all of the two or more heteroatoms can each be different from the others . the term heteroaryl includes optionally substituted fused and non - fused heteroaryl radicals having at least one heteroatom . the term heteroaryl also includes fused and non - fused heteroaryls having from five to about twelve skeletal ring atoms , as well as those having from five to about ten skeletal ring atoms . bonding to a heteroaryl group can be via a carbon atom or a heteroatom . thus , as a non - limiting example , an imidazole group may be attached to a parent molecule via any of its carbon atoms ( imidazol - 2 - yl , imidazol - 4 - yl or imidazol - 5 - yl ), or its nitrogen atoms ( imidazol - 1 - yl or imidazol - 3 - yl ). likewise , a heteroaryl group may be further substituted via any or all of its carbon atoms , and / or any or all of its heteroatoms . a fused heteroaryl radical may contain from two to four fused rings where the ring of attachment is a heteroaromatic ring and the other individual rings may be alicyclic , heterocyclic , aromatic , heteroaromatic or any combination thereof . a non - limiting example of a single ring heteroaryl group includes pyridyl ; fused ring heteroaryl groups include benzimidazolyl , quinolinyl , acridinyl ; and a non - fused bi - heteroaryl group includes bipyridinyl . further examples of heteroaryls include , without limitation , furanyl , thienyl , oxazolyl , acridinyl , phenazinyl , benzimidazolyl , benzofuranyl , benzoxazolyl , benzothiazolyl , benzothiadiazolyl , benzothiophenyl , benzoxadiazolyl , benzotriazolyl , imidazolyl , indolyl , isoxazolyl , isoquinolinyl , indolizinyl , isothiazolyl , isoindolyloxadiazolyl , indazolyl , pyridyl , pyridazyl , pyrimidyl , pyrazinyl , pyrrolyl , pyrazolyl , purinyl , phthalazinyl , pteridinyl , quinolinyl , quinazolinyl , quinoxalinyl , triazolyl , tetrazolyl , thiazolyl , triazinyl , thiadiazolyl and the like , and their oxides , such as for example pyridyl - n - oxide and the like . the term “ heterocyclyl ” as used herein , alone or in combination , refers collectively to heteroalicyclyl and heteroaryl groups . herein , whenever the number of carbon atoms in a heterocycle is indicated ( e . g ., c 1 - c 6 heterocycle ), at least one non - carbon atom ( the heteroatom ) must be present in the ring . designations such as “ c 1 - c 6 heterocycle ” refer only to the number of carbon atoms in the ring and do not refer to the total number of atoms in the ring . designations such as “ 4 - 6 membered heterocycle ” refer to the total number of atoms that are contained in the ring ( i . e ., a four , five , or six membered ring , in which at least one atom is a carbon atom , at least one atom is a heteroatom and the remaining two to four atoms are either carbon atoms or heteroatoms ). for heterocycles having two or more heteroatoms , those two or more heteroatoms can be the same or different from one another . heterocycles can be optionally substituted . non - aromatic heterocyclic groups include groups having only three atoms in the ring , while aromatic heterocyclic groups must have at least five atoms in the ring . bonding ( i . e . attachment to a parent molecule or further substitution ) to a heterocycle can be via a heteroatom or a carbon atom . the term “ alkoxy ” as used herein , alone or in combination , refers to an alkyl ether radical , o - alkyl , including the groups o - aliphatic and o - carbocycle , wherein the alkyl , aliphatic and carbocycle groups may be optionally substituted , and wherein the terms alkyl , aliphatic and carbocycle are as defined herein . non - limiting examples of alkoxy radicals include methoxy , ethoxy , n - propoxy , isopropoxy , n - butoxy , iso - butoxy , sec - butoxy , tertbutoxy and the like . the term “ mek inhibitor ” as used herein refers to a compound that exhibits an ic 50 , with respect to mek activity , of no more than about 100 μm or not more than about 50 μm , as measured in the mek1 kinase assay described generally herein . “ ic 50 ” is that concentration of inhibitor which reduces the activity of an enzyme ( e . g ., mek ) to half - maximal level . compounds described herein have been discovered to exhibit inhibition against mek . compounds of the present invention preferably exhibit an ic 50 with respect to mek of no more than about 10 μm , more preferably , no more than about 5 μm , even more preferably not more than about 1 μm , and most preferably , not more than about 200 nm , as measured in the mek1 kinase assay described herein . the term “ selective ,” “ selectivity ,” or “ selectivity ” as used herein refers to a compound of this invention having a lower ic 50 value for a mek enzyme as compared to any other enzymes ( e . g ., at least 2 , 5 , 10 or more - fold lower ). the term may also refer to a compound of this invention having a lower ic 50 value for a mek1 enzyme as compared to a mek2 enzyme ( e . g ., at least 2 , 5 , 10 or more - fold ) or alternatively having a lower ic 50 value for a mek2 enzyme as compared to a mek1 enzyme ( e . g ., at least 2 , 5 , 10 or more - fold lower ). the term “ subject ”, “ patient ” or “ individual ” as used herein in reference to individuals suffering from a disorder , a disorder , a condition , and the like , encompasses mammals and non - mammals . examples of mammals include , but are not limited to , any member of the mammalian class : humans , non - human primates such as chimpanzees , and other apes and monkey species ; farm animals such as cattle , horses , sheep , goats , swine ; domestic animals such as rabbits , dogs , and cats ; laboratory animals including rodents , such as rats , mice and guinea pigs , and the like . examples of non - mammals include , but are not limited to , birds , fish and the like . in one embodiment of the methods and compositions provided herein , the mammal is a human . the terms “ treat ,” “ treating ” or “ treatment ,” and other grammatical equivalents as used herein , include alleviating , abating or ameliorating a disease or condition symptoms , preventing additional symptoms , ameliorating or preventing the underlying metabolic causes of symptoms , inhibiting the disease or condition , e . g ., arresting the development of the disease or condition , relieving the disease or condition , causing regression of the disease or condition , relieving a condition caused by the disease or condition , or stopping the symptoms of the disease or condition , and are intended to include prophylaxis . the terms further include achieving a therapeutic benefit and / or a prophylactic benefit . by therapeutic benefit is meant eradication or amelioration of the underlying disorder being treated . also , a therapeutic benefit is achieved with the eradication or amelioration of one or more of the physiological symptoms associated with the underlying disorder such that an improvement is observed in the patient , notwithstanding that the patient may still be afflicted with the underlying disorder . for prophylactic benefit , the compositions may be administered to a patient at risk of developing a particular disease , or to a patient reporting one or more of the physiological symptoms of a disease , even though a diagnosis of this disease may not have been made . the terms “ effective amount ”, “ therapeutically effective amount ” or “ pharmaceutically effective amount ” as used herein , refer to a sufficient amount of at least one agent or compound being administered which will relieve to some extent one or more of the symptoms of the disease or condition being treated . the result can be reduction and / or alleviation of the signs , symptoms , or causes of a disease , or any other desired alteration of a biological system . for example , an “ effective amount ” for therapeutic uses is the amount of the composition comprising a compound as disclosed herein required to provide a clinically significant decrease in a disease . an appropriate “ effective ” amount in any individual case may be determined using techniques , such as a dose escalation study . the terms “ administer ,” “ administering ”, “ administration ,” and the like , as used herein , refer to the methods that may be used to enable delivery of compounds or compositions to the desired site of biological action . these methods include , but are not limited to oral routes , intraduodenal routes , parenteral injection ( including intravenous , subcutaneous , intraperitoneal , intramuscular , intravascular or infusion ), topical and rectal administration . those of skill in the art are familiar with administration techniques that can be employed with the compounds and methods described herein , e . g ., as discussed in goodman and gilman , the pharmacological basis of therapeutics , current ed . ; pergamon ; and remington &# 39 ; s , pharmaceutical sciences ( current edition ), mack publishing co ., easton , pa . in preferred embodiments , the compounds and compositions described herein are administered orally . the term “ acceptable ” as used herein , with respect to a formulation , composition or ingredient , means having no persistent detrimental effect on the general health of the subject being treated . the term “ pharmaceutically acceptable ” as used herein , refers to a material , such as a carrier or diluent , which does not abrogate the biological activity or properties of the compounds described herein , and is relatively nontoxic , i . e ., the material may be administered to an individual without causing undesirable biological effects or interacting in a deleterious manner with any of the components of the composition in which it is contained . the term “ pharmaceutical composition ,” as used herein , refers to a biologically active compound , optionally mixed with at least one pharmaceutically acceptable chemical component , such as , though not limited to carriers , stabilizers , diluents , dispersing agents , suspending agents , thickening agents , and / or excipients . the term “ carrier ” as used herein , refers to relatively nontoxic chemical compounds or agents that facilitate the incorporation of a compound into cells or tissues . the term “ agonist ,” as used herein , refers to a molecule such as a compound , a drug , an enzyme activator or a hormone modulator which enhances the activity of another molecule or the activity of a receptor site . the term “ antagonist ,” as used herein , refers to a molecule such as a compound , a drug , an enzyme inhibitor , or a hormone modulator , which diminishes , or prevents the action of another molecule or the activity of a receptor site . the term “ modulate ,” as used herein , means to interact with a target either directly or indirectly so as to alter the activity of the target , including , by way of example only , to enhance the activity of the target , to inhibit the activity of the target , to limit the activity of the target , or to extend the activity of the target . the term “ modulator ,” as used herein , refers to a molecule that interacts with a target either directly or indirectly . the interactions include , but are not limited to , the interactions of an agonist and an antagonist . the term “ pharmaceutically acceptable salt ” as used herein , refers to salts that retain the biological effectiveness of the free acids and bases of the specified compound and that are not biologically or otherwise undesirable . compounds described herein may possess acidic or basic groups and therefore may react with any of a number of inorganic or organic bases , and inorganic and organic acids , to form a pharmaceutically acceptable salt . these salts can be prepared in situ during the final isolation and purification of the compounds of the invention , or by separately reacting a purified compound in its free base form with a suitable organic or inorganic acid , and isolating the salt thus formed . examples of pharmaceutically acceptable salts include those salts prepared by reaction of the compounds described herein with a mineral or organic acid or an inorganic base , such salts including , acetate , acrylate , adipate , alginate , aspartate , benzoate , benzenesulfonate , bisulfate , bisulfite , bromide , butyrate , butyn - 1 , 4 - dioate , camphorate , camphorsulfonate , caprylate , chlorobenzoate , chloride , citrate , cyclopentanepropionate , decanoate , digluconate , dihydrogenphosphate , dinitrobenzoate , dodecylsulfate , ethanesulfonate , formate , fumarate , glucoheptanoate , glycerophosphate , glycolate , hemisulfate , heptanoate , hexanoate , hexyne - 1 , 6 - dioate , hydroxybenzoate , hydroxybutyrate , hydrochloride , hydrobromide , hydro iodide , 2 - hydroxyethanesulfonate , iodide , isobutyrate , lactate , maleate , malonate , methanesulfonate , mandelate . metaphosphate , methoxybenzoate , methylbenzoate , monohydrogenphosphate , 1 - napthalenesulfonate , 2 - napthalenesulfonate , nicotinate , nitrate , palmoate , pectinate , persulfate , 3 - phenylpropionate , phosphate , picrate , pivalate , propionate , pyrosulfate , pyrophosphate , propiolate , phthalate , phenylacetate , phenylbutyrate , propanesulfonate , salicylate , succinate , sulfate , sulfite , suberate , sebacate , sulfonate , tartrate , thiocyanate , tosylate undeconate and xylenesulfonate . other acids , such as oxalic , while not in themselves pharmaceutically acceptable , may be employed in the preparation of salts useful as intermediates in obtaining the compounds of the invention and their pharmaceutically acceptable acid addition salts ( see examples at berge et al ., j . plum . sci . 1977 , 66 , 1 - 19 .). further , those compounds described herein which may comprise a free acid group may react with a suitable base , such as the hydroxide , carbonate or bicarbonate of a pharmaceutically acceptable metal cation , with ammonia , or with a pharmaceutically acceptable organic primary , secondary or tertiary amine . representative alkali or alkaline earth salts include the lithium , sodium , potassium , calcium , magnesium , and aluminum salts and the like . illustrative examples of bases include sodium hydroxide , potassium hydroxide , choline hydroxide , sodium carbonate , iv ′ ( c 1 — 4 alkyl ) 4 , and the like . representative organic amines useful for the formation of base addition salts include ethylamine , diethylamine , ethylenediamine , ethanolamine , diethanolamine , piperazine and the like . it should be understood that the compounds described herein also include the quaternization of any basic nitrogen - containing groups they may contain . water or oil - soluble or dispersible products may be obtained by such quaternization . see , for example , berge et al ., supra . the term “ solvate ” as used herein refers to a combination of a compound of this invention with a solvent molecule formed by solvation . in some situations , the solvate refers to a hydrate , i . e ., the solvent molecule is a water molecule , the combination of a compound of this invention and water forms a hydrate . the term “ polymorph ” or “ polymorphism ” as used herein refers to a compound of this invention present in different crystal lattice forms . the term “ ester ” as used herein refers to a derivative of a compound of this invention derived from an oxoacid group and a hydroxyl group , either one of which can be present at the compound of this invention . the term “ tautomer ” as used herein refers to an isomer readily interconverted from a compound of this invention by e . g ., migration of a hydrogen atom or proton . the term “ pharmaceutically acceptable derivative or prodrug ” as used herein , refers to any pharmaceutically acceptable salt , ester , salt of an ester or other derivative of a compound of this invention , which , upon administration to a recipient , is capable of providing , either directly or indirectly , a compound of this invention or a pharmaceutically active metabolite or residue thereof . particularly favored derivatives or prodrugs are those that increase the bioavailability of the compounds of this invention when such compounds are administered to a patient ( e . g ., by allowing orally administered compound to be more readily absorbed into blood ) or which enhance delivery of the parent compound to a biological compartment ( e . g ., the brain or lymphatic system ). pharmaceutically acceptable prodrugs of the compounds described herein include , but are not limited to , esters , carbonates , thiocarbonates , n - acyl derivatives , n - acyloxyalkyl derivatives , quaternary derivatives of tertiary amines , n - mannich bases , schiff bases , amino acid conjugates , phosphate esters , metal salts and sulfonate esters . various forms of prodrugs are well known in the art . see for example design of prodrugs , bundgaard , a . ed ., elseview , 1985 and method in enzymology , widder , k . et al ., ed . ; academic , 1985 , vol . 42 , p . 309 - 396 ; bundgaard , h . “ design and application of prodrugs ” in a textbook of drug design and development , krosgaard - larsen and h . bundgaard , ed ., 1991 , chapter 5 , p . 113 - 191 ; and bundgaard , h ., advanced drug delivery review , 1992 , 8 , 1 - 38 , each of which is incorporated herein by reference . the prodrugs described herein include , but are not limited to , the following groups and combinations of these groups ; amine derived prodrugs : hydroxy prodrugs include , but are not limited to acyloxyalkyl esters , alkoxycarbonyloxyalkyl esters , alkyl esters , aryl esters and disulfide containing esters . the terms “ enhance ” or “ enhancing ,” as used herein , means to increase or prolong either in potency or duration of a desired effect . thus , in regard to enhancing the effect of therapeutic agents , the term “ enhancing ” refers to the ability to increase or prolong , either in potency or duration , the effect of other therapeutic agents on a system . an “ enhancing - effective amount ,” as used herein , refers to an amount adequate to enhance the effect of another therapeutic agent in a desired system . the terms “ pharmaceutical combination ”, “ administering an additional therapy ”, “ administering an additional therapeutic agent ” and the like , as used herein , refer to a pharmaceutical therapy resulting from mixing or combining more than one active ingredient and includes both fixed and non - fixed combinations of the active ingredients . the term “ fixed combination ” means that at least one of the compounds described herein , and at least one co - agent , are both administered to a patient simultaneously in the form of a single entity or dosage . the term “ non - fixed combination ” means that at least one of the compounds described herein , and at least one co - agent , are administered to a patient as separate entities either simultaneously , concurrently or sequentially with variable intervening time limits , wherein such administration provides effective levels of the two or more compounds in the body of the patient . these also apply to cocktail therapies , e . g . the administration of three or more active ingredients . the terms “ co - administration ”, “ administered in combination with ” and their grammatical equivalents or the like , as used herein , are meant to encompass administration of the selected therapeutic agents to a single patient , and are intended to include treatment regimens in which the agents are administered by the same or different route of administration or at the same or different times . in some embodiments the compounds described herein will be co - administered with other agents . these terms encompass administration of two or more agents to an animal so that both agents and / or their metabolites are present in the animal at the same time . they include simultaneous administration in separate compositions , administration at different times in separate compositions , and / or administration in a composition in which both agents are present . thus , in some embodiments , the compounds of the invention and the other agent ( s ) are administered in a single composition . the term “ metabolite ,” as used herein , refers to a derivative of a compound which is formed when the compound is metabolized . the term “ active metabolite ,” as used herein , refers to a biologically active derivative of a compound that is formed when the compound is metabolized . the term “ metabolized ,” as used herein , refers to the sum of the processes ( including , but not limited to , hydrolysis reactions and reactions catalyzed by enzymes ) by which a particular substance is changed by an organism . thus , enzymes may produce specific structural alterations to a compound . for example , cytochrome p450 catalyzes a variety of oxidative and reductive reactions while uridine diphosphate glucuronyltransferases catalyze the transfer of an activated glucuronic - acid molecule to aromatic alcohols , aliphatic alcohols , carboxylic acids , amines and free sulfhydryl groups . further information on metabolism may be obtained from the pharmacological basis of therapeutics , 9th edition , mcgraw - hill ( 1996 ). scheme 1 above illustrates the preparation of pyridone hydroxamate derivatives of ( 7 ). alkylation of diethylacetone 1 , 3dicarboxylate afford intermediate ( 2 ). condensation with iminoaniline derivatives ( 3 ) affords the pyridone ( 4 ). the iminoaniline derivatives ( 3 ) can be prepared in two steps from anilines by coupling to form the urea followed by reaction with carbon tetrabromide and triphenylphosphine to afford intermediates ( 3 ) [ scheme 2 ]. o - alkylation of ( 4 ) affords compound ( 5 ) which upon treatment with an amine affords the desired compounds ( 7 ). scheme 3 illustrates the preparation of the dihydrofuro pyridinone derivatives represented by ( 13 ). alkylation of dimethylacetone 1 , 3dicarboxylate ( 8 ) with 2 - halo carboxaldehydes ( 9 ) affords intermediate ( 10 ). subsequent condensation with iminoaniline derivatives ( 3 ) generates the bicyclic dihydro pyridinone ( 11 ). hydrolysis of the ester yields ( 12 ) which upon coupling with an amine affords the requisite analogs ( 13 ). to n , n ′- carbonyldiimidazole ( 51 . 3 g , 316 mmol ) in dry dmf ( 52 ml ) was added tea ( 3 . 55 ml , 25 . 5 mmol ) after addition of a solution of 2 - fluoro - 4 - iodoaniline ( 50 . 0 g , 211 mmol ) in dry dmf ( 52 ml ) at 0 ° c . under a n 2 atmosphere . the reaction mixture was stirred at room temperature for 16 h followed by the addition of a solution of 40 % methylamine ( 24 . 5 g , 316 mmol ) at 0 ° c . after stirring for 1 h at room temperature , the reaction mixture was added to water / toluene ( v / v = 2 / 1 ) while stirring . the resulting solid was collected by filtration , rinsed with water and dried in vacuo to give 1 -( 2 - fluoro - 4 - iodophenyl )- 3 - methylurea ( 57 . 6 g , 93 %) as a white solid , which was used for the next reaction without further purification . 1 h nmr ( dmso - d 6 , varian 400 mhz ) δ 2 . 64 ( 3h , d , j = 2 . 4 hz ), 6 . 45 - 6 . 49 ( 1h , m ), 7 . 40 - 7 . 42 ( 1h , m ), 7 . 55 ( 1h , dd , j = 5 . 4 , 2 . 0 hz ), 7 . 95 ( 1h , t , j = 8 . 8 hz ), 8 . 36 ( 1h , brs ). to a solution of 1 -( 2 - fluoro - 4 - iodophenyl )- 3 - methylurea ( 15 . 0 g , 51 . 0 mmol ) and tea ( 28 . 3 ml , 204 mmol ) in dcm ( 250 ml ) was added cbr 4 ( 33 . 8 g , 102 mmol ) and pph 3 ( 26 . 8 g , 102 mmol ) at room temperature . the reaction mixture was stirred at room temperature for 4 h . the solvent was removed by reduce pressure and the residue purified by flash column chromatography on sio 2 ( hex : etoac = 20 : 1 to 5 : 1 ) to give 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( 9 . 00 g , 64 %) as a red oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 3 . 17 ( 3h , s ), 6 . 78 ( 1h , t , j = 8 . 4 hz ), 7 . 33 - 7 . 36 ( 1h , m ), 7 . 38 - 7 . 41 ( 1h , m ). to a solution of 2 -( vinyloxy ) ethanol ( 20 . 4 ml , 227 mmol ), triphenylphosphine ( 59 . 5 g , 227 mmol ), and n - hydroxyphthalimide ( 37 . 0 g , 227 mmol ) in thf ( 450 ml ) was added dead ( 35 . 9 ml , 227 mmol ) at 0 ° c . under a n 2 atmosphere . after stirring for 16 h at room temperature , the reaction mixture was concentrated in vacuo . the residue was filtered , washed with chloroform and the filtrate was concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 2 : 1 ) to give 2 -( 2 -( vinyloxy ) ethoxy ) isoindoline - 1 , 3 - dione ( 32 . 5 g , 61 . 4 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 4 . 04 - 4 . 08 ( 3h , m ), 4 . 19 ( 1h , dd , j = 14 . 4 , 2 . 2 hz ), 4 . 45 - 4 . 48 ( 2h , m ), 6 . 47 ( 1h , dd , j = 14 . 0 , 6 . 8 hz ), 7 . 53 - 7 . 78 ( 2h , m ), 7 . 80 - 7 . 87 ( 2 m , m ). to a solution of 2 -( 2 -( vinyloxy ) ethoxy ) isoindoline - 1 , 3 - dione ( 32 . 0 g , 137 mmol ) in dcm ( 96 . 0 ml ) was added dropwise an aqueous solution of methylhydrazine ( 15 . 8 ml , 137 mmol ) at room temperature . after being stirred for 1 h at room temperature , the resultant suspension was diluted with diethyl ether and filtered . the filtrate was concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 3 : 2 to 1 : 1 ) to give o -( 2 -( vinyloxy ) ethyl )- hydroxylamine ( 10 . 7 g , 76 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 3 . 85 - 3 . 93 ( 4h , m ), 4 . 03 ( 1h , dd , j = 6 . 8 , 2 . 0 hz ), 4 . 22 ( 1h , dd , j = 14 . 2 , 2 . 0 hz ), 5 . 51 ( 2h , brs ), 6 . 50 ( 1h , dd , j = 14 . 2 , 6 . 8 hz ). to a solution of dimethyl 3 - oxopentanedioate ( 55 . 0 g , 316 mmol ) in pyridine ( 113 ml ) was added 2 - chloropropanal ( 91 . 0 g , 524 mmol ) dropwise at 0 ° c . the reaction mixture was stirred at 50 ° c . for 24 h . the residue was diluted with etoac and washed with water and brine , dried over mgso 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 to give methyl 2 -( 2 - methoxy - 2 - oxoethyl ) furan - 3 - carboxylate ( 45 . 0 g , 72 %) as a yellow oil . 1 h - nmr ( cdcl 3 , varian , 400 mhz ) δ 3 . 73 ( 3h , s ), 3 . 83 ( 3h , s ), 4 . 09 ( 2h , s ), 6 . 70 ( 1h , d , j = 2 . 0 hz ), 7 . 34 ( 1h , d , j = 2 . 0 hz ). to a solution of methyl 2 -( 2 - methoxy - 2 - oxoethyl ) furan - 3 - carboxylate ( 9 . 94 g , 50 . 1 mmol ) in dry thf ( 200 ml ) was added nah ( 55 wt % dispersion in mineral oil , 2 . 29 g , 52 . 6 mmol ) at 0 ° c . the reaction mixture was stirred at room temperature for 30 min , and then 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 13 . 8 g , 50 . 1 mmol ) was added slowly with a dropping funnel . the reaction mixture was stirred at room temperature for 3 h . the reaction mixture was quenched with water and extracted with etoac and brine ( 50 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residual solid was suspended in water , collected by filtration , rinsed with water and dried in vacuo to give methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 11 . 8 g , 53 %) as a yellow solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 3 . 35 ( 3h , s ), 3 . 96 ( 3h , s ), 6 . 45 ( 1h , t , j = 8 . 4 hz ), 6 . 96 ( 2h , d , j = 1 . 2 hz ), 7 . 36 - 7 . 38 ( 1h , d , j = 4 . 2 hz ), 7 . 48 - 7 . 51 ( 1h , m ), 7 . 53 ( 1h , d , j = 1 . 0 hz ), 9 . 85 ( 1h , s ). a solution of the 3 - chlorobut - 1 - ene ( 1 . 11 ml , 11 . 0 mmol ) in dcm ( 12 . 0 ml ) was cooled to − 60 ° c . a mixture of o 3 / o 2 was then bubbled through the solution for 20 min . the solution was purged with nitrogen , warmed to room temperature , treated with triphenylphosphine ( 3 . 48 g , 13 . 2 mmol ) and stirred vigorously for 30 min . the mixture was used for the next reaction without further purification . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 61 ( 3h , d , j = 7 . 2 hz ), 4 . 28 ( 1h , qd , j = 1 . 0 , 0 . 8 , 0 . 8 , 0 . 8 hz ), 9 . 53 ( 1h , m ). to a cooled ( 0 ° c .) and stirred solution of prop - 2 - yn - 1 - ol ( 5 . 19 ml , 89 . 0 mmol ) and pyridine ( 14 . 4 ml , 178 mmol ) in diethyl ether ( 90 . 0 ml ) was added methyl chloroformate ( 6 . 91 ml , 89 . 0 mmol ) dropwise over 10 min . the mixture was stirred at room temperature for 15 hours and then dilute hydrochloric acid was added . after extraction with ether , the organic layer was washed with brine and dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 3 : 1 ) to give methyl prop - 2 - ynyl carbonate ( 5 . 27 g , 52 %) as a colorless liquid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 53 ( 1h , t , j = 2 . 2 hz ), 3 . 82 ( 3h , s ), 4 . 74 ( 2h , d , j = 2 . 8 hz ). to n , n ′- carbonyldiimidazole ( 480 mg , 2 . 96 mmol ) in dry dmf ( 0 . 7 ml ) was added tea ( 0 . 33 ml , 2 . 38 mmol ) after addition of a solution of 2 - chloro - 4 - iodoaniline ( 500 mg , 1 . 97 mmol ) in dry dmf ( 0 . 7 ml ) at 0 ° c . under a n 2 atmosphere . the reaction mixture was stirred at room temperature for 16 hour followed by the addition of a solution of 40 % methylamine ( 230 mg , 2 . 96 mmol ) at 0 ° c . after stiffing for 1 hour at room temperature , the reaction mixture was added to water / toluene ( v / v = 2 / 1 ) while stiffing . the resulting solid was collected by filtration , rinsed with water and dried in vacuo to give 1 -( 2 - chloro - 4 - iodophenyl )- 3 - methylurea ( 530 mg , 87 %) as a yellow solid , which was used for the next reaction without further purification . 1 h nmr ( dmso - d 6 , varian 400 mhz ) δ 2 . 64 ( 3h , d , j = 4 . 8 hz ), 6 . 90 - 6 . 93 ( 1h , m ), 7 . 54 - 7 . 57 ( 1h , m ), 7 . 73 ( 1h , d , j = 1 . 6 hz ), 7 . 97 ( 1h , d , j = 8 . 8 hz ), 8 . 07 ( 1h , s ). to a solution of 1 -( 2 - chloro - 4 - iodophenyl )- 3 - methylurea ( 530 mg , 51 . 0 mmol ) and tea ( 0 . 95 ml , 6 . 83 mmol ) in dcm ( 9 ml ) was added cbr 4 ( 1 . 13 g , 3 . 41 mmol ) and pph 3 ( 0 . 89 g , 3 . 41 mmol ) at room temperature . the reaction mixture was stirred at room temperature for 4 hours . the solvent was removed by reduce pressure and the residue purified by flash column chromatography on sio 2 ( hex : etoac = 20 : 1 to 5 : 1 ) to give 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( 340 mg , 68 %) as a red oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 3 . 15 ( 3h , s ), 6 . 80 ( 1h , d , j = 8 . 4 hz ), 7 . 41 - 7 . 43 ( 1h , dd , j = 8 . 2 , 2 . 2 hz ), 7 . 63 - 7 . 68 ( 1h , m ). to a solution of dimethyl 3 - oxopentanedioate ( 55 . 0 g , 316 mmol ) in pyridine ( 113 ml ) was added 2 - chloropropanal ( 91 . 0 g , 524 mmol ) dropwise at 0 ° c . the reaction mixture was stirred at 50 ° c . for 24 hours . the residue was diluted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 to give methyl 2 -( 2 - methoxy - 2 - oxoethyl ) furan - 3 - carboxylate ( 45 . 0 g , 72 %) as a yellow oil . 1 h - nmr ( cdcl 3 , varian , 400 mhz ) δ 3 . 73 ( 3h , s ), 3 . 83 ( 3h , s ), 4 . 09 ( 2h , s ), 6 . 70 ( 1h , d , j = 2 . 0 hz ), 7 . 34 ( 1h , d , j = 2 . 0 hz ). to a solution of methyl 2 -( 2 - methoxy - 2 - oxoethyl ) furan - 3 - carboxylate ( 305 mg , 1 . 53 mmol ) in dry thf ( 8 . 0 ml ) was added nah ( 55 wt % dispersion in mineral oil , 67 . 1 mg , 1 . 53 mmol ) at 0 ° c . the reaction mixture was stirred at room temperature for 30 min , and then 2 - chloro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 6 , 450 mg , 1 . 53 mmol ) was added slowly . the reaction mixture was stirred at room temperature for 2 hours . the reaction mixture was quenched with water and extracted with etoac and brine ( 50 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residual solid was suspended in water , collected by filtration , rinsed with water and dried in vacuo to give methyl 6 -( 2 - chloro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 320 mg , 45 %) as a yellow solid . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ): δ 3 . 24 ( 3h , s ), 3 . 76 ( 3h , s ), 6 . 60 ( 1h , d , j = 8 . 4 hz ), 7 . 01 - 7 . 02 ( 1h , m ), 7 . 50 - 7 . 52 ( 1h , dd , j = 8 . 4 , 2 . 0 hz ), 7 . 87 ( 1h , m ), 7 . 94 ( 1h , m ), 9 . 25 ( 1h , s ). to 2 - hydroxyisoindoline - 1 , 3 - dione ( 300 mg , 1 . 84 mmol ) and ( bromomethyl ) cyclopropane ( 0 . 180 ml , 1 . 84 mmol ) in dmf ( 1 . 00 ml ) was added et 3 n ( 0 . 306 ml , 2 . 21 mmol ) dropwise at room temperature . the mixture was stirred at 65 ° c . for 15 hours . and then the reaction mixture was cooled and precipitate was filtered and washed with water . the solid obtained was dried in vacuo to give 2 -( cyclopropylmethoxy ) isoindoline - 1 , 3 - dione ( 193 mg , 48 %) as a light brown solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 0 . 38 ( 2h , m ), 0 . 63 ( 2h , m ), 1 . 29 ( 1h , m ), 4 . 05 ( 2h , d , j = 7 . 2 hz ), 7 . 75 ( 2h , m ), 7 . 85 ( 2h , m ). to a solution of 2 -( cyclopropylmethoxy ) isoindoline - 1 , 3 - dione ( 1 . 07 g , 4 . 93 mmol ) in dcm ( 6 . 00 ml ) at room temperature was added n - methylhydrazine sulfate ( 0 . 710 g , 4 . 93 mmol ). and the mixture was stirred at room temperature for 1 hour . the reaction mixture was diluted with diethyl ether and filtered . the filtrate was concentrated in vacuo . the residue was suspended in etoac and filtered again . 4m hcl in 1 , 4 - dioxane ( 1 . 35 ml , 5 . 42 mmol ) was added to the filtrate and the resulting precipitate was collected by filtration and dried under vacuum to give o -( cyclopropylmethyl ) hydroxylamine hydrochloride ( 55 . 9 mg , 9 . 2 %) as a yellow solid . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ): δ 0 . 29 ( 2h , m ), 0 . 57 ( 2h , m ), 1 . 06 ( 1h , m ), 3 . 79 ( 2h , d , j = 7 . 2 hz ), 10 . 69 ( 2h , br ). to a solution of tert - butyl hydroxycarbamate ( 300 mg , 2 . 25 mmol ) in etoh ( 17 . 0 ml ) was added koh ( 152 mg , 2 . 70 mmol ) and stirred at room temperature till the koh dissolved into solution . to this was added 2 - bromoisobutyricacid ethyl ester ( 0 . 397 ml , 2 . 70 mmol ) and refluxed 15 hours . the white solid was discarded and the filterate was concentrated . the residue was partitioned between water and etoac . the combined etoac layer was dried with na 2 so 4 , filtered and filtrate was concentrated to give ethyl 2 -( tert - butoxycarbonylaminooxy )- 2 - methylpropanoate ( 410 mg , 74 %) as a colorless oil . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 29 ( 3h , t , j = 1 . 3 hz ), 1 . 47 ( 9h , s ), 1 . 49 ( 6h , s ), 4 . 20 ( 2h , q , j = 7 . 1 hz ), 7 . 37 ( 1h , s ). to a solution of ethyl 2 -( tert - butoxycarbonylaminooxy )- 2 - methylpropanoate ( 410 mg , 1 . 66 mmol ) in anhydrous thf ( 4 . 20 ml ) at 0 ° c . under n 2 was added lialh 4 ( 83 . 0 mg , 2 . 19 mmol ) slowly and stirred for 1 hour . to this was added h 2 o ( 1 . 00 ml ), after aq . naoh ( 1 . 00 ml ), h 2 o ( 3 . 00 ml ) and the mixture was stirred for 30 min at room temperature . then filtered washed with etoac , the filtrate was extracted with etoac for 3 times , the combined organic extracts were dried , filtered and concentrated in vacuo to give tert - butyl 1 - hydroxy - 2 - methylpropan - 2 - yloxycarbamate ( 310 mg , 91 %) as a white solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 14 ( 6h , s ), 1 . 42 ( 9h , s ), 3 . 33 ( 2h , d , j = 7 . 2 hz ), 4 . 41 ( 1h , br ). * nh peak was not observed . to a solution of tert - butyl 1 - hydroxy - 2 - methylpropan - 2 - yloxycarbamate ( 310 mg , 1 . 51 mmol ) in dcm ( 1 . 60 ml ) was added 4 m hcl in 1 , 4 - dioxane ( 2 . 79 ml , 11 . 2 mmol ) at room temperature and stirred for 1 h . the reaction was concentrated under reduced pressure and the residue was filtered with diethyl ether , and solid was concentrated in vacuum to give 2 -( aminooxy )- 2 - methylpropan - 1 - ol hydrochloride ( 236 mg , 110 %) as a colorless oil . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 24 ( 6h , s ), 3 . 48 ( 2h , s ), 10 . 66 ( 3h , s ). * oh peak was not observed . to a solution of ( r )-( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methanol ( 1 . 00 g , 7 . 57 mmol ), triphenylphosphine ( 1 . 99 g , 7 . 57 mmol ), and n - hydroxyphthalimide ( 1 . 23 g , 7 . 57 mmol ) in thf ( 5 . 2 ml ) was added dead ( 2 . 64 ml , 15 . 1 mmol ) at 0 ° c . under a n 2 atmosphere . after stiffing for 16 h at room temperature , the reaction mixture was concentrated in vacuo . the residue was filtered , washed with chloroform and the filtrate was concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 9 : 1 ˜ 1 : 1 ) to give ( r )- 2 -(( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methoxy ) isoindoline - 1 , 3 - dione ( 1 . 44 g , 68 . 6 %) as a white solid . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 1 . 35 ( 3h , s ), 1 . 41 ( 3h , s ), 3 . 98 ( 1h , dd , j = 8 . 8 , 5 . 2 hz ), 4 . 12 - 4 . 20 ( 2h , m ), 4 . 32 ( 1h , dd , j = 10 . 2 , 5 . 8 hz ), 4 . 47 - 4 . 53 ( 1h , m ), 7 . 74 - 7 . 79 ( 2h , m ), 7 . 83 - 7 . 86 ( 2h , m ). to a solution of ( r )- 2 -(( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methoxy ) isoindoline - 1 , 3 - dione ( 1 . 44 g , 5 . 19 mmol ) in dcm ( 10 . 4 ml ) was added hydrazine hydrate ( 0 . 26 g , 5 . 19 mmol ) at room temperature . the reaction mixture was stirred at room temperature for 30 min . the solvent was removed by reduce pressure . the resultant suspension was diluted with diethyl ether and filtered to remove insoluble solid . the filtrate was concentrated in vacuo to give ( r )— o -(( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methyl ) hydroxylamine ( 700 mg , 92 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 1 . 37 ( 3h , s ), 1 . 44 ( 3h , s ), 3 . 68 - 3 . 79 ( 3h , m ), 4 . 05 - 4 . 09 ( 1h , m ), 4 . 32 - 4 . 38 ( 1h , m ), 5 . 56 ( 2h , brs ). to a solution of methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( intermediate 3 , 7 . 00 g , 15 . 8 mmol ) in meoh ( 500 ml ) was added k 2 co 3 ( 8 . 75 g , 63 . 3 mmol ) at room temperature followed by the addition of water ( 500 ml ) via dropping funnel . the reaction mixture was stirred at 70 ° c . for 3 h . the reaction mixture was quenched with water and then acidified with 10 % aq . hcl until ph 1 ˜ 2 . the resulting solid was collected by filtration , rinsed with water and dried in vacuo to give 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( 5 . 48 g , 81 %) as a yellow solid , which was used for the next reaction without further purification . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ) δ 3 . 25 ( 3h , s ), 6 . 69 ( 1h , t , j = 8 . 8 hz ), 6 . 98 ( 1h , d , j = 1 . 2 hz ), 7 . 41 ( 1h , d , j = 4 . 2 hz ), 7 . 69 ( 1h , dd , j = 10 . 6 , 1 . 0 hz ), 7 . 90 ( 1h , d , j = 1 . 0 hz ), 9 . 66 ( 1h , s ), 13 . 2 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( 4 . 00 g , 9 . 34 mmol ) in dmf ( 110 ml ) was added o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 1 . 15 g , 11 . 2 mmol ) at room temperature and then was cooled to 0 ° c . to the reaction mixture was added edc ( 2 . 14 g , 11 . 2 mmol ), hobt ( 1 . 71 g , 11 . 2 mmol ), and tea ( 1 . 56 ml , 11 . 2 mmol ). the mixture was stirred at room temperature for 3 h . the reaction was extracted with etoac , washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo to give 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 2 . 43 g , 50 %) as a white solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 3 . 32 ( 3h , s ), 3 . 99 - 4 . 01 ( 2h , m ), 4 . 07 - 4 . 27 ( 2h , m ), 4 . 29 - 4 . 31 ( 2h , m ), 6 . 48 - 6 . 55 ( 2h , m ), 7 . 01 ( 1h , d , j = 1 . 2 hz ), 7 . 37 ( 1h , d , j = 4 . 2 hz ), 7 . 47 ( 1h , dd , j = 5 . 0 , 1 . 0 hz ), 7 . 50 ( 1h , d , j = 1 . 2 hz ), 10 . 0 ( 1h , s ), 10 . 9 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 1 . 57 g , 3 . 06 mmol ) in meoh ( 15 ml ) was added 2n aq . hcl at room temperature . the mixture was stirred at room temperature for 30 min . the residue was diluted with dcm and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo to give 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 1 . 35 g , 91 %) as a white solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ) δ 3 . 30 ( 3h , s ), 3 . 75 - 3 . 78 ( 2h , m ), 4 . 05 ( 1h , t , j = 6 . 4 hz ), 4 . 09 - 4 . 11 ( 2h , m ), 6 . 55 ( 1h , t , j = 8 . 4 hz ), 7 . 01 ( 1h , d , j = 0 . 8 hz ), 7 . 38 - 7 . 40 ( 1h , m ), 7 . 49 ( 1h , dd , j = 4 . 8 , 1 . 0 hz ), 7 . 52 ( 1h , d , j = 1 . 0 hz ), 9 . 86 ( 1h , s ), 10 . 8 ( 1h , s ). m / z = 487 . 8 [ m + h ] + to a solution of diethyl 3 - oxopentanedioate ( 20 . 0 g , 99 . 0 mmol ) in dry thf ( 198 ml ) was added nah ( 55 %, 4 . 53 g , 104 mmol ) at 0 ° c . the mixture was stirred for 30 minutes at 0 ° c . after dropwise addition of mei ( 14 . 0 g , 99 . 0 mmol ) at 0 ° c ., the reaction mixture was stirred at room temperature for 2 days , and then quenched saturated aq . nh 4 cl ( 200 ml ). the mixture was extracted with etoac ( 3 × 50 ml ). the combined organic layers were washed water ( 300 ml ) and brine ( 300 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 9 : 1 ) to afford diethyl 2 - methyl - 3 - oxopentanedioate ( 11 . 1 g , 52 %) as a colorless oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 1 . 28 ( 6h , t , j = 7 . 2 hz ), 1 . 38 ( 3h , d , j = 7 . 2 hz ), 3 . 57 ( 1h , d , j = 16 . 0 hz ), 3 . 66 ( 1h , d , j = 16 . 0 hz ), 3 . 72 ( 1h , q , j = 7 . 2 hz ), 4 . 16 - 4 . 24 ( 4h , m ). to a solution of diethyl 2 - methyl - 3 - oxopentanedioate ( 9 . 56 g , 44 . 2 mmol ) in dry thf ( 88 ml ) was added nah ( 55 %, 2 . 02 g , 46 . 4 mmol ) at 0 ° c . the mixture was stirred for 30 minutes at 0 ° c . after dropwise addition of 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 12 . 2 g , 44 . 2 mmol ) at 0 ° c ., the reaction mixture was stirred at room temperature overnight , and then quenched with saturated 1n aq . hcl ( 60 ml ). the mixture was extracted with etoac ( 3 × 30 ml ). the combined organic layers were washed water ( 100 ml ) and brine ( 100 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 7 : 3 to 1 : 1 ) to afford ethyl 2 -( 2 - fluoro - 4 - iodophenylamino )- 4 - hydroxy - 1 , 5 - dimethyl - 6 - oxo - 1 , 6 - dihydropyridine - 3 - carboxylate ( 2 . 98 g , 15 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 1 . 36 ( 3h , t , j = 7 . 2 hz ), 2 . 05 ( 3h , s ), 3 . 35 ( 3h , s ), 4 . 40 ( 2h , q , j = 7 . 2 hz ), 6 . 33 ( 1h , t , j = 8 . 4 hz ), 7 . 36 ( 1h , d , j = 8 . 4 hz ), 7 . 50 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 8 . 28 ( 1h , brs ), 11 . 20 ( 1 m , brs ). a mixture of ethyl 2 -( 2 - fluoro - 4 - iodophenylamino )- 4 - hydroxy - 1 , 5 - dimethyl - 6 - oxo - 1 , 6 - dihydropyridine - 3 - carboxylate ( 2 . 78 g , 6 . 23 mmol ), dimethyl sulfate ( 0 . 60 ml , 6 . 23 mmol ) and k 2 co 3 ( 1 . 72 , 12 . 5 mmol ) in acetone ( 31 ml ) was refluxed for 1 hour , cooled to room temperature , and then partitioned between etoac and water . the separated aqueous layer was extracted with etoac . the combined organic layers were washed with brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 3 : 2 ) to afford ethyl 2 -( 2 - fluoro - 4 - iodophenylamino )- 4 - methoxy - 1 , 5 - dimethyl - 6 - oxo - 1 , 6 - dihydropyridine - 3 - carboxylate ( 1 . 04 g , 36 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 1 . 35 ( 3h , t , j = 7 . 2 hz ), 2 . 09 ( 3h , s ), 3 . 32 ( 3h , s ), 3 . 78 ( 3h , s ), 4 . 31 ( 2h , q , j = 7 . 2 hz ), 6 . 35 ( 1h , t , j = 8 . 4 hz ), 7 . 34 ( 1h , d , j = 8 . 4 hz ), 7 . 46 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 8 . 88 ( 1h , brs ). to a mixture of ethyl 2 -( 2 - fluoro - 4 - iodophenylamino )- 4 - methoxy - 1 , 5 - dimethyl - 6 - oxo - 1 , 6 - dihydropyridine - 3 - carboxylate ( 1 . 29 g , 2 . 80 mmol ) and o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 433 mg , 4 . 20 mmol ) in dry thf ( 14 ml ) was added lihmds ( 16 . 8 ml , 16 . 8 mmol , 1 . 0 m solution in hexane ) at 0 ° c . the reaction mixture was stirred for 2 hours at room temperature , and then quenched with saturated 1n aq . hcl ( 50 ml ). the mixture was extracted with etoac ( 3 × 20 ml ). the combined organic layers were washed with water ( 50 ml ) and brine ( 50 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 1 to 1 : 2 ) to afford 2 -( 2 - fluoro - 4 - iodophenylamino )- 4 - methoxy - 1 , 5 - dimethyl - 6 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 1 , 6 - dihydropyridine - 3 - carboxamide ( 850 mg , 54 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 2 . 08 ( 3h , s ), 3 . 27 ( 3h , s ), 3 . 79 ( 3h , s ), 3 . 94 - 3 . 96 ( 2h , m ), 4 . 06 ( 1h , dd , j = 6 . 8 , 2 . 4 hz ), 4 . 19 - 4 . 26 ( 3h , m ), 6 . 41 ( 1h , t , j = 8 . 4 hz ), 6 . 50 ( 1h , dd , j = 14 . 6 , 6 . 8 hz ), 7 . 34 ( 1h , d , j = 8 . 4 hz ), 7 . 45 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 10 . 18 ( 1h , brs ), 10 . 52 ( 1h , brs ). m / z = 517 . 9 [ m + h ] + to a solution of 2 -( 2 - fluoro - 4 - iodophenylamino )- 4 - methoxy - 1 , 5 - dimethyl - 6 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 1 , 6 - dihydropyridine - 3 - carboxamide ( 400 mg , 0 . 773 mmol ) in meoh ( 8 . 0 ml ) was added 2m aq . hcl ( 2 . 3 ml , 4 . 64 mmol ) at room temperature . the reaction mixture was stirred for 15 minutes at room temperature , and then concentrated in vacuo . the residue was dissolved in dcm , neutralized with saturated aq . nahco 3 at 0 ° c . the separated aqueous layer was extracted with dcm . the combined organic layers were washed with brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residual solid was suspended in et 2 o , collected by filtration , and washed with et 2 o to afford 2 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 4 - methoxy - 1 , 5 - dimethyl - 6 - oxo - 1 , 6 - dihydropyridine - 3 - carboxamide ( 357 mg , 94 %) as a yellow solid . 1 h nmr ( dmso - d 6 , varian 400 mhz ) δ 1 . 95 ( 3h , s ), 3 . 25 ( 3h , s ), 3 . 40 - 3 . 46 ( 2h , m ), 3 . 59 - 3 . 61 ( 2h , m ), 3 . 73 ( 3h , s ), 4 . 64 ( 1h , brs ), 6 . 40 ( 1h , t , j = 8 . 8 hz ), 7 . 31 ( 1h , dd , j = 8 . 4 , 1 . 2 hz ), 7 . 45 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 8 . 25 ( 1h , brs ), 11 . 13 ( 1h , brs ). m / z = 491 . 9 [ m + h ] + to a solution of dimethyl 3 - oxopentanedioate ( 1 . 30 ml , 8 . 83 mmol ) in pyridine ( 2 . 28 ml ) was added crude 2 - chloropropanal ( intermediate 4 , 817 mg , 8 . 83 mmol ) dropwise at 0 ° c . the reaction mixture was stirred at 40 ° c . for 15 hours . the residue was diluted with dcm and washed with water and brine , dried over mgso 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 5 : 1 ) to give methyl 5 - ethyl - 2 -( 2 - methoxy - 2 - oxoethyl ) furan - 3 - carboxylate ( 420 mg , 22 %) as a colorless liquid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 28 ( 3h , s ), 3 . 72 ( 3h , s ), 3 . 80 ( 3h , s ), 4 . 02 ( 2h , s ), 6 . 27 ( 1h , s ). to a solution of 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 1 . 22 g , 5 . 75 mmol ) in dry thf ( 25 . 0 ml ) was added nah ( 55 wt % dispersion in mineral oil , 0 . 263 g , 6 . 04 mmol ) at 0 ° c . the reaction mixture was stirred at room temperature for 30 min , and then methyl 5 - ethyl - 2 -( 2 - methoxy - 2 - oxoethyl ) furan - 3 - carboxylate ( 1 . 59 g , 5 . 75 mmol ) was added slowly with dropping funnel . the reaction mixture was stirred at room temperature for 15 hours . the reaction mixture was quenched with water , extracted with etoac . the resulting solid was collected by filtration , rinsed with water and dried in vacuo to give methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 833 mg , 32 %) as a yellow solid , which was used for the next reaction without further purification . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 45 ( 3h , d , j = 1 . 2 hz ), 3 . 36 ( 3h , s ), 3 . 95 ( 3h , s ), 6 . 40 ( 1h , t , j = 8 . 4 hz ), 6 . 54 ( 1h , m ), 7 . 34 ( 1h , d , j = 8 . 4 hz ), 7 . 57 ( 1h , m ), 9 . 72 ( 1h , s ). to a solution of methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 273 mg , 0 . 599 mmol ) in meoh ( 18 . 0 ml ) was added k 2 co 3 ( 331 mg , 2 . 40 mmol ) at room temperature . and then water ( 18 . 0 ml ) was added slowly with dropping funnel . the reaction mixture was stirred at 70 ° c . for 1 hour . the reaction mixture was quenched with water and then concentrated in vacuo to give potassium 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 554 mg , 192 %) as a white solid . lc - ms : calcd . 441 . 98 . found 442 . 72 [ m + h ] + . to a solution of potassium 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 280 mg , 0 . 583 mmol ) in dmf ( 6 . 50 ml ) was added o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 66 . 1 mg , 0 . 641 mmol ) at room temperature and then was cooled to 0 ° c . to a reaction mixture was added edci ( 168 mg , 0 . 875 mmol ), hobt ( 134 mg , 0 . 875 mmol ) and tea ( 0 . 143 ml , 1 . 02 mmol ). the mixture was stirred at 40 ° c . for 15 h . the residue was extracted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 2 : 1 ) to give 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 42 . 3 mg , 14 %) as a brown solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 46 ( 3h , s ), 3 . 32 ( 3h , s ), 4 . 00 ( 2h , m ), 4 . 07 - 4 . 27 ( 2h , m ), 4 . 29 - 4 . 31 ( 2h , m ), 6 . 48 - 6 . 55 ( 2h , m ), 7 . 36 ( 1h , d , j = 12 . 8 hz ), 7 . 46 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 7 . 70 ( 1h , d , j = 8 . 0 hz ), 10 . 0 ( 1h , s ), 10 . 8 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 42 . 3 mg , 0 . 0800 mmol ) in meoh ( 0 . 400 ml ) was added 1 n aq . hcl ( 0 . 52 ml , 0 . 515 mmol ) at room temperature . the reaction mixture was stirred at room temperature for 10 min . the solvent was evaporated , diluted with dcm , and aq . nahco 3 was added until ph 7 at 0 ° c . dcm was evaporated and solidify with ether / hexane to give 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 15 . 2 mg , 37 . 8 %) as a light brown solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 49 ( 3h , s ), 3 . 30 ( 3h , s ), 3 . 77 ( 2h , m ), 4 . 06 ( 1h , t , j = 6 . 4 hz ), 4 . 11 ( 2h , t , j = 4 . 4 hz ), 6 . 50 ( 1h , t , j = 8 . 6 hz ), 7 . 58 ( 1h , m ), 7 . 39 ( 1h , d , j = 4 . 0 hz ), 7 . 48 ( 1h , d , j = 9 . 8 , 1 . 8 hz ), 9 . 84 ( 1h , s ), 10 . 7 ( 1h , s ). m / z = 501 . 8 [ m + h ] + . a mixture of pd 2 ( dba ) 3 ( 0 . 239 g , 0 . 261 mmol ) and 1 , 2 - bis ( diphenylphosphino ) ethane ( 0 . 208 g , 0 . 521 mmol ) in thf ( 226 ml ) was added methyl prop - 2 - ynyl carbonate ( intermediate 5 , 5 . 94 g , 52 . 1 mmol ) and diethyl 3 - oxopentanedioate ( 10 . 5 g , 52 . 1 mmol ) at room temperature . the reaction mixture was heated to reflux overnight under nitrogen atmosphere . after being cooled to room temperature , the reaction mixture was filtered through a celite pad and washed with etoac . the filtrate was concentrated in vacuo , and the residue was purified by column chromatography on sio 2 ( hex : etoac = 4 : 1 ) to give ethyl 2 -( 2 - ethoxy - 2 - oxoethyl )- 4 - methylfuran - 3 - carboxylate ( 4 . 67 g , 37 %) as a yellow oil . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 26 ( 3h , t , j = 9 . 0 hz ), 1 . 34 ( 3h , t , j = 6 . 0 hz ), 2 . 16 ( 3h , s ), 4 . 01 ( 2h , s ), 4 . 18 ( 2h , q ), 4 . 28 ( 2h , q ), 7 . 12 ( 1h , s ). to a solution of ethyl 2 -( 2 - ethoxy - 2 - oxoethyl )- 4 - methylfuran - 3 - carboxylate ( 4 . 67 g , 19 . 4 mmol ) in dry thf ( 100 ml ) was added nah ( 55 wt % dispersion in mineral oil , 0 . 891 g , 20 . 4 mmol ) at 0 ° c . the reaction mixture was stirred at room temperature for 30 min , and then 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 6 . 98 g , 25 . 3 mmol ) was added slowly . the reaction mixture was stirred at room temperature for 15 hours . the reaction mixture was quenched with water , extracted with etoac . the resulting solid was collected by filtration , rinsed with water and dried in vacuo to give ethyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 3 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 1 . 22 g , 13 %) as a yellow solid , which was used for the next reaction without further purification . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 41 ( 3h , t , j = 7 . 2 hz ), 2 . 36 ( 3h , s ), 3 . 33 ( 3h , s ), 4 . 39 ( 2h , q ), 6 . 43 ( 1h , t , j = 8 . 4 hz ), 7 . 27 ( 1h , m ), 7 . 35 ( 1h , m ), 7 . 48 ( 1h , m ), 9 . 78 ( 1h , s ). to a solution of ethyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 3 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 1 . 22 g , 2 . 59 mmol ) in thf ( 12 . 0 ml ) and meoh ( 12 . 0 ml ) was added k 2 co 3 ( 1 . 43 g , 10 . 4 mmol ) at room temperature . and then water ( 12 . 0 ml ) was added slowly with dropping funnel . the reaction mixture was stirred at 65 ° c . for 9 hours . the reaction mixture was quenched with water and then acidified with 1n aq . hcl until ph 1 ˜ 2 . the resulting solid was collected by filtration , rinsed with water and dried in vacuo to give 6 -( 2 - fluoro - 4 - iodophenylamino )- 3 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( 860 mg , 75 %) as a white solid , which was used for the next reaction without further purification . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 21 ( 3h , s ), 3 . 19 ( 3h , s ), 6 . 64 ( 1h , t , j = 8 . 2 hz ), 7 . 37 ( 1h , m ), 7 . 60 ( 1h , m ), 7 . 65 ( 1h , m ), 9 . 59 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 3 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( 680 mg , 1 . 54 mmol ) in dmf ( 35 . 0 ml ) was added o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 190 mg , 1 . 85 mmol ) at room temperature and then was cooled to 0 ° c . to a reaction mixture was added edci ( 442 mg , 2 . 31 mmol ), hobt ( 353 mg , 2 . 31 mmol ) and tea ( 0 . 322 ml , 2 . 31 mmol ). the mixture was stirred at room temperature for 15 hours . the residue was extracted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 2 : 1 ) to give 6 -( 2 - fluoro - 4 - iodophenylamino )- 3 , 5 - dimethyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 382 mg , 47 %) as a brown solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 37 ( 3h , s ), 3 . 30 ( 3h , s ), 4 . 00 ( 2h , m ), 4 . 09 ( 1h , m ), 4 . 22 ( 1h , m ), 4 . 29 ( 2h , m ), 6 . 49 ( 2h , m ), 7 . 27 ( 1h , m ), 7 . 37 ( 1h , m ), 7 . 47 ( 1h , m ), 10 . 0 ( 1h , s ), 10 . 9 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 3 , 5 - dimethyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 200 mg , 0 . 379 mmol ) in meoh ( 11 . 1 ml ) and thf ( 11 . 1 ml ) was added 1n aq . hcl ( 2 . 20 ml , 2 . 20 mmol ) at room temperature . the reaction mixture was stirred at room temperature for 10 min . the reaction mixture was added aq . nahco 3 until ph 7 at 0 ° c . the residue was extracted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 1 ) to give 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 3 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 84 . 1 mg , 44 %) as a light brown solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 26 ( 3h , s ), 3 . 34 ( 3h , s ), 3 . 48 ( 2h , t , j = 4 . 6 hz ), 3 . 65 ( 2h , t , j = 4 . 8 hz ), 6 . 53 ( 1h , t , j = 8 . 8 hz ), 7 . 33 ( 1h , m ), 7 . 58 ( 1h , dd , j = 10 . 8 , 1 . 6 hz ), 7 . 64 ( 1h , m ). * oh alcohol , nh amide , nh peak were not observed . m / z = 501 . 8 [ m + h ] + . a mixture of dimethyl 3 - oxopentanedioate ( 13 . 7 g , 79 . 0 mmol ), 1 , 4 - dithiane - 2 , 5 - diol ( 4 . 00 g , 26 . 3 mmol ), libr ( 685 mg , 7 . 88 mmol ) in 1 , 4 - dioxane ( 132 ml ) was refluxed overnight , cooled to room temperature . the insoluble solid was filtered and washed with et 2 o , and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 85 : 15 ) to give the methyl 2 -( 2 - methoxy - 2 - oxoethyl ) thiophene - 3 - carboxylate ( 5 . 07 g , 90 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 74 ( 3h , s ), 3 . 84 ( 3h , s ), 4 . 22 ( 2h , s ), 7 . 15 ( 1h , d , j = 5 . 2 hz ), 7 . 44 ( 1h , d , j = 5 . 2 hz ). to a solution of methyl 2 -( 2 - methoxy - 2 - oxoethyl ) thiophene - 3 - carboxylate ( 1 . 00 g , 4 . 67 mmol ) in dry thf ( 23 . 0 ml ) was added nah ( 55 %, 224 mg , 5 . 13 mmol ) at 0 ° c . the mixture was stirred for 30 minutes at 0 ° c . after dropwise addition of 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 1 . 29 g , 4 . 67 mmol ) at 0 ° c ., the reaction mixture was stirred at room temperature for 30 min , and then quenched saturated aq . nh 4 cl ( 30 ml ). the mixture was extracted with etoac ( 2 × 20 ml ). the combined organic layers were washed water ( 50 ml ) and brine ( 50 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 4 : 1 ) to give the methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothieno [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 654 mg , 31 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 38 ( 3h , s ), 3 . 97 ( 3h , s ), 6 . 45 ( 1h , t , j = 8 . 4 hz ), 7 . 19 ( 1h , d , j = 5 . 2 hz ), 7 . 36 ( 1h , d , j = 8 . 4 hz ), 7 . 49 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 7 . 61 ( 1h , d , j = 8 . 4 hz ), 9 . 70 ( 1h , brs ). a mixture of methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothieno [ 3 , 2 - c ] pyridine - 7 - carboxylate ( 1 . 36 g , 2 . 96 mmol ) and o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 458 mg , 4 . 44 mmol ) in dry thf ( 20 ml ) was added lihmds ( 17 . 8 ml , 17 . 8 mmol , 1 . 0 m solution in hexane ) at 0 ° c . the reaction mixture was stirred for 1 hour at room temperature , and then quenched saturated 1n aq . hcl ( 50 ml ). the mixture was extracted with etoac ( 2 × 20 ml ). the combined organic layers were washed water ( 50 ml ) and brine ( 50 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 3 : 7 ) to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrothieno [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 575 mg , 37 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 41 ( 3h , s ), 3 . 94 - 3 . 97 ( 2h , m ), 4 . 07 ( 1h , dd , j = 6 . 8 , 2 . 4 hz ), 4 . 18 - 4 . 25 ( 3h , m ), 6 . 37 ( 1h , t , j = 8 . 4 hz ), 6 . 46 ( 1h , dd , j = 14 . 6 , 6 . 8 hz ), 7 . 28 ( 1h , d , j = 5 . 2 hz ), 7 . 32 ( 1h , d , j = 8 . 4 hz ), 7 . 47 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 7 . 62 ( 1h , d , j = 5 . 2 hz ), 8 . 71 ( 1h , brs ), 9 . 21 ( 1h , brs ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrothieno [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 300 mg , 0 . 567 mmol ) in meoh ( 6 . 0 ml ) was added 2n aq . hcl ( 1 . 7 ml , 3 . 40 mmol ) at room temperature , the reaction mixture was stirred for 30 minutes at room temperature , then concentrated in vacuo . the residue was dissolved in dcm , neutralized with saturated aq . nahco 3 at 0 ° c . the separated aqueous layer was extracted with dcm . the combined organic layers were washed with brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residual solid was suspended in meoh , collected by filtration , and washed with meoh to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothieno [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 217 mg , 76 %) as a white solid . 1 h nmr ( dmso - d 6 , varian 400 mhz ): δ 3 . 43 ( 3h , s ), 3 . 40 - 3 . 47 ( 2h , m ), 3 . 57 - 3 . 64 ( 2h , m ), 4 . 67 ( 1h , brs ), 6 . 51 ( 1h , t , j = 8 . 8 hz ), 7 . 31 ( 1h , dd , j = 8 . 4 , 1 . 2 hz ), 7 . 49 ( 1h , d , j = 5 . 2 hz ), 7 . 57 ( 1h , dd , j = 10 . 8 , 2 . 0 hz ), 7 . 62 ( 1h , d , j = 5 . 2 hz ), 8 . 30 ( 1h , brs ), 11 . 30 ( 1h , brs ). m / z = 503 . 7 [ m + h ] + . to a solution of dimethyl 3 - oxopentanedioate ( 25 . 0 g , 144 mmol ) in acetic acid ( 50 ml ) was added a solution of nano 2 ( 10 . 4 g , 151 mmol ) in water ( 25 ml ) at 0 ° c . the reaction mixture was stirred overnight at room temperature . after evaporation of volatile solvents , the residue was partitioned between etoac ( 50 ml ) and water ( 50 ml ). the separated aqueous layer was extracted ( 2 × 30 ml ). the combined organic layers were washed water ( 100 ml ) and brine ( 100 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 3 : 2 ) to give the dimethyl 2 -( hydroxyimino )- 3 - oxopentanedioate ( 15 . 3 g , 52 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 76 ( 3h , s ), 3 . 84 ( 2h , s ), 3 . 93 ( 3h , s ), 9 . 74 ( 1h , brs ). a mixture of dimethyl 2 -( hydroxyimino )- 3 - oxopentanedioate ( 15 . 3 g , 75 . 0 mmol ) and 10 % pd / c ( 1 . 50 g ) in acetic anhydride ( 377 ml ) was stirred at room temperature for 3 hours under hydrogen atmosphere ( balloon ). the reaction mixture was filtered through a celite pad , washed with etoac ( 200 ml ), and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 9 ) to give the dimethyl 2 - acetamido - 3 - oxopentanedioate ( 9 . 28 g , 53 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 2 . 09 ( 1h , s ), 3 . 75 ( 3h , s ), 3 . 76 ( 2h , s ), 3 . 83 ( 3h , s ), 5 . 42 ( 1h , d , j = 6 . 4 hz ), 6 . 64 ( 1h , brs ). to a solution of dimethyl 2 - acetamido - 3 - oxopentanedioate ( 9 . 28 g , 40 . 2 mmol ) in chloroform ( 200 ml ) was added socl 2 ( 8 . 79 ml , 120 mmol ) at 0 ° c . the mixture was refluxed for 6 hours , cooled to room temperature . after evaporation of volatile solvents , the residue was diluted with dcm ( 50 ml ), neutralized with saturated aq . nahco 3 at 0 ° c ., and extracted with dcm ( 2 × 30 ml ). the combined organic layers were washed water ( 100 ml ) and brine ( 100 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 2 ) to give the methyl 5 -( 2 - methoxy - 2 - oxoethyl )- 2 - methyloxazole - 4 - carboxylate ( 4 . 06 g , 47 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 2 . 49 ( 3h , s ), 3 . 75 ( 3h , s ), 3 . 90 ( 3h , s ), 4 . 10 ( 2h , s ). to a solution of methyl 5 -( 2 - methoxy - 2 - oxoethyl )- 2 - methyloxazole - 4 - carboxylate ( 2 . 00 g , 4 . 67 mmol ) in dry thf ( 47 ml ) was added nah ( 55 %, 450 mg , 10 . 3 mmol ) at 0 ° c . the mixture was stirred for 30 minutes at 0 ° c . after dropwise addition of 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 3 . 11 g , 11 . 3 mmol ) at 0 ° c ., the reaction mixture was stirred at 0 ° c . for 30 min , and then quenched saturated aq . nh 4 cl ( 50 ml ). the mixture was extracted with etoac ( 2 × 30 ml ). the combined organic layers were washed water ( 70 ml ) and brine ( 70 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residual was suspended in et 2 o , collected by filtration , and washed with et 2 o to give the methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxylate ( 1 . 85 g , 43 %) as a brown solid . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 2 . 64 ( 3h , s ), 3 . 36 ( 3h , s ), 3 . 96 ( 3h , s ), 6 . 50 ( 1h , t , j = 8 . 4 hz ), 7 . 40 ( 1h , d , j = 8 . 4 hz ), 7 . 50 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 9 . 92 ( 1h , brs ). to a solution of methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxylate ( 1 . 60 g , 3 . 50 mmol ) in a mixture of thf ( 40 ml ), meoh ( 40 ml ) and h 2 o ( 40 ml ) was added 2 m aq . k 2 co 3 ( 2 . 62 ml , 5 . 25 mmol ) at room temperature . the reaction mixture was stirred at 70 ° c . for 3 hours . the mixture was extracted with etoac ( 2 × 40 ml ). the aqueous layer was acidified with 3 n aq . hcl until ph 3 . the resulting solid was collected by filtration , washed with water and et 2 o to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxylic acid ( 1 . 21 g , 78 %) as a yellow solid . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ): δ 2 . 56 ( 3h , s ), 3 . 25 ( 3h , s ), 6 . 75 ( 1h , t , j = 8 . 8 hz ), 7 . 44 ( 1h , d , j = 8 . 8 hz ), 7 . 69 ( 1h , dd , j = 10 . 8 , 2 . 0 hz ), 9 . 70 ( 1h , s ), 13 . 33 ( 1h , brs ). a mixture of 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxylic acid ( 1 . 21 g , 2 . 74 mmol ), o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 424 mg , 4 . 11 mmol ), hobt ( 630 mg , 4 . 11 mmol ), and edc ( 788 mg , 4 . 11 mmol ) in dmf ( 14 ml ) was added tea ( 0 . 764 ml , 5 . 48 mmol ) at room temperature . the mixture was stirred at room temperature for 1 h , and quenched with saturated aq . nh 4 cl ( 20 ml ). the mixture was extracted with etoac ( 3 × 10 ml ), and the combined organic layers were washed with water ( 3 × 30 ml ) and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residual was suspended in etoac , collected by filtration , and washed with etoac to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxamide ( 826 g , 57 %) as a yellow solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 2 . 66 ( 3h , s ), 3 . 33 ( 3h , s ), 4 . 00 - 4 . 02 ( 2h , m ), 4 . 09 - 4 . 12 ( 1h , m ), 4 . 26 ( 1h , dd , j = 14 . 4 , 2 . 4 hz ), 4 . 30 - 4 . 33 ( 2h , m ), 6 . 50 - 6 . 57 ( 2h , m ), 7 . 40 ( 1h , d , j = 8 . 4 hz ), 7 . 48 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 9 . 70 ( 1h , s ), 10 . 96 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 2 , 5 - dimethyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxamide ( 300 mg , 0 . 568 mmol ) in meoh ( 6 . 0 ml ) was added 2n aq . hcl ( 1 . 7 ml , 3 . 40 mmol ) at room temperature , the reaction mixture was stirred for 30 minutes at room temperature , then concentrated in vacuo . the residue was dissolved in dcm , neutralized with saturated aq . nahco 3 at 0 ° c . the separated aqueous layer was extracted with dcm . the combined organic layers were washed with brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( dcm : meoh = 95 : 5 ) to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 2 , 5 - dimethyl - 4 - oxo - 4 , 5 - dihydrooxazolo [ 4 , 5 - c ] pyridine - 7 - carboxamide ( 186 mg , 65 %) as a white solid . 1 h nmr ( dmso - d 6 , varian 400 mhz ): δ 2 . 56 ( 3h , s ), 3 . 39 ( 3h , s ), 3 . 47 - 3 . 50 ( 2h , m ), 3 . 59 - 3 . 62 ( 2h , m ), 4 . 68 ( 1h , t , j = 5 . 6 hz ), 6 . 63 ( 1h , t , j = 8 . 8 hz ), 7 . 35 ( 1h , d , j = 8 . 4 hz ), 7 . 60 ( 1h , dd , j = 10 . 8 , 2 . 0 hz ), 9 . 00 ( 1h , brs ), 11 . 34 ( 1h , brs ). m / z = 502 . 9 [ m + h ] + . to a solution of compound cubr 2 ( 11 . 5 g , 51 . 7 mmol ) in etoac ( 160 ml ) was added a solution of dimethyl 2 - oxopentanedioate ( 3 . 00 g , 17 . 2 mmol ) in chcl 3 ( 80 ml ) at room temperature . the reaction mixture was refluxed overnight , cooled to room temperature . after evaporation of volatile solvents , the residue was purified by column chromatography on sio 2 ( hex : etoac = 3 : 2 ) to give the dimethyl 3 - bromo - 2 - oxopentanedioate ( 4 . 36 g , quant .) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 06 ( 1h , a bx , j ab = 17 . 3 hz , j ax = 9 . 3 hz ), 3 . 34 ( 1h , a b x , j ab = 17 . 3 hz , j bx = 5 . 9 hz ), 3 . 71 ( 3h , s ), 3 . 95 ( 3h , s ), 5 . 40 ( 1h , ab x , j ax = 9 . 3 hz , j bx = 5 . 9 hz ). a mixture of dimethyl 3 - bromo - 2 - oxopentanedioate ( 4 . 36 g , 17 . 2 mmol ) and methanethioamide ( 1 . 6 m in dioxane , 53 . 8 ml , 86 . 0 mmol ) in etoh ( 86 ml ) was refluxed overnight , cooled to room temperature . after evaporation of volatile solvents , the residue was purified by column chromatography on sio 2 ( hex : etoac = 2 : 3 ) to give the methyl 5 -( 2 - methoxy - 2 - oxoethyl ) thiazole - 4 - carboxylate ( 2 . 02 g , 54 %) as a yellow oil . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 77 ( 3h , s ), 3 . 96 ( 3h , s ), 4 . 37 ( 2h , s ), 8 . 73 ( 1h , s ). to a solution of methyl 5 -( 2 - methoxy - 2 - oxoethyl ) thiazole - 4 - carboxylate ( 2 . 02 g , 9 . 40 mmol ) in dry thf ( 47 ml ) was added nah ( 55 %, 490 mg , 11 . 3 mmol ) at 0 ° c . the mixture was stirred for 30 minutes at 0 ° c . after dropwise addition of 2 - fluoro - 4 - iodo - n -(( methylimino ) methylene ) aniline ( intermediate 1 , 2 . 59 g , 9 . 40 mmol ) at 0 ° c ., the reaction mixture was stirred at room temperature for 1 hour , and then quenched saturated aq . nh 4 cl ( 50 ml ). the mixture was extracted with etoac ( 2 × 30 ml ). the combined organic layers were washed water ( 70 ml ) and brine ( 70 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residual was purified by column chromatography on sio 2 ( hex : etoac = 2 : 3 to 1 : 2 ) to give the methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxylate ( 434 mg , 10 %) as an orange solid . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 41 ( 3h , s ), 3 . 97 ( 3h , s ), 6 . 54 ( 1h , t , j = 8 . 8 hz ), 7 . 41 ( 1h , d , j = 8 . 4 hz ), 7 . 52 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 9 . 94 ( 1h , brs ). to a solution of methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxylate ( 100 mg , 0 . 218 mmol ) in a mixture of thf ( 2 ml ), meoh ( 2 ml ) and h 2 o ( 2 ml ) was added 2 m aq . k 2 co 3 ( 0 . 163 ml , 0 . 327 mmol ) at room temperature . the reaction mixture was stirred at 70 ° c . for 3 hours . the mixture was extracted with etoac ( 2 × 10 ml ). the aqueous layer was acidified with 3 n aq . hcl until ph 3 . the resulting solid was collected by filtration , washed with water and et 2 o to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxylic acid ( 66 . 9 mg , 69 %) as a yellow solid . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ): δ 3 . 28 ( 3h , s ), 6 . 75 ( 1h , t , j = 8 . 8 hz ), 7 . 40 ( 1h , d , j = 8 . 4 hz ), 7 . 69 ( 1h , dd , j = 10 . 6 , 2 . 0 hz ), 9 . 07 ( 1h , s ), 9 . 62 ( 1h , brs ). a mixture of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxylic acid ( 66 . 9 mg , 0 . 150 mmol ), o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 23 . 0 mg , 0 . 225 mmol ) in dmf ( 1 ml ) was added hatu ( 171 mg , 0 . 450 mmol ) at room temperature . the mixture was stirred at room temperature for 4 hours , and quenched with saturated aq . nh 4 cl ( 10 ml ). the mixture was extracted with etoac ( 2 × 10 ml ), and the combined organic layers were washed with water ( 3 × 10 ml ) and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residual was purified by column chromatography on sio 2 ( dcm : meoh = 95 : 5 ) to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxamide ( 14 mg , 17 %) as a brown solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 3 . 69 ( 3h , s ), 3 . 90 - 3 . 93 ( 2h , m ), 3 . 98 - 4 . 02 ( 3h , m ), 4 . 13 ( 1h , dd , j = 14 . 4 , 2 . 4 hz ), 6 . 47 - 6 . 52 ( 2h , m ), 7 . 31 ( 1h , d , j = 8 . 8 hz ), 7 . 43 ( 1h , dd , j = 10 . 0 , 2 . 0 hz ), 8 . 90 ( 1h , s ). to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxamide ( 14 . 0 mg , 0 . 026 mmol ) in meoh ( 0 . 5 ml ) was added 2n aq . hcl ( 0 . 079 ml , 0 . 158 mmol ) at room temperature , the reaction mixture was stirred for 1 hour at room temperature , then concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( dcm : meoh = 93 : 7 to 9 : 1 ) to give the 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrothiazolo [ 4 , 5 - c ] pyridine - 7 - carboxamide ( 5 . 2 mg , 39 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ): δ 3 . 40 - 3 . 47 ( 2h , m ), 3 . 74 ( 3h , s ), 3 . 76 - 3 . 81 ( 2h , m ), 6 . 52 ( 1h , t , j = 8 . 8 hz ), 7 . 34 ( 1h , d , j = 8 . 4 hz ), 7 . 44 ( 1h , dd , j = 10 . 0 , 1 . 6 hz ), 8 . 94 ( 1h , s ), 9 . 20 ( 1h , brs ), 11 . 06 ( 1h , brs ). m / z = 504 . 6 [ m + h ] + . to a solution of methyl 6 -( 2 - chloro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylate ( intermediate 7 , 320 mg , 0 . 69 mmol ) in dry thf ( 17 . 0 ml ) was added o -( 2 -( vinyloxy ) ethyl ) hydroxylamine ( intermediate 2 , 108 mg , 1 . 04 mmol ) at room temperature and then was cooled to 0 ° c . to the reaction mixture was added lihmds ( 3 . 50 g , 4 . 19 mmol ) at 0 ° c . under a n 2 atmosphere . the mixture was stirred at room temperature for 1 hour . the reaction mixture was quenched with water and extracted with etoac , washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo to give 6 -( 2 - chloro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 310 mg , 84 %) as a white solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 3 . 99 - 4 . 01 ( 2h , m ), 4 . 07 - 4 . 09 ( 1h , dd , j = 6 . 8 , 2 . 4 hz ), 4 . 25 - 4 . 26 ( 1h , dd , j = 14 . 4 , 2 . 4 hz ), 6 . 36 ( 1h , d , j = 8 . 4 hz ), 6 . 49 - 6 . 54 ( 1h , m ), 7 . 01 ( 1h , m ), 7 . 43 - 7 . 45 ( 1h , dd , j = 8 . 6 , 1 . 8 hz ), 7 . 51 ( 1h , m ), 7 . 77 ( 1h , m ), 10 . 0 ( 1h , s ), 10 . 8 ( 1h , s ). to a solution of 6 -( 2 - chloro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - n -( 2 -( vinyloxy ) ethoxy )- 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 200 mg , 0 . 37 mmol ) in meoh ( 4 ml ) was added 2n aq . hcl ( 1 . 21 ml ) at room temperature . the mixture was stirred at room temperature for 30 min . the residue was neutralized with aq . nahco 3 at 0 ° c . the separated aqueous layer was extracted with dcm . the combined organic layers were washed with brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residual solid was suspended in et 2 o , collected by filtration , and washed with et 2 o to give 6 -( 2 - chloro - 4 - iodophenylamino )- n -( 2 - hydroxyethoxy )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 170 mg , 89 %) as a white solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ) δ 3 . 29 ( 3h , s ), 3 . 50 - 3 . 51 ( 2h , m ), 3 . 70 - 3 . 72 ( 2h , m ), 4 . 66 - 4 . 681 ( 1h , m ), 6 . 46 ( 1h , t , j = 8 . 4 hz ), 7 . 03 ( 1h , m ), 7 . 45 - 7 . 48 ( 1h , dd , j = 8 . 4 , 2 . 0 hz ), 7 . 78 ( 1h , m ), 7 . 96 ( 1h , m ), 8 . 91 ( 1h , s ), 11 . 3 ( 1h , s ). m / z = 503 . 6 [ m + h ] + . to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( example 1 , step a ; 150 mg , 0 . 350 mmol ) in dmf ( 1 . 00 ml ) was added o -( cyclopropylmethyl ) hydroxylamine hydrochloride ( intermediate 8 , 47 . 6 mg , 0 . 385 mmol ) at room temperature and then was cooled to 0 ° c . to a reaction mixture was added edci ( 101 mg , 0 . 526 mmol ), hobt ( 80 . 0 mg , 0 . 526 mmol ) and tea ( 0 . 146 ml , 1 . 05 mmol ). the mixture was stirred at room temperature for 15 hours . the residue was extracted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 2 : 1 ) to give n -( cyclopropylmethoxy )- 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 30 . 3 mg , 16 %) as a purple solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ); δ 0 . 35 ( 2h , m ), 0 . 63 ( 2h , m ), 3 . 32 ( 3h , s ), 3 . 87 ( 2h , d , j = 7 . 2 hz ), 6 . 50 ( 1h , t , j = 8 . 4 hz ), 7 . 01 ( 1h , m ), 7 . 36 ( 1h , m ), 7 . 47 ( 1h , m ), 7 . 53 ( 1h , m ), 9 . 86 ( 1h , s ), 10 . 9 ( 1h , s ). * nh peak was not observed . m / z = 497 . 90 [ m + h ] + . to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( example 1 , step a ; 150 mg , 0 . 350 mmol ) in dmf ( 3 . 50 ml ) was added o -( 1 - hydroxy - 2 - methylpropan - 2 - yl ) hydroxylammonium chloride ( intermediate 9 , 74 . 4 mg , 0 . 526 mmol ) at room temperature and then was cooled to 0 ° c . to a reaction mixture was added edci ( 101 mg , 0 . 526 mmol ), hobt ( 80 . 0 mg , 0 . 526 mmol ) and tea ( 0 . 0730 ml , 0 . 526 mmol ). the mixture was stirred at room temperature for 15 hours . the residue was extracted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 1 ) to give 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 1 - hydroxy - 2 - methylpropan - 2 - yloxy )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 30 . 1 mg , 17 %) as a white solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 1 . 34 ( 6h , s ), 3 . 31 ( 3h , s ), 3 . 39 ( 2h , d , j = 6 . 8 hz ), 6 . 55 ( 1h , t , j = 8 . 4 hz ), 7 . 02 ( 1h , d , j = 2 . 0 hz ), 7 . 39 ( 1h , d , j = 8 . 4 hz ), 7 . 48 ( 1h , m ), 7 . 52 ( 1h , m ), 9 . 46 ( 1h , s ), 10 . 80 ( 1h , s ). m / z = 515 . 9 . 0 [ m + h ] + . to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( example 1 , step a ; 150 mg , 0 . 350 mmol ) in dmf ( 3 . 50 ml ) was added methoxymethanamine hydrochloride ( 51 . 3 mg , 0 . 526 mmol ) at room temperature and then was cooled to 0 ° c . to a reaction mixture was added edci ( 101 mg , 0 . 526 mmol ), hobt ( 80 . 0 mg , 0 . 526 mmol ) and tea ( 0 . 0730 ml , 0 . 526 mmol ). the mixture was stirred at room temperature for 15 hours . the residue was extracted with etoac and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 1 ) to give 6 -( 2 - fluoro - 4 - iodophenylamino )- n - methoxy - 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 66 . 2 mg , 41 %) as a purple solid . 1 h - nmr ( cdcl 3 , varian , 400 mhz ): δ 3 . 34 ( 3h , s ), 3 . 90 ( 3h , s ), 6 . 51 ( 1h , t , j = 8 . 4 hz ), 7 . 01 ( 1h , s ), 7 . 38 ( 1h , d , j = 14 hz ), 7 . 49 ( 2h , m ), 9 . 88 ( 1h , s ), 10 . 98 ( 1h , s ). m / z = 458 . 0 [ m + h ] + . to a mixture of methyl 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carb ( example 1 , step a ; 1 . 30 g , 2 . 94 mmol ) and ( r )— o -(( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methyl ) hydroxylamine ( intermediate 10 , 0 . 65 g , 4 . 41 mmol in dry thf ( 7 . 35 ml ) was added lihmds ( 17 . 6 ml , 16 . 6 mmol , 1 . 06 m solution in hexane ) at 0 ° c . the reaction mixture was stirred for 20 min at 0 ° c ., and then quenched with saturated 1n aq . hcl ( 50 ml ). the mixture was extracted with etoac ( 3 × 20 ml ). the combined organic layers were washed with water ( 50 ml ) and brine ( 50 ml ), dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 1 to 1 : 2 ) to give ( r )— n -(( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methoxy )- 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 1 . 07 g , 65 . 3 %) as a yellow solid . 1 h nmr ( cdcl 3 , varian 400 mhz ) δ 1 . 40 ( 3h , s ), 1 . 47 ( 3h , s ), 3 . 32 ( 3h , s ), 3 . 85 ( 1h , dd , j = 8 . 4 , 6 . 4 hz ), 4 . 05 - 4 . 18 ( 3h , m ), 4 . 43 - 4 . 48 ( 1h , m ), 6 . 51 ( 1h , t , j = 8 . 4 hz ), 7 . 01 ( 1h , d , j = 2 . 0 hz ), 7 . 37 ( 1h , d , j = 8 . 4 hz ), 7 . 46 - 7 . 50 ( 2h , m ), 10 . 14 ( 1h , s ), 10 . 96 ( 1h , brs ). to a solution of ( r )— n -(( 2 , 2 - dimethyl - 1 , 3 - dioxolan - 4 - yl ) methoxy )- 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 1 . 07 g , 1 . 92 mmol ) in meoh ( 28 ml ) was added 1 n aq . hcl ( 9 . 31 ml , 9 . 31 mmol ) at room temperature . the mixture was stirred at room temperature for 14 hours . the residue was diluted with dcm and washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo to give ( r )— n -( 2 , 3 - dihydroxypropoxy )- 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 580 mg , 58 . 4 %) as a white solid . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ) δ 2 . 42 ( 1h , t , j = 5 . 8 hz ), 3 . 30 ( 3h , s ), 3 . 62 - 3 . 67 ( 1h , m ), 3 . 73 - 3 . 79 ( 1h , m ), 3 . 97 - 4 . 02 ( 1h , m ), 4 . 03 - 4 . 14 ( 2h , m ), 4 . 44 ( 1h , d , t , j = 2 . 0 hz ), 6 . 56 ( 1h , t , t , j = 8 . 4 hz ), 7 . 01 ( 1h , d , t , j = 2 . 0 hz ), 7 . 40 ( 1h , d , t , j = 8 . 4 hz ), 7 . 49 ( 1h , dd , j = 9 . 8 , 1 . 8 hz ), 7 . 52 ( 1h , d , t , j = 2 . 0 hz ), 10 . 00 ( 1h , s ), 10 . 79 ( 1h , brs ). m / z = 517 . 8 [ m + h ] + . to a solution of 6 -( 2 - fluoro - 4 - iodophenylamino )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxylic acid ( example 1 , step a ; 1 . 18 g , 2 . 76 mmol ) in dmf ( 21 . 5 ml ) was added 3 - aminopropan - 1 - ol ( 228 mg , 3 . 03 mmol ) at room temperature and then was cooled to 0 ° c . to the reaction mixture was added edc ( 792 mg , 4 . 13 mmol ), hobt ( 633 g , 4 . 13 mmol ), and tea ( 0 . 77 ml , 5 . 51 mmol ). the mixture was stirred at room temperature for 2 hours . the reaction was extracted with etoac , washed with water and brine , dried over na 2 so 4 , filtered and concentrated in vacuo . the residue was purified by column chromatography on sio 2 ( hex : etoac = 1 : 1 ˜ 1 : 2 ) to give to give 6 -( 2 - fluoro - 4 - iodophenylamino )- n -( 3 - hydroxypropyl )- 5 - methyl - 4 - oxo - 4 , 5 - dihydrofuro [ 3 , 2 - c ] pyridine - 7 - carboxamide ( 130 mg , 9 . 7 %) as a violet solid . 1 h - nmr ( dmso - d 6 , varian , 400 mhz ) δ 1 . 53 - 1 . 60 ( 2h , m ), 3 . 24 ( q , 2h , j = 6 . 4 hz ), 3 . 34 ( 3h , s ), 3 . 42 - 3 . 46 ( 2h , m ), 4 . 50 ( 1h , t ), 6 . 60 ( 1h , t , j = 8 . 8 hz ), 7 . 02 ( 1h , d , j = 2 . 4 hz ), 7 . 36 ( 1h , dd , j = 1 . 0 hz ), 7 . 63 ( 1h , dd , j = 1 . 8 hz ), 7 . 92 ( 1h , d , j = 2 . 0 hz ), 8 . 22 ( 1h , t , j = 5 . 6 hz ), 9 . 93 ( 1h , s ). m / z = 486 . 0 [ m + h ] + . the kinase glo plus assay kit was purchased from promega . the substrate , apt , dtt , and dimethylsulfoxide were purchased from sigma - aldrich . the map2k1 ( mek1 ) kinase , europium labeled antibody , tracer 236 and binding buffer a were purchased from invitrogen . the recombinant human epithelial growth factor ( egf ) was purchased from r & amp ; d system . the surefire phospho - erk1 / 2 assay kit and the alphascreen general igg ( protein a ) detection kit were both purchased from perkinelmer . a mek1 kinase assay ( lance , perkinelmer ) was developed for supporting compound profiling and lead optimization . in this assay , un - phosphorylated / inactive erk1 ( millipore ) was used as the substrate for mek1 ( millipore ). then the phosphorylated erk1 was able to phosphorylate ulight ™- mbp peptide ( perkinelmer ). the phosphorylated peptide was detected by europium - anti - phospho - mbp ( perkinelmer ). in a reaction , the activity of mek1 ( 0 . 25 nm ) was measured in a buffer containing 50 μm atp , 2 nm inactive erk1 , 50 nm ulight ™- mbp peptide , and a compound for 90 min at 23 ° c . after quenching the reaction , 2 nm europium - anti - phospho - mbp was added to the reaction mixture and incubated for 60 min , followed by a detection using envision . the ic 50 values were derived through a curve fitting using grafit . to investigate whether a compound is able to inhibit the activity of mek in cells , a mechanism - based assay using a375 cell line ( melanoma ) was developed . in this assay ( alphascreen , perkinelmer ), inhibition of mek was detected by reduced erk phosphorylation . a375 cells were cultured in a tissue culture flask to 80 % confluence in dmem plus 10 % fetal bovine serum . cells were collected and plated onto 96 well culture plates at 3 × 10 4 cells / well . plates were incubated overnight at 37 ° c . with 5 % co 2 to allow cells to adhere . compounds were added to the plates and incubated at 37 ° c . for 1 hour . after removing the medium , 100 μl of cell lysis buffer were added to each well and 4 μl of cell lysate were transferred into a 384 well white proxiplate ( perkinelmer ). the phospho - erk levels were determined by following the standard protocol supplied with the perkinelmer surefire phospho - erk 1 / 2 assay kit ®. plates were read out by envision ( perkinelmer ). the data were analyzed using graphpad prism . select compounds prepared as described above were assayed according to the biological procedures described herein . the results are given in the table below : | 2 |
referring to fig1 there is shown a schematic layout of a floor plan for an integrated memory circuit device 10 of the present invention . as is well known , the device 10 is fabricated from silicon and is an integrated circuit device or a chip 10 . in the preferred embodiment , the device or chip 10 is an 8m × 8 - bit flash eeprom , using non - volatile memory cells of the split gate type arranged in a nor array 12 as disclosed in u . s . pat . no . 5 , 668 , 757 , which disclosure is incorporated by reference . as disclosed in u . s . pat . no . 5 , 668 , 757 programming of the memory cell occurs by hot channel electron tunneling . further , in the preferred embodiment , although the device 10 has its non - volatile memory cells arranged in a nor array 12 , the device 10 emulates the operation of a nand type page mode device . however , it should be noted that the present invention is not limited to this specific density or configuration or mode of operation . the memory cell array 12 is located in the center of the device 10 . on the left side of the array 12 , a control gate decoder 14 is located . on the right side of the array 12 , a word - line decoder 16 is located . a plurality of page buffers 18 are placed on the upper side of the array 12 . in the preferred embodiment , there are 512 × 8 page buffers that correspond to a page of 1024 × 8 memory cells . peripheral circuits 24 are located on the upper side of the device 10 . on the left side of the device 10 , charge pumps 22 are placed . on the right side of the device 10 , the current pumps 20 are placed . in the vicinity of corners of the device 10 , pads ( such as i / o , power and control ) are placed . since the memory cell array is configured as 8m × 8 - bit , the entire memory cell array 12 is divided into 8 identical sub - arrays ( sub - array 12 - 0 sub - array 12 - 1 , . . . sub - array 12 - 7 ). each sub - array has a corresponding i / o . thus , sub - array 12 - 0 corresponds to i / o - 0 , . . . sub - array 12 - 7 corresponds to i / o - 7 . although the memory cell array 12 is divided into 8 identical sub - arrays 12 - n , each word line from the word line decoder 16 , and each control gate line from the control gate decoder 14 runs “ horizontally ” across all eight identical sub - arrays 12 - n . in the preferred embodiment , a word line and a control line crosses 1024 × 8 cells , with each cell each having an associated bit line . thus , there are 1024 cells in each sub - array 12 - n . within each sub - array 12 - n , there are 512 page buffers 18 . thus , there are two memory cells associated with each page buffer 18 . to simplify the illustration , only one of the 8 sub - arrays 12 - n and its corresponding page buffers 18 - n is described and shown in the following drawings . referring to fig2 a , a plurality of adjacent signal lines pdb 0 to pdb 511 are connected to page buffers 18 l . each signal line pdb is connected to one page buffer 18 l . therefore , there are 512 page buffers 18 l . each signal line pdb is further eventually connected to a pair of immediately adjacent bit lines blj and bl ( j + 1 ) through bit line switches 46 l , sense amplifiers 36 u , and bit line switches 46 u and 44 to the memory array 12 ( see fig3 ). thus , the 512 pdb lines connected the 512 page buffers to 1024 bit lines bl . each bit line ( blx ) is in turn connected to a column of non - volatile memory cells . when a particular row of memory cells is selected there are 1024 memory cells associated with the 512 pdb lines . all the 512 ( from # 0 to # 511 ) page buffers 18 l that are connected to the signal lines pdb 0 - pdb 511 are further grouped into 16 interleaved sub - pages 18 l - n . thus , each sub - page 18 l - n comprises 32 page buffers 18 l . the grouping of each sub - page 18 l - n and its members are as follows : thus , sub - page 18 l - 0 comprises page buffers 18 l connected to pdb [ 0 ], [ 16 ], [ 32 ], [ 48 ], . . . [ 496 ] sub - page 18 l - 1 comprises page buffers 18 l connected to pdb [ 1 ], [ 17 ], [ 33 ], [ 49 ], . . . ,[ 497 ] sub - page 18 l - 2 comprises page buffers 18 l connected to pdb [ 2 ], [ 18 ], [ 34 ], [ 50 ], . . . ,[ 498 ] finally , sub - page 18 l - 15 comprises page buffers 18 l connected to pdb [ 15 ], [ 31 ], [ 47 ], [ 63 ], . . . , [ 511 ] as can be seen from the foregoing , each sub - page 18 l - n comprises page buffers 18 l that are not located immediately adjacent to one another . instead , page buffers 18 l of the same sub - page 18 l - n are connected to signal lines pdb that are spaced equal distance apart ( namely by the size of 15 page buffers 18 l ) from one another and are grouped together to form a sub - page . thus , the 16 sub - pages 18 l - 0 - 18 l - 15 are interleaved with one another . with this arrangement , the current drawn by selected memory cells during a sub - page pre - fetch can be spread out evenly across the whole memory cell sub - array 12 - n rather than being crowded over an area as narrow as the pitch of 32 adjacent pdb signal lines . the distance between two adjacent pdbs is carefully selected based on the sheet resistance of source diffusion area of memory cells . referring to fig2 a , the source line of each memory cell is connected together by a local diffusion path . a metal strapping runs through the cell array horizontally . periodic vss taps are made to connect the local diffusion path to vss . if the sub - page distance l is long enough to accommodate 1 vss tap for each selected bit line as depicted in the figure , the vss bounce ( or ground bounce ) will be minimized down to icell × rdiff . where icell is the cell current and rdiff is the diffusion resistance . if the sub - page distance is reduced to l / 4 , 1 vss tap is shared among 4 selected bit lines , the vss bounce increases differently for those 4 bit lines as depicted in fig2 b . therefore , an optimal value of l could be resulted from the trade off between the layout area penalty of vss taps and the vss bounce . referring to fig3 there is shown a schematic diagram of the interconnection of the bit lines bl 0 . . . bl 1023 from the memory array 12 ( shown in fig1 ) to the output of the device 10 . the 1024 bit lines from the memory array 12 are first supplied to bit line switches 44 . the 1024 bit lines supplied to the bit line switches 44 are reduced to 512 signal lines mblx ( x = 0 , 511 ). thus , each pair of adjacent bit lines blj and bl ( j + 1 ) are connected to a signal line mblx . the 512 signal lines mblx are supplied to a first column decoder 46 u . the first column decoder 46 u also receives the column signals yls ( 0 . . . 15 ). each 16 adjacent mbl signal lines is assigned to 1 xdl line . thus , the 512 mbl signal lines are decoded to 32 xdl lines . the first column decoder 46 u functions as a multiplexer / de - multiplexer in selecting one of 16 mbl lines to be connected to a single xdl line . each of the 32 xdl lines is supplied to a respective sensing circuit 36 u . thus , there are 32 sensing circuits 36 u in the first section 18 u of the page buffer 18 u / 18 l . since each sensing circuit 36 u is associated with 32 bit lines bl , the size ( width ) of each sensing circuit 36 u can be 32 times the pitch or size ( width ) of each memory cell . therefore , the sensing circuit 36 u can be very large compared to each memory cell . fig3 a is a schematic circuit diagram showing the bit - line pre - charge circuits 36 u - 8 / 36 u - 9 / 36 u - 10 . these pre - charge transistors are used to pre - charge the selected bit - lines to the predetermined voltage level biasp before starting the page - mode read operation . the pre - charge transistor is activated by the signal xdlpb . each sensing circuit 36 u has an output sdlbx ( 0 . . . 31 ). the 32 sdlb lines are supplied to a second column decoder 46 l which is also decoded by the column signals yls ( 0 . . . 15 ), and connect the 32 sdlb lines to 512 pdbx ( 0 . . . 511 ) lines . the second column decoder also functions s a multiplexer / de - multiplexer in connecting a single output of a qclt 36 u to one of selected 16 pdb lines . the 512 pdb lines are supplied to a plurality of latches 34 in the second section 18 l of the page buffer 18 u / 18 l , with one latch 34 associated with each of the 512 pdb lines . the 512 latches 34 are grouped into 32 sub - pages 36 l . each sub - page 36 l comprises 32 latches 34 with each latch 34 associated with a pdb line spaced apart from one another , all as discussed with reference to fig2 a . the output of the each latch 34 is connected to an output line pdx ( in reality the output line pdx is a pair of output lines , comprising pdx and pdx ( bar )). since there are 512 latches , there are 512 output lines pdx . 16 adjacent latches 34 and their associated output lines pd ( x , x + 15 ) are grouped together to form a group . in total there are 32 groups of output lines pdx . the 32 groups of output lines pdx are supplied to a third column decoder 38 , which also functions as a multiplexer / de - multiplexer . the third column decoder 38 selects one of the output lines pdx from each group 36 l , based upon the select signals yl 0 . . . yl 15 . thus , the third column decoder 38 selects 32 outputs , one from each group 36 lx , representing all of the outputs of the latches 34 from the same selected sub - page 18 - n . the 32 outputs of the third column decoder 38 are supplied to a pre - charge circuit 38 p , which outputs the 32 signals at nodes dlu 0 . . . dlu 15 , dlu 0 . . . dlu 15 . ( shown in fig3 b ) ( again , each line represents a pair of output lines .) the pre - charge transistors of the pre - charge circuit 38 p are used to pre - charge the intermediate nodes dlux before switching the third column decoders 38 . fig3 b is a schematic circuit diagram showing the dlux pre - charge circuits 38 p / 40 p . from the output of the pre - charge circuit 38 p , the signals dlu 0 . . . dlu 15 , dlu 0 . . . dlu 15 are supplied to the fourth column decoder 40 . the fourth column decoder 40 selects one of the output lines from the first group of 16 dlu signals , and one of the output lines from the second group of 16 dlu signals , based upon the select signals yu 0 . . . yu 15 . thus , the fourth column decoder 40 selects 2 outputs , with each being a pair of lines . the two outputs from the fourth column decoder 40 are supplied to a pre - charge circuit 40 p , which outputs the 2 signals at nodes dll 0 and dll 1 . the pre - charge transistors of the pre - charge circuit 40 p are used to pre - charge the intermediate nodes dllx before switching the fourth column decoders 40 . from the pre - charge circuit 40 p , the signals dll 0 and dll 1 are supplied to the fifth column decoder 42 , which selects one of the signals as the output dl ( a pair output lines : dl and dlb ), based upon the select signals z 0 and z 1 . the selected signal dl ( dl and dlb ) from the fifth column decoder 42 is supplied to the output buffer 48 . thus , through the action of the third , fourth and fifth column decoders 38 / 40 / 42 one signal ( both the signal and its complement ) stored in a latch 34 from a selected sub page 18 l - n is outputted from the device 10 . the pre - charge circuits 38 p / 40 p serve only to pre - charge certain nodes before the column decoders 38 / 40 / 42 are activated . since all these intermediate nodes dlux / dllx are loaded with large parasitic capacitance , any switching on the column decoders 38 / 40 / 42 will cause disturbance to the data latches 34 . to prevent this disturbance , all dlux / dllx nodes must be pre - charged to vcc − vtn before switching . fig3 c is a schematic circuit diagram showing in detail the output buffer 48 . the pair of output signals dl and dlb , representing the data and data inverse signals from the output of a latch from the selected page buffer 18 l , are supplied to a differential amplifier 48 sa . the output , dout , of the differential amplifier 48 sa , is supplied to a series of latches and is then supplied to a multiplexer / de - multiplexer 48 m . in the page mode of operation , this would be the path of the signal . however , the device 10 can also operate in a non - page mode , wherein the signal from a non - volatile memory cell is read out directly and not stored in the page buffer 18 l . in that event , the signal from the non - volatile memory cell along with the signal from a reference cell are supplied to a sense amplifier 48 na . the output of the sense amplifier 48 na is supplied to a series of latches and to another input to the multiplexer / de - multiplexer 48 m . the output of the multiplexer / de - multiplexer 48 m is supplied as the output of the device 10 . the latched signal , csaout , from the sense amplifier 48 na , is also supplied in a feedback manner to a feedback circuit 48 r , which is connected to the output lines dl and dlb , and is used in a read - modify - write mode during programming operation , which will be discussed greater detail hereinafter . referring to fig4 there is shown a detailed circuit diagram of the sensing circuit 36 u shown in fig3 . the sensing circuit or quick current level translators ( qclt ) 36 u receives data on the input line xdl and supplies its output to sdlb . each xdl is connected to a plurality of bit lines through the first column decoder 46 u . each sdlb is connected to a plurality of page latches 36 l through the second column decoder 46 l . page latches are connected to corresponding output buffers through the column decoders 38 / 40 / 42 . the qclt 36 u is a current - mode analog - to - digital converter that converts the input current signal at local data line xdl to binary codes and stores the codes in the q - latches 36 u - 2 shown in fig4 . the data stored in q - latches 36 u - 2 will be transferred to page latches 34 for clocking out . in the prior arts of page - mode non - volatile memory , current sensing devices are usually combined with data storage devices to form a complicated page buffer . this complicated page buffer is often found difficult to layout within the tight bit line pitch . at the same time , the tight pitch also limits the delicacy of the page buffer design . furthermore , in order to fit in the pitch , the current sensing devices are often made primitive . unlike the prior arts , in the present invention , the sensing devices ( qclt ) 36 u are completely separated from the data storage devices ( page latches 34 ). every 32 bit - lines share 1 qclt . the pitch for qclt is greater . with this design , the sensing device qclt can perform high precision current sensing while the page latch design can be made as simple as possible to fit in the tight pitch . fig4 is a schematic circuit diagram of the qclt 36 u . each qclt comprises a q latch 36 u - 2 , a current - mode comparator 36 u - 1 , a program driving circuit 36 u - 12 , a program verifying circuit 36 u - 13 , a pre - charging transistor 36 u - 10 , a pmos transistor in diode connection 36 u - 7 , a tri - state inverter 36 u - 3 , pass - gate transistors 36 u - 8 / 36 u - 9 / 36 u - 11 / 36 u - 4 / 36 u - 17 , a latch reset circuit 36 u - 6 , two latch preset circuits 36 u - 5 / 36 u - 14 , all as connected and as shown in fig4 . the operation of the qclt 36 u will be discussed hereinafter . fig4 a is a schematic circuit diagram of a page latch 34 . this page latch 34 is simply an sram cell . the program / read operation of the qclt 36 u is as follows : referring to fig4 b there is shown a detailed timing diagram of the read operation for the present invention . to perform the read operation , data node qd of the q latch 36 u - 2 is first reset to 0v by reset circuit 36 u - 6 . the selected bit line blx ( connected by xdl ) is pre - charged to biasl − vtn by pre - charge circuit 36 u - 10 . pmos transistor 36 u - 7 mirrors the cell current into the comparator 36 u - 1 . if the selected cell conducts no current , output vo of the comparator 36 u - 1 stays at 0v . if the selected cell conducts current higher than a pre - determined value , vo becomes vcc . the data at node vo is supplied to the preset circuit 36 u - 5 and when signal latrd is high , the data at node qd will be supplied to vcc . while latrd is high , inverter 36 u - 3 is tri - stated to avoid noise feeding back to the comparator 36 u - 1 . data node qd will be transferred to node pd of page latch 34 ( shown in fig4 a ) through data line sdlb by switching signal xtlat and pglat both to high . once data node qd becomes high after sensing , the pass gate transistor 36 u - 8 will be cut off and the comparator 36 u - 1 will be disconnected from the selected bit line xdl , and from the selected memory cell . by doing this , the selected memory cell will conduct no more current after sensing and the power consumption is greatly reduced . referring to fig4 c there is shown a detailed timing diagram for the programming operation for the present invention . before starting the program operation , all the page latches 34 are reset by signal rstpgb . then data to be programmed are loaded from io pads to the selected page latches 34 through the third column decoder 38 / 40 / 42 . since node sdlb of each qclt 36 u is connected to a plurality of page latches 34 , only one data from a page latch 34 can be uploaded to q latch 36 u - 2 for programming during one program iteration . to upload the selected page latch data , pglat and xtlat are switched to high and q latch 36 u - 2 is tri - stated by switching ph 2 to low ( ph 2 b to high ). next , signal pgmd turns on the pass gate transistor 36 u - 11 that connects the program driver circuit 36 u - 12 to local data line xdl . xdl is connected to the selected bit line through the first column decoder 46 u . depending the data stored in q latch 36 u - 2 , the selected bit line will be driven to either vcc − vtn or 0v . if the selected cell is to be programmed to higher threshold voltage than its original value , its bit line will be pulled down to 0v ( this is the program state ). if the threshold voltage of the selected cell is not to be modified , its bit line will be pulled up to vcc − vtn ( this is the program inhibit state ). referring to fig4 d there is shown a detailed timing diagram for the program verification operation for the present invention . the program verification operation is similar to the current sensing operation depicted in fig4 b except that data node qd of q latch 36 u - 2 is modified in a different way . in fig4 b , node qd will be flipped to 0v if the selected cell conducts current higher than a pre - determined value . in fig4 d , node qd will be flipped to vcc if the selected cell conducts no current . if the selected cell is successfully programmed , its threshold voltage will be higher than a pre - determined value and will conduct no more current under verification condition . once this no - current state is reached , node qd will be flipped to vcc and its corresponding bit line will be pulled up to vcc − vtn (“ program inhibit ” state ). each qdb is wired - nor to pvdt , as shown in fig4 e . if all qdb are high , pvdt will also become high . by checking pvdt , program iterations can be determined to be “ pass ” or “ fail ”. referring to fig4 f there is shown a detailed circuit diagram of the current - mode comparator 36 u - 1 . the comparator 36 u - 1 receives the input voltage line ( shown as vin in fig4 ) and the reference voltage vref ( shown as biasr in fig4 ), converting to current signals lin and iref respectively , and based upon the comparison generates an output voltage vout ( shown as vo in fig4 ). fig5 is a circuit block diagram showing various circuits for performing program and read operations according a preferred embodiment of the present invention . the device of the present invention is also capable of performing what is termed “ gapless read ” fig6 is a timing chart for performing a page - mode gapless read operation . fig7 is a flow chart for performing the page - mode read operation shown in fig6 . in a “ gapless read ” operation , the pre - charge transistors of 36 u - 10 ( shown in fig3 a ) are used to pre - charge the selected bit - lines to the pre - determined voltage level biasl − vtn before starting the page - mode read operation . the pre - charge transistor is activated by the signal xdlpb . the signal ylsx is a decoded signal which represents the selection of the particular sub - page 18 l - x . when the particular ylsx is activated , it pre - charges those 32 bit lines associated with sub - page 18 l - x . for example , if yls 0 is activated , then bit lines bl 0 , bl 16 , bl 32 , bl 48 , . . . , bl 496 are all pre - charged to biasl − vtn . to perform the page - mode read operation , the q latch 36 u - 2 is first reset by the latch reset circuit 36 u - 6 and the selected bit - line is pre - charged to the voltage level of biasl − vtn by bit - line pre - charge circuits 36 u - 10 . depending on the data stored in the selected memory cell , mbl ( or the bit line or column line ) will be driven to either one of the two binary voltage levels : high or low after bit - line pre - charging . the data stored in memory cells can be in one of two states : on or off . each state represents one of the binary data : 1 or 0 . if the selected memory cell is in an on condition , this cell will draw current to discharge mbl from pre - charged level of biasl − vtn down to 0v ( low level ). if the selected memory is in an off condition , this cell draws no current and mbl stays at the pre - charged level of biasl − vtn ( high level ). after the pre - charged bit - line reach electrical steady state , the data stored in the selected memory cell is translated into the corresponding voltage level on xdl . in the period shown as “ sense out sub - page ( 0 ) yls & lt ; 0 & gt ;” a particular sub - page x is selected . when the signal xdlpb goes low , the selected bit line is pre - charged . when yls & lt ; 0 & gt ; first goes high , reset of latch 36 u - 2 occurs by rstqclt being high , and the transistors in the first column decoder 46 u are turned on . the memory cells from the selected sub - page x are then read and stored in the associated latches 34 . in the next period shown as “ sense out sub - page ( 1 ) yls & lt ; 1 & gt ;” a second particular sub - page x + 1 is selected . the memory cells from the selected sub - page x + 1 are then read and stored in the associated latches 34 . in the next time period shown as “ clock out sub - page yl & lt ; 0 & gt ;” the data stored in the latches 34 associated with sub - page x is clocked out . in the next time period shown as “ clock out sub - page yl & lt ; 1 & gt ;” the data stored in the latches 34 associated with sub - page x + 1 is clocked out . at the same time , however , the data in the memory cells from a third particular sub - page x + 2 is selected . the memory cells from the selected sub - page x + 2 are then read and stored in the associated latches 34 . thereafter , in each time period , a read of the data from the latches 34 occurs while at the same time data from memory cells associated with another sub - page group is read and is stored in their associated latches . fig8 is a flow chart for performing the page - mode program operation related to fig4 c ˜ 4 d . this flow chart comprises 2 main loops . before starting the program operation , all the page latches must be reset to “ program inhibit ” state and a starting address must be input to the on - chip address counter . the starting address for programming will be latched by a first set of on - chip address registers . in loop 1 , bytes of data will be loaded into page latches sequentially . as the address counter increments , a second set of address registers store the latest address as the end address for programming . in loop 2 , consecutive sub - pages will be programmed successively . as stated above , 2 sets of address registers are used to store both the starting and end address for programming . therefore , in this loop , only those sub - pages that are previously loaded with data in loop 1 will be programmed . program verification is also embedded for each sub - page program in loop 2 . the circuits described heretofore can also be used to store multi - levels in a memory cell . in the following description , embodiments capable of performing multi - level page - mode read and program operation will be detailed . fig9 shows typical threshold voltage distribution of a multi - level cells in a flash memory array . the cell threshold voltage falls into one of 4 groups . two bits of binary codes are assigned to each group . in this figure , the group of lowest threshold voltage value is assigned state ‘ 11 ’ while the group of highest threshold voltage value is assigned state ‘ 00 ’. with this state assignment , two bits of binary data are mapped to 4 threshold voltage levels . hence , 2 - bit binary data could be stored in the form of four different threshold voltage levels . to manipulate the threshold voltage level , cells are first erased to their lowest threshold level ‘ 11 ’. then multi - step program iterations are used to boost up the threshold voltage incrementally until it reaches the desired level . to read a multi - level cell , a multi - step sensing operation is adopted to detect and convert the threshold voltage level into a two - bit binary code . during the multi - step sensing , a multi - level voltage source is applied to cong terminal . the variable voltage level applied to cong is used as reference to detect the threshold voltage . the detecting algorithm is commonly known as “ successive approach ”. at the beginning , cong is set to vcr 1 and sensing circuitry is turned on to detect whether the selected cell conducts current or not . if the cell conducts current , the threshold voltage belongs to group ‘ 11 ’. if the cell conducts no current , cong will be set to vcr 2 to sense a higher level . step by step , cong level is raised higher each time to sense higher threshold voltage level . once the threshold voltage level of the selected cell is found , the corresponding binary codes will be assigned and stored fig1 is a schematic view of a qclt 36 u modified from fig4 for multi - level read / program operation . the basic structure is mostly identical to the embodiment shown in fig4 except that the q latch related circuitry 36 u - 2 is duplicated , shown as 36 u - 2 h and 36 u - 2 l , and pattern - recognition circuitry ptr 36 u - 15 / 36 u - 16 h / 36 u - 16 l is added . fig1 a shows the page latches 34 for multi - level operation . fig1 b is a schematic circuit diagram of the pattern - recognition device ptr . the ptr circuit is used to selectively accept or reject some specific data paterns . the ptr circuit accepts only specific patterns of data loaded into q latches 36 u - 2 h / 36 u - 2 l before program iteration starts . if the data loaded into q latches 36 u - 2 h / 36 u - 2 l is not accepted by ptr , q latches 36 u - 2 h / 36 u - 2 l will be reset to “ program inhibit ” state . this pattern selection device could eliminate over - programming to those cells that need not to be programmed . the program / read operation of this multi - level qclt 36 is detailed below . refer to fig1 c ˜ 10 f for detail timing diagram of cell current sensing . the multi - level read operation is divided into 3 serial sections . in the first section , the inputs { qdh , qdl } of q latches 36 u are first reset to { 0 , 0 } state , respectively , by 36 u - 6 h / 36 u - 6 l . cong is connected to vcr 1 output of the multi - level voltage source and the selected bit line is pre - charged to biasl − vtn by 36 u - 10 . pmos transistor 36 u - 7 mirrors the cell current into the comparator 36 u - 1 . if the threshold voltage of the selected cell is higher than vcr 1 , vo of the comparator 36 u - 1 stays at 0v . otherwise , as shown in fig1 c , vo becomes vcc and the inputs { qdh , qdl } to q latches 36 u - 2 h / 36 u - 2 l will be flipped to { 1 , 1 } state when signal lat 11 ( supplied to 36 u - 5 h / 36 u - 5 l ) is high . while lat 11 is high , inverter 36 u - 3 h / 36 u - l is tri - stated to avoid noise feeding back to the comparator 36 u - 1 . once the inputs { qdh , qdl } to q latches 36 u - 2 h / 36 u - 2 l become { 1 , 1 } after sensing , pass gate transistor 36 u - 8 h / 36 u - 8 l will be cut off and the comparator 36 u - 1 will be disconnected from the selected memory cell . by doing this , the selected cell will conduct no more current after sensing and the data { qdh , qdl } is frozen during the rest of the sensing operation . in the second section , cong is raised to vcr 2 and the selected bit line is pre - charged . if threshold voltage of the selected cell is higher than vcr 2 , vo of the comparator 36 u - 1 stays at 0v . otherwise , as depicted in fig1 d , vo becomes vcc and inputs { qdh , qdl } to q latches 36 u - 2 h / 36 u - 2 l will be flipped to { 1 , 0 } state , respectively , when signal lat 10 is high . once inputs { qdh , qdl } become { 1 , 0 } after sensing , pass gate transistor 36 u - 8 h will be cut off . the data { qdh , qdl } is frozen during the rest of sensing operation . in the third section , cong is raised to vcr 3 and the selected bit line is pre - charged . if threshold voltage of the selected cell is higher than vcr 3 , vo of the comparator 36 u - 1 stays at 0v . otherwise , as depicted in fig1 e , vo becomes vcc and { qdh , qdl } will be flipped to { 0 , 1 } state when signal lat 01 is high . once { qdh , qdl } becomes { 0 , 1 } after sensing , pass gate transistor 36 u - 8 l will be cut off . the data { qdh , qdl } is frozen during the rest of sensing operation . if the threshold voltage of the selected cell is higher than vcr 3 , { qdh , qdl } stays at { 0 , 0 } state as depicted in fig1 f . data { qdh , qdl } will be transferred to node { pdh , pdl } of page latches 34 h / 34 l through local data line sdlb while signal xtlath / xlatl and pglath / pglatl become high . for programming a cell to multi - levels , refer to fig1 g ˜ 10 i for detail program timing diagram . before starting the program operation , all the page latches 34 are reset by signal rstpgb . then data to be programmed are loaded from io pads to the selected page latches 34 through the third column decoder 38 / 40 / 42 . since node sdlb of each qclt 36 u is connected to a plurality of page latches , only one { pdh , pdl } pair of those page latch data can be uploaded to { qdh , qdl } for programming during one program iteration . to upload the selected { pdh , pdl }, pglath / pglatl and xtlath / xlatl are switched to high and q latches 36 u - 2 h / 36 u - 2 l are tri - stated by switching ph 2 / ph 3 to low ( ph 2 b / ph 3 b to high ). after { qdh , qdl } is loaded , ptr 36 u - 15 is activated to check the data pattern of { qdh , qdl } by properly switching signal loadpatl , loadpatm , loadpath and patrec . different { qdh , qdl } patterns represent different threshold voltage levels to which the cells are about to be programmed . the multi - level program algorithm of the present invention will selectively accept specific { qdh , qdl } patterns according the target threshold voltage level . if the { qdh , qdl } pattern is not accepted by ptr , { qdh , qdl } will be set to “ program inhibit ” state (“ 11 ” state ) by 36 u - 16 h / 36 u - 16 l . for instance , as depicted in fig1 g , the target threshold voltage level is “ 10 ”. data pattern “ 10 ”, “ 01 ”, “ 00 ” will be accepted and data pattern “ 11 ” is “ program inhibit ” state . in fig1 h , the target level is “ 01 ”. data pattern “ 01 ” and “ 00 ” are accepted . pattern “ 10 ” is rejected because level 10 is lower than the target level and should not be over - programmed to level “ 01 ”. in fig1 i , the target level is “ 00 ”, data pattern “ 01 ”, “ 10 ” will be rejected to prevent over - programming to level “ 00 ”. next , signal pgmd turns on the pass gate transistor 36 u - 11 that connects the programming circuit 36 u - 12 to local data line xdl . xdl is connected to the selected bit line through the first column decoder 46 u . depending the { qdh , qdl } data stored in q latches , the selected bit line will be driven to either vcc − vtn or 0v . if the selected cell is about to be programmed to higher threshold voltage than its original value , its bit line will be pulled down to 0v . if the threshold voltage of the selected cell is not to be modified , its bit line will be pulled up to vcc − vtn . fig1 j is a timing diagram of multi - level program verification . the program verification operation is similar to the current sensing operation depicted in fig1 c except that data { qdh , qdl } is modified in a different way . cong is set to one of vcr 1 , vcr 2 or vcr 3 according the target threshold voltage level . { qdh , qdl } will be flipped to “ program inhibit ” state (“ 11 ” state ) if the selected cell conducts no current . if the selected cell is successfully programmed , its threshold voltage will be higher than the target level and will conduct no more current under verification condition . once this no - current state is reached , { qdh , qdl } will be flipped to “ 11 ” and its corresponding bit line will be pulled up to vcc − vtn (“ program inhibit ” state ). each qdhb / qdlb is wired - nor to pvdt . if all qdh / qdl become high , pvdt will also become high . by checking pvdt , program iterations can be determined to be “ pass ” or “ fail ”. fig1 k shows how the qdhb / qdlb nodes are wired to form a nor logic . fig1 is a flow chart for performing the multi - level page - mode program operation . this flow chart is mostly identical to fig8 except that an extra section of data pattern recognition algorithm is added to eliminate over - programming ( refer to ptr fig1 b ). fig1 a is another flow chart modified from fig1 . in this chart , the data pattern recognition algorithm is changed and new ptr depicted in fig1 b is used to replace ptr of fig1 b . in this new algorithm , only one specific pattern is accepted for each target threshold voltage level . for instance , if the target level is “ 10 ”, only pattern “ 10 ” will be accepted and all the other patterns will be rejected ( flipped to “ program inhibit ” state ). referring to fig1 b there is shown one embodiment of the ptr 36 u - 15 . the signal loadpatall is supplied to the gate of transistor 80 . transistor 80 connects the output signal hitb to node 98 . at node 98 there are 6 parallel branch paths : designated as a , b , c , d , e and f . the signal loadpatl is supplied to the gate of transistors 82 a , 82 b , and 82 c . the signal loadpatm is supplied to the gate of transistors 84 d and 84 e . the signal loadpath is supplied to the gate of transistor 86 f . the data signal qdh is supplied to the gate of transistor 88 c . the inverse of the signal qdh , qdhb is supplied to the gate of transistors 90 a , 90 b , 90 d , 90 e and 90 f . the signal qdl is supplied to the gate of transistor 92 b and 92 e . the inverse of the signal qdl , qdlb is supplied to the gate of transistors 94 a , 94 c , 94 d , and 94 f . as can be seen from fig1 b , all the transistors in the same current path ( a , b , c , d , e , or f ) are connected in series . thus , transistors 82 a , 90 a and 94 a are connected in series . similarly , transistors 82 b , 90 b , and 92 b are connected in series . although there is shown in fig1 b the designations “ 00 ”,“ 01 ”, and “ 10 ”. it should be noted that these are not inputs . rather they are comments showing when the states of { qdh , qdl } connect hitb to ground , as explained hereinbelow . in fig1 b , when loadpatall = 1 , then transistor 80 connects hitb to node 98 . further if loadpatl = 1 , and if qdhb =“ 1 ” and qdlb =“ 1 ”, then hitb will be connected to vss through transistors 82 a , 90 a , and 94 a . when qdhb =“ 1 ” and qdlb =“ 1 ”, then this means that the inverse of the signals or qdh and qdl are both “ 0 ”. thus hitb is connected to ground when { qdh , qdl } are in the state of { 0 , 0 }. similarly , if loadpatl = 1 , and { qdh , qdl } are in the state of { 0 , 1 }, then hitb is connected to ground through transistors 82 b , 90 b , and 92 b . if loadpatl = 1 , and { qdh , qdl } are in the state of { 1 , 0 }, then hitb is connected to ground through transistors 82 c , 88 c , and 94 c . the other three conditions when hitb is connected to ground occurs when loadpatm = 1 , and { qdh , qdl } are in the states of { 0 , 0 }; or when loadpatm = 1 , and { qdh , qdl } are in the states of { 0 , 1 }; or when loadpath = 1 , and { qdh , qdl } are in the states of { 0 , 0 }. once hitb = 0 , the data of { qdh , qdl } is accepted and will be programmed into memory cells . in contrast in fig1 b , when loadpatall = 1 , and loadpatl = 1 , if the states of { qdh , qdl } are “ 10 ”, hitb will become 0 . when loadpatall = 1 , loadpatm = 1 , if the states of { qdh , qdl } are “ 01 ”, hitb will become 0 . finally , when loadpatall = 1 , and loadpath = 1 , if the states of { qdh , qdl } are “ 00 ”, hitb will become 0 . once hitb = 0 , the data of { qdh , qdl } is accepted and will be programmed into memory cells . with reference to the algorithm of programming shown in fig1 , the ptr of fig1 b is adopted . when program level =“ 10 ”, loadpatall = 1 and loadpatl = 1 , hitb will be 0 if { qdh , qdl } equal to any one of “ 00 ”,“ 01 ”, or “ 10 ”. cells which are going to be programmed to three different levels “ 00 ”,“ 01 ”,“ 10 ” are first programmed to level “ 01 ” as shown in fig1 g . when program level =“ 01 ”, loadpatall = 1 , and loadpatm = 1 , hitb will be 0 if { qdh , qdl } equal to either one of “ 00 ” or “ 01 ”. if { qdh , qdl }=“ 10 ”, hitb will be 1 and { qdh , qdl } will be flipped to “ 11 ”. cells which are going to be programmed to two different level “ 00 ” or “ 01 ” are then programmed to level “ 01 ” as shown in fig1 h . when program level =“ 00 ”, loadpatall = 1 and loadpath = 1 , hitb will be 0 if { qdh , qdl } equal to “ 00 ”. if { qdh , qdl }=“ 01 ” or “ 10 ”, hitb will be 1 and { qdh , qdl } will be flipped to “ 11 ”. cells which are going to be programmed to level “ 00 ” are then programmed to level “ 00 ” as shown in fig1 i . in this algorithm , cells which are to be programmed to different levels (“ 00 ”,“ 01 ”,“ 10 ”) are programmed in such a manner that all those cells are first programmed to the lowest level ( in this case “ 10 ”) regardless of their individual target level . then , in the following program interval , cells are programmed to the middle level (“ 01 ”). during this program interval , cells targeted for level “ 10 ” will be selectively rejected by ptr device ( when hitb = 1 ). only cells with target level “ 00 ” and “ 01 ” will be programmed to level “ 01 ”. similarly , in the final program interval , only cells targeted for level “ 00 ” will be programmed to level “ 00 ”, while cells targeted for level “ 10 ” and “ 01 ” will be selectively rejected . the programming algorithm of fig1 a differs from that shown in fig1 only in the ptr device portion and the method of operation based upon this difference . in the programming algorithm shown in fig1 a , the ptr of fig1 b is adopted . when program level =“ 10 ”, loadpatall = 1 and loadpatl = 1 , hitb will be 0 only if { qdh , qdl } equal to “ 10 ”. cells which are going to be programmed to level “ 10 ” are programmed to level “ 01 ”. when program level =“ 01 ”, loadpatall = 1 , and loadpatm = 1 , hitb will be 0 only if { qdh , qdl } equal to “ 01 ”. cells which are going to be programmed to level “ 01 ” are then programmed to level “ 01 ”. when program level =“ 00 ”, loadpatall = 1 and loadpath = 1 , hitb will be 0 only if { qdh , qdl } equal to “ 00 ”. cells which are going to be programmed to level “ 00 ” are then programmed to level “ 00 ”. in this algorithm , cells which are to be programmed to different levels (“ 00 ”,“ 01 ”,“ 10 ”) are programmed in such a manner that cells of the same target level are programmed to their individual target level in one program interval . during program interval for level “ 10 ”, level “ 00 ” and “ 01 ” will be rejected ( hitb = 1 ). during program interval for level “ 01 ”, level “ 00 ” and “ 10 ” will be rejected . during program interval for level “ 00 ”, level “ 01 ” and “ 10 ” will be rejected . | 6 |
next , an embodiment of a surrounding environment recognition device of the invention will be described below with reference to the drawings . further , in the embodiment below , an example will be described in which the surrounding environment recognition device of the invention is applied to an in - vehicle environment recognition device mounted on a vehicle such as an automobile , but the invention is not limited to the in - vehicle environment recognition device . for example , the surrounding environment recognition device can be also applied to a construction machine , a robot , a monitoring camera , an agricultural machine , and the like . fig1 is a block diagram showing an internal function of the surrounding environment recognition device . an in - vehicle surrounding environment recognition device 10 of the embodiment is used to recognize a surrounding environment of a vehicle on the basis of an image obtained by capturing an external environment by an in - vehicle camera . the surrounding environment recognition device 10 includes an in - vehicle camera which captures an outside image of the vehicle and a recognition device which recognizes a surrounding environment on the basis of an image captured by the in - vehicle camera . however , the in - vehicle camera is not essentially necessary for the surrounding environment recognition device as long as only an outside image captured by the in - vehicle camera or the like can be acquired . the surrounding environment recognition device 10 includes , as illustrated in fig1 , an image capturing unit 100 , a lens state diagnosis unit 200 , a sensing range determination unit 300 , an application execution unit 400 , and a notification control unit 500 . the image capturing unit 100 captures a vehicle surrounding image acquired by , for example , in - vehicle cameras 101 ( see fig6 ) attached to front , rear , left , and right sides of a vehicle body ( an image acquisition unit ). the application execution unit 400 recognizes an object from the image acquired by the image capturing unit 100 and executes various applications for detecting a pedestrian or a vehicle ( hereinafter , referred to as an application ). the lens state diagnosis unit 200 diagnoses a lens state of each in - vehicle camera 101 on the basis of the image acquired by the image capturing unit 100 . the in - vehicle camera 101 includes an imaging element such as a cmos and a lens of an optical system disposed at the front side of the imaging element . further , the lens of the embodiment is not limited to a focus adjusting lens and generally also includes a glass of an optical system ( for example , a stain preventing filter lens or a polarizing lens ) disposed at the front side of the imaging element . the lens state diagnosis unit 200 diagnoses a stain caused by a particulate deposit , cloudness , or a water droplet of the lens . when the in - vehicle camera 101 is disposed , for example , outside the vehicle , there is concern that a particulate deposit of mud , trash , or bugs may adhere to the lens or the lens may become cloudy like obscure glass due to dust or a water stain . further , there is concern that the water droplet adheres to the lens so that the lens becomes dirty . when the lens of the in - vehicle camera 101 becomes dirty , a part or the entirety of a background captured in an image is hidden or a background image becomes dim due to low sharpness or becomes distorted . as a result , there is concern that the object may not be easily recognized . the sensing range determination unit 300 determines a sensing enabled range capable of recognizing a recognition object on the basis of the lens state diagnosed by the lens state diagnosis unit 200 . the sensing enabled range changes in response to a stain degree including a particulate deposit adhering position and a particulate deposit size with respect to the lens . also , the sensing enabled range also changes in response to the application executed by application execution unit 400 . for example , even when the lens stain degree and the distance from the lens to the object are the same , the sensing enabled range becomes wider when the recognition object of the application is a large object such as a vehicle compared to a small object such as a pedestrian . the notification control unit 500 executes a control that notifies at least one of the sensing enabled range and the sensing disabled range to a user on the basis of information from the sensing range determination unit 300 . the notification control unit 500 notifies a change in sensing enabled range to the user , for example , in such a manner that the sensing enabled range is displayed or a warning sound or a message is generated for the user by the use of an in - vehicle monitor or a warning device . in this way , the information can be provided for the vehicle control device in response to the sensing enabled range so that the vehicle control device can use the information for a vehicle control . fig6 is a schematic diagram showing an example of a system configuration of the vehicle and an entire configuration of the in - vehicle camera system . the surrounding environment recognition device 10 has an internal configuration of the image processing device 2 that executes an image process of the in - vehicle camera 101 and an internal function of the vehicle control device 3 that executes a vehicle control or a notification to a driver on the basis of a process result transmitted from the image processing device . the image processing device 2 includes , for example , the lens state diagnosis unit 200 , the sensing range determination unit 300 , and the application execution unit 400 and the vehicle control device 3 includes the notification control unit 500 . the vehicle 1 includes a plurality of in - vehicle cameras 101 , for example , four in - vehicle cameras 101 including a front camera 101 a capturing a front image of the vehicle 1 , a rear camera 101 b capturing a rear image thereof , a left camera 101 c capturing a left image thereof , and a right camera 101 d capturing a right image thereof . accordingly , the peripheral image of the vehicle 1 can be continuously captured . in addition , the in - vehicle camera 101 may not be provided at a plurality of positions , but may be provided at one position . further , only the front or rear image maybe captured instead of the peripheral image . the left and right in - vehicle cameras 101 may be configured as cameras attached to side mirrors or cameras installed instead of the side mirrors . the notification control unit 500 is a user interface and is mounted on hardware different from the image processing device 2 . the notification control unit 500 executes a control that realizes a preventive safety function or a convenience function by the use of a result obtained by the application execution unit 400 . fig7 is a diagram showing an example of a screen displayed on the in - vehicle monitor . from the past , there is known an overview display method of suggesting a sensing enabled range of an application obtained when a predetermined application is executed during a normal operation of the system while a distance space is viewed from the upside of an own vehicle ( the vehicle 1 ) to the in - vehicle monitor 700 . a minimum sensing line 701 in which an object closest to the vehicle 1 can be sensed ( recognized ) by a predetermined application is indicated by a small oval surrounding the periphery of the vehicle 1 and a maximum sensing line 702 in which an object farthest from the vehicle 1 can be sensed ( recognized ) by the same application is indicated by a large oval . when a space between the minimum sensing line 701 and the maximum sensing line 702 becomes a sensing range 704 and the lens is in a normal state without a stain , the entire sensing range 704 becomes the sensing enabled range . in addition , a reference numeral 703 indicated by the dashed line in the drawing indicates a part in which the image capturing ranges of the adjacent in - vehicle cameras overlap each other . the sensing range 704 is set in response to the application in execution . for example , when the object of the application is relatively large like the vehicle 1 , the maximum sensing line 702 and the minimum sensing line 701 respectively increase in size . further , when the object is relatively small like a pedestrian or the like , the maximum sensing line 702 and the minimum sensing line 701 respectively decrease in size . when a stain or the like exists on the lens of the in - vehicle camera 101 , it is difficult to detect a recognition object in a background part hidden by the stain or the like even within the sensing range 704 . as a result , there is concern for a performance deterioration state in which the application cannot exhibit predetermined performance . in the surrounding environment recognition device of the invention , a control of notifying the performance deterioration state of the application to the user is executed . as a notification method , for example , a method can be employed in which the sensing enabled range and the sensing disabled range of the sensing range 704 are visually displayed on the in - vehicle monitor or the like so that the performance deterioration state is accurately notified to the user . in this display method , a detectable distance from the vehicle 1 can be easily checked and a sensing ability deterioration degree caused by deterioration in performance can be easily suggested to the user . further , the performance deterioration state of the application may be notified to the user in such a manner that an led provided on a meter panel or the like inside a vehicle interior is turned on or a warning sound or a vibration is generated . fig8 is a diagram showing an example of a screen displayed on the in - vehicle monitor . an in - vehicle monitor 801 displays an image 802 captured by the in - vehicle camera 101 installed at the front part of the vehicle and also displays a sensing enabled region 803 and a sensing disabled region 804 to be displayed to overlap the image 802 . the image 802 includes a road r at the front side of the vehicle 1 and left and right white lines wl indicating a travel vehicle lane . by such a display , the sensing enabled region 803 set in response to the lens state can be notified to the driver while the lens state of the in - vehicle camera 101 ( see fig6 ) is viewed . then , since the sensing enabled region 803 and the lens state indicating , for example , a message that “ wiping is necessary since a far place is not visible in such a stain degree ” are viewed simultaneously , the sensing ability of the in - vehicle camera 101 can be easily notified to the driver . fig9 is a diagram showing an example of an image displayed on a front glass of the vehicle . here , a scene which is viewed from the vehicle interior through a front glass 901 by the use of a head up display ( hud ) overlaps a real world . since the sensing enabled region 803 or the sensing disabled region 804 are viewed while overlapping a road of the real world , the sensing enabled region or the sensing distance of the actual in - vehicle camera 101 can be easily and visually checked . here , since a projection type head up display for the front glass 901 shields a driver &# 39 ; s view , a display on the entire face of the front glass 901 is difficult . for this reason , as illustrated in fig9 the overlap display with the road using the lower side of the front glass 901 may be performed in such a manner that the sensing enabled region 803 is suggested to overlap the real world by the use of the overlap display at the upper side of the front glass 901 . next , the execution content of the lens state diagnosis unit 200 , the sensing range determination unit 300 , the application execution unit 400 , and the notification control unit 500 illustrated in fig1 will be described sequentially . fig2 is a block diagram showing an internal function of the lens state diagnosis unit 200 . the lens state diagnosis unit 200 includes a particulate deposit detector 210 , a sharpness detector 220 , and a water droplet detector 230 and diagnoses a stain state in accordance with the type of stain adhering to the lens of the in - vehicle camera 101 on the basis of the image acquired by the image capturing unit 100 . fig1 ( a ) to 10 ( c ) are diagrams showing a method of detecting a particulate deposit adhering to the lens . here , fig1 ( a ) shows an image 1001 at the front side of the in - vehicle camera 101 and fig1 ( b ) and 10 ( c ) show a method of detecting the particulate deposit . as illustrated in fig1 ( a ) , the image 1001 is dirty since a plurality of particulate deposits 1002 adhere to the lens . the particulate deposit detector 210 detects the particulate deposit adhering to the lens , for example , the particulate deposit 1002 such as mud shielding the appearance of the background . when the particulate deposit 1002 such as mud adheres to the lens , the background is not easily visible and the brightness is continuously low compared to the periphery . thus , it is possible to detect the particulate deposit 1002 by detecting a region having a small brightness change amount . first , the particulate deposit detector 210 divides an image region of the image 1001 into a plurality of blocks a ( x , y ) as illustrated in fig1 ( b ) . next , the brightness values of the pixels of the image 1001 are detected and a total sum i t ( x , y ) of the brightness values of the pixels included in the block a ( x , y ) is calculated for each block a ( x , y ). then , a difference δi ( x , y ) between the total sum i t ( x , y ) calculated for a captured image of a current frame and a total sum i t - 1 ( x , y ) calculated for a captured image of a previous frame is calculated for each block a ( x , y ). then , the block a ( x , y ) in which the difference δi ( x , v ) is smaller than those of the peripheral blocks is detected and a score sa ( x , y ) corresponding to the block a ( x , y ) is increased by a predetermined value , for example , “ 1 ”. the particulate deposit detector 210 calculates an elapse time ta from the initialization of the score sa ( x , y ) of each block a ( x , y ) after the above - described determination for all pixels of the image 1001 . then , a time average sa ( x , y )/ ta of the score sa ( x , y ) is calculated in such a manner that the score sa ( x , y ) of each block a ( x , y ) is divided by the elapse time ta . the particulate deposit detector 210 calculates a total sum of the time average sa ( x , y )/ ta of all blocks a ( x , y ) and divides the total sum by the number of all blocks of the captured image to calculate a score average sa_ave . when a stain 1002 such as mud continuously adheres to the lens of the in - vehicle camera 101 , the score average sa_ave increases in each of the sequentially captured frames . in other words , when the score average sa_ave is large , there is a high possibility that mud or the like adheres to the lens for a long period of time . it is determined whether the time average sa ( x , y )/ ta exceeds a predetermined threshold value . here , a region in which the time average exceeds the threshold value is determined as a region ( a particulate deposit region ) in which a background is not visible due to mud . this region is used to calculate the sensing enabled range of each application in response to the size of the region in which the time average exceeds the threshold value . further , a final determination is made for the operation of each application by the use of the score average sa_ave . fig1 ( c ) shows a score example in which all blocks are depicted as color gradation depending on the score . then , when the score is equal to or larger than a predetermined threshold value , a region 1012 is determined in which the background is not visible due to the particulate deposit . next , an operation of the sharpness detector 220 will be described with reference to fig1 ( a ) and 11 ( b ) . fig1 ( a ) and 11 ( b ) are diagrams showing a method of detecting the sharpness of the lens . the sharpness detector 220 detects the lens state on the basis of a sharpness index representing whether the lens is clear or unclear . a state where the lens is not clear indicates , for example , a state where a lens surface becomes cloudy due to the stain and a contrast becomes low . accordingly , an outline of an object is dimmed and the degree is indicated by the sharpness . as illustrated in fig1 ( a ) , the sharpness detector 220 sets a left upper detection region bg_l ( background left ), an upper detection region bg_t ( background top ), and a right upper detection region bg_r ( background right ) at a position where a horizontal line is reflected on the image 1001 . the upper detection region bg_t is set to a position including a horizontal line and a vanishing point where two lane marks wl are provided in parallel on the road intersect each other at a far position . the left upper detection region bg_l is set to the left side of the upper detection region bg_t and the right upper detection region bg_r is set to the right side of the upper detection region bg_t . the regions including the horizontal line are set so that edges are essentially included on the image . further , the sharpness detector sets a left lower detection region rd_l ( road left ) and a right lower detection region rd_r ( road right ) at a position where the lane mark wl is reflected on the image 1001 . the sharpness detector 220 executes an edge detection process on pixels within each region of the left upper detection region bg_l , the upper detection region bg_t , the right upper detection region bg_r , the left lower detection region rd_l , and the right lower detection region rd_r . in the edge detection for the left upper detection region bg_l , the upper detection region bg_t , and the right upper detection region bg_r , an edge such as a horizontal line is essentially detected . further , in the edge detection for the left lower detection region rd_l and the right lower detection region rd_r , the edge of the lane mark wl or the like is detected . the sharpness detector 220 calculates an edge strength value for each pixel included in the detection regions bg_l , bg_t , bg_r , rd_l , and rd_r . then , the sharpness detector 220 calculates an average value blave of the edge strength values of each of the detection regions bg_l , bg_t , bg_r , rd_l , and rd_r and determines a sharpness degree on the basis of the average value blave . as illustrated in fig1 ( b ) , the sharpness is set so that the lens is clear as the edge strength becomes strong and the lens nclear as the edge strength becomes weak . it is determined that the application recognition performance is influenced when the calculated average value blave is lower than standard sharpness . then , the application performance deterioration degree is determined for each application by the use of the sharpness average value for each region . when the sharpness is lower than minimal sharpness α2 , it is determined that the recognition in each application is difficult . fig1 ( a ) to 12 ( c ) are diagrams showing a method of detecting a water droplet adhering to the lens . the water droplet detector 230 of fig2 extracts a water droplet feature amount by comparing the brightness of the peripheral pixels on an imaging screen illustrated in fig1 ( a ) . the water droplet detector 230 sets pixels which are separated from an interest point by a predetermined distance ( for example , three pixels ) in the up direction , the right up direction , the right down direction , the left up direction , and the left down direction as inner reference points pi and sets pixels which are further separated therefrom by a predetermined distance ( for example , pixels more than three pixels ) in the five directions as outer reference points po . next , the water droplet detector 230 compares the brightness for each inner reference point pi and each outer reference point po . there is a high possibility that the vicinity of the inside of the edge of the water droplet 1202 is brighter than the outside due to a lens effect . here , the water droplet detector 230 determines whether the brightness of the inner reference point pi at the inside of the edge of the water droplet 1202 is higher than the brightness of the outer reference point po in each of five directions . in other words , the water droplet detector 230 determines whether the interest point is at the center of the water droplet 1202 . when the brightness of the inner reference point pi in each direction is higher than the brightness of the outer reference point po in the same direction , the water droplet detector 230 increases a score sb ( x , y ) of a region b ( x , y ) included in the interest point in fig1 ( b ) by a predetermined value , for example , “ 1 ”. as for the score of b ( x , y ), an instantaneous value at a predetermined time tb is stored and a past score stored for the time tb or more is discarded . the water droplet detector 230 executes the above - described determination for all pixels in a captured image . then , the water droplet detector obtains a total sum of the score sb ( x , y ) of each block b ( x , y ) for an elapse time tb , calculates a time average score sb ( x , y ) by dividing the total sum by the time tb , and calculates a score average sb_ave by dividing the time average score by the number of all blocks in the captured image . a degree in which the score sb ( x , y ) of each divided region exceeds a specific threshold value thrb is determined as a score . then , the divided region exceeding the threshold value and the score are depicted on a map as illustrated in fig1 ( c ) and a sum sb 2 of the scores on the map is calculated . when the water droplet continuously adheres to the lens of the in - vehicle camera 101 , the score average sb_ave for each frame increases . in other words , when the score average sb_ave is large , there is a high possibility that the water droplet adheres to the lens position . the water droplet detector 230 determines whether many water droplets adhere to the lens by the use of the score average sb_ave . the sum sb 2 is appropriate when the water droplet adhering amount on the lens is large and a failure determination on the entire system is made by the use of this value . in the determination of each logic , a separate water droplet occupying ratio is used to determine a maximal detection distance . both the water droplet adhering amount and the score average sb_ave are used in the determination for deterioration in performance of the recognition application due to the stain of the lens . the a method of calculating the sensing enabled range is considered . fig1 ( c ) shows a score example in which all blocks are depicted as color gradation depending on the score . then , when the score is equal to or larger than a predetermined threshold value , a region in which a background is not visible due to the water droplet is determined . fig3 is a diagram showing an internal function of the sensing range determination unit . the sensing range determination unit 300 includes a particulate deposit distance calculation unit 310 , a sharpness distance calculation unit 320 , and a water droplet distance calculation unit 330 and executes a process of determining the sensing enabled range by the use of a diagnosis result of the lens state diagnosis unit 200 . in the particulate deposit distance calculation unit 310 , a sensing enabled range capable of guaranteeing the detection of each application by the use of the detection result of the particulate deposit detector 210 is converted . in the sharpness distance calculation unit 320 , a sensing enabled range capable of guaranteeing the detection of each application by the use of the detection result of the sharpness detector 220 is converted . in the water droplet distance calculation unit 330 , a sensing enabled range capable of guaranteeing the detection of each application by the use of the detection result of the water droplet detector 230 is converted . the particulate deposit distance calculation unit 310 calculates the sensing enabled range in response to the detection result of the particulate deposit detector 210 . it is determined whether the time average sa ( x , y )/ ta exceeds a predetermined threshold value by the use of the result of the particulate deposit detector 210 . then , a region exceeding the threshold value is determined as a region in which a background is not visible due to mud . for example , as illustrated in fig1 - 1 ( a ), when a particulate deposit 1302 such as mud adheres to a left upper side of an image 1301 , it is determined that the time average sa ( x , y )/ ta corresponding to the region of the particulate deposit 1302 exceeds a predetermined threshold value . accordingly , as indicated by a dark region 1303 in fig1 - 1 ( b ), a region in which a background is not visible due to the particulate deposit 1302 is selected on the image . next , the sensing enabled range in this case is defined for each application . an important point herein is that the size of the recognition object in each application is different . first , an example for a pedestrian detection application will be described . as illustrated in fig1 - 2 ( a ) and 13 - 2 ( b ), a pedestrian p overlaps a region in which a background is not visible due to the particulate deposit 1302 . on the image , the size of the pedestrian p becomes different in response to a distance in the depth direction . since a percentage ( a ratio ) in which the particulate deposit 1302 shields the pedestrian p increases as the pedestrian p is located at a far position , it is difficult to guarantee a detection at a far position and a detection in the left direction of the front fish - eye camera . in the example illustrated in fig1 - 2 ( a ), a pedestrian is separated from an own vehicle by 6 . 0 m and most part of the pedestrian is hidden by the shade of the particulate deposit 1302 so that only a shape smaller than 40 % of the size of the pedestrian is visible . for this reason , the pedestrian detector 430 of the application execution unit 400 cannot recognize the pedestrian ( an unrecognizable state ). meanwhile , as illustrated in fig1 - 2 ( b ) when the pedestrian is separated from the own vehicle by 1 . 0 m , a shape equal to or larger than 40 % of the size of the pedestrian is visible . for this reason , the pedestrian detector 430 can recognize the pedestrian ( a recognizable state ). this process is executed for each depth distance z . as the pedestrian , a pedestrian having a body shape ( a standard size ) with a height of 1 . 8 m is supposed . then , the size of the pedestrian p on the image 1301 in appearance is calculated for each depth distance z from 1 m to 5 m . here , a maximal percentage of the pedestrian p hidden by the particulate deposit 1302 ( a ratio in which a recognition object having a standard size is hidden by a particulate deposit region ) is calculated by the comparison of the shape of the pedestrian p in each depth and a region part ( a particulate deposit region ) in which a background ot visible due to the particulate deposit 1302 such as mud . for example , a depth in which 30 % or more of the pedestrian p is not visible to maximal and a viewing angle θ from the camera 101 are calculated . fig1 - 3 ( a ) and 13 - 3 ( b ) illustrated examples in which a sensing disabled range 1331 incapable of recongnizing ( sensing ) the pedestrian and a sensing enabled range 1332 capable of recognizing ( sensing ) the pedestrian are displayed on a display unit 1330 such as an in - vehicle monitor . the sensing range determination unit 300 determines the sensing enabled range capable of sensing the pedestrian and the sensing disabled range incapable of sensing the pedestrian by the lens state diagnosed by the lens state diagnosis unit 200 when the application is executed . in the example illustrated in fig1 - 3 ( a ), the sensing disabled range 1331 is set such that the pedestrian farther than a predetermined distance 705 is not visible in response to the shape or the size of the particulate deposit . the predetermined distance 705 is set such that a position moves close to the vehicle 1 as the size of the particulate deposit becomes large and a position moves away from the vehicle 1 as the size of the particulate deposit becomes small . an angle θ determining the horizontal width of the sensing disabled range 1331 is set in response to the size of the particulate deposit . then , in the example of fig1 - 3 ( b ), particulate deposit adheres to the in - vehicle camera 101 a attached to the front part of the vehicle 1 . here , since there is a high possibility that a far position is not visible due to the influence of the particulate deposit , a position farther than the predetermined distance 705 of the image captured by the in - vehicle camera 101 installed at the front part of the vehicle cannot be used . a concept of a vehicle detection is similar to that of the pedestrian detection and a vehicle m corresponding to a recognition object has a width of 1 . 8 m and a depth of 4 . 7 m . then , a difference from the pedestrian p is that a direction of the vehicle m corresponding to the detection object is the same as a direction in which a lane is recognized or an own vehicle travels . a calculation is made on the assumption that the vehicle is a preceding vehicle or a preceding vehicle traveling on an adjacent vehicle lane in the same direction . for example , as illustrated in fig1 - 1 ( a ), a case in which a preceding vehicle m traveling on a lane wl overlaps the left upper particulate deposit 1302 will be examined in each depth . since the vehicle n is larger than the pedestrian p , it is possible to detect a position farther than the pedestrian p . here , when 40 % or more of the vehicle body is hidden , it is determined that the detection is not easily guaranteed . since the vehicle m is a rigid body compared to the pedestrian p and an artificial object , it is possible to guarantee the detection even when the hidden percentage ( ratio ) increases compared to the pedestrian p . for example , as illustrated in fig1 - 2 ( a ) and 14 - 2 ( b ), since the percentage in which the particulate deposit 1302 shields the vehicle m increases as the vehicle m is located at a far position , it is difficult to guarantee a detection at a far position and a detection in the front direction of the front fish - eye camera . in the example illustrated in fig1 - 2 ( a ), since the preceding vehicle is separated from the own vehicle by 7 . 0 m , a vehicle detector 420 cannot recognize the vehicle ( an unrecognizable state ). further , in the example illustrated in fig1 - 2 ( b ), since the preceding vehicle is separated from the own vehicle by 3 . 0 m , the vehicle detector 420 can recognize the vehicle ( a recognizable state ). a basic concept of a lane recognition is similar to that of the pedestrian detection or the vehicle detection . a difference is that a size of the recognition object is not set . however , it is important that , since the lane wl is recognized from a far position of 10 m to the vicinity of 50 cm , an invisible range from a certain meter position to a certain meter position is detected . then , it is determined whether a stain region on a screen is hidden in a certain range on the road by the use of the geometry of the camera . in the case of a white line ( the lane wl ), the right recognition performance using parallelism is influenced when a far left side is not visible . for this reason , when it is determined that a left position farther than 5 m is not visible , it is determined that a far right side of the white line cannot be recognized due to the same performance . even in an actual image process , an erroneous detection may be reduced by an image process excluding a position farther than 5 m . alternatively , only the stain region maybe excluded from the sensing region . while a detection guarantee range is suggested , it is determined whether the detection guarantee range can be used for a control , can be used for a warning instead of a control , or cannot be used for any purpose in consideration of the accuracy of the horizontal position , the yaw angle , and the curvature of the lane recognition deteriorating as a detection guarantee region becomes narrow . a parking frame exists on the road as in the white line , but an approximate size of an object can be regarded as a given size differently from the white line . of course , there is a slight difference in the size of the parking frame depending on a place . however , for example , a parking frame having a width of 2 . 2 m and a depth of 5 m is defined and the possibility of the hidden percentage inside the frame of the region is calculated . in fact , since only a frame line is important , the parking frame can be detected even when only the inside of the frame becomes dirty due to mud . however , when the parking frame is not visible due to the movement of the vehicle , the performance of the application cannot be guaranteed . thus , the possibility of the hidden percentage inside the frame due to mud is calculated . when the percentage exceeds 30 %, an operation cannot be guaranteed . this calculation is also executed for each depth . further , the application using the parking frame is used for a parking assist in many cases while the vehicle is turned . for this reason , even when 30 % or more of mud adheres to a position farther than 7 m at the left side of the front camera in the depth direction , a range capable of guaranteeing the application is defined as the vicinity within 7 m in the front camera . in a barrier detection , all three - dimensional objects existing around the vehicle are defined as detection objects and thus the size of the detection object cannot be defined . for this reason , in the barrier detection , a case in which a foot of a three - dimensional object existing on the road cannot be specified is defined as a case in which the barrier detection performance cannot be guaranteed . for this reason , a basic concept is supposed on the assumption that a road region having a certain size is reflected on a mud detection region . then , an invisible distance due to a shielding ratio increasing at a certain range from the own vehicle is obtained by conversion and thus the barrier detection performance guarantee range is determined . for example , as illustrated in fig1 ( a ) , when the particulate deposit 1302 adheres to the lens so that a region in which an arrow in the up direction is not visible exist , this region can be determined as a region in which a background is not visible due to the particulate deposit , that is , a sensing disabled range 1303 can be determined as illustrated in fig1 ( b ) . in this way , in the vehicle detection or the pedestrian detection capable of assuming the approximate three - dimensional size of the detection object corresponding to the three - dimensional object , the three - dimensional object having a certain size and corresponding to the detection object is assumed and a percentage in which the three - dimensional object is shielded by a certain degree of a stain on the image is calculated when the three - dimensional position is changed in the depth direction on the road and the horizontal direction perpendicular thereto . here , an unrecognizable three - dimensional position is determined when the percentage shielded by the particulate deposit exceeds a threshold value and a recognizable three - dimensional position is determined when the percentage does not exceed the threshold value . in this way , when the durable shielding ratio of the object in each application illustrated in fig1 is calculated in the particulate deposit state , a position where a detection object detection rate decreases is estimated as a three - dimensional region based on the own vehicle . here , when the object size is not defined as in the barrier detection , a certain size at a foot position is assumed and the visible state of the region may be determined instead . fig1 is a table showing a durable shielding ratio and a standard size of the recognition object of the application . here , the durable shielding ratio indicates a state where the recognition object can be recognized when the size of the particulate deposit on the image is smaller than the size of the recognition object by a certain percentage . for example , when the particulate deposit is 50 % or less of the size of the vehicle in the vehicle detection , the vehicle can be recognized . further , when the particulate deposit is 40 % or less of the size of the pedestrian in the pedestrian detection , the vehicle can be recognized . in this way , when the sensing enabled range of the camera is estimated in the three - dimensional region on the image , the sensing enabled range changing in response to the lens state of the camera can be easily notified to the user . in the sharpness distance calculation unit 320 illustrated in fig3 , a guaranteed detection distance is calculated on the basis of the average value blave of the sharpness obtained by the sharpness detector 220 . first , standard sharpness α1 of the lens sharpness necessary for obtaining the edge strength used to recognize the recognition object to the maximal detection distance in each application is set . fig1 ( a ) is a diagram showing a relation between the maximal detection distance and the edge strength of each application . then , when the sharpness is equal to or larger than the standard sharpness α1 , each application can guarantee a sensing operation to the maximal detection distance . however , the guaranteed detection distance from the maximal detection distance becomes shorter as the sharpness becomes lower than the standard sharpness α1 . the sharpness distance calculation unit 320 shortens the guaranteed detection distance as the sharpness decreases from the standard sharpness α1 . fig1 ( b ) is a graph showing a relation between a detection distance and sharpness . here , when the sharpness blave exists between the standard sharpness al and the minimal sharpness α2 , the guaranteed detection distance of the application changes . regarding the setting of each application , as illustrated in the table of fig1 ( a ) , when the maximal detection distance of each application exists and a range of the maximal detection distance is guaranteed , the standard sharpness α1 or more set for each application needs to be indicated by the average value blave of the sharpness . as the average value blave of the sharpness decreases from the standard sharpness α1 , the guaranteed detection distance decreases . when the sharpness reaches the minimal sharpness α2 of the target application , the detection is not available . for example , when the application is for the vehicle detection , the maximal detection distance becomes 10 m when the standard sharpness is 0 . 4 and the minimal detection distance becomes 0 m when the minimal sharpness is 0 . 15 . then , when the application is for the pedestrian detection , the maximal detection distance becomes 5 m when the standard sharpness is 0 . 5 and the minimal detection distance becomes 0 m when the minimal sharpness is 0 . 2 . fig1 ( a ) and 17 ( b ) are diagrams showing a method of determining the sensing enabled range by the sensing range determination unit 300 in response to the sharpness . fig1 ( a ) shows an example in which the low sharpness state is displayed on the in - vehicle monitor and fig1 ( b ) shows an example in which the sensing disabled range 1331 incapable of recognizing ( sensing ) the pedestrian and the sensing enabled range 1332 capable of recognizing ( sensing ) the pedestrian are displayed on the display unit 1330 such as an in - vehicle monitor . for example , when the sharpness is low due to cloudness as illustrated in fig1 ( a ) , there is a high possibility that a far position is not visible . for this reason , as illustrated in fig1 ( b ) it is defined that a position farther than the predetermined distance 705 in the image captured by the in - vehicle camera 101 installed at the front part of the vehicle cannot used . the predetermined distance 705 is set such that a position moves close to the vehicle 1 as the sharpness becomes closer to the minimal sharpness and a position moves away from the vehicle 1 as the sharpness becomes closer to the standard sharpness . in the water droplet distance calculation unit 330 illustrated in fig3 , the sensing enabled range for each application is calculated on the basis of the result of the water droplet detector 230 . a region within a process region of each application and having a score sb ( x , y ) exceeding the threshold value thrb is calculated on the basis of the threshold value thrb and the score sb ( x , y ) obtained as a result of the water droplet detection . since this is obtained as a numerical value indicating the amount of the water droplet within the process region of each application , the water droplet occupying ratio is obtained for each application ( each recognition application ) in such a manner that an area of a water droplet adhering region ( an area of a water droplet region corresponding to a region in which the water droplet adheres ) within the process region of the application is divided by an area of the process region . by using the water droplet occupying ratio , the maximal detection distance is determined . as illustrated in fig1 ( a ) , there is a high possibility that the lens state promptly changes in the case of a water droplet 1902 . for example , the lens state may change due to the water droplet of falling rain or from the road or the water droplet amount may be reduced due to the opposite traveling wind or the heat generated during the activation of the camera . likewise , there is a high possibility that the lens state may change at all times . for this reason , it is possible to prevent a determination that the position 1903 is in a region which is out of a viewing angle or cannot be detected due to the position of the current water droplet . in the lens state involving with the current water droplet adhering amount , a far position or a small object position cannot be correctly determined . accordingly , an operation depending on the lens state is guaranteed in such a manner that the detection distance is set to be short . since the process region is different for each application , the water droplet distance calculation unit 330 calculates the guaranteed detection distance from the water droplet occupying ratio obtained in consideration of the process region . further , the water droplet occupying ratio capable of guaranteeing the maximal detection distance of the application from the value of the water droplet occupying ratio is set as the durable water droplet occupying ratio illustrated in fig2 ( a ) . further , the water droplet occupying ratio incapable of guaranteeing the detection and the operation of the application is set as the limited water droplet occupying ratio . the limited water droplet occupying ratio state indicates a state where the guaranteed detection distance is 0 m . here , the guaranteed detection distance from the durable water droplet occupying ratio to the limited water droplet occupying ratio decreases linearly as illustrated in fig2 ( b ) . the image of the background is not easily visible when the water droplet adheres to the lens . thus , the image may be erroneously detected or may not be detected for an image recognition logic as the water droplet adhering amount on the lens increases . for this reason , since the water droplet adhering amount within the range of the image process for recognizing the recognition object among the water droplets adhering to the lens is obtained , the water droplet adhering amount is used while being converted to a degree causing an erroneous detection or a non - detection in each application ( water droplet durability ). for example , when the water droplet occupying ratio within the process region of the lane recognition is high , a large water droplet amount exists in the region where a lane exists on the image . accordingly , there is a possibility that the lane cannot be appropriately recognized . here , as for the detection of a far position which can be easily influenced by the distortion of the water droplet , the guaranteed target is not ensured at a level in which the water droplet occupying ratio is slightly raised and the guaranteed target is not ensured even in a near distance in response to an increase in water droplet occupying ratio . for example , even when the application in execution is the vehicle detection , the maximal detection distance of 10 m can be guaranteed until the water droplet occupying ratio becomes 35 % or less of the durable water droplet occupying ratio 35 %. here , when the water droplet occupying ratio becomes larger than 60 % of the limited water droplet occupying ratio , the minimal detection distance becomes 0 m . then , when the application is the pedestrian detection , the maximal detection distance of 5 m can be guaranteed when the water droplet occupying ratio becomes 30 % of the durable water droplet occupying ratio . then , the minimal detection distance becomes 0 m when the water droplet occupying ratio becomes larger than 50 % of the limited water droplet occupying ratio . fig4 is a block diagram showing an internal function of the application execution unit 400 . the application execution unit 400 includes , for example , a lane recognition unit 410 , a vehicle detector 420 , a pedestrian detector 430 , a parking frame detector 440 , and a barrier detector 450 to be executed on the basis of a predetermined condition . the application execution unit 400 executes various applications used for recognizing the image in order to improve the preventive safety or the convenience by using the image captured by the in - vehicle camera 101 as an input . the lane recognition unit 410 executes , for example , the lane recognition used to warn or prevent a vehicle lane departure , to conduct a vehicle lane keep assist , and to conduct a deceleration before a curve . in the lane recognition unit 410 , a feature amount of the white line wl is extracted from the image and the linear property or the curved property of the feature amount is evaluated in order to determine whether the own vehicle exists at a certain horizontal position within the vehicle lane or to estimate a yaw angle representing an inclination with respect to the vehicle lane and a curvature of a travel vehicle lane . then , when there is a possibility that the own vehicle may depart from the vehicle lane in response to the vehicle horizontal position , the yaw angle , or the curvature , an alarm for warning the risk to the driver is generated . alternatively , when there is a possibility that the vehicle lane departure may occur , a control of returning the own vehicle to the own vehicle lane in order to prevent the departure is executed . here , when the vehicle is controlled , there is a need to stabilize the vehicle lane recognition performance and to highly accurately obtain the horizontal position and the yaw angle . further , when the vehicle lane to a far position can be extracted with high accuracy , an assist may be executed which has high curvature estimation accuracy , can be used for a control on a curve , and can support a smooth curve travel operation . the vehicle detector 420 extracts a square shape on the image of the rear face of the preceding vehicle as a feature amount in order to extract a vehicle candidate . it is determined that the candidate is not a stationary object by checking whether the candidate moves on the screen at the own vehicle speed differently from the background . further , the candidate may be narrowed by the pattern matching for a candidate region . in this way , when the vehicle candidate is narrowed to estimate the relative position with respect to the own vehicle , it is determined whether the own vehicle may contact or collide with the vehicle candidate . accordingly , it is determined whether the vehicle candidate becomes a warning target or a control target . in the application used to follow the preceding vehicle , an automatic following operation with respect to the preceding vehicle is executed by the control of the own vehicle speed in response to the relative distance of the preceding vehicle . the pedestrian detector 430 narrows a pedestrian candidate by extracting a feature amount based on a head shape or a leg shape of a pedestrian . further , a moving pedestrian is detected on the basis of a determination reference indicating a state whether the pedestrian candidate moves in a collision direction by the use of a comparison of a movement of a background of a stationary object moving along with the movement of the own vehicle . by the pattern matching , the stationary pedestrian may be also used as a target . in this way , when the pedestrian is detected , it is possible to execute a warning or control process depending on whether the pedestrian jumps into the own vehicle lane . further , it is possible to obtain an application which is very helpful for a low - speed region such as a parking place or an intersection instead of a road travel state . the parking frame detector 440 extracts a white line feature amount similarly to the white line recognition when the vehicle travels at a low speed , for example , 20 km or less . next , all lines having different inclination degrees and existing on the screen are extracted by hough transformation . further , a parking frame is checked to assist the driver &# 39 ; s parking operation instead of searching for a simple white line . it is checked whether the horizontal width of the parking frame is a width in which the vehicle 1 needs to be stopped or the vehicle 1 can be parked in a parking region by detecting a bumper block or a white line at the front or rear side of the vehicle 1 . when the parking frame is visible to a far position in a wide parking lot , the user can select a suitable parking frame from a plurality of parking frame candidates . however , only when a near parking frame is visible , the user needs to approach a near parking space in order to recognize the parking frame . further , since the recognition is basically used for the parking control of the vehicle 1 , the user is informed of the non - control state when the recognition is not stable . the barrier detector 450 extracts a feature point on an image . the feature point having an original feature on an image including an angle for an object may be considered as a feature point having the same feature when a change on the image is small even at the next frame . by the use of the feature points between two frames or multiple frames , a three - dimensional restoration is executed . at this time , a barrier which may collide with the own vehicle is detected . fig5 is a block diagram showing an internal function of the notification control unit 500 . the notification control unit 500 includes , for example , a warning unit 510 , a control unit 520 , a display unit 530 , a stain removing unit 540 , an led display unit 550 , and the like . the notification control unit 500 is an interface unit that receives the determination result of the sensing range determination unit 300 and transmits the information to the user . for example , in a normal state where a sensing disabled range does not exist in a sensing range necessary for the application and the entire sensing range becomes a sensing enabled range , a green led is turned on . then , a green led is turned on and off in a suppression mode . then , in a system give - up state having a temporary possibility of an early return due to a rain or the like , an orange led is turned on . meanwhile , in a system give - up state having a low possibility of a return unless the lens is wiped by the user due to a durable stain such as mud or cloudness on the lens , a red led is turned on . in this way , a system configuration is obtained in order to warn a current preventive safety application operation state and an abnormal state caused by the stain of the lens of a current system to the user . in addition , the system give - up state indicates a state where an application for recognizing a recognition object is stopped for the preventive safety when it is determined that an image suitable for an image recognition cannot be captured due to the particulate deposit on the lens surface . further , the system give - up state indicates a state where a can output is stopped even when the recognition is not stopped or a warning corresponding to a final output or a recognition object recognition result is not transmitted to the user during a vehicle control or a display on a screen or even when a can output is generated . in the system give - up state , the give - up state of the recognition system may be notified to the user through a display or a voice while the recognition object recognition result is not notified to the user . in addition , when the preventive safety application is temporarily changed to the system give - up state , this transition state may be notified to the user through a display for warning the stop of the preventive safety application or a voice for warning the stop of the preventive safety application while not disturbing the driving operation of the driver . in this way , a function of notifying the transition of the application of the lane recognition or the vehicle detection to the stop state to the user may be provided . further , a return state may be notified to the user through a display or a voice . further , in a situation in which visibility is not improved by a road structure tracking unit although the lens state is improved when it is determined that a durable stain adheres to the lens , the lens may be improved after an orange display is selected as a failure display in a durable give - up state . in fact , there is also a possibility influenced by the light source or the background . further , when it is determined that a durable stain other than a water droplet adheres to the lens so that a particularly red led is turned on , an instruction may be given to the user so that the lens is wiped by the user when the vehicle is stopped or before the vehicle starts to travel . since the user is informed of the application operation state based on the lens state diagnosed by the lens state diagnosis unit 200 and the sensing enabled range determined by the sensing range determination unit 300 , it is possible to prevent a problem in which a preventive safety function is stopped without a notice to the user . when the user is informed of the current system state so that the user does not doubt the failure of the system and the vehicle lane departure is warned to the user during the operation of the vehicle lane recognition , an improvement treatment method using a lens wiping and clearing hardware is notified to the user . when a situation is not easily improved unless the user removes the stain of the lens surface in the system give - up state caused by the stain of the lens , this state is notified to the user . accordingly , a further improvement request is notified to the user and a non - operation state of a current application is notified to the user . fig2 is a diagram comparing the sensing enabled range in response to the recognition object . when the particulate deposit adhering to the front in - vehicle camera 101 has the same size and position and the recognition object of the application corresponds to three kinds of recognition objects , that is , a vehicle , a pedestrian , and a barrier , the size of the recognition object is different in each application and thus the sensing range is also different . for example , when the recognition object is the vehicle , a forward vehicle length la 2 of a minimum sensing range 2101 and a forward vehicle length la 1 of a maximum sensing range 2102 are longer than a forward vehicle length lp 2 of a minimum sensing range 2111 and a forward vehicle length lp 1 of a maximum sensing range 2112 of the pedestrian and a forward vehicle length lm 2 of a minimum sensing range 2121 and a forward vehicle length lm 1 of a maximum sensing range 2122 of the barrier are smaller than the forward vehicle length lp 2 of the minimum sensing range 2111 and the forward vehicle length lp 1 of the maximum sensing range 2112 of the pedestrian . meanwhile , an angle θ in which a background is hidden by the particulate deposit is substantially the same among the applications , but is corrected in response to the size of the recognition object . according to the surrounding environment recognition device 10 of the invention , it is possible to notify the sensing enabled range set in response to the stain of the lens of the in - vehicle camera 101 to the user and to allow the user to check a range capable of recognizing the recognition object of the application . thus , it is possible to allow the user to drive the vehicle while further keeping an eye on the surrounding environment by preventing a careless attention on the surrounding environment due to the overestimation of the application . while the embodiment of the invention has been described , the invention is not limited to the above - described embodiment and various modifications in design can be made without departing from the spirit of the invention of claims . for example , the above - described embodiment has been carefully explained for the easy comprehension of the invention and all configurations may not be essentially provided . further , a part of a configuration of a certain embodiment may be replaced as a configuration of the other embodiment and a configuration of the other embodiment may be added to a configuration of a certain embodiment . furthermore , the other configurations may be added to , deleted from , or replaced by a part of a configuration of each embodiment . | 6 |
the b lymphocyte donor is selected from anti - rh ( d ) donors undergoing plasmapheresis , based on the activity of his or her anti - rh ( d ) serum antibodies in the adcc activity assay described in § 33 . after a whole blood donation , in 1998 , the “ buffy coat ” fraction ( leukocyte concentrate ) was recovered . the peripheral blood mononuclear cells are separated from the other elements by centrifugation on ficoll plus ( pharmacia ). they are then diluted to 10 6 cell / ml in imdm containing 20 % ( v / v ) of fetal calf serum ( fcs ), to which 20 % of culture supernatant of the b95 - 8 line ( atcc - crl1612 ), 0 . 1 μg / ml of cyclosporin a ( sandoz ), 50 μg / ml of gentamycin sulfate ( life technologies ) are added , and distributed into round - bottomed 96 - well plates or 24 - well plates ( p24 greiner ). they are then placed in an incubator at 37 ° c ., 7 % co 2 . after 3 weeks , the presence of anti - rh ( d ) antibodies is sought by adcc . each one of the 16 microwells of a positive p24 plate well is transferred into a new p24 well . this enrichment is repeated after 10 to 15 days of culturing and each microwell is amplified in a p96 and then in a p24 . the positive p96 wells are taken up and amplified in a flat - bottomed p24 ( nunc ). after a few days of culturing , the presence of anti - rh ( d ) antibodies is sought by adcc . the cells derived from one or more p24 wells are enriched in specific cells by the formation and separation of rosettes with papain - treated rh ( d )- positive red blood cells : one volume of red blood cells washed in 0 . 9 % nacl is incubated for 10 minutes at 37 ° c . with 1 volume of papain ( merck ) solution at 1 / 1 000th ( m / v ), and then washed 3 times in 0 . 9 % nacl . the cells were then washed once in hanks solution , suspended in fcs and mixed with the papain - treated red blood cells in a ratio of 1 cell to 33 red blood cells . the mixture is placed in a cone - bottomed centrifuged tube , centrifuged for 5 minutes at 80 g and incubated for one hour in melting ice . the mixture is then carefully agitated and ficoll is deposited at the bottom of the tube for separation at 900 g for 20 minutes . the pellet containing the rosettes is hemolyzed in a solution of nh 4 cl for 5 minutes and the cells are placed in culture again in a p24 containing irradiated human mononuclear cells . after approximately 1 week , the supernatants are evaluated in cela ( paragraph 3 . 2 ) and adcc assays for the presence of anti - rh ( d ) antibodies having good activity . a further cycle of enrichment is carried out if the percentage of cells forming rosettes significantly increases compared to the preceding cycle . the ir - enriched cells are distributed at 5 and 0 . 5 cells per well in round - bottomed 96 - well plates containing irradiated human mononuclear cells . after approximately 4 weeks of culturing , the supernatants from the wells containing cell aggregates are evaluated by adcc assay . the wells from cloning the ebv - transformed cells exhibiting an advantageous adcc activity are amplified in culture and then fused with the heteromyeloma k6h6 - b5 ( atcc crl - 1823 ) according to the standard peg technique . after fusion , the cells are distributed , in a proportion of 2 × 10 4 cells / well , into flat - bottomed p96s containing murine intraperitoneal macrophages and in a selective medium containing aminopterin and ouabain ( sigma ). after 3 to 4 weeks of culturing , the supernatants of the wells containing cell aggregates are evaluated by adcc assay . cloning by limiting dilution is carried out at 4 , 2 and 1 cell / well in flat - bottomed p96s . after 2 weeks , the microscopic appearance of the wells is examined in order to identify the single clones , and the medium is then renewed . after approximately 2 weeks , the supernatants of the wells containing cell aggregates are evaluated by adcc assay . ebv transformation of the cells of donor d13 made it possible to select a well , designated t125 2a2 , on which the following were successively carried out : 2 enrichments , 3 cycles of ir , and cloning at 5 cells / well to give 2 clones : 1 ) t125 2a2 ( 5 / 1 ) a2 from which the dna was extracted in order to prepare the recombinant vector ; 2 ) t125 ( 5 / 1 ) a2 which was fused with k6h6 - b5 to give f60 2f6 and then , after 5 rounds of cloning , f60 2f6 ( 5 ) 4c4 , a clone selected for constituting a cell stock prior to preparing libraries . a line producing an igg3 was prepared according to the same method as that used to prepare the antibody of igg1 isotype . the cells of origin originate from a donation of whole blood , from a designated donor , from which the “ buffy coat ” fraction ( leukocyte concentrate ) was recovered . after purification by affinity chromatography on protein a sepharose ( pharmacia ) and dialysis in 25 mm tris buffer , 150 mm nacl , ph 7 . 4 , the concentration of the antibody t125 is determined by the elisa technique . the biological activity in vitro is then measured by the adcc technique . coating : anti - igg ( calbiochem ) at 2 μg / ml in 0 . 05m carbonate buffer , ph 9 . 5 , overnight at 4 ° c . saturation : dilution buffer ( pbs + 1 % bsa + 0 . 05 % tween 20 , ph 7 . 2 ), 1 h at ambient temperature . washing ( to be renewed at each step ): h 2 o + 150 mm nacl + 0 . 05 % tween 20 . dilution of the samples , in dilution buffer to approximately 100 ng / ml and of the control range made up of lfb polyvalent human iggs prediluted to 100 ng / ml . incubation for 2 h at ambient temperature . conjugate : anti - igg ( diagnostic pasteur ) diluted to 1 / 5 000 , 2 hours at ambient temperature . substrate : opd at 0 . 5 mg / ml ( sigma ) in phosphate - citrate buffer containing sodium perborate ( sigma ), 10 minutes in the dark . reaction stopped with 1n hcl , and read at 492 nm . coating : anti - kappa ( caltag lab ) at 5 μg / ml in 0 . 05m carbonate buffer , ph 9 . 5 , overnight at 4 ° c . saturation : dilution buffer ( pbs + 1 % bsa + 0 . 05 % tween 20 , ph 7 . 2 ), 1 h at ambient temperature . the washing ( to be renewed at each step ): h 2 o + 150 mm nacl + 0 . 05 % tween 20 . dilution of the samples , in dilution buffer , to approximately 100 ng / ml and of the control range made up of the lfb monoclonal antibody ad3t1 ( kappa / gamma 3 ) prediluted to 100 ng / ml . incubation for 2 h at ambient temperature . conjugate : biotinylated anti - kappa ( pierce ) diluted to 1 / 1 000 in the presence of streptavidin - peroxidase ( pierce ) diluted to 1 / 1 500 , 2 hours at ambient temperature . substrate : opd at 0 . 5 mg / ml ( sigma ) in phosphate - citrate buffer containing sodium perborate ( sigma ), 10 minutes in the dark . the reaction is stopped with 1n hcl , and read at 492 nm . 3 . 2 — specific assaying of anti - d by the cela ( cellular enzyme linked assay ) technique : this method is used for specifically assaying the anti - d antibodies in particular when this involves a culture supernatant at culturing stages at which other non - anti - d immunoglobulins are present in the solution ( early stages after ebv transformation ). principle : the anti - d antibody is incubated with rhesus - positive red blood cells and then revealed with an alkaline phosphatase - labeled anti - human ig . 100 μl of rh + red blood cells at 10 % diluted in liss - 1 % bsa dilution buffer . dilution of the samples , in dilution buffer , to approximately 500 ng / ml and of the control range made up of a purified monoclonal human anti - d igg ( df5 , lfb ) prediluted to 500 ng / ml . incubation for 45 min at ambient temperature . washing ( to be renewed at each step ): h 2 o + 150 mm nacl . conjugate : anti - igg alkaline phosphatase ( jackson ) diluted to 1 / 4 000 in pbs + 1 % bsa , 1 h 30 at ambient temperature . substrate : pnpp at 1 mg / ml ( sigma ) in 1m diethanolamine , 0 . 5 mm mgcl 2 , ph 9 . 8 . the reaction is stopped with 1n naoh , and read at 405 nm . the adcc ( antibody - dependent cellular cytotoxicity ) technique makes it possible to evaluate the ability of the ( anti - d ) antibodies to induce lysis of rh - positive red blood cells , in the presence of effector cells ( mononuclear cells or lymphocytes ). briefly , the red blood cells of an rh - positive cell concentrate are treated with papain ( 1 mg / ml , 10 min at 37 ° c .) and then washed in 0 . 9 % nacl . the effector cells are isolated from a pool of at least 3 buffy - coats , by centrifugation on ficoll ( pharmacia ), followed by a step of adhesion in the presence of 25 % fcs , so as to obtain a lymphocyte / monocyte ratio of the order of 9 . the following are deposited , per well , into a microtitration plate ( 96 well ): 100 μl of purified anti - d antibody at 200 ng / ml , 25 μl of rh + papain - treated red blood cells ( i . e . 1 × 10 6 ), 25 μl of effector cells ( i . e . 2 × 10 6 ) and 50 μl of polyvalent igg ( tegeline , lfb , for example ) at the usual concentrations of 10 and 2 mg / ml . the dilutions are made in imdm containing 0 . 25 % fcs . after overnight incubation at 37 ° c ., the plates are centrifuged , and the hemoglobin released into the supernatant is then measured in the presence of a substrate specific for peroxidase activity ( 2 , 7 - diaminofluorene , daf ). the results are expressed as percentage lysis , 100 % corresponding to total red blood cell lysis in nh 4 cl ( 100 % control ), and 0 % to the reaction mixture without antibody ( 0 % control ). the specific lysis is calculated as a percentage according to the following formula : the results given in fig1 show the activity of the antibody produced by the heterohybrid f60 compared to those of the reference antibodies : the anti - rh ( d ) polyclonal antibodies poly - d lfb 51 and winrho w03 ( cangene )= positive controls the monoclonal antibody df5 ( inactive in vivo on clearance of rh ( d )- positive red blood cells ( brossard / fnts , 1990 , not published ))= negative control the igg1s purified ( separated from the igg3s ) from the polyclonal winrho w03 . two concentrations of human iggs ( tegeline lfb ) are used to show that inhibition of activity of the negative control is linked to the binding of competing iggs to the fcγ type i receptors . this assay makes it possible to assess the binding of the anti - rh ( d ) antibodies of igg1 isotype to fcγriii , and in particular to differentiate igg3 antibodies . given the low affinity of this receptor for monomeric iggs , prior binding of the antibodies to the d antigen is necessary . principle : the antibody to be tested ( anti - d ) is added to membranes of rh + red blood cells coated with a microtitration plate , followed by transfected jurkat cells expressing the fcγriii receptor at their surface . after centrifugation , the “ rh + membrane / anti - d / cd16 jurkat ” interaction is visualized by a homogeneous plating of the cd16 jurkats in the well . in the absence of interaction , the cells are , on the contrary , grouped at the center of the well . the intensity of the reaction is expressed as numbers of +. method : 1 ) incubation for 1 h at 37 ° c . of the anti - d antibody ( 50 μl at 1 μg / ml in imdm ) on a capture r plate ( immunochim ), and then washes in water + 0 . 9 % nacl . addition of cd16 jurkat ( 2 × 10 6 cells / ml ) in imdm + 10 % fcs . incubation for 20 min at 37 ° c . and then centrifugation and evaluation of cell adhesion ( against a control range ). 2 ) revelation of the anti - d bound to the capture r plates by an elisa - type technique using anti - human igg - peroxidase at 1 / 5 000 ( sanofi diagnostics pasteur ) after having lysed the cd16 jurkat cells with 0 . 2m tris - hcl , 6m urea , ph 5 . 3 - 5 . 5 . opd revelation and then reading of optical density ( o . d .) at 492 nm . expression of results : an arbitrary value of 0 to 3 is allotted as a function of the binding and of the plating of the cd16 jurkat cells . these values are allotted at each od interval defined ( increments of 0 . 1 ). the following are plotted : either a curve : adhesion of the jurkat cells ( y ) as a function of the amount of anti - d bound to the red blood cell membranes ( x ). or a histogram of the “ binding indices ” corresponding , for each antibody , to the sum of each jurkat cell binding value ( 0 to 3 ) allotted per od interval ( over a portion common to all the antibodies tested ). an example of a histogram is given in fig2 . the anti - rh ( d ) antibodies of igg1 isotype ( f60 and t125 yb2 / 0 ) show a binding index close to that of the polyclonal igg1s ( winrho ), whereas the negative control antibodies df5 and ad1 do not bind . similarly , the antibody of igg3 isotype ( f41 ) exhibits a good binding index , slightly less than that of the igg3s purified from the polyclonal winrho and greater than that of the antibody ad3 ( other igg3 tested and ineffective in clinical trial , in a mixture with ad1 ( biotest / lfb , 1997 , not published ). 1 — isolation and amplification of the cdnas encoding the heavy and light chains of the ab the total rnas were extracted from an anti - d ab - producing clone ( igg g1 / kappa ) obtained by ebv transformation : t125 a2 ( 5 / 1 ) a2 ( see paragraph 2 , example 1 ). the corresponding cdnas were synthesized by reverse transcription of the total rnas using oligo dt primers . the vh / t125 - a2 sequence is obtained by amplification of the t125 - a2 cdnas using the following primers : primer a2vh5 , located 5 ′ of the leader region of the vh gene of t125 - a2 , introduces a consensus leader sequence ( in bold ) deduced from leader sequences already published and associated with vh genes belonging to the same vh3 - 30 family as the vh gene of t125 - a2 ; this sequence also comprises an eco ri restriction site ( in italics ) and a kozak sequence ( underlined ): antisense primer gsp2anp , located 5 ′ of the constant region ( ch ) of t125 - a2 : the ch / t125 - a2 sequence is obtained by amplification of the t125 - a2 cdnas using the following primers : the first g base of the ch sequence is here replaced with a c ( underlined ) in order to recreate , after cloning , an eco ri site ( see paragraph 2 . 1 . 1 ). antisense primer h3 ′ xba , located 3 ′ of the ch of t125 - a2 , introduces an xba i site ( underlined ) 3 ′ of the amplified sequence : the entire kappa chain of t125 - a2 ( k / t125 - a2 sequence ) is amplified from the t125 - a2 cdnas using the following primers : primer a2vk3 , located 5 ′ of the leader region of the vk gene of t125 - a2 , introduces a consensus sequence ( in bold ) deduced from the sequence of several leader regions of vk vh genes belonging to the same vk1 subgroup as the vk gene of t125 - a2 ; this sequence also comprises an eco ri restriction site ( in italics ) and a kozak sequence ( underlined ): anti sense primer kse1 , located 3 ′ of kappa , introduces an eco ri site ( underlined ): fig1 gives a diagrammatic illustration of the strategies for amplifying the heavy and light chains of t125 - a2 . the construction of t125 - h26 is summarized in fig2 . it is carried out in two stages : first of all , construction of the intermediate vector v51 - ch / t125 - a2 by insertion of the constant region of t125 - a2 into the expression vector v51 derived from pci - neo ( fig3 ) and then cloning of the variable region into v51 - ch / t125 - a2 . the amplified ch / t125 - a2 sequence is inserted , after phosphorylation , at the eco ri site of the vector v51 ( fig3 ). the ligation is performed after prior treatment of the eco ri sticky ends of v51 with the klenow polymerase in order to make them “ blunt - ended .” the primer g1 used for amplifying ch / t125 - a2 makes it possible to recreate , after its insertion into v51 , an eco ri site 5 ′ of ch / t125 - a2 . the vh / t125 - a2 sequence obtained by amplification is digested with eco ri and apa i and then inserted at the eco ri and apa i sites of the vector v51 - g1 / t125 - a2 . the construction of t125 - k47 is given in fig4 . the k / t125 - a2 sequence obtained by pcr is digested with eco ri and inserted at the eco ri site of the expression vector v47 derived from pci - neo ( fig5 ). the construction of t125 - ig24 is illustrated diagrammatically in fig6 . this vector , which contains the two transcription units for the heavy and kappa chains of t125 - a2 , is obtained by inserting the sal i - xho i fragment of t125 - k47 , containing the transcription unit for k / t125 - a2 , at the xho i and sal i sites of t125 - h26 . thus , the heavy and light chains of t125 - a2 are expressed under the control of the cmv promoter ; other promoters may be used : rsv , igg heavy chain promoter , mmlv ltr , hiv , β - actin , etc . a second vector for expressing t125 - a2 is also constructed , in which the consensus leader sequence of the kappa chain is replaced with the real sequence of the leader region of t125 - a2 determined beforehand by sequencing products from “ pcr 5 ′- race ” ( rapid amplification of cdna 5 ′ ends ). the construction of this t125 - ls4 vector is described in fig7 . it is carried out in two stages : first of all , construction of a new vector for expressing the t125 - a2 kappa chain , t125 - kls18 , and then assembly of the final expression vector , t125 - ls4 , containing the two heavy chain and modified light chain transcription units . the 5 ′ portion of the kappa consensus leader sequence of the vector t125 - k47 is replaced with the specific leader sequence of t125 ( kls / t125 - a2 ) during a step of amplification of the k / t125 - a2 sequence carried out using the following primers : primer a2vk9 , modifies the 5 ′ portion of the leader region ( in bold ) and introduces an eco ri site ( underlined ) and also a kozak sequence ( in italics ): the vector t125 - kls18 is then obtained by replacing the eco ri fragment of t125 - k47 , containing the k / t125 - a2 sequence of origin , with the new sequence kls / t125 - a2 digested via eco ri . the sal i - xho i fragment of t125 - kls18 , containing the modified kls / t125 - a2 sequence , is inserted into t125 - h26 at the xho i and sal i sites . the two expression vectors t125 - ig24 and t125 - ls4 were used to transfect cells of the yb2 / 0 line ( rat myeloma , atcc line no . 1662 ). after transfection by electroporation and selection of transformants in the presence of g418 ( neo selection ), several clones were isolated . the production of recombinant anti - d abs is approximately 0 . 2 μg / 10 6 cells / 24 h ( value obtained for clone 3b2 of r270 ). the adcc activity of this recombinant ab is greater than or equal to that of the poly - d controls ( fig1 ). the abs produced using the two expression vectors are not significantly different in terms of level of production or of adcc activity . the gene amplification system used is based on the selection of transformants resistant to methotrexate ( mtx ). it requires the prior introduction of a transcription unit encoding the dhfr ( dihydrofolate reductase ) enzyme into the vector for expressing the recombinant ab ( shitari et al ., 1994 ). the scheme shown in fig8 describes the construction of the vector for expressing t125 - a2 , containing the murine dhfr gene . a first vector ( v64 ) was constructed from a vector derived from pci - neo , v43 ( fig9 ), by replacing , 3 ′ of the sv40 promoter and 5 ′ of a synthetic polyadenylation sequence , the neo gene ( hind iii - csp 45 i fragment ) with the cdna of the murine dhfr gene ( obtained by amplification from the plasmid pmt2 ). this vector is then modified so as to create a cla i site 5 ′ of the dhfr transcription unit . the cla i fragment containing the dhfr transcription unit is then inserted at the cla i site of t125 - ls4 . yb2 / 0 cells transfected by electroporation with the vector t125 - dhfr13 are selected in the presence of g418 . the recombinant ab - producing transformants are then subjected to selection in the presence of increasing doses of mtx ( from 25 nm to 25 μm ). the progression of the recombinant ab production , reflecting the gene amplification process , is followed during the mtx selection steps . the mtx - resistant transformants are then cloned by limiting dilution . the level and the stability of the recombinant ab production are evaluated for each clone obtained . the anti - d antibody productivity after gene amplification is approximately 13 (+/− 7 ) μg / 10 6 cells / 24 h . yb2 / 0 cells transfected by electroporation with vector t125 - dhfr13 are selected in the presence of g418 . the best recombinant ab - producing transformants are cloned by limiting dilution before selection in the presence of increasing doses of mtx . the progression of the production by each clone , reflecting the gene amplification process , is followed during the mtx selection steps . the level and the stability of the recombinant ab production are evaluated for each mtx - resistant clone obtained . after purification by affinity chromatography on protein a sepharose ( pharmacia ) and dialysis into 25 mm tris buffer , 150 mm nacl , ph 7 . 4 , the concentration of the t125 antibody is determined by the elisa technique . the biological activity in vitro is then measured by the adcc assay described above . the results are given in fig1 . several studies describe the effect of enzymatic inhibitors on the glycosylation of immunoglobulins and on their biological activity . an increase in adcc activity is reported by rothman et al ., 1989 , this being an increase which cannot be attributed to an enhancement of the affinity of the antibody for its target . the modification of glycosylation caused by adding dmm consists of inhibition of the α - 1 , 2 mannosidase i present in le golgi . it leads to the production of a greater proportion of polymannosylated , nonfucosylated structures . various anti - rh ( d ) antibody - producing lines were brought into contact with dmm and the functional activity of the monoclonal antibodies produced was evaluated in the form of culture supernatants or after purification . the cells ( heterohybrid or lymphoblastoid cells ) are seeded at between 1 and 3 × 10 5 cell / ml , and cultured in imdm culture medium ( life technologies ) with 10 % of fcs and in the presence of 20 μg / ml of dmm ( sigma , boehringer ). after having renewed the medium 3 times , the culture supernatants are assayed by human igg elisa and then by adcc . the addition of dmm may make it possible to restore the adcc activity of an antibody derived from the cloid t125 = t125 ri ( 3 ) ( described in example 1 ) and which has lost this activity through sustained culturing . the strong activity of the antibody produced by the heterohybridoma f60 ( the production of which is described in example 1 ) is not modified by culturing in the presence of dmm . the nucleotide sequence of the antibody df5 , a negative control in the adcc assay , is used to study the transfection of this antibody into some lines , in parallel to transfection of the antibody t125 . the sequences encoding the ab df5 are isolated and amplified according to the same techniques used for the recombinant ab t125 - a2 . the corresponding cdnas are first of all synthesized from total rna extracted from the anti - d ab -( igg g1 / lambda )- producing clone 2mdf5 obtained by ebv transformation . amplification of the heavy and light chains is then carried out from these cdnas using the primers presented below . amplification of the variable region of the heavy chain of df5 ( vh / df5 sequence ): primer df5vh1 , located 5 ′ of the leader region ( in bold ) of the vh gene of df5 ( sequence published : l . chouchane et al . ); this primer also comprises an eco ri restriction site ( in italics ) and a kozak sequence ( underlined ): antisense primer gsp2anp , located 5 ′ of the constant region ( ch ) already described in paragraph 1 . 2 ( example 2 ). amplification of the constant region ch of df5 ( ch / df5 sequence ): primers g1 and h3 ′ xba already described in paragraph 1 . 3 ( example 2 ). primer df5vlbd1 , located 5 ′ of the leader region of the vl gene of df5 , introduces a consensus sequence ( in bold ) deduced from the sequence of several leader regions of vl genes belonging to the same vl1 subgroup as the vl gene of 2mdf5 ; this sequence also comprises an eco ri restriction site ( in italics ) and a kozak sequence ( underlined ): antisense primer lse1 , located 3 ′ of lambda , introduces an eco ri site ( underlined ): the construction of the vectors for expressing the heavy chain ( df5 - h31 ), light chain ( df5 - l10 ) and heavy and light chains ( df5 - ig1 ) of the ab df5 is carried out according to a construction scheme similar to vectors expressing the ab t125 - a2 . all the leader sequences of origin ( introduced in the amplification primers ) are conserved in these various vectors . 2 . 2 — transfection of various cell lines with the antibodies t125 and df5 the three expression vectors t125 - ig24 , t125 - ls4 and df5 - igg1 are used to transfect cells of various lines : stable or transient transfections are performed by electroporation or using a transfection reagent . the modification of effector activity of a humanized monoclonal antibody as a function of the expressing cell has been described by crowe et al . ( 1992 ), with the cho , nso and yb2 / 0 cell lines . the results obtained here confirm the importance of the expressing cell line with respect to the functional characteristics of the antibody to be produced . among the cells tested , only the vero , yb2 / 0 and cho lec - 1 lines make it possible to express recombinant anti - rh ( d ) monoclonal antibodies with strong lytic activity in the adcc assay ( see example 1 and table 4 ). characterization of the glycan structures of the anti - rh - d antibody was carried out on four purified products having an adcc activity ( f60 , and three recombinant proteins derived from t125 ) in comparison with two purified products inactive or very weakly active in the adcc assay according to the invention ( d31 and df5 ). in practice , the oligosaccharides are separated from the protein by specific enzymatic deglycosylation with pngase f at asn 297 . the oligosaccharides thus released are labeled with a fluorophore , separated and identified by various complementary techniques which allow : fine characterization of the glycan structures by matrix - assisted laser desorption ionization ( maldi ) mass spectrometry by comparison of the experimental masses with the theoretical masses . determination of the degree of sialylation by ion exchange hplc ( glycosep c ) separation and quantification of the oligosacharride forms according to hydrophilicity criteria by normal - phase hplc ( glycosep n ) separation and quantification of the oligosaccharides by high performance capillary electrophoresis - laser induced fluorescence ( hpce - lif ). the various active forms studied are f60 and three recombinant antibodies , r 290 , r 297 and r 270 , derived from t125 and produced in yb2 / 0 . fine characterization of the glycan structures by mass spectrometry ( fig7 ) shows that these forms are all of the bi - antennary type . in the case of r 270 , the major form is of the agalactosylated , nonfucosylated type ( g0 , exp . mass 1459 . 37 da , fig1 ). three other structures are identified : agalactosylated , fucosylated ( g0f at 1605 . 41 da ), monogalactosylated , nonfucosylated ( g1 at 1621 . 26 da ) and monogalactosylated , fucosylated ( g1f at 1767 . 43 da ) in minor amount . these same four structures are characteristic of r 290 , f 60 and r 297 ( fig1 ). these four antibodies which are active in adcc are also characterized by the absence of oligosaccharides having a bisecting n - acetylglucosamine residue . quantification of the glycan structures by the various techniques of hplc and hpce - lif ( table 1 ) confirms the presence of the four forms identified by mass : g0 , g0f , g1 and g1f . the degree of sialylation is very low , in particular for the recombinant products , from 1 to 9 . 4 %, which is confirmed by the similarity of the mass spectra obtained before and after enzymatic desialylation . the degree of fucosylation ranges from 34 to 59 %. the various inactive forms studied are d31 and df5 . quantification of the glycan structures by the various chromatographic and capillary electrophoresis techniques ( table 1 ) reveals , for these two antibodies , a degree of sialylation close to 50 %, and a degree of fucosylation of 88 and 100 % for d31 and df5 , respectively . these degrees of sialylation and fucosylation are much higher than those obtained from the active forms . characterization of the glycan structures shows that the major form is , for the two antibodies , of the bi - antennary , monosialylated , digalactosylated , fucosylated type ( g2s1f , table 1 ). the characterization by mass spectrometry of d31 ( fig7 ) reveals that the neutral forms are mainly of the monogalactosylated , fucosylated type ( gif at 1767 . 43 da ) and digalactosylated , fucosylated type ( g2f at 1929 . 66 da ). the inactive antibody df5 is characterized by the presence of oligosaccharides having an intercalated glcnac residue . in particular , the mass analysis ( fig8 ) reveals the presence of a major neutral form of the monogalactosylated , fucosylated , bisecting , intercalated glcnac type ( g1fb at 1851 . 03 da ). on the other hand , these structural forms are undetectable or present in trace amounts on the active antibodies studied . the adcc activity of d31 after the action of dmm increases from 10 % to 60 %. the glycan structures of dmm d31 differ from those of d31 by the presence of oligomannose forms ( man 5 , man 6 and man 7 ) ( see fig9 ). the various active antibodies are modified on asn 297 with n - 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278 ( 1994 ). thompson , k . m ., hough , d . w ., maddison , p . j ., mclamed , m . d . and hughes - jones , n . c . production of human monoclonal igg and igm antibodies with anti - d ( rhesus ) specificity using heterohybridomas . immunology 58 : 157 - 160 ( 1986 ). thomson , a ., contreras , m ., gorick , b ., kumpel , b ., chapman , g . e ., lane , r . s ., teesdale , p . hughes - jones , n . c . and mollison , p . l . clearance of rh d - positive red cells with monoclonal anti - d . lancet 336 : 1147 - 1150 ( 1990 ). tippett , p . sub - divisions of the rh ( d ) antigen . med . lab . sci . 45 : 88 - 93 ( 1988 ). ware , r . e . and zimmerman , s . a . anti - d : mechanisms of action . seminars in hematology , vol . 35 , no . 1 , supp . 1 : 14 - 22 ( 1998 ). yu , i . p . c ., miller , w . j ., silberklang , m ., mark , g . e ., ellis , r . w ., huang , l ., glushka , j ., van halbeek , h ., zhu , j . and alhadeff , j . a . structural characterization of the n - glycans of a humanized anti - cd18 murine immunoglobulin g . arch . biochem . biophys . 308 , 387 - 399 ( 1994 ). zupanska , b ., thompson , e ., brojer , e . and merry , a . h . phagocytosis of erythrocytes sensitized with known amounts of igg1 and igg3 anti - rh antibodies . vox sang . 53 : 96 - 101 ( 1987 ). | 2 |
referring to the drawings it will be appreciated that a method and apparatus for detecting the presence or absence of an object at a predetermined location can be implemented in various forms . the following embodiments are described by way of example only . references herein to ‘ light ’ are not intended to be limited to visible light but are to be understood as also including non - visible radiation , including infrared and ultraviolet radiation having wavelengths outside the visible spectrum , for example . references to ‘ reflection ’ include scattering of light or radiation from a surface . fig1 shows a schematic diagram of a first preferred embodiment of an optical arrangement for determining the presence or absence of a die at a predetermined location . in this embodiment the predetermined location is at a die - handling collet of a collet assembly for die placement . the collet assembly is used to pick up individual dice fabricated from a silicon or sapphire wafer , and to place the dice at a bonding position where , for example , the die is attached to a substrate , such as a lead frame . a light source 1 , for example a laser diode , is arranged to illuminate at least a portion of a site in the collet . as shown in fig1 , the site is occupied by a die 2 . the light from the source is preferably collimated or focused , such as by a lens 22 ( see fig3 ) into a narrow incident beam 3 . in a preferred application the collimated or focused beam is between 0 . 02 to 0 . 5 mm wide , and most preferably 0 . 05 mm wide . the incident beam is directed through the collet , whose inner diameter can be as small as 0 . 02 mm , at a small portion of the die 2 . noise caused by reflections of light from the inner surface of the collet other than at the die site in the collet , are minimised by making the diameter of the beam sufficiently small so that very little , other than the die , is illuminated . in the case shown in fig1 , the illuminating light is incident upon the surface 4 of the die substantially normal to the orientation of the surface 4 . however , other angles of incident light that are close to normal incidence may be used , in which case the light will be reflected from the die surface at a corresponding angle , as long as angles of incidence and reflection are sufficiently small to allow the light to be received . the light source illuminates the die surface after passing through a beam splitter 5 . in the case shown in fig1 , where the die 2 is transparent , a major fraction 6 of the light is transmitted through the die 2 . however , a smaller fraction 7 of the incident source light is reflected from the die surface 4 back toward the beam splitter 5 which reflects the light to a light detector , which may be in the form of a photo - sensor 8 . fig1 shows this reflected fraction or beam 7 offset from the incident beam 3 . this offset is only shown for clarity of the explanation provided by fig1 , and in practice the incident and reflected beams coincide , at least at the die surface 4 . an output signal from the photo - sensor 8 is connected to an electronic amplifier 9 which produces an amplified output 10 for further processing to make a determination of the presence or absence of a die at the collet , based on the light received by the photo - sensor 8 . the photo - sensor 8 can be an image sensor or a general light power sensor . in the case of the preferred application , where the optical arrangement monitors the presence or absence of a die fabricated from a wafer made of sapphire , the die is substantially transparent . in general , the reflectivity r of a surface of a transparent body can be expressed as : typically for sapphire , n is between 1 . 55 to 1 . 7 . if n = 1 . 55 , then r = 0 . 047 ( or 4 . 7 %). however reflection occurs at both the top and bottom surfaces of the sapphire die giving a total reflectivity of about 9 . 4 %. thus , even if the die is substantially transparent and as long as its refractive index is not equal to 1 , the die will still reflect a fraction of the incident light beam back for detection by the photo - sensor . this reflectivity by the die allows a determination of the presence or absence of a transparent object such as a sapphire die in the collet to be based upon reflected rather than the traditional transmitted light . determination based upon scattering of light by an object is also possible , as long as an intensity of the scattered light is sufficient to reach the photo - sensor . a second arrangement is shown in fig2 . corresponding features in fig1 and 2 are labelled alike . in this arrangement the positions of the illuminating light source 1 and the photo - sensor 8 are interchanged , so that light from the illuminating source 1 is directed to the beam splitter 5 which reflects the incident beam 3 toward the surface 4 of the die 2 . a major fraction 6 of the incident light is transmitted through the die , while a minor fraction 7 of the incident light is reflected back through the beam splitter 5 to the photo - sensor 8 . fig3 shows a cross - sectional side view of a collet assembly 20 utilising the arrangement of the first preferred embodiment . the light source or laser diode 1 is arranged at the top of the collet assembly 20 to project a beam of light through the collet assembly 20 . the light from the source is collimated or focused by a lens 22 into a narrow incident beam . the incident beam passes through the beam splitter 5 and is directed through the collet 21 such that at least a portion of a site at the opening of the collet 21 is illuminated . a die 2 is located at the said opening . the incident beam is reflected from the surface of the die 2 back toward the beam splitter 5 which reflects the light to the photo - sensor 8 . in fig3 , the light source 1 and photo - sensor 8 are integrated with and located on the collet assembly 20 . fig4 shows a cross - sectional side view of a collet assembly 20 where the light source 1 and light detector 8 are located remotely from the collet assembly 20 . an optical fibre 23 is used to direct incident light from the remotely located laser diode 1 to the surface of the die 2 at the collet 21 . another optical fibre 24 is used to direct light reflected from the surface of the die 2 to the photo - sensor 8 , which is also remotely located . in another alternative arrangement ( not shown ), a single fibre directs both incident light to , and reflected light from , the die . in alternative arrangements ( not shown ), optical systems such as light guides , mirrors , etc , can be used to direct the incident light from the light source 1 , or to direct light reflected by the die surface back to the photo - sensor 8 . an advantage of using optical fibres 23 , 24 is that the light source and / or the sensor need not be mounted on the collet assembly 20 so that heavier and more complicated designs can be used without burdening a bond arm controlling it . it should be appreciated that either or both of the light source 1 and the photo - sensor 8 may be mounted on the collet assembly 20 or may be located remotely . fig5 is a schematic view of the layout of a placement apparatus that uses the missing die detection arrangements described above . a bond arm 11 is mounted to rotate about an axis 12 . a collet assembly 20 is carried at the distal end 13 of the bond arm . the illuminating light source and the photo - sensor are mounted in the collet assembly 20 . the illuminated light is collimated or focused into a beam providing a small spot size which is projected through the collet and onto the position to be occupied by a die . signal - to - noise ratio of the detecting signal is high because background noise is reduced by the use of the collimated or focused beam and small spot size . fig5 shows the bond arm 11 in three positions . in a first bond arm position 11 a , the pick - up head and collet are located over a selected die ( not shown ) on a sapphire wafer 14 on which individual dice have been fabricated and diced . the collet is operated in an attempt to pick up the selected die and the bond arm 11 is rotated to move the collet toward a third bond arm position 11 c . the sapphire wafer has a highly specular surface which can interfere with measurements of light reflected from an individual die above the wafer . therefore , a dark background 15 is arranged under an intermediate second position 11 b through which the bond arm moves when passing from the first position 11 a to a third position 11 c . while the collet is moving over the dark background , the photo - sensor signal processor is triggered , for example by a signal from a host controller or a bond arm controller , to make a measurement of light reflected from the die , if present , in the collet . the measurement is undertaken while the bond arm keeps moving as it is moving over the dark background . the measurement is compared to a reference signal , representing a reference level of detected light intensity in the absence of a die plus a reasonable margin , that can be manually preset or automatically learned by the signal processor . if the reflection measurement is greater than the reference signal this is taken as an indication that a die is present in the collet , otherwise a missing die alarm is raised and the bond arm is returned to the first bond arm position 11 a , to make another attempt to pick up a die . if the indication derived from the reflection measurement is that a die is present in the collet , the bond arm continues moving to the third bond arm position 11 c at which the collet is released to place the die in a bonding position . the bond arm then begins to return back to the first bond arm position 11 a . while the collet is returning over the dark background 15 , the photo - sensor signal processor is again triggered to make a second measurement of light reflected from the die , if present , in the collet . again the measurement is undertaken while the bond arm keeps moving and the measurement compared to the reference signal . if the reflection measurement is less than the reference signal this is taken as an indication that a die is not present in the collet , and that the die was well placed . otherwise , a reflection signal greater than the reference is taken as an indication that the die was not placed and an unplaced die alarm is raised . if the reflection measurement is less than the reference signal , indicating that a die is not present in the collet , then the reference signal may be replaced by this reflection measurement with a reasonable margin added . in this way the reference signal may be continually updated to accommodate variations in ambient conditions , for example background light levels , and to accommodate drift of the apparatus performance parameters , for example in the light source and the photo - sensor . the bond arm returns to the first position 11 a to complete one die placement cycle . although the embodiment refers to a transparent die , it should be appreciated that a presence of a non - transparent die can also be detected by an apparatus and method according to the invention . the foregoing describes the invention including preferred forms thereof . alterations and modifications as will be obvious to those skilled in the art are intended to be incorporated within the scope hereof as defined in the accompanying claims . | 7 |
embodiments of the present invention will be described in detail on the basis of the following drawings . first , a configuration of an x - ray ct apparatus 1 will be described with reference to fig1 and fig2 . as illustrated in fig1 , the x - ray ct apparatus 1 includes a scanner 2 on which an x - ray tube 11 and a detector 12 are loaded , a bed 4 on which a test object 10 is placed , an arithmetic device 5 that processes data obtained from the detector 12 , an input device 6 such as a mouse , a trackball , a keyboard , a touch panel and so forth , a display device 7 that displays a reconstructed image and so forth and others . an operator inputs imaging conditions , reconstruction parameters and so forth via the input device 6 . the imaging conditions are , for example , a bed feed rate , a tube current , a tube voltage , a slice position and so forth . in addition , the reconstruction parameters are , for example , a region of interest , a reconstructed image size , a back projection phase width , a reconstruction filter function and so forth . as illustrated in fig2 , the x - ray ct apparatus 1 includes the scanner 2 , an operation unit 3 and the bed 4 when broadly classified . the scanner 2 includes the x - ray tube 11 ( an x - ray source ), the detector 12 ( an x - ray detector ), a collimator 13 , a drive device 4 , a central control device 15 , an x - ray control device 16 , a high - voltage generation device 17 , a scanner control device 18 , a bed control device 19 , a bed movement measuring device 20 , a collimator control device 21 , a preamplifier 22 , an a / d converter 23 and so forth . the x - ray ct apparatus 1 is broadly classified into a multislice ct using the detector 12 that detection elements are arrayed in two - dimensional directions and a single slice ct using the detector 12 that the detection elements are arrayed in line , that is , in one - dimensional direction ( only in a channel direction ). in the multislice ct , x - ray beams which spread in a cone - like form or in a pyramid - like form are irradiated from the x - ray tube 11 which is an x - ray source conforming with the detector 12 . in the single slice ct , the x - ray beams which spread in a fan - like form are irradiated from the x - ray tube 11 . in general , in imaging using the x - ray ct apparatus 1 , x - ray irradiation is performed while a gantry part is going around the test object 10 placed on the bed 4 . the central control device 15 controls to input the imaging conditions and the reconstruction parameters through the input device 6 in the operation unit 3 and to transmit control signals desired for imaging to the collimator control device 21 , the x - ray control device 16 , the scanner control device 18 and the bed control device 19 . the collimator control device 21 controls the position of the collimator 13 on the basis of the control signal . when imaging is started by receiving an imaging start signal , the x - ray control device 16 controls the high - voltage generation device 17 on the basis of the control signal . the high - voltage generation device 17 applies the tube voltage and the tube current to the x - ray tube 11 . in the x - ray tube 11 , electrons of energy according to the applied tube voltage are emitted from a cathode and the emitted electrons strike a target ( an anode ), thereby irradiating the test object 10 with the x - ray of energy according to the energy of the electrons . in addition , the scanner control device 18 controls the drive device 14 on the basis of the control signal . the drive device 14 drives the gantry part on which the x - ray tube 11 , the detector 12 , the preamplifier 22 and so forth are loaded so as to go around the test object 10 . the bed control device 19 controls the bed 4 on the basis of the control signal . the x - ray irradiated from the x - ray tube 11 is controlled by the collimator 13 in irradiation region , is absorbed ( attenuated ) in accordance with an x - ray attenuation coefficient into each tissue in the test object 10 , passes through the test object 10 and is detected by the detector 12 arranged at a position facing the x - ray tube 11 . the detector 12 includes the plurality of detection elements which are arrayed in the two - dimensional directions ( the channel direction and a column direction orthogonal to the channel direction . the x - ray received by each detection element is converted into real projection data . that is , the x - ray detected by the detector 12 is converted into current , is amplified by the preamplifier 22 , is converted into digital data by the a / d converter 23 , is subjected to logarithmic transformation , is calibrated and is input into the arithmetic device 5 as the real projection data . at that time , since the mutually facing x - ray tube 11 and detector 12 rotate around the test object 10 , the real projection data is collected at discrete x - ray tube positions ( and corresponding detector positions ) in a rotation direction . a real projection data acquisition unit at each x - ray tube position is called a “ view ”. the arithmetic device 5 includes a reconstruction arithmetic device 31 , an image processing device 32 and so forth . in addition , an input / output device 9 includes the input device 6 , the display device 7 , a memory device 8 ( a memory unit ) and so forth . the reconstruction arithmetic device 31 performs an image reconstructing process using the real projection data and generates a reconstructed image . the reconstruction arithmetic device 31 generates filtered projection data by superimposing a reconstruction filter on the real projection data of each view and performs back projection processing on the filtered projection data by adding weight in a view direction , thereby non - destructively imaging a tomographic image as a distribution map of an x - ray attenuation coefficient in the test object 10 . the reconstruction arithmetic device 31 stores the generated reconstructed image into the memory device 8 . in addition , the reconstruction arithmetic device 31 displays the reconstructed image as a ct image on the display device 7 . alternatively , the image processing device 32 may perform image processing on the reconstructed image stored in the memory device 8 and displays the image so processed as the ct image on the display device 7 . in the following , an image processing method that adds respective mutually corresponding pixels of an original image generated from original information acquired by the x - ray ct apparatus 1 and so forth and a smoothed image which is generated from the same original information and is reduced at least in streak artifact with weighting by using a weighting coefficient and generate a target image that the edge of the structure is maintained and the streak artifact is removed will be described . in the image processing method according to the embodiment of the present invention , the target image is generated so as to meet the following three constraint conditions . ( constraint condition 1 ) the pixel value of the target image is to be within a range of pixel values of mutually corresponding pixels in the original image and the smoothed image . ( constraint condition 2 ) the target image is to be an image which is smooth spatially ( that is , in one image space ). ( constraint condition 3 ) the target image is to be suppressed in increase in noise such as the streak artifact and so forth in a region (= one of the flat regions ) which is thought to be the same organ in comparison with the smoothed image . the constraint condition 1 is a condition which has been defined in order not to lose the original image ( however , the noise is excluded ) acquired by the x - ray ct apparatus 1 and so forth . the constraint condition 1 may be expressed in such a different form as min ( a minimum pixel value of the original image and a minimum pixel value of the smoothed image ) s a pixel value of the target image 5 max ( a maximum pixel value of the original image and a maximum pixel value of the smoothed image ). incidentally , min ( ) is an operator for outputting a minimum value and max ( ) is an operator for outputting a maximum value . the constraint condition 2 is a condition which has been defined in order to avoid discontinuity which would occur in the target image . the constraint condition 3 is a condition which has been defined in order to remove mainly the granular noise and the streak artifact . the image processing method according to the embodiment of the present invention features to meet the constraint condition 3 in particular . the weighting coefficient used for weighted addition is determined by condition coefficients indicating the conditions of the original image and the smoothed image . the condition coefficient has a value of a nonlinear function that a difference in pixel value between a pixel of interest of the original image or the smoothed image and an adjacent pixel thereof is set as a variable . in the embodiment of the present invention , a generalized gaussian function is used as the nonlinear function . however , any nonlinear function will do as long as it is a smooth continuous function , has a plurality of arbitrary parameters and is arbitrarily adjustable in shape , and there is no particular limit thereon . if the nonlinear function is the smooth continuous function , the aforementioned “( constraint condition 2 ) the target image is to be an image which is smooth spatially ( that is , in one image space )” will be met . as other examples of the nonlinear function , a logistic function and so forth may be given . an image vector is put as x =( x 1 , . . . , x j ), a set of adjacent pixels r relative to a pixel of interest s is put as n s and a condition coefficient g s ( x ) of the pixel of interest s is defined by the following formula using the generalized gaussian function . here , p is an arbitrary parameter for adjusting the gradient of the generalized gaussian function and is set to have the same value for all slices . ν is an arbitrary parameter for adjusting a bending position of the generalized gaussian function . w sr is a weighting coefficient according to a distance between the pixel of interest s and the adjacent pixel r and is defined , for example , as in the following formula . here , l sr is the distance between the pixel of interest s and the adjacent pixel r . l is a ratio of the size of a pixel to the size of an element of the detector . however , w sr may not necessarily be limited to the formula ( 2 ) and may be a function whose value is increased as the adjacent pixel r is closer to the pixel of interest s . in addition , the set n s of pixels adjacent to the pixel of interest s and the gradient p of the generalized gaussian function may be empirically determined . in the formula ( 1 ), if the pixel values of the pixel of interest s and the adjacent pixel r are equal to each other , the condition coefficient will become 1 , and the larger the difference in pixel value between the pixel of interest s and the adjacent pixel r is , the more the condition coefficient will approach 0 . one example of a change in shape of functions when ν has been set to arbitrary constants c , 2c and 4c for the difference in pixel value between the pixel of interest s and the adjacent pixel r is illustrated in fig3 . thinking of the situation by fixing the difference in pixel value , the more ν is increased , the more the condition coefficient is liable to have a value close to 1 . according to the embodiment of the present invention , the parameter ν for adjusting the bending position of the function is determined such that the condition coefficient has a value almost close to 1 relative to the difference in pixel value between the pixel of interest s and the adjacent pixel r which would occur due to the presence of the streak artifact in one tomographic image . in the following , the first embodiment of the present invention will be described following the stream of a processing flow illustrated in fig4 while appropriately referring to other drawings . the arithmetic device 5 of the x - ray ct apparatus 1 ( hereinafter , referred to as the “ arithmetic device 5 ) determines the shape of the nonlinear function on the basis of feature amounts of the original image and the smoothed image . a process of determining the shape of the nonlinear function will be described later with reference to fig5 . the arithmetic device 5 divides regions of the original image and the smoothed image into mutually corresponding small regions . for example , as illustrated in fig6 , the arithmetic device 5 partitions the regions of an original image 41 and a smoothed image 42 in a lattice shape and divides them into small regions . the size of the small region is empirically determined . however , the method of dividing one region into small regions is not limited to this example . in the embodiment of the present invention , the regions of the original image 41 and the smoothed image 42 may be just divided into the small regions by the same dividing method . in addition , the shape of the small region is not limited to a rectangle . in the embodiment of the present invention , the plurality of adjacent pixels may be included in the same small region . in addition , one pixel may be included in the plurality of small regions redundantly . the arithmetic device 5 calculates variation values of the original image 421 and the smoothed image 42 from the pixel values of the pixels included in the small region for each of the respective small regions pertaining to both of the original image 41 and the smoothed image 42 . the variation value is , for example , a standard deviation value , ( the maximum value − the minimum value ) and so forth . the variation value is a value indicating a variation of each small region and may be a statistic calculated from the pixel values of the pixels included in each small region . in the following , description will be made by giving the standard deviation value as an example in order to avoid confusion . here , for the convenience of explanation , serial numbers i = 1 , . . . are allocated to the small regions and attention will be paid to an i - th small region . the standard deviation value of the original image 41 in the i - th small region is put as σ i ( org ) and the standard deviation value of the smoothed image 42 is put as σ i ( smt ) . the arithmetic device 5 calculates a decreasing rate of the variation value of the smoothed image 42 based on the variation value of the original image 41 for every small region . in the present embodiment , the decreasing rate of the standard deviation value is calculated . for the i - th small region , the decreasing rate of the standard deviation value of the smoothed image 42 based on the standard deviation value of the original image 41 is put as ρ i and is calculated by the following formula . the arithmetic device 5 calculates the decreasing rate ρ i of the standard deviation value in all of the small regions on the basis of the formula ( 3 ). the shape of the nonlinear function is determined using a feature amount ( for example , the decreasing rate ρ i ) calculated from the pixel values of the pixels in both of the original image 41 and the smoothed image 42 as in the formula ( 3 ) and the processing illustrated in fig4 is performed , thereby meeting the aforementioned “( constraint condition 3 ) the target image is to be suppressed in increase in noise such as the streak artifact and so forth in a region (= one of the flat regions ) which is thought to be the same organ in comparison with the smoothed image ”. incidentally , in related art ( for example , japanese patent no . 3700798 and japanese patent application laid - open no . hei07 - 93543 ) relating to the technique of mixing together two images which are the same as each other in original information , only the feature amount calculated from the pixel values of the pixels included in only one of the images is used . for example , with the standard deviation value calculated from the pixel values of the pixels included in only one of the images , it is difficult to discriminate between whether the noise has been reduced and whether the structure has blurred as a result of execution of an arbitrary smoothing process . accordingly , it is difficult for related art to generate such a target image that the streak artifact is removed as generated in the embodiment of the present invention . the arithmetic device 5 extracts a feature amount calculation region from the set of small regions on the basis of the decreasing rate ρ i . in the first embodiment , the arithmetic device 5 extracts a small region whose decreasing rate has a maximum value in the small regions included within a predetermined range ( for example , in the same slice ) as the feature amount calculation region . incidentally , the predetermined range may be either in a plurality of slices or in all of the slices . in the following , description will be made assuming that a k - th small region has been extracted as the feature amount calculation region . the arithmetic device 5 determines the shape of the nonlinear function from the feature amount calculated from the pixel values of the pixels included in the feature amount calculation region ( the k - th small region ). in the following , an example that the feature amount is calculated by using a standard deviation value σ k ( org ) of the original image 41 calculated in step s 202 and a standard deviation value σ k ( smt ) of the smoothed image 42 calculated in step s 203 will be described . however , the present invention is not limited to this example and another variation value ( for example , the difference between the maximum value and the minimum value of the pixels in the small region concerned ) may be used in place of the standard deviation value . an arbitrary constant is putt as α ( 0 & lt ; α & lt ; 1 ) and the shape of the nonlinear function is set such that the condition coefficient takes the value of α when the difference in pixel value is σ k ( a general notation of σ k ( org ) and σ k ( smt ) ( see fig3 ). α is an actual value such as , for example , 0 . 99 , 0 . 98 , 0 . 97 or the like . for example , for the generalized gaussian function in the formula ( 1 ), the parameter ν for adjusting the bending position of the function is defined as in the following formula . here , t is a positive coefficient which is not 1 and is empirically determined from statistical information obtained from already photographed images by taking the influence of the noise such as the streak artifact and so forth into account . for example , for an image that only gaussian noise ( the granular noise ) is generated , t = 1 is put and introduction of t into the formula ( 4 ) may be unnecessary . however , the embodiment of the present invention targets on the image that the streak artifact which is the noise stronger than the gaussian noise is generated , t of a value larger than 1 is introduced into the formula ( 4 ). in the formula ( 4 ), the parameters for adjusting the bending positions of the nonlinear functions calculated in the original image 41 and the smoothed image 42 respectively are put as σ k ( org ) and σ k ( smt ) . the arithmetic device 5 dynamically determines the shape of the nonlinear function for every predetermined range ( for example , for every slice ) by executing the processing illustrated in fig5 . one of the features of the first embodiment lies in the point that the region whose decreasing rate ρ i of the standard deviation value of the smoothed image 42 to the standard deviation value of the original image 41 has a maximum value is extracted as the feature amount calculation region and the shape of the nonlinear function is determined using the standard deviation value of the feature amount calculation region . the aforementioned projection data smoothing filter has such a characteristic that it greatly decreases the streak artifact . owing to this characteristic , the decreasing rate ρ i of the standard deviation value is increased in the small region including the streak artifact . in addition , the projection data smoothing filter also has such a characteristic that blurring of the structure is involved . owing to this characteristic , since the standard deviation value of the original image is increased in the small region including the structure and the denominator in the formula ( 3 ) is increased , the decreasing rate ρ i of the standard deviation value is decreased consequently . that is , the possibility that the region whose the decreasing rate ρ i of the standard deviation value has the maximum value may include the streak artifact is high . therefore , extraction of the region whose decreasing rate ρ i of the standard deviation value has the maximum value as the feature amount calculation region leads to extraction of the small region which includes the streak artifact as the feature amount calculation region . then , it is possible to obtain the target image that the streak artifact is removed eventually by substituting the standard deviation value of the small region which includes the streak artifact into the formula ( 4 ) and determining the value of the parameter ν for adjusting the bending position of the nonlinear function . getting back to the description of the flow in fig4 , in the following , processes of calculating the condition coefficients indicating the respective conditions of the original image 41 and the smoothed image 42 using the nonlinear function and calculating the weighting coefficient for weighted addition from the condition coefficients of the original image 41 and the smoothed image 42 will be described . the arithmetic device 5 calculates the condition coefficients of the original image 41 and the smoothed image 42 using the nonlinear function whose shape is determined in step s 101 . the process of calculating the condition coefficients is executed following the formula ( 1 ). the arithmetic device 5 calculates the weighing coefficient of each pixel of the original image 41 and the smoothed image 42 by using the condition coefficients calculated in step s 102 . the image vector of the original image 41 is put as x ( org ) ={ x 1 ( org ) , . . . , x j ( org ) and the image vector of the smoothed image 42 is put as x ( smt ) ={ x 1 ( smt ) , . . . , x j ( smt ) . in weighted addition of the images , the weighting coefficient pertaining to the pixel of interest s is put as λ s . the process of calculating λ s is executed following any one of the following formula ( 5 ), formula ( 6 ) and formula ( 7 ). λ s ≡ g s ( x ( org ) , ν k ( org ) )· g s ( x ( smt ) , ν k ( smt ) ) ( 5 ) λ s ≡{ g s ( x ( org ) , ν k ( org ) + g s ( x ( smt ) , ν k ( smt ) )}/ 2 ( 6 ) λ s ≡{ g s ( x ( org ) , ν k ( org ) )· g s ( x ( smt ) , ν k ( smt ) } 1 / 2 ( 7 ) one of the features of the embodiment of the present invention lies in the point that the values of the weighting coefficients of the mutually corresponding pixels are calculated using the condition coefficients of both of the original image 41 and the smoothed image 42 as expressed in the formula ( 5 ) to the formula ( 7 ). in the formula ( 5 ) and the formula ( 7 ), in a case where the condition coefficient takes a value close to 1 in at least either of the original image 41 and the smoothed image 42 and it is decided that the pixel of interest s corresponds to an edge part of the structure , the weighting coefficient takes a value close to 0 . on the other hand , in a case where the condition coefficients of both of the original image 41 and the smoothed image 42 take values close to 1 and it is decided that the pixel of interest s corresponds to a flat region ( for example , a region which is thought to be the same organ ), the weighting coefficient takes a value close to 1 . in the formula ( 6 ), in a case where the condition coefficients of both of the original image 41 and the smoothed image 42 take values close to 0 , the weighting coefficient takes a value close to 0 . in addition , in the formula ( 6 ), in a case where the condition coefficients of both of the original image 41 and the smoothed image 42 tales values close to 1 , the weighting coefficient takes a value close to 1 . on the other hand , in the formula ( 6 ), in a case where a difference in value of condition coefficient between the original image 41 and the smoothed image 42 is large , a mean value of the both is defined as the weighting coefficient . considering from the above , in a case where it is desired to sharply recover the edge of the structure in the target image , it is desirable to use the formula ( 5 ) or the formula ( 7 ). on the other hand , in a case where it is desired to smoothly recover the edge of the structure in the target image , it is desirable to use the formula ( 6 ). the both ways of recovering the edge may be properly used depending on the application . the arithmetic device 5 generates the target image by performing weighed addition of the original image 41 and the smoothed image 42 by using the weighting coefficient calculated in step s 103 . the image vector of the target image after weighted addition has been performed is set as x ( mrg ) ={ x 1 ( mrg ) , . . . , x j ( mrg ) }. the arithmetic device 5 performs weighted addition for the pixel of interest s of the target image by using the following formula . x s ( mrg ) = λ s ( x s ( smt ) − x s ( org ) )+ x s ( org ) ( 8 ) the aforementioned “( constraint condition 1 ) the pixel value of the target image is to be within a range of pixel values of mutually corresponding pixels in the original image and the smoothed image ” is met by performing weighted addition by using the formula ( 8 ). examples of schematic diagrams of the original image 41 , the smoothed image 42 and a target image 43 are illustrated in fig7 . as illustrated in fig7 , a streak artifact 51 is being generated in the original image 41 . in addition , a blur 52 of the edge of the structure is being generated in the smoothed image 42 . it is possible to generate the target image 43 that the edge of the structure is maintained and the streak artifact 51 is removed from such original image 41 and smoothed image 42 as mentioned above by the image processing method according to the embodiment of the present invention illustrated in fig4 . as illustrated in fig7 , the edge of the structure is maintained and the streak artifact 51 is removed in the target image 43 . in the following , the second embodiment of the present invention will be described . incidentally , description of the contents which are common to the first embodiment is omitted . in the first embodiment , the small region whose decreasing rate of the variation value of the smoothed image 42 to the variation value of the original image 41 has the maximum value is extracted as the feature amount calculation region and the parameter ν for adjusting the bending position of the nonlinear function is determined on the basis of the feature amount of the feature amount calculation region . at that time , the feature amount calculation region is extracted by analyzing in more detail the relation between the decreasing rate of the variation value and the variation value of the original image 41 or the smoothed image 42 . owing to this , the precision that the flat region including the streak artifact 51 is extracted as the feature amount calculation region is improved . in the second embodiment , the arithmetic device 5 extracts m higher - rank small regions which are higher in decreasing rate ρ i of the standard deviation value in the small regions included within the predetermined range ( for example , in the same slice ) in step s 205 in fig5 . that is , the arithmetic device 5 extracts the small regions counted from the small region whose decreasing rate ρ i of the standard deviation value has the maximum value down to an m - th ranked small region . here , m is an arbitrary constant and is empirically determined . next , the arithmetic device 5 extracts the small region whose standard deviation value has a maximum value in m higher - rank small regions as the feature amount calculation region in each of the original image 41 and the smoothed image 42 . the feature amount calculation process , the nonlinear function shape determination process , the condition coefficient calculation process , the weighing coefficient calculation process , the weighted addition process and so forth which are succeeding processes are the same as those in the first embodiment . according to the second embodiment , the precision that the flat region including the streak artifact 51 is extracted as the feature amount calculation region is improved . it is apparent that the object of the present invention is attained from the above - mentioned description relating to the various embodiments of the present invention . although the present invention has been described and illustrated in detail , they simply aim at description and illustration and the present invention is not limited to them . in addition , the gist of the present invention is to be limited only by the scope of the patent claims . 1 : x - ray ct apparatus , 2 : scanner , 3 : operation unit , 4 : bed , 5 : arithmetic device , 6 : input device , 7 : display device , 8 : memory device , 10 : test object , 11 : x - ray tube , 41 : original image , 42 : smoothed image , 43 : target image , 51 : streak artifact , 52 : blur of structure edge | 6 |
the general organization of the exemplified year - round air conditioner will become apparent upon consideration of fig1 and 2 . broadly it comprises : 1 . a housing 10 having a filter - screened air inlet 12 and a louvered air outlet 14 . 2 . a water receptacle 16 withdrawably mounted on the bottom 18 of the housing 10 . 3 . a wet band assembly 20 also withdrawably mounted within the housing 10 in partial immersion in the water w contained in the receptacle 16 . 4 . a fan 22 within the housing 10 for producing an airflow a from air inlet 12 to air outlet 14 through the wet band assembly 20 . 5 . a damper 24 pivotally mounted at the air outlet 14 for dividing the same into a cool air outlet 26 and a warm air outlet 28 and for selectively communicating the cool and warm air outlets with the air inlet 12 . 6 . an electric heater 30 mounted on the damper 24 for heating the air as it is expelled through the warm air outlet 28 . the housing 10 is of generally boxlike shape , mounted on casters 32 for portability . the air inlet 12 is defined in the rear wall 34 of the housing midway between its top and bottom ends . a filter screen 36 covers the air inlet 12 for removal of dust from the incoming room air . the air outlet 14 , on the other hand , is defined in the front wall 38 of the housing 10 in the vicinity of its top end . this air outlet is fitted with a dual louver assembly 40 comprising a set of vertical slats 42 and a set of horizontal slats 44 . during cooling or heating operation of the air conditioner the vertical slats 42 are to be jointly and repeatedly oscillated about their vertical pivots by an electric motor drive unit 46 for correspondingly oscillating the conditioning airstream being discharged through the cool air outlet 26 or warm air outlet 28 . the horizontal slats 44 are to be manually turned about their horizontal pivots for varying the angle of the conditioning air - stream either upwardly or downwardly . molded of plastic material , the water receptacle 16 is to be inserted in the housing 10 through an aperture 48 in its rear wall 34 . a lid 50 openably closes the aperture 48 . a pair of guide plates 52 are firmly erected on the bottom 18 of the housing 10 , one on each side of the water receptacle 16 . placed on the bottom 18 of the housing through the aperture 48 , the water receptacle 16 is to be slid along the pair of upstanding guide plates 52 to its preassigned working position best depicted in fig1 . the lid 50 has a pusher 54 projecting interiorly therefrom to butt on the rear wall of the water receptacle 16 . upon closure of the lid 50 , therefore , the pusher 54 pushes the water receptacle 16 to its working position . open at the top , the water receptacle 16 has its top edge bent outwardly into an l - shaped rim 56 ( fig2 ) for ease of handling by the user . the rim 56 is crimped or curled at 58 for reinforcement . closing the open top of the water receptacle 16 is a cover 60 which may also be molded of plastics material and which rests on the ledge 62 formed by part of the l - shaped rim 56 of the water receptacle . the cover 60 has an elongate aperture 64 defined therein for the passage of the wet band assembly 20 with considerable clearance . a plate 66 depending from the cover 60 in the vicinity of the aperture 64 functions to minimize the waving of the water w in the receptacle 16 upon exertion of external forces on the air conditioner . further , the cover 60 is formed to include a depression 68 for the receipt of water from a replenishing vessel 70 removably mounted thereon . this replenishing vessel has a built - in valve mechanism , not shown , whereby the water receptacle 16 is replenished through an opening 72 in the cover depression 68 to keep the water at a constant level . the housing 10 has an aperture 74 defined in its front wall 38 for the insertion and withdrawal of the replenishing vessel 70 to and from its illustrated working position on the water receptacle cover 60 . a hinged or otherwise openable lid 76 normally holds the aperture 74 closed . the wet band assembly 20 is formed as a discrete unit and is readily withdrawable from within the housing 10 for servicing . as shown in both fig1 and 2 and on an enlarged scale in fig3 the wet band assembly 20 comprises : 1 . a pair of elongate , channeled side frames 78 in parallel spaced relation to each other . 2 . a drive roll 80 and an idler roll 82 rotatably mounted at the opposite extremities of the pair of side frames 78 . 3 . a relatively wide , endless band 84 of generally porous , water - absorbent , air - permeable material , such as that normally used for filtration purposes , wrapped around and extending between the drive and idler rolls 80 and 82 . 4 . a small motor drive unit 86 ( hereinafter referred to as the band motor ) mounted on one of the side frames 78 and coupled to the drive roll 80 for imparting rotation thereto and hence for driving the endless porous band 84 in the direction of the arrows in fig1 . on the opposite sides of the wet band assembly 20 there are provided a pair of support plates 88 in fixed relation to the housing 10 . a pair of channeled guides 90 are affixed respectively to the opposed surfaces of the support plates 88 , sloping rearwardly as they extend upwardly . the wet band assembly 20 , or its pair of side frames 78 , is to slide along the guideways 92 defined by the channeled guides 90 to and away from its working position indicated in fig1 and 2 . preferably the side frames 78 of the wet band assembly should have some transverse play with respect to the respective channeled guides 90 . the rear wall 34 of the housing 10 is further apertured at 94 , fig1 for the introduction and withdrawal of the wet band assembly 20 to and away from its working position . the aperture 94 is provided with a hinged lid 96 pivotable about a pin 98 . disposed immediately interiorly of the aperture 94 is a slot 100 in alignment with the pair of guideways 92 defined by the channeled guides 90 . the wet band assembly 20 has its top end portion held engaged in the slot 100 when it is in the working position . preferably the pair of side frames 78 of the wet band assembly 20 should have their top end portions flared in order that the wet band assembly may not drop too far into the slot 100 . either or both of these top ends of the side frames 78 may be provided with a handle or handles 102 to facilitate the manipulation of the wet band assembly 20 into and out of the housing 10 . thus , on being inserted into the slot 100 in the housing 10 through the aperture 94 , the wet band assembly 20 slides along the pair of opposed guideways 92 until the flaring top end portions of its side frames 78 become caught at the entrance of the slot 100 . in this operating position of the wet band assembly 20 , its idler roll 82 lies wholly in the water w in the receptacle 16 , so that the endless porous band 84 is partly submerged in the water through the aperture 64 in the receptacle cover 60 . as the band motor 86 revolves the drive roll 80 , therefore , the porous band 84 travels over the rolls 80 and 82 while being constantly wetted by the water in the receptacle 16 . it will also be observed from fig1 that the wet band assembly 20 intervenes between air inlet 12 and air outlet 14 in the housing 10 . consequently the airflow a , induced by the fan 22 , passes the porous band 84 on its way from air inlet 12 to air outlet 14 . the fan 22 is mounted within a curved , tapering air duct 104 which functions to guide the airflow a from the wet band assembly 20 to the air outlet 14 . the air duct 104 has a larger entrance end 106 open toward the wet band assembly 20 and a smaller exit end or air passage 108 open toward the air outlet 14 . the fan 22 lies at or adjacent the entrance end 106 of the air duct 104 . mounted exteriorly of the air duct 104 , on one side thereof , is a motor drive unit 110 for the fan 22 . this motor drive unit will hereinafter be referred to as the fan motor in contradistinction to the band motor 86 . with reference to fig1 the damper 24 extends horizontally across the air outlet 14 and so partitions the same into the upper , cool air outlet 26 and the lower , warm air outlet 28 . arranged at or adjacent to the exit end or air passage 108 of the air duct 104 , the damper 24 pivots about a horizontal axis at 112 for selectively communicating the cool air outlet 26 and warm air outlet 28 with the air inlet 12 in coaction with the air duct . fig1 indicates the two operating positions of the damper 24 by the solid and phantom lines . in the solid - line slanting position the damper 24 places the warm air outlet 28 in communication with the air inlet 12 . when pivoted clockwise to the phantom horizontal position , on the other hand , the damper 24 establishes communication between the cool air outlet 26 and air inlet 12 . the electric heater 30 is mounted on that surface of the damper 24 which is directed downwardly when the damper is in the horizontal position in this particular embodiment . the heater 30 is to be energized only when the damper 24 is in the slanting position , heating the air - stream a being discharged through the warm air outlet 28 . in the horizontal position of the damper 24 , on the other hand , the heater 30 is held deenergized and retracted away from the path of the airstream flowing through the cool air outlet 26 . such energization and deenergization of the heater 30 take place automatically as the damper 24 is manually activated between its two working positions . the following description will make clear how the heater 30 is automatically set into and out of operation with the pivotal motion of the damper 24 . fig4 illustrates a manual actuating mechanism 114 for the damper 24 . the manual actuating mechanism 114 includes an arm 116 rigidly anchored at one end on the pivot pin 112 of the damper 24 for joint pivotal motion therewith . the other end of the arm 116 is pin jointed at 118 to one end of a link 120 , the other end of which is likewise pin jointed at 122 to one end of a hand lever 124 . medially pivoted at 126 , the hand lever 124 has a knob 128 on the other end which projects out of the conditioner housing 10 for manipulation by the user . a heater switch 130 is positioned adjacent the hand lever 124 of the damper actuating mechanism 114 . the hand lever 124 has an abutment 132 secured thereto for movement into and out of abutting engagement with the actuator arm 134 of the heater switch 130 . it is clear from the foregoing discussion of fig4 that the manual actuation of the hand lever 124 to the solid line position results in the pivotal motion of the damper 24 to the phantom horizontal position of fig1 . the damper 24 , when in this position , places the cool air outlet 26 in communication with the air inlet 12 . also , when turned to the solid line position of fig4 the hand lever 124 causes the heater switch 130 to deenergize the heater 30 . when pivoted counterclockwise to the phantom position of fig4 on the other hand , the hand lever 124 causes the damper 24 to pivot to the solid - line slanting position of fig1 and hence to communicate the warm air outlet 28 with the air inlet 12 . the heater switch 130 becomes closed upon counterclockwise turn of the hand lever 124 , so that the heater 30 becomes energized to heat the airstream being discharged through the warm air outlet 28 . fig5 is a schematic diagram of a plug - in electric circuitry to be incorporated into the year - round air conditioner of the above - described mechanical construction . the circuitry has a plug 136 for insertion in a service outlet or the like . a pair of supply lines 138 and 140 are connected to the plug 136 , with the supply line 138 having a power switch 142 . connected between the pair of supply lines 138 and 140 are : 1 . a line 144 having a timer switch 146 , a lid switch 148 , a relay coil 150 associated with the power switch 142 , and a current limit switch 152 . 3 . a line 158 having the heater switch or warm switch 130 , the heater 30 and , in parallel with the latter , a warm pilot lamp 160 . 4 . lines 162 and 164 having the fan motor 110 capable of operation at a high or low speed , and a capacitor 166 . 6 . a line 170 having a cool switch 172 and a cool pilot lamp 174 . as shown also in fig1 the lid switch 148 on the line 144 is to be activated by the hinged lid 96 normally closing the aperture 94 through which the wet band assembly 20 is inserted in and withdrawn from the conditioner housing 10 . the warm switch 130 and the cool switch 172 are coordinated with each other in such a manner that one is opened when the other is closed , and vice versa . the circuitry of fig5 further includes a rotary multicontact switch 176 for the on - off control of the two - speed fan motor 110 and the band motor 86 . the rotary switch comprises an annular row of fixed contacts designated 1 through 7 , and a dual movable contact 178 capable of simultaneous engagement with any two diametrically opposed fixed contacts . the operational description of the year - round air conditioner follows . for the production of warm , moist air the user may close the power switch 142 , operate the movable contact 178 of the rotary switch 176 into engagement either with the fixed contacts 1 and 5 or with the fixed contacts 2 and 6 , and turn the hand lever 124 of the damper actuating mechanism 114 to the phantom position of fig4 . the power pilot lamp 156 glows upon closure of the power switch 142 . the simultaneous engagement of the movable contact 178 of the rotary switch 176 with the fixed contacts 1 and 5 , or 2 and 6 , results in the operation of both the band motor 86 and the fan motor 110 . driven by the fan motor 110 at high or low speed , the fan 22 draws room air into the conditioner housing 10 through the filter screen 36 at the air inlet 12 . within the housing 10 the filtered airstream a passes the wetted porous band 84 traveling over the pair of rolls 80 and 82 , thereby to be both moistened and refiltered . then the dust - free moist air enters the duct 104 . as the hand lever 124 of the damper actuating mechanism 114 is activated as above , the damper 24 pivots to the solid - line slanting position of fig1 thereby placing the warm air outlet 28 in communication with the air inlet 12 . simultaneously the warm switch 130 becomes closed by the hand lever 124 to cause the heater 30 to be energized and the warm pilot lamp 160 to glow . thus the heater 30 heats the filtered , moistened air as it flows through the warm air outlet 28 out into the room . positioned at the relatively constricted part of the airflow path , the heater 30 can effectively heat the air to a required temperature range in spite of its limited capacity . further , the damper 24 in its slanting position coacts with the air duct 104 to direct the stream of warm , moist air downwardly through the warm air outlet 28 , toward the floor , for most efficiently heating the room . for the production of warm air without humidification the user may operate the rotary switch 176 to move one of the arms of its movable contact 178 into engagement with either the fixed contact 4 or 7 . then only the fan motor 110 will be set into operation , with the band motor 86 held out of operation . for cooling the room , on the other hand , the user may close the power switch 142 , actuate the movable contact 178 of the rotary switch 176 into engagement either with the fixed contacts 1 and 5 or with the fixed contacts 2 and 6 , and manipulate the hand lever 124 of the damper actuating mechanism 114 to the solid line position of fig4 . thus the band motor 86 and the fan motor 110 are both set into operation as in the above described case of warm , moist air supply . drawn by the fan 22 into the conditioner housing 10 through the filter screen 36 at the air inlet 12 , the air passes the wetted porous band 84 thereby to be cooled by the evaporative cooling process , besides being refiltered . the hand lever 124 when turned to the solid line position of fig4 causes the damper 24 to pivot to the phantom horizontal position of fig1 . thereupon the exit end 108 of the air duct 104 opens to the cool air outlet 26 . the hand lever 124 also opens the warm switch 130 . as has been stated , the opening of the warm switch 130 results in the closure of the cool switch 172 , with the consequent glowing of the cool pilot lamp 174 . after passing the air duct 104 , the cool , clean air is directed by the damper 24 into and through the cool air outlet 26 out into the room . it should be appreciated that the cool airstream encounters no obstacle at all on its way from fan 22 to cool air outlet 26 . accordingly the cool air will be produced noiselessly at a sufficiently high flow rate . while one embodiment of the invention has been shown and described herein , it will be understood that it is illustrative only and not to be taken as a definition of the scope of the invention . a variety of modifications will readily occur to one skilled in the art on the basis of this disclosure . an example is the location of the heater 30 . although this heater is shown to be mounted on the pivotal damper 24 in the illustrated embodiment , it may be fixedly positioned anywhere at or adjacent the warm air outlet so as not to run counter to the objectives of the invention . this and other modifications or alterations of the invention may be resorted to within the broad teaching hereof ; hence the invention should be accorded the full scope of the following claims so as to embrace any and all equivalent devices . | 5 |
all numbers used herein , including those in the examples and claims , should be understood as being modified by the term “ about ” unless otherwise stated , such as with a specified precision . unless expressly stated to the contrary , all ranges cited herein are inclusive . as used herein , the singular forms “ a ,” “ an ,” and “ the ” include plural reference unless the context dictates otherwise . the terms “ scy - 078 ” and “ compound 1 ” refer to the compound shown below , and refer to the freebase form unless otherwise indicated . another name for scy - 078 is ( 1s , 4ar , 6as , 7r , 8r , 10ar , 10br , 12ar , 14r , 15r )- 15 -[[( 2r )- 2 - amino - 2 , 3 , 3 - trimethylbutyl ] oxy ]- 8 -[( 1r )- 1 , 2 - dimethylpropyl ]- 1445 -( 4 - pyridinyl )- 1h - 1 , 2 , 4 - triazol - 1 - yl ]- 1 , 6 , 6a , 7 , 8 , 9 , 10 , 10a , 10b , 11 , 12 , 12a - dodecahydro - 1 , 6a , 8 , 10a - tetramethyl - 4h - 4a - propano - 2h - phenanthro [ 1 , 2 - c ] pyran - 7 - carboxylic acid . the terms “ pharmaceutically acceptable salt ” and the like should be understood to include , but not limited to , citrate salts , hippurate salts , fumarate salts , glycolate salts , mesylate salts , and calcium salts . as used here , phrases such as “ scy - 078 salt ,” “ scy - 078 salts ,” “ salt of scy - 078 ,” “ salts of scy - 078 ,” “ pharmaceutically acceptable salt of scy - 078 ,” and “ pharmaceutically acceptable salts thereof ” should be understood to be salts in various forms , for example , the polymorphs disclosed herein . in addition , as used here , phrases such as “ scy - 078 phosphate ,” “ scy - 078 citrate ,” “ scy - 078 hippurate ,” “ scy - 078 glycolate ,” “ scy - 078 mesylate ,” “ scy - 078 fumarate ,” and “ scy - 078 calcium ” should be understood to be salts in various forms , for example , the polymorphs disclosed herein . the term “ solvent ” and the like refer to any appropriate aqueous or organic solvent . solvents include , but are not limited to , methanol , acetic acid , tetrahydrofuran , 2 methyl - tetrahydrofuran , 1 , 4 - dioxane , n - methyl - 2 - pyrrolidone , dimethyl sulfoxide , dimethylacetamide , isopropyl alcohol , acetonitrile , acetone , ethyl acetate , water and mixtures thereof . the term “ pharmaceutically acceptable carrier ” and the like refer to an ingredient that is compatible with scy - 078 and is not harmful to a patient &# 39 ; s health . pharmaceutically acceptable carriers include , but are not limited to , one or more of the following : aqueous vehicles and solvents , such as water , saline solutions , and alcohols ; buffers ; surface active agents ; dispersing agents ; inert diluents ; preservatives ; suspending agents ; emulsifying agents ; demulcents ; thickening agents ; emulsifying agents ; antioxidants ; and stabilizing agents . other additional ingredients that may be included in the pharmaceutical compositions of the disclosure are generally known in the art and may be described , for example , in remington &# 39 ; s pharmaceutical sciences , mack publishing co ., easton , pa ., which is incorporated by reference herein . the term “ injection ” and the like refer to the insertion of a composition into the body by syringe , hollow needle , or the like . the term “ injection ” and the like include , but are not limited to , intravenous injections , including those entailing administering using an iv bag containing a diluent . the term “ effective amount ” refers to an amount of the active ingredient that , when administered to a subject , alleviates at least some of the symptoms or stops the progression of the identified disease or condition . the terms “ disease ” or “ condition ” include , but are not limited to , infections such as fungal infections . exemplary dosage amounts can be found , for example , in u . s . pat . no . 8 , 188 , 085 , the relevant portions of which are incorporated herein by reference . the term “ å ” refers to angstroms . terms such as “ 2θ ” or “ 2 th .” refer to degrees 2 theta . the xrpd peaks recited herein should be understood to reflect a precision of ± 0 . 2 for the 2 theta peaks , and the equivalent precision for d - spacings as per bragg &# 39 ; s law . the present disclosure also fully incorporates section 941 of the united states pharmacopeia . the national formulary from 2014 ( usp 37 / nf 32 , volume 1 ) relating to characterization of crystalline and partially crystalline solids by x - ray powder diffraction . the present disclosure relates to , among other things , pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , glycolate , mesylate , fumarate , and calcium . in one embodiment , the salt is selected from citrate , hippurate , mesylate , and fumarate . in a further embodiment , the scy - 078 salt is selected from scy - 078 hippurate type a , scy - 078 hippurate type b , and scy - 078 hippurate type c . in another embodiment , the scy - 078 salt is selected from scy - 078 fumarate type a and scy - 078 fumarate type b . in yet another embodiment , the salt is a scy - 078 citrate salt . in yet a further embodiment , the salt is scy - 078 citrate type a . the present disclosure further relates to pharmaceutically acceptable salts of scy - 078 that have a chemical purity of at least 90 %. in another embodiment , pharmaceutically acceptable salts of scy - 078 have a chemical purity of at least 95 %. in a further embodiment , pharmaceutically acceptable salts of scy - 078 have a chemical purity of at least 98 %. in yet another embodiment , pharmaceutically acceptable salts of scy - 078 have a chemical purity of at least 99 %. in still another embodiment , the present disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a chemical purity of at least 90 %, at least 95 %, at least 98 %, or at least 99 %. the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 that have a kinetic solubility of at least 2 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 4 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 2 mg / ml to 5 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 4 mg / ml to 5 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in still another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility greater than scy - 078 ( as a freebase ) at 4 hours in dextrose buffer at ph 5 . 5 . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 that have a kinetic solubility of at least 2 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 4 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 8 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in a further embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 2 mg / ml to 9 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 4 mg / ml to 9 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in still another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 8 mg / ml to 9 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 2 mg / ml to 5 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in one embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 4 mg / ml to 5 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in yet another embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 2 mg / ml to 9 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in still another embodiment , the disclosure also relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 4 mg / ml to 9 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in another embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 8 mg / ml to 9 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 that have a kinetic solubility of at least 2 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 4 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 2 mg / ml to 5 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 4 mg / ml to 5 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in still another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 4 . 5 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 7 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 4 . 5 mg / ml to 8 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 7 mg / ml to 8 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 1 mg / ml to 5 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in one embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 4 mg / ml to 5 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in another embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 4 mg / ml to 8 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . in yet another embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 7 mg / ml to 8 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 that have a kinetic solubility of at least 16 mg / ml at 1 hour in sgf media . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 17 mg / ml at 1 hour in sgf media . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 18 mg / ml at 1 hour in sgf media . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 20 mg / ml at 1 hour in sgf media . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 that have a kinetic solubility of from 17 mg / ml to 21 mg / ml at 1 hour in sgf media . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 18 mg / ml to 21 mg / ml at 1 hour in sgf media . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 20 mg / ml to 21 mg / ml at 1 hour in sgf media . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 12 mg / ml to 21 mg / ml at 1 hour in sgf media . in one embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 13 mg / ml to 21 mg / ml at 1 hour in sgf media . in another embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 18 mg / ml to 21 mg / ml at 1 hour in sgf media . in yet another embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 20 mg / ml to 21 mg / ml at 1 hour in sgf media . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 that have a kinetic solubility of at least 17 mg / ml at 24 hours in fassif media . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of at least 22 mg / ml at 24 hours in fassif media . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 17 mg / ml to 22 mg / ml at 24 hours in fassif media . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a kinetic solubility of from 21 mg / ml to 22 mg / ml at 24 hours in fassif media . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 17 mg / ml to 22 mg / ml at 24 hours in fassif media . in one embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a kinetic solubility of from 21 mg / ml to 22 mg / ml at 24 hours in fassif media . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 having any of the disclosed kinetic solubilities and having a water sorption of not greater than 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . in one embodiment , the pharmaceutically acceptable salts of scy - 078 have a water sorption of from 2 % to 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . in another embodiment , the pharmaceutically acceptable salts of scy - 078 have a water sorption of from 3 % to 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . in yet another embodiment , the pharmaceutically acceptable salts of scy - 078 have a water sorption of from 6 % to 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . the present disclosure additionally relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a water sorption of from 2 % to 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . in one embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a water sorption of from 3 % to 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . in one embodiment , the disclosure relates to pharmaceutically acceptable salts of scy - 078 , wherein the salt is selected from citrate , hippurate , mesylate , and fumarate , and wherein the salt has a water sorption of from 6 % to 7 % at 25 ° c . and 80 % relative humidity as determined by dvs . the present disclosure further relates to hippurate salts of scy - 078 , such as scy - 078 hippurate type a , scy - 078 hippurate type b , and scy - 078 hippurate type c . in one embodiment , the scy - 078 hippurate type a has an xrpd pattern comprising peaks at one or more of the following locations : table a fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 6 . 276484 353 . 472400 0 . 102336 14 . 08226 12 . 90 7 . 023845 139 . 782300 0 . 307008 12 . 58545 5 . 10 7 . 900725 1475 . 766000 0 . 127920 11 . 19048 53 . 85 8 . 241444 302 . 522300 0 . 102336 10 . 72859 11 . 04 9 . 723080 945 . 921800 0 . 089544 9 . 09681 34 . 52 11 . 283030 414 . 659200 0 . 102336 7 . 84238 15 . 13 11 . 492390 300 . 886600 0 . 076752 7 . 69998 10 . 98 12 . 610210 2740 . 558000 0 . 089544 7 . 01982 100 . 00 12 . 910370 765 . 158500 0 . 063960 6 . 85728 27 . 92 13 . 561180 243 . 791900 0 . 153504 6 . 52963 8 . 90 14 . 149930 371 . 812900 0 . 102336 6 . 25924 13 . 57 15 . 182550 1607 . 490000 0 . 102336 5 . 83577 58 . 66 15 . 806230 690 . 955800 0 . 179088 5 . 60688 25 . 21 16 . 673670 482 . 323700 0 . 179088 5 . 31709 17 . 60 17 . 068480 365 . 833300 0 . 127920 5 . 19498 13 . 35 18 . 200570 206 . 779900 0 . 153504 4 . 87432 7 . 55 18 . 933070 395 . 979900 0 . 153504 4 . 68736 14 . 45 19 . 293830 277 . 037400 0 . 102336 4 . 60052 10 . 11 19 . 924160 251 . 428800 0 . 204672 4 . 45638 9 . 17 20 . 583290 158 . 800000 0 . 204672 4 . 31514 5 . 79 21 . 951230 220 . 614300 0 . 153504 4 . 04923 8 . 05 23 . 477450 72 . 922780 0 . 409344 3 . 78934 2 . 66 24 . 511240 99 . 987140 0 . 255840 3 . 63181 3 . 65 24 . 954920 117 . 325600 0 . 153504 3 . 56824 4 . 28 25 . 993010 108 . 058000 0 . 204672 3 . 42804 3 . 94 28 . 257860 72 . 489400 0 . 409344 3 . 15822 2 . 65 31 . 063590 95 . 037750 0 . 179088 2 . 87907 3 . 47 31 . 653730 62 . 090590 0 . 307008 2 . 82673 2 . 27 for example , the scy - 078 hippurate type a has an xrpd pattern comprising one or more peaks at d - spacings of 11 . 20 , 7 . 02 , and 5 . 84 a . in another example , the scy - 078 hippurate type a has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 90 , 12 . 6 , and 15 . 18 . in one embodiment , the scy - 078 hippurate type b has an xrpd pattern comprising peaks at one or more of the following locations : table b fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 887601 118 . 925500 0 . 102336 15 . 01151 9 . 56 6 . 889384 462 . 675400 0 . 063960 12 . 83077 37 . 19 7 . 277837 251 . 176000 0 . 051168 12 . 14678 20 . 19 8 . 767134 927 . 066800 0 . 076752 10 . 08643 74 . 52 9 . 945603 1143 . 995000 0 . 102336 8 . 89377 91 . 96 10 . 843500 681 . 448200 0 . 102336 8 . 15925 54 . 78 11 . 822440 140 . 502200 0 . 127920 7 . 48575 11 . 29 12 . 417990 1244 . 014000 0 . 089544 7 . 12805 100 . 00 13 . 714490 435 . 466500 0 . 089544 6 . 45698 35 . 00 14 . 608760 1242 . 496000 0 . 102336 6 . 06367 99 . 88 15 . 050420 474 . 015800 0 . 102336 5 . 88670 38 . 10 16 . 071560 476 . 890000 0 . 127920 5 . 51491 38 . 33 16 . 476910 708 . 831400 0 . 102336 5 . 38014 56 . 98 16 . 857150 185 . 689200 0 . 102336 5 . 25963 14 . 93 17 . 289970 422 . 781900 0 . 127920 5 . 12893 33 . 99 17 . 612420 996 . 474200 0 . 089544 5 . 03575 80 . 10 18 . 405510 186 . 288500 0 . 153504 4 . 82051 14 . 97 19 . 118560 303 . 851800 0 . 127920 4 . 64230 24 . 43 19 . 623870 158 . 474700 0 . 153504 4 . 52389 12 . 74 20 . 218430 314 . 377200 0 . 153504 4 . 39218 25 . 27 21 . 746130 200 . 050600 0 . 153504 4 . 08695 16 . 08 23 . 075880 129 . 668200 0 . 204672 3 . 85436 10 . 42 23 . 853540 106 . 856400 0 . 204672 3 . 73044 8 . 59 25 . 372290 96 . 670350 0 . 204672 3 . 51048 7 . 77 29 . 216870 66 . 396300 0 . 230256 3 . 05670 5 . 34 32 . 714200 31 . 053470 0 . 614016 2 . 73748 2 . 50 for example , the scy - 078 hippurate type b has an xrpd pattern comprising one or more peaks at d - spacings of 8 . 90 , 7 . 13 , and 6 . 10 a . in another example , the scy - 078 hippurate type b has an xrpd pattern comprising one or more peaks at degrees 2 theta of 9 . 95 , 12 . 42 , and 14 . 61 . in one embodiment , the scy - 078 hippurate type c has an xrpd pattern comprising peaks at one or more of the following locations : table c pos . fwhm [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 3 . 027072 11818 . 150000 0 . 051168 29 . 18766 100 . 00 5 . 916137 351 . 270000 0 . 102336 14 . 93916 2 . 97 6 . 916698 947 . 910600 0 . 102336 12 . 78016 8 . 02 7 . 251646 624 . 847700 0 . 076752 12 . 19059 5 . 29 8 . 761702 1828 . 733000 0 . 076752 10 . 09268 15 . 47 9 . 962105 2404 . 236000 0 . 102336 8 . 87907 20 . 34 10 . 897800 1593 . 408000 0 . 102336 8 . 11872 13 . 48 11 . 868550 552 . 254500 0 . 102336 7 . 45677 4 . 67 12 . 432300 2880 . 441000 0 . 127920 7 . 11988 24 . 37 12 . 857840 525 . 634600 0 . 076752 6 . 88518 4 . 45 13 . 091360 511 . 764400 0 . 115128 6 . 76288 4 . 33 13 . 709840 1112 . 219000 0 . 102336 6 . 45916 9 . 41 14 . 555290 3086 . 294000 0 . 153504 6 . 08582 26 . 11 14 . 984610 1215 . 693000 0 . 102336 5 . 91241 10 . 29 15 . 341160 506 . 870800 0 . 153504 5 . 77579 4 . 29 16 . 136210 1315 . 742000 0 . 089544 5 . 49296 11 . 13 16 . 453540 1710 . 358000 0 . 153504 5 . 38772 14 . 47 16 . 897030 606 . 324900 0 . 102336 5 . 24730 5 . 13 17 . 280760 1171 . 798000 0 . 127920 5 . 13164 9 . 92 17 . 591700 2258 . 867000 0 . 102336 5 . 04163 19 . 11 18 . 190770 538 . 754800 0 . 127920 4 . 87692 4 . 56 18 . 425670 516 . 831300 0 . 179088 4 . 81528 4 . 37 19 . 151570 950 . 084500 0 . 102336 4 . 63437 8 . 04 19 . 602330 487 . 956400 0 . 127920 4 . 52881 4 . 13 20 . 234760 861 . 917600 0 . 153504 4 . 38867 7 . 29 20 . 860030 424 . 598600 0 . 153504 4 . 25851 3 . 59 21 . 725360 459 . 496200 0 . 307008 4 . 09081 3 . 89 22 . 532320 498 . 240700 0 . 102336 3 . 94610 4 . 22 23 . 078810 380 . 947900 0 . 127920 3 . 85388 3 . 22 23 . 551950 208 . 488500 0 . 409344 3 . 77752 1 . 76 23 . 874020 377 . 598600 0 . 102336 3 . 72728 3 . 20 25 . 381750 351 . 553600 0 . 102336 3 . 50919 2 . 97 25 . 844490 207 . 070300 0 . 204672 3 . 44740 1 . 75 27 . 188450 192 . 463400 0 . 153504 3 . 27997 1 . 63 27 . 681830 144 . 369000 0 . 307008 3 . 22262 1 . 22 29 . 319670 172 . 870900 0 . 511680 3 . 04622 1 . 46 30 . 833510 86 . 432220 0 . 307008 2 . 90002 0 . 73 34 . 979000 90 . 330020 0 . 204672 2 . 56525 0 . 76 35 . 588330 69 . 479680 0 . 307008 2 . 52271 0 . 59 37 . 270360 55 . 666410 0 . 307008 2 . 41264 0 . 47 for example , the scy - 078 hippurate type c has an xrpd pattern comprising one or more peaks at d - spacings of 29 . 19 , 8 . 88 , 7 . 12 , and 6 . 09 å . in another example , the scy - 078 hippurate type c has an xrpd pattern comprising one or more peaks at degrees 2 theta of 3 . 03 , 9 . 96 , 12 . 43 , and 14 . 56 . the present disclosure further relates to fumarate salts of scy - 078 , such as scy - 078 fumarate type a and scy - 078 fumarate type b . in one embodiment , the scy - 078 fumarate type a has an xrpd pattern comprising peaks at one or more of the following locations : table d fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 7 . 747007 167 . 350400 0 . 153504 11 . 41218 2 . 00 8 . 493147 8373 . 572000 0 . 102336 10 . 41119 100 . 00 9 . 346397 181 . 715800 0 . 204672 9 . 46257 2 . 17 9 . 931064 167 . 355100 0 . 153504 8 . 90676 2 . 00 10 . 442940 371 . 960600 0 . 089544 8 . 47130 4 . 44 10 . 706620 463 . 482500 0 . 076752 8 . 26326 5 . 54 11 . 231160 490 . 618200 0 . 153504 7 . 87848 5 . 86 13 . 030860 311 . 426800 0 . 102336 6 . 79415 3 . 72 13 . 700070 569 . 254300 0 . 102336 6 . 46374 6 . 80 14 . 895760 234 . 024600 0 . 153504 5 . 94748 2 . 79 15 . 204970 269 . 752200 0 . 153504 5 . 82722 3 . 22 16 . 350790 434 . 953000 0 . 127920 5 . 42135 5 . 19 16 . 976580 3015 . 489000 0 . 115128 5 . 22289 36 . 01 17 . 726110 1152 . 135000 0 . 230256 5 . 00370 13 . 76 18 . 205910 303 . 920500 0 . 102336 4 . 87290 3 . 63 18 . 863510 267 . 939100 0 . 153504 4 . 70449 3 . 20 20 . 164360 63 . 804870 0 . 409344 4 . 40383 0 . 76 20 . 898390 184 . 877000 0 . 102336 4 . 25078 2 . 21 21 . 419940 168 . 417300 0 . 102336 4 . 14844 2 . 01 22 . 228150 318 . 867400 0 . 127920 3 . 99940 3 . 81 23 . 936960 77 . 330220 0 . 307008 3 . 71763 0 . 92 25 . 533030 318 . 681700 0 . 089544 3 . 48874 3 . 81 26 . 114530 59 . 303240 0 . 204672 3 . 41236 0 . 71 26 . 883130 111 . 136200 0 . 204672 3 . 31652 1 . 33 30 . 876670 38 . 684340 0 . 614016 2 . 89607 0 . 46 for example , the scy - 078 fumarate type a has an xrpd pattern comprising one or more peaks at d - spacings of 10 . 41 , 5 . 22 , and 5 . 00 a . in another example , the scy - 078 fumarate type a has an xrpd pattern comprising one or more peaks at degrees 2 theta of 8 . 49 , 16 . 98 , and 17 . 73 . in one embodiment , the scy - 078 fumarate type b has an xrpd pattern comprising peaks at one or more of the following locations : table e fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 449312 94 . 567020 0 . 307008 16 . 21786 19 . 92 6 . 318422 110 . 456500 0 . 409344 13 . 98888 23 . 26 9 . 799620 153 . 670200 0 . 614016 9 . 02593 32 . 36 10 . 577440 403 . 264100 0 . 255840 8 . 36388 84 . 93 10 . 995710 322 . 682700 0 . 089544 8 . 04665 67 . 96 11 . 970210 133 . 555200 0 . 307008 7 . 39367 28 . 13 13 . 136230 472 . 855300 0 . 102336 6 . 73989 99 . 58 13 . 551710 408 . 076200 0 . 102336 6 . 53417 85 . 94 14 . 201760 320 . 510900 0 . 204672 6 . 23651 67 . 50 15 . 712210 472 . 732700 0 . 076752 5 . 64022 99 . 56 16 . 216750 474 . 828900 0 . 076752 5 . 46586 100 . 00 16 . 849640 211 . 687300 0 . 204672 5 . 26195 44 . 58 20 . 391740 103 . 586500 0 . 358176 4 . 35524 21 . 82 21 . 343910 97 . 997770 0 . 409344 4 . 16305 20 . 64 28 . 564840 34 . 739620 0 . 614016 3 . 12498 7 . 32 for example , the scy - 078 fumarate type b has an xrpd pattern comprising one or more peaks at d - spacings of 8 . 36 , 6 . 74 , 6 . 53 , 5 . 64 , and 5 . 47 å . in another example , the scy - 078 fumarate type b has an xrpd pattern comprising one or more peaks at degrees 2 theta of 10 . 58 , 13 . 14 , 13 . 55 , 15 . 71 , and 16 . 22 . the present disclosure further relates to glycolate salts of scy - 078 . in one embodiment , the scy - 078 glycolate has an xrpd pattern comprising peaks at one or more of the following locations : table f fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 7 . 879599 291 . 814000 0 . 127920 11 . 22044 54 . 74 8 . 983378 233 . 086200 0 . 204672 9 . 84412 43 . 72 9 . 855934 117 . 677600 0 . 153504 8 . 97448 22 . 07 11 . 483230 269 . 580500 0 . 204672 7 . 70610 50 . 56 12 . 311460 163 . 106800 0 . 358176 7 . 18949 30 . 59 14 . 259570 285 . 813400 0 . 179088 6 . 21136 53 . 61 14 . 651000 437 . 366100 0 . 102336 6 . 04628 82 . 04 15 . 433320 533 . 138100 0 . 102336 5 . 74151 100 . 00 16 . 892280 103 . 441500 0 . 614016 5 . 24877 19 . 40 18 . 826490 177 . 863500 0 . 204672 4 . 71365 33 . 36 20 . 401140 101 . 236100 0 . 307008 4 . 35325 18 . 99 21 . 743970 54 . 436950 0 . 614016 4 . 08735 10 . 21 24 . 981860 29 . 298130 0 . 614016 3 . 56445 5 . 50 for example , the scy - 078 glycolate has an xrpd pattern comprising one or more peaks at d - spacings of 11 . 22 , 6 . 21 , 6 . 05 , and 5 . 74 a . in another example , the scy - 078 glycolate has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 88 , 14 . 26 , 14 . 65 , and 15 . 43 . the present disclosure further relates to mesylate salts of scy - 078 . in one embodiment , the scy - 078 mesylate has an xrpd pattern comprising peaks at one or more of the following locations : table g fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 321569 44 . 016770 0 . 307008 16 . 60688 3 . 75 6 . 654286 233 . 467600 0 . 076752 13 . 28355 19 . 89 8 . 041747 243 . 835400 0 . 204672 10 . 99455 20 . 77 9 . 224843 236 . 712900 0 . 153504 9 . 58698 20 . 16 10 . 179890 547 . 128100 0 . 089544 8 . 68960 46 . 60 10 . 532080 592 . 551800 0 . 089544 8 . 39980 50 . 47 11 . 692820 225 . 932500 0 . 409344 7 . 56843 19 . 24 12 . 670270 361 . 926000 0 . 102336 6 . 98668 30 . 83 14 . 316750 537 . 652200 0 . 102336 6 . 18668 45 . 80 14 . 751260 1174 . 011000 0 . 102336 6 . 00541 100 . 00 15 . 645660 347 . 928600 0 . 204672 5 . 66406 29 . 64 16 . 537910 485 . 586600 0 . 179088 5 . 36043 41 . 36 17 . 477180 328 . 731900 0 . 127920 5 . 07441 28 . 00 18 . 838670 252 . 134300 0 . 307008 4 . 71063 21 . 48 19 . 613670 351 . 448500 0 . 153504 4 . 52622 29 . 94 21 . 008230 254 . 102200 0 . 204672 4 . 22880 21 . 64 22 . 068870 130 . 646600 0 . 307008 4 . 02791 11 . 13 23 . 475460 151 . 601600 0 . 204672 3 . 78965 12 . 91 25 . 592960 130 . 952000 0 . 153504 3 . 48071 11 . 15 for example , the scy - 078 mesylate has an xrpd pattern comprising one or more peaks at d - spacings of 10 . 99 , 6 . 99 , and 6 . 01 å . in another example , the scy - 078 mesylate has an xrpd pattern comprising one or more peaks at degrees 2 theta of 8 . 04 , 12 . 67 , and 14 . 75 . the present disclosure further relates to calcium salts of scy - 078 . in one embodiment , the scy - 078 calcium has an xrpd pattern comprising peaks at one or more of the following locations : table h fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 330948 1222 . 647000 0 . 063960 16 . 57768 100 . 00 8 . 684942 82 . 143680 0 . 307008 10 . 18170 6 . 72 9 . 624508 215 . 229600 0 . 127920 9 . 18975 17 . 60 10 . 625810 286 . 722000 0 . 153504 8 . 32591 23 . 45 13 . 358050 110 . 336200 0 . 307008 6 . 62846 9 . 02 14 . 092620 101 . 325400 0 . 307008 6 . 28456 8 . 29 15 . 952080 1188 . 492000 0 . 153504 5 . 55594 97 . 21 16 . 282720 334 . 685300 0 . 153504 5 . 44386 27 . 37 17 . 853110 104 . 842700 0 . 153504 4 . 96839 8 . 58 19 . 638160 74 . 407610 0 . 307008 4 . 52063 6 . 09 29 . 434800 171 . 668200 0 . 204672 3 . 03457 14 . 04 30 . 178030 59 . 353870 0 . 153504 2 . 96150 4 . 85 31 . 428330 37 . 765730 0 . 307008 2 . 84648 3 . 09 for example , the scy - 078 calcium has an xrpd pattern comprising one or more peaks at d - spacings of 16 . 58 , 5 . 56 , and 5 . 44 a . in another example , the scy - 078 calcium has an xrpd pattern comprising one or more peaks at degrees 2 theta of 5 . 33 , 15 . 95 , and 16 . 28 . the present disclosure further relates to citrate salts of scy - 078 , such as scy - 078 citrate type a , type b , type e , type f , type m , type n , type 0 , type q , type r , and type s . in one embodiment , the citrate salt of scy - 078 comprises at least one of type a , type b , type e , type f , type m , type n , type 0 , type q , type r , and type s . the present disclosure further relates to a citrate salt of scy - 078 comprising type a . in one embodiment , the citrate salt of scy - 078 consists essentially of type a . in another embodiment , the citrate salt of scy - 078 comprises at least 98 % type a . in a further embodiment , the citrate salt of scy - 078 comprises at least 99 % type a . in one embodiment , the scy - 078 citrate type a is stable for at least 1 week when stored at 60 ° c . in another embodiment , the scy - 078 citrate type a is stable for at least 1 week when stored at 25 ° c . and 60 % relative humidity . in a further embodiment , the scy - 078 citrate type a is stable for at least 1 week when stored at 40 ° c . and 75 % relative humidity . in a further embodiment , the scy - 078 citrate type a has an equilibrium solubility of 38 mg / ml in non - buffered water at ambient temperature . in yet another embodiment , the scy - 078 citrate type a has an approximate solubility of from 40 mg / ml to 42 mg / ml at room temperature in at least one solvent selected from methanol , isopropyl alcohol , acetic acid , tetrahydrofuran , 2 methyl - tetrahydrofuran , 1 , 4 - dioxane , n - methyl - 2 - pyrrolidone , dimethyl sulfoxide , and dimethylacetamide . in still another embodiment , the scy - 078 citrate type a has a water sorption of 6 % at 25 ° c . and 80 % relative humidity as determined by dvs . in one embodiment , the scy - 078 citrate type a has a kinetic solubility of 4 mg / ml at 4 hours in dextrose buffer at ph 5 . 5 . in another embodiment , the scy - 078 citrate type a has a kinetic solubility of 8 mg / ml at 24 hours in dextrose buffer at ph 5 . 5 . in a further embodiment , the scy - 078 citrate type a has a kinetic solubility of 5 mg / ml at 4 hours in phosphate buffer at ph 6 . 0 . in still another embodiment , the scy - 078 citrate type a has a kinetic solubility of 8 mg / ml at 24 hours in phosphate buffer at ph 6 . 0 . in one embodiment , the scy - 078 citrate type a has a kinetic solubility of 21 mg / ml at 1 hour in sgf media . in another embodiment , the scy - 078 citrate type a has a kinetic solubility of 4 mg / ml at 24 hours in fessif media . in yet another embodiment , the scy - 078 citrate type a has a kinetic solubility of 10 mg / ml at 1 hour in fassif media . in a further embodiment , the scy - 078 citrate type a has a kinetic solubility of 21 mg / ml at 4 hours in fassif media . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type a . in one embodiment , the scy - 078 citrate type a has an xrpd pattern comprising peaks at one or more of the following locations : table i pos . fwhm [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 400273 434 . 322700 0 . 102336 16 . 36502 3 . 34 7 . 453872 13000 . 820000 0 . 191880 11 . 86031 100 . 00 9 . 201639 691 . 948300 0 . 204672 9 . 61110 5 . 32 10 . 831710 404 . 555000 0 . 153504 8 . 16811 3 . 11 11 . 485080 936 . 115200 0 . 179088 7 . 70486 7 . 20 12 . 491050 954 . 805500 0 . 179088 7 . 08652 7 . 34 13 . 191360 1776 . 320000 0 . 204672 6 . 71184 13 . 66 15 . 020350 1342 . 537000 0 . 204672 5 . 89842 10 . 33 15 . 664830 532 . 278900 0 . 179088 5 . 65717 4 . 09 15 . 955570 613 . 057500 0 . 127920 5 . 55474 4 . 72 16 . 751250 951 . 729000 0 . 153504 5 . 29264 7 . 32 17 . 978130 170 . 323300 0 . 204672 4 . 93412 1 . 31 19 . 591770 472 . 971000 0 . 204672 4 . 53123 3 . 64 22 . 213400 146 . 982900 0 . 204672 4 . 00202 1 . 13 23 . 845740 34 . 469910 0 . 614016 3 . 73164 0 . 27 25 . 160050 117 . 741100 0 . 307008 3 . 53961 0 . 91 28 . 761350 129 . 234400 0 . 255840 3 . 10407 0 . 99 30 . 356250 332 . 945100 0 . 230256 2 . 94452 2 . 56 32 . 317870 87 . 151140 0 . 307008 2 . 77014 0 . 67 34 . 725480 74 . 664570 0 . 511680 2 . 58339 0 . 57 for example , the scy - 078 citrate type a has an xrpd pattern comprising one or more peaks at d - spacings of 11 . 86 , 7 . 70 , 7 . 09 , 6 . 71 , 5 . 90 , and 5 . 29 å . in another example , the scy - 078 citrate type a has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 45 , 11 . 49 , 12 . 49 , 13 . 19 , 15 . 02 , and 16 . 75 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type b . in one embodiment , the scy - 078 citrate type b has an xrpd pattern comprising peaks at one or more of the following locations : table j fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 561437 214 . 772000 0 . 127920 15 . 89114 18 . 87 6 . 920576 1138 . 274000 0 . 115128 12 . 77301 100 . 00 9 . 319721 77 . 009080 0 . 307008 9 . 48959 6 . 77 11 . 144180 155 . 075600 0 . 153504 7 . 93978 13 . 62 11 . 729970 201 . 281900 0 . 153504 7 . 54455 17 . 68 13 . 405240 187 . 402700 0 . 358176 6 . 60523 16 . 46 15 . 225970 237 . 746900 0 . 204672 5 . 81923 20 . 89 16 . 813690 449 . 144100 0 . 153504 5 . 27312 39 . 46 18 . 219030 148 . 764600 0 . 204672 4 . 86942 13 . 07 19 . 324790 108 . 017600 0 . 153504 4 . 59322 9 . 49 20 . 531330 143 . 254500 0 . 127920 4 . 32594 12 . 59 23 . 721410 34 . 728650 0 . 307008 3 . 75092 3 . 05 26 . 000800 68 . 151450 0 . 204672 3 . 42703 5 . 99 29 . 343000 18 . 852780 0 . 614016 3 . 04385 1 . 66 for example , the scy - 078 citrate type b has an xrpd pattern comprising one or more peaks at d - spacings of 15 . 89 , 12 . 77 , 7 . 54 , 5 . 82 , and 5 . 27 å . in another example , the scy - 078 citrate type b has an xrpd pattern comprising one or more peaks at degrees 2 theta of 5 . 56 , 6 . 92 , 11 . 73 , 15 . 23 , and 16 . 81 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type e . in one embodiment , the scy - 078 citrate type e has an xrpd pattern comprising peaks at one or more of the following locations : table k fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 524293 92 . 779970 0 . 307008 15 . 99790 5 . 74 7 . 256628 1616 . 341000 0 . 179088 12 . 18224 100 . 00 11 . 438900 216 . 111400 0 . 281424 7 . 73586 13 . 37 14 . 135060 246 . 012400 0 . 255840 6 . 26579 15 . 22 15 . 755470 336 . 295500 0 . 255840 5 . 62483 20 . 81 16 . 331430 208 . 920100 0 . 255840 5 . 42773 12 . 93 17 . 088060 99 . 712520 0 . 409344 5 . 18907 6 . 17 21 . 127980 46 . 130650 0 . 614016 4 . 20511 2 . 85 31 . 562360 23 . 421260 0 . 614016 2 . 83470 1 . 45 for example , the scy - 078 citrate type e has an xrpd pattern comprising one or more peaks at d - spacings of 12 . 18 , 7 . 74 , 6 . 27 , 5 . 62 , and 5 . 43 a . in another example , the scy - 078 citrate type e has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 26 , 11 . 44 , 14 . 14 , 15 . 76 , and 16 . 33 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type f . in one embodiment , the scy - 078 citrate type f has an xrpd pattern comprising peaks at one or more of the following locations : table l fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 3 . 633823 273 . 473300 0 . 204672 24 . 31535 100 . 00 8 . 094996 83 . 291080 0 . 307008 10 . 92235 30 . 46 14 . 004250 57 . 266020 0 . 818688 6 . 32402 20 . 94 17 . 742840 88 . 241520 0 . 307008 4 . 99902 32 . 27 for example , the scy - 078 citrate type f has an xrpd pattern comprising one or more peaks at d - spacings of 24 . 32 and 5 . 00 å . in another example , the scy - 078 citrate type f has an xrpd pattern comprising one or more peaks at degrees 2 theta of 3 . 63 and 17 . 74 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type m . in one embodiment , the scy - 078 citrate type m has an xrpd pattern comprising peaks at one or more of the following locations : table m fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 572099 251 . 586000 0 . 179088 15 . 86076 9 . 89 7 . 341430 2543 . 546000 0 . 332592 12 . 04171 100 . 00 9 . 506812 193 . 442600 0 . 307008 9 . 30326 7 . 61 11 . 507120 612 . 058600 0 . 281424 7 . 69016 24 . 06 12 . 151790 217 . 504900 0 . 255840 7 . 28359 8 . 55 14 . 166310 475 . 291100 0 . 179088 6 . 25204 18 . 69 15 . 796090 798 . 112100 0 . 255840 5 . 61046 31 . 38 16 . 373100 704 . 236700 0 . 179088 5 . 41401 27 . 69 17 . 342680 236 . 560600 0 . 511680 5 . 11346 9 . 30 18 . 264100 127 . 099200 0 . 307008 4 . 85751 5 . 00 20 . 028560 111 . 330700 0 . 307008 4 . 43338 4 . 38 21 . 230190 166 . 125100 0 . 255840 4 . 18509 6 . 53 22 . 124240 151 . 032300 0 . 358176 4 . 01795 5 . 94 23 . 019390 107 . 550400 0 . 307008 3 . 86369 4 . 23 25 . 286220 144 . 601600 0 . 511680 3 . 52223 5 . 69 27 . 656070 79 . 447100 0 . 358176 3 . 22556 3 . 12 28 . 430390 56 . 622940 0 . 409344 3 . 13945 2 . 23 29 . 646340 75 . 432070 0 . 614016 3 . 01339 2 . 97 32 . 376530 74 . 417430 0 . 307008 2 . 76525 2 . 93 36 . 534050 34 . 760060 0 . 614016 2 . 45955 1 . 37 38 . 139080 26 . 017290 0 . 614016 2 . 35966 1 . 02 for example , the scy - 078 citrate type m has an xrpd pattern comprising one or more peaks at d - spacings of 12 . 04 , 7 . 69 , 6 . 25 , 5 . 61 , and 5 . 41 a . in another example , the scy - 078 citrate type m has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 34 , 11 . 51 , 14 . 17 , 15 . 80 , and 16 . 37 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type n . in one embodiment , the scy - 078 citrate type n has an xrpd pattern comprising peaks at one or more of the following locations : table n fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 410849 486 . 098000 0 . 076752 16 . 33306 9 . 13 7 . 067553 5326 . 844000 0 . 089544 12 . 50771 100 . 00 10 . 838060 670 . 175200 0 . 063960 8 . 16333 12 . 58 11 . 383920 1260 . 568000 0 . 089544 7 . 77310 23 . 66 11 . 924900 315 . 766000 0 . 153504 7 . 42166 5 . 93 12 . 367310 352 . 822800 0 . 153504 7 . 15714 6 . 62 12 . 923310 1574 . 956000 0 . 089544 6 . 85044 29 . 57 14 . 132120 1282 . 157000 0 . 102336 6 . 26708 24 . 07 15 . 162450 1604 . 350000 0 . 102336 5 . 84346 30 . 12 16 . 256930 1496 . 153000 0 . 089544 5 . 45244 28 . 09 16 . 676790 891 . 116500 0 . 115128 5 . 31610 16 . 73 16 . 898590 608 . 961300 0 . 102336 5 . 24682 11 . 43 17 . 769210 633 . 106100 0 . 127920 4 . 99166 11 . 89 18 . 512560 1119 . 245000 0 . 102336 4 . 79287 21 . 01 20 . 764100 264 . 835400 0 . 102336 4 . 27797 4 . 97 21 . 599360 277 . 781400 0 . 127920 4 . 11439 5 . 21 22 . 726850 204 . 007000 0 . 102336 3 . 91276 3 . 83 23 . 066060 336 . 013100 0 . 153504 3 . 85598 6 . 31 24 . 489610 243 . 365100 0 . 127920 3 . 63497 4 . 57 28 . 491330 175 . 736200 0 . 179088 3 . 13287 3 . 30 30 . 668850 84 . 372280 0 . 307008 2 . 91522 1 . 58 33 . 097360 34 . 363080 0 . 614016 2 . 70666 0 . 65 36 . 308500 40 . 510880 0 . 716352 2 . 47431 0 . 76 for example , the scy - 078 citrate type n has an xrpd pattern comprising one or more peaks at d - spacings of 12 . 51 , 7 . 77 , 6 . 85 , 6 . 27 , 5 . 84 , 5 . 45 , and 4 . 79 å . in another example , the scy - 078 citrate type n has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 07 , 11 . 38 , 12 . 92 , 14 . 13 , 15 . 16 , 16 . 26 , and 18 . 51 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type o in one embodiment , the scy - 078 citrate type o has an xrpd pattern comprising peaks at one or more of the following locations : table o fwhm pos . [° 2th .] height [ cts ] left [° 2th .] d - spacing [ å ] rel . int . [%] 3 . 214240 359 . 101800 0 . 409344 27 . 48844 9 . 56 5 . 562890 564 . 632100 0 . 102336 15 . 88699 15 . 03 7 . 082335 3757 . 717000 0 . 115128 12 . 48164 100 . 00 11 . 908250 1208 . 103000 0 . 089544 7 . 43200 32 . 15 14 . 197590 602 . 552700 0 . 115128 6 . 23833 16 . 04 16 . 178670 447 . 137400 0 . 179088 5 . 47864 11 . 90 16 . 755170 956 . 290800 0 . 115128 5 . 29141 25 . 45 28 . 567280 48 . 759020 0 . 307008 3 . 12472 1 . 30 for example , the scy - 078 citrate type 0 has an xrpd pattern comprising one or more peaks at d - spacings of 12 . 48 , 7 . 43 , and 5 . 29 a . in another example , the scy - 078 citrate type o has an xrpd pattern comprising one or more peaks at degrees 2 theta of 7 . 08 , 11 . 91 , and 16 . 76 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type q . in one embodiment , the scy - 078 citrate type q has an xrpd pattern comprising peaks at one or more of the following locations : table p fwhm left pos . [° 2th .] height [ cts ] [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 686347 449 . 970600 0 . 102336 15 . 54234 13 . 51 6 . 300879 3329 . 599000 0 . 140712 14 . 02779 100 . 00 6 . 890776 1871 . 585000 0 . 076752 12 . 82818 56 . 21 8 . 441730 95 . 233120 0 . 153504 10 . 47449 2 . 86 9 . 785571 136 . 396600 0 . 153504 9 . 03885 4 . 10 11 . 334590 1386 . 986000 0 . 140712 7 . 80682 41 . 66 11 . 733060 826 . 632000 0 . 102336 7 . 54257 24 . 83 12 . 939760 265 . 781600 0 . 409344 6 . 84177 7 . 98 13 . 691820 190 . 778000 0 . 153504 6 . 46762 5 . 73 14 . 156830 332 . 781500 0 . 153504 6 . 25620 9 . 99 14 . 496570 455 . 453300 0 . 102336 6 . 11034 13 . 68 15 . 135910 594 . 105600 0 . 153504 5 . 85365 17 . 84 15 . 903400 540 . 737100 0 . 127920 5 . 57284 16 . 24 17 . 010910 1588 . 263000 0 . 127920 5 . 21243 47 . 70 17 . 296950 476 . 914900 0 . 127920 5 . 12687 14 . 32 18 . 962100 570 . 585000 0 . 204672 4 . 68025 17 . 14 20 . 190720 395 . 466100 0 . 102336 4 . 39814 11 . 88 20 . 646480 601 . 591200 0 . 153504 4 . 30207 18 . 07 21 . 298380 208 . 197100 0 . 153504 4 . 17185 6 . 25 22 . 025220 160 . 183700 0 . 307008 4 . 03579 4 . 81 22 . 719750 205 . 611500 0 . 204672 3 . 91397 6 . 18 23 . 633070 128 . 288000 0 . 307008 3 . 76474 3 . 85 25 . 991160 157 . 744000 0 . 204672 3 . 42828 4 . 74 27 . 462080 37 . 389280 0 . 307008 3 . 24790 1 . 12 28 . 950740 597 . 140100 0 . 140712 3 . 08419 17 . 93 34 . 085010 29 . 835660 0 . 511680 2 . 63046 0 . 90 for example , the scy - 078 citrate type q has an xrpd pattern comprising one or more peaks at d - spacings of 14 . 03 , 12 . 83 , 7 . 81 , 7 . 54 , and 5 . 21 å . in another example , the scy - 078 citrate type q has an xrpd pattern comprising one or more peaks at degrees 2 theta of 6 . 30 , 6 . 89 , 11 . 33 , 11 . 73 , and 17 . 01 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type r . in one embodiment , the scy - 078 citrate type r has an xrpd pattern comprising peaks at one or more of the following locations : table q fwhm left pos . [° 2th .] height [ cts ] [° 2th .] d - spacing [ å ] rel . int . [%] 6 . 143884 611 . 904200 0 . 153504 14 . 38589 100 . 00 11 . 248800 143 . 606900 0 . 255840 7 . 86616 23 . 47 14 . 059410 351 . 488100 0 . 204672 6 . 29933 57 . 44 14 . 636960 372 . 993000 0 . 204672 6 . 05205 60 . 96 16 . 413500 550 . 672100 0 . 102336 5 . 40078 89 . 99 17 . 742000 362 . 377400 0 . 614016 4 . 99926 59 . 22 19 . 697290 248 . 048100 0 . 307008 4 . 50719 40 . 54 22 . 159300 133 . 589200 0 . 409344 4 . 01167 21 . 83 30 . 197650 27 . 706020 0 . 614016 2 . 95963 4 . 53 for example , the scy - 078 citrate type r has an xrpd pattern comprising one or more peaks at d - spacings of 14 . 39 , 6 . 05 , 5 . 40 , and 5 . 00 å . in another example , the scy - 078 citrate type r has an xrpd pattern comprising one or more peaks at degrees 2 theta of 6 . 14 , 14 . 64 , 16 . 41 , and 17 . 74 . the present disclosure further relates to a citrate salt of scy - 078 comprising scy - 078 citrate type s . in one embodiment , the scy - 078 citrate type s has an xrpd pattern comprising peaks at one or more of the following locations : table r fwhm left pos . [° 2th .] height [ cts ] [° 2th .] d - spacing [ å ] rel . int . [%] 5 . 512446 1020 . 013000 0 . 089544 16 . 03226 16 . 16 7 . 296105 6310 . 710000 0 . 153504 12 . 11641 100 . 00 8 . 443163 252 . 219900 0 . 230256 10 . 47272 4 . 00 11 . 057440 582 . 228600 0 . 179088 8 . 00186 9 . 23 12 . 004950 2714 . 326000 0 . 166296 7 . 37235 43 . 01 14 . 346070 536 . 999100 0 . 204672 6 . 17410 8 . 51 16 . 812800 1626 . 861000 0 . 127920 5 . 27340 25 . 78 19 . 482230 106 . 142000 0 . 358176 4 . 55646 1 . 68 22 . 188280 88 . 048920 0 . 409344 4 . 00650 1 . 40 24 . 046320 53 . 183810 0 . 818688 3 . 70096 0 . 84 for example , the scy - 078 citrate type s has an xrpd pattern comprising one or more peaks at d - spacings of 16 . 03 , 12 . 12 , 7 . 37 , and 5 . 27 a . in another example , the scy - 078 citrate type s has an xrpd pattern comprising one or more peaks at degrees 2 theta of 5 . 51 , 7 . 30 , 12 . 00 , and 16 . 81 . the present disclosure further relates to a method for preparing a pharmaceutically acceptable salt of scy - 078 comprising combining at least components : ( i ) a free base of scy - 078 ; ( ii ) a weak organic acid ; and ( iii ) a liquid carrier . the weak organic acid may be chosen from those known in the art . in one embodiment , the weak organic acid is selected from citric acid , fumaric acid , methanesulfonic acid , and hippuric acid . in another embodiment , the weak organic acid is citric acid . in a further embodiment , the liquid carrier is a solvent or solvent mixture , and at least one of the free base of scy - 078 and the weak organic acid is soluble in the solvent or solvent mixture . in still another embodiment , the liquid carrier comprises at least one of ethanol , isopropyl alcohol , acetonitrile , acetone , ethyl acetate , and tetrahydrofuran / water mixture . in yet another embodiment , the liquid carrier comprises ethanol . in one embodiment , the method further comprises combining ( iv ) an anti - solvent . in another embodiment , the anti - solvent comprises n - heptane . in one embodiment , the method further comprises agitating the combination of at least components ( i )-( iii ). in a further embodiment , the method further comprises agitating the combination of at least components ( i )-( iii ) for at least 24 hours . in another embodiment , the method further comprises agitating and heating the combination of at least components ( i )-( iii ). in a further embodiment , the method further comprises agitating and heating the combination of at least components ( i )-( iii ) to a temperature of from 40 ° c . to 60 ° c . in still another embodiment , the method further comprises agitating and heating the combination of at least components ( i )-( iii ) to a temperature of from 40 ° c . to 60 ° c . for at least 60 minutes . in one embodiment , the method further comprises agitating and heating the combination of at least components ( i )-( iii ) and adding to the combination of at least components ( i )-( iii ) an anti - solvent after at least 14 hours . in yet another embodiment , the anti - solvent is n - heptane . in one embodiment , the method further comprises agitating and heating the combination of at least components ( i )-( iii ); adding to the combination of at least components ( i )-( iii ) an anti - solvent after at least 14 hours ; and cooling the combination of at least components ( i )-( iii ). in a further embodiment , the cooling is from 0 ° c . to 20 ° c . in another embodiment , the cooling is from 0 ° c . to 20 ° c . at a rate of 0 . 25 ° c ./ min . the present disclosure further relates to methods for preparing citrate type a salt of scy - 078 . in one embodiment , the method comprises desolvating at least one of type b , type n , and type q citrate salt of scy - 078 . in a further embodiment , the desolvating comprises drying under nitrogen . in yet another embodiment , the desolvating comprises drying under vacuum filtration . the present disclosure additionally relates to pharmaceutical compositions comprising a pharmaceutically acceptable salt of scy - 078 , and a pharmaceutically acceptable carrier . the pharmaceutically acceptable carrier may be chosen from , among other things , one or more of the following : water , saline solutions , buffers , and alcohols . in one embodiment , the pharmaceutically acceptable salt in the pharmaceutical composition is selected from citrate , hippurate , mesylate , and fumarate . in yet another embodiment , the pharmaceutically acceptable salt is a citrate salt . in still another embodiment , the pharmaceutically acceptable salt of scy - 078 is scy - 078 citrate type a . according to certain embodiments , the pharmaceutically acceptable salt of scy - 078 may consist essentially of a specified crystal form . according to certain embodiments , the pharmaceutically acceptable salt of scy - 078 may comprise a specified crystal in combination with one or more other crystal forms . the pharmaceutically acceptable salt of scy - 078 may , for example , contain a specified crystal form together with less than 10 % of another crystal form ( s ), such as less than 5 %, less than 2 %, or less than 1 %. in one embodiment , the pharmaceutical composition is made by dissolving the pharmaceutically acceptable salt of scy - 078 in a pharmaceutically acceptable carrier . the pharmaceutically acceptable carrier may be chosen from , among other things , one or more of the following : water , saline solutions , buffers , and alcohols . in another embodiment , the pharmaceutical composition is suitable for injection into a human . in a further embodiment , the pharmaceutical composition is suitable for intravenous injection into a human . in another embodiment , the pharmaceutically acceptable salt is a citrate salt . in still another embodiment , the pharmaceutically acceptable salt of scy - 078 is scy - 078 citrate type a . the present disclosure further relates to methods of preparing a pharmaceutical composition comprising pharmaceutically acceptable salts of scy - 078 , and a pharmaceutically acceptable carrier . the pharmaceutically acceptable carrier may be chosen from , among other things , one or more of the following : water , saline solutions , buffers , and alcohols . in one embodiment , the pharmaceutically acceptable salt of scy - 078 is dissolved in the pharmaceutically acceptable carrier within 1 hour . in another embodiment , the pharmaceutically acceptable salt of scy - 078 is dissolved in the pharmaceutically acceptable carrier within 24 hours . in a further embodiment , the pharmaceutically acceptable salt is a citrate salt . in still another embodiment , the pharmaceutically acceptable salt of scy - 078 is scy - 078 citrate type a . the present disclosure additionally relates to methods of treating a fungal infection in a patient in need thereof . for example , the methods include treating invasive candidiasis and invasive aspergillosis . in one embodiment , the method comprises administering to the patient in need thereof a pharmaceutical composition comprising an effective amount of a pharmaceutically acceptable salt of scy - 078 . in another embodiment , the pharmaceutically acceptable salt is a citrate salt . in a further embodiment , the pharmaceutically acceptable salt of scy - 078 is scy - 078 citrate type a . in another embodiment , the pharmaceutical composition is suitable for injection into a human . in yet another embodiment , the pharmaceutical composition is suitable for intravenous injection into a human . the following describes the materials and methods used for all examples unless otherwise stated . differential scanning calorimetry ( dsc )— dsc was performed with a ta q2000 dsc from ta instruments . to perform dsc , the sample was ramped from room temperature to the desired temperature at a heating rate of 10 ° c ./ min , using n 2 as the purge gas and with the pan crimped . universal analysis 2000 ( ta instruments ) was used to analyze the results . thermogravimetric analysis ( tga )— tga was performed with a ta q500 / q5000 tga from ta instruments . to perform tga , the sample was ramped from room temperature to the desired temperature at a heating rate of 10 ° c ./ min , using n 2 as the purge gas . universal analysis 2000 ( ta instruments ) was used to analyze the results . the temperature was calibrated using nickel and the weight using ta - supplied standard weights and verified against calcium oxalate monohydrate dehydration and decomposition . dynamic vapor sorption ( dvs )— the term “ dvs ” means the procedure described in below . the relative humidity at 25 ° c . was calibrated against deliquescence point of licl , mg ( no 3 ) 2 and kcl . the dvs of scy - 078 salts were tested according to the above method , using a 10 - 20 mg sample size . the dvs was measured using a surface measurement systems ( sms ) dvs intrinsic . high power liquid chromatography ( hplc ) method — an agilent 1260 hplc with dad detector was utilized to test solubility or to test purity and stability . for all compounds tested other than the trifluoroacetate salts ( type a and b ) and the hcl type i and ii salts , the conditions and parameters used for measuring solubility are shown in table 2a and for measuring stability are showing in table 3a . the conditions and parameters used for the solubility of the trifluoroacetate salts ( type a and b ) and the hcl type i and ii salts are shown in table 2b and for stability are shown in table 3b . system suitability was tested by injecting standard solutions five times in each sample sequence , and the relative standard deviation of the peak areas was less than 2 %. a : 0 . 1 % hclo 4 in h 2 o b : acn sgf media preparation — the term “ sgf media ” means a solution prepared according to the following method . sodium chloride ( 0 . 2 g ) and triton x - 100 ( 0 . 1 g ) were combined in a 100 ml flask . then deionized water was added . the mixture was stirred until all solids were dissolved . then 12 n hcl ( 200 μl ) was added and the ph value was checked with a ph meter . the ph was adjusted to 1 . 8 with 1n hcl or 1n naoh . once the desired ph was established , the solution was diluted to volume with deionized water . fassif media preparation — the term “ fassif media ” means a solution prepared according to the following method . a fassif dissolving buffer was prepared by dissolving maleic acid ( 0 . 222 g ) in 45 ml of purified water . the ph was adjusted to exactly 6 . 4 using 1n naoh . fassif media was prepared by adding sodium taurocholate ( 0 . 161 g ), sodium chloride ( 0 . 398 g ), and lecithin ( 0 . 0156 g ) into a 100 - ml volumetric flask . then 40 ml of deionized water was added . the solution was sonicated until clear . next 45 ml of the fassif dissolving buffer was added . the ph was adjusted to 6 . 5 with 1n naoh or 1n hcl . once the desired ph was reached , the solution was diluted to volume with deionized water . an alternative media (“ fassif alternative media ”) was used to study the trifluoroacetate salts ( type a and b ) and the hcl type i salt . more specifically , the media was prepared by weighing 0 . 17 g of sodium phosphate monobasic ( nah2po4 , anhydrous ), 0 . 021 g of sodium hydroxide , and 0 . 31 g of sodium chloride into a 50 - ml volumetric flask and was dissolve with approximately 48 ml of purified water . the ph was adjusted to exactly 6 . 5 using 1 m hcl or 1 m naoh and diluted to volume with purified water . 0 . 11 g of sif powder was then added , stirred and sonicated until all the powder was completely dissolved . the solution was equilibrated for 2 hours at rt before use . the solution can be stored at rt for 48 hours or 4 ° c . for 7 days and should be equilibrated to rt before use fessif preparation — the term “ fessif media ” means a solution prepared according to the following method . a fessif dissolving buffer was prepared by dissolving maleic acid ( 0 . 638 g ) and nacl ( 0 . 728 g ) in 100 ml of purified water . the ph was adjusted to exactly 5 . 8 using 1n naoh or 1n hcl . fessif media was prepared by adding sodium taurocholate ( 0 . 269 g ), lecithin ( 0 . 078 g ), sodium oleate ( 0 . 012 g ), and glyceryl monooleate ( 0 . 089 ) into a 50 - ml flask . then 2 . 5 ml of the fessif dissolving buffer was added . the solution was sonicated . an additional 12 . 5 ml of the fessif dissolving buffer was then added 1 ml stepwise forming an emulsion . the solution was transferred to a 50 - ml volumetric flask and diluted to volume with the fessif dissolving buffer . an alternative media (“ fessif alternative media ”) was used to study the trifluoroacetate salts ( type a and b ) and the hcl type i salt . more specifically , the media was prepared by transferring 0 . 41 ml of glacial acid and weighing 0 . 20 g of sodium hydroxide , 0 . 59 g of sodium chloride into a 50 - ml volumetric flask . this was dissolved with approximately 48 ml of purified water . the ph was adjusted to exactly 5 . 0 using 1 m hcl or 1 m naoh and diluted to volume with purified water . 0 . 56 g of sif powder was added , stirred and sonicated until all the powder is completely dissolved . the solution can be stored at rt for 48 hours or 4 ° c . for 7 days and should be equilibrated to rt before use . dextrose buffer ( ph 5 . 5 ) preparation — the terms “ dextrose buffer at ph 5 . 5 ” and “ dextrose buffer ( ph 5 . 5 )” mean a solution prepared according to the following method . dextrose ( 0 . 5 g ) was added to a 100 - ml volumetric flask . then 1m hcl or 1m naoh was added to adjust the ph of the buffer to ph 5 . 5 . acetate buffer ( ph 5 . 5 ) preparation — the acetate buffer ( ph 5 . 5 ) used for the trifluoroacetate salts ( type a and b ) and the hcl type i salt was prepared by placing 0 . 60 g sodium acetate ( nac 2 h 3 o 2 . 3h 2 o ) in a 100 - ml volumetric flask , adding 3 ml of 2 m acetic acid solution , and then adding purified water to volume . phosphate buffer ( ph 6 . 0 ) preparation — the terms “ phosphate buffer at ph 6 . 0 ” and “ phosphate buffer ( ph 6 . 0 )” mean a solution prepared according to the following method . a solution of 0 . 2 m kh 2 po 4 ( 25 ml ) and 0 . 2 m naoh ( 5 . 6 ml ) was prepared in a 100 - ml volumetric flask . the ph was checked by ph meter . then water was added to volume . an alternative media (“ phosphate ( ph 6 . 0 ) alternative media ”) was used to study the trifluoroacetate salts ( type a and b ) and the hcl type i salt . more specifically , the media was prepared by dissolving 2 . 72 g of 0 . 2 m monobasic potassium phosphate ( kh 2 po 4 ) in purified water , and diluting with purified water to 100 ml . 0 . 8 g of 0 . 2 m sodium hydroxide in purified water was diluted with purified water to 100 ml . then 50 ml of the 0 . 2 m monobasic potassium phosphate solution was placed in a 200 - ml volumetric flask , 5 . 6 ml of 0 . 2 m sodium hydroxide solution was added , and then purified water was added to volume . phosphate buffer ( ph 7 . 5 ) preparation — the terms “ phosphate buffer at ph 7 . 5 ” and “ phosphate buffer ( ph 7 . 5 )” mean a solution prepared according to the following method . a solution of 0 . 2 m kh 2 po 4 ( 25 ml ) and 0 . 2 m naoh ( 40 . 2 ml ) was prepared in a 100 - ml volumetric flask . the ph was checked by ph meter . then water was added to volume . kinetic solubility of scy - 078 salts — the term “ kinetic solubility ” with respect to scy - 078 salts means the following procedure . first , 15 mg , 50 mg , or 100 mg of one of the scy - 078 salts was placed into a 4 - ml plastic centrifuge tubes along with 1 . 7 ml of relevant media or 2 . 0 ml of water . for dextrose buffer at ph 5 . 5 , phosphate buffer at ph 6 . 0 , and phosphate buffer at ph 7 . 5 , 15 mg of the scy - 078 salt was used . for sgf media , fessif media , and fassif media , 50 mg of the scy - 078 salt was used . for water , 100 mg of the scy - 078 salt was used . the actual weight of each sample was recorded . the tube was subsequently capped and the suspension samples were stirred on a rolling incubator ( 25 rpm ) at room temperature . samples were taken at 1 hour , 4 hours , and 24 hours respectively . for each sample , a 0 . 5 ml aliquot of the suspension was transferred into a 1 . 5 - ml centrifuge filtration tube and centrifuged . the samples were then filtered through the centrifuge filtration tube ( 0 . 45 μm ) at 8 , 000 rpm at room temperature for 3 minutes . the trifluoroacetate salts ( type a and b ) and the hcl type i salt were tested using the following alternative procedure . first , 15 mg , 36 mg or 90 mg solid was weighted into a 4 - ml plastic tube , and 3 ml of relevant media was added before leaving the suspension on a rolling incubator ( 25 r / min ). for scf , 90 mg of solid was used . for fassif , acetate buffer ( ph 5 . 5 ), and phosphate buffer ( ph 6 . 0 ), 15 mg solid was used . for fessif , 36 mg of solid was used . 1 . 0 ml aliquot of the suspension was sampled for centrifugation with the supernatant submitted for hplc and ph measurement and solid for xrpd characterization at 1 hr , 4 hr and / or 24 hrs . approximate solubility of scy - 078 salts — the term “ approximate solubility ” with respect to scy - 078 salts means the procedure described in this paragraph . to conduct each experiment , a sample of a scy - 078 salt (˜ 2 mg ) was added into a 3 - ml glass vial . then a solvent was added step - wise ( 100 μl per step ) into the vials until the solids were dissolved or a total volume of 2 ml was reached . equilibrium solubility of scy - 078 salts — the term “ equilibrium solubility ” with respect to scy - 078 salts means the procedure described in this paragraph . the equilibrium solubility of a scy - 078 salt was evaluated in water at room temperature . first , the scy - 078 salt (˜ 50 mg ) was weighed into a 1 . 5 - ml vial followed by addition of 1 . 0 ml water , and then the sample was stirred ( 800 rpm ) at room temperature for 24 hours . the sample was centrifuged with the residual solid analyzed by xrpd and supernatant concentration measured by hplc . polarized light microscopic imaging — polarized light microscopic ( plm ) images was captured at room temperature using axio lab a1 upright microscope equipped with progres ® ct3 camera . the sample was sandwiched between a glass slide and a top cover before placed under the polarized light microscopy for imaging . scy - 078 phosphate : the phosphate salt of scy - 078 was prepared from scy - 078 freebase , which was prepared using known procedures . see , e . g ., u . s . pat . no . 8 , 188 , 085 . scy - 078 freebase ( 10 . 0 g ) was placed in a 250 ml reactor . ethanol ( 50 ml ), ethyl acetate ( 30 ml ), acetic acid ( 1 . 5 ml ) and water ( 1 ml ) were added and the mixture was stirred at room temperature over 10 minutes . the resulting homogeneous solution was heated to 50 ° c . and phosphoric acid ( 1 . 74 g ) solution in ethyl acetate was slowly added to the solution at 50 ° c . for 1 hour . the resulting slurry was slowly cooled to room temperature and stirred overnight at room temperature . the slurry was filtered , and the wet cake was washed with 20 ml mixed solvents ( ethanol : ethyl acetate : water = 5 : 5 : 0 . 1 ) two times , then twice with ethyl acetate ( 1 ml ). the wet cake was dried under vacuum with nitrogen sweep over three hours , and then dried in a vacuum oven overnight to obtain 11 . 08 g of an off - white crystal . the retention time of the compound was 4 . 08 minutes , as measured by hplc using an ascentis express c18 column with standard gradient : 10 - 95 % of b in 6 minutes ( a = 0 . 1 % phosphoric acid , b = acetonitrile ), 2 minute hold 2 minute post ; flow rate : 1 . 8ml / minute ( uv detection at 245 nm , 40 ° c .). scy - 078 phosphate was characterized by xrpd , which evidenced that the compound is crystalline ( fig1 ). the 2 theta and d - spacing values are summarized in table 4 . the dsc curve of scy - 078 phosphate exhibited two endothermic peaks at 48 . 1 ° c . and 267 ° c . ( fig2 ). a weight loss of 6 . 6 % was observed up to 155 . 4 ° c . in the tga curve ( fig2 ). scy - 078 crystalline freebase ( meoh desolvate ): the meoh desolvate was prepared as follows . scy - 078 phosphate salt ( 10 . 0 g ) was charged into a 250 ml reactor . sodium carbonate ( 50 ml of a 10 % solution ) was added at 20 ° c . and agitated . 2 - methyltetrahydrofuan ( 100 ml ) was added and agitated strongly at 20 ° c . until all the solids dissolved . the mixture was left to stand for 30 minutes to leave two clear layers which were separated and the organic layer was washed twice with deionized water ( 40 ml ). the washed organic layer was transferred to a 125 - ml reaction vessel and agitated at 500 rpm , heated to 50 ° c . and distilled under partial vacuum at 50 ° c . down to 40 ml volume . methanol ( 80 ml ) was added to the reaction vessel at 50 ° c ., which was then cooled to 40 ° c . ; after 2 hours , crystals formed . the volume was then distilled down to 50 ml at 40 ° c . under partial vacuum over 16 hours . there was then constant volume distillation at 40 ° c . while adding methanol ( 40 ml ) over 2 hours . water ( 20 ml ) was then added over 2 hours . the reaction vessel was then cooled to 20 ° c . over 2 hours and then slurry aged at 20 ° c . for 2 hours . the mixture was then filtered and the resulting wet cake washed with 20 ml of a 4 : 1 solution of methanol and water . the wet cake was dried under nitrogen sweep at room temperature for 16 hours . xrpd analysis confirmed that the dry cake is desolvated methanol solvate ( yield 89 %, purity : 99 . 1 %). two batches of meoh desolvate were prepared and characterized by xrpd , dsc , and tga ( fig3 - 5 ). xrpd patterns evidenced that the compound is crystalline . the 2 theta and d - spacing values from batch 1 and batch 2 are summarized in tables 5a and 5b , respectively . the dsc curve of meoh desolvate batch 1 exhibited an endotherm at ˜ 55 . 0 ° c . and an exotherm at ˜ 281 . 5 ° c . the dsc curve of meoh desolvate batch 2 exhibited an endotherm at ˜ 56 . 1 ° c . and an exotherm at ˜ 279 . 2 ° c . the tga curve of batch 1 showed a weight loss of 4 . 7 % before 120 ° c . the tga curve of batch 1 showed a weight loss of 6 . 6 % before 120 ° c . the tga curve of batch 2 showed a weight loss of 4 . 9 % before 120 ° c . scy - 078 amorphous freebase : to prepare scy - 078 amorphous freebase , meoh desolvate ( 50 mg ) was added to a 3 - ml vial . then dcm ( 0 . 5 ml ) was added to the vial of meoh desolvate . the resulting solution of meoh desolvate and dcm formed a clear solution . the solution was evaporated to dryness from an open vial at 50 ° c . the solid obtained after evaporation was characterized by xrpd , tga , dsc , and dvs . the xrpd pattern evidenced that the tested sample is amorphous . the dsc and tga curves of the amorphous sample exhibited a glass transition at ˜ 189 . 1 ° c . ( fig6 ). the tga curve demonstrated a weight loss of 4 . 2 % before 150 ° c . the dvs curve demonstrated that the sample is hygroscopic with a water uptake of ˜ 4 . 8 % at 80 % rh , 25 ° c . an xrpd pattern performed after dvs demonstrated no form change . kinetic solubility of scy - 078 freebase : the kinetic solubility of scy - 078 meoh desolvate and scy - 078 amorphous freebase was evaluated in sgf media , fassif media , fessif media , dextrose buffer ( ph 5 . 5 ), phosphate buffer ( ph 6 . 0 ), and phosphate buffer ( ph 7 . 5 ) at room temperature . first , solid scy - 078 meoh desolvate or scy - 078 amorphous freebase (˜ 15 mg ) was weighed into a 4 - ml vial . then the relevant media ( 3 . 0 ml ) was added and the suspensions were stirred on a rolling incubator ( 25 rpm ) at room temperature for 1 hour , 4 hours , and 24 hours respectively . after stirring , 0 . 5 ml of suspension was centrifuged and filtered ( 0 . 45 μm ). the residual solids were analyzed by xrpd , and the supernatant was measured by hplc and ph meter . the results ( table 6 ) suggested that both the meoh desolvate and the amorphous freebase display high solubility in sgf and fessif . the results also showed that both the meoh desolvate and the amorphous freebase are only sparingly soluble in fassif and ph 5 . 5 , ph 6 . 0 , and ph 7 . 5 buffers . solid form change was observed during the solubility measurements of the meoh desolvate in fessif , fassif , ph 5 . 5 and 6 . 0 buffers . additionally , three new crystal forms were discovered ( table 6 ). the three new forms are identified as new form 1 , 2 , and 3 . approximate solubility of scy - 078 meoh desolvate : the approximate solubility of scy - 078 meoh desolvate was measured in 20 solvents at room temperature ( 25 ± 3 ° c .). first , meoh desolvate (˜ 2 mg ) was added to a 3 - ml glass vial . then the corresponding solvent was added step wise ( 100 μl ) until the solution was visually clear or a total volume of 2 ml was reached . the results appear in table 7 . salt study of scy - 078 freebase : a salt study of the scy - 078 meoh desolvate freebase was performed using 108 different conditions developed through 18 acids in 6 solvents ( table 8 ). the salt study was performed by first preparing a solution of scy - 078 meoh desolvate freebase and mixing with an equi - molar acid solution . this solution was stirred at room temperature overnight . for precipitates , the solids were isolated and analyzed by xrpd . clear solutions were evaporated slowly to dryness at room temperature . the salt study ( table 8 ) showed that seven crystalline salts ( eight crystal forms ) of scy - 078 were found : hcl type a , citrate type a , hippurate type a , fumarate type a , fumarate type b , glycolate type a , mesylate type a , and ca salt type a . four crystal forms of scy - 078 freebase were discovered during the salt study and were identified as freebase (“ fb ”) type a , b , c , and d . scy - 078 hcl type a : scy - 078 hcl type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig7 - 8 ). the resulting xrpd pattern evidenced that scy - 078 hcl type a is weakly crystalline and has a unique form as compared to the freebase meoh desolvate . the 2 theta and d - spacing values are summarized in table 9 . the dsc curve displayed an endotherm at 48 . 5 ° c . ( onset temperature ). the tga curve showed a weight loss of 14 . 4 % before 130 ° c . scy - 078 citrate type a ( molar equivalency — counter ion / api 1 ): scy - 078 citrate type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig9 - 10 ). the resulting xrpd pattern evidenced that scy - 078 citrate type a is crystalline and is a unique form compared to the freebase meoh desolvate . the 2 theta and d - spacing values are summarized in table 10 . the dsc curve displayed two endotherms at 36 . 2 ° c . and 194 . 8 ° c . ( onset temperature ). the tga curve demonstrated 5 . 1 % before 100 ° c . a sample was heated to 100 ° c . and then cooled to room temperature . xrpd was performed after heating and cooling to room temperature . the resulting xrpd pattern showed that there was no change in form . dsc and tga characterization was also performed after heating and cooling . the dsc curve demonstrated two endotherms at 39 . 9 ° c . and 194 . 8 ° c . ( onset temperatures ). the tga curve showed a weight loss of 5 . 3 % before 100 ° c . scy - 078 hippurate type a ( molar equivalency counter ion / api 2 . 0 ): scy - 078 hippurate type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig1 - 12 ). the xrpd pattern of scy - 078 hippurate type a indicated that the sample is crystalline and has a unique form as compared to the freebase meoh desolvate . the dsc curve displayed three endotherms at 36 . 3 ° c ., 104 . 6 ° c ., and 165 . 5 ° c . ( onset temperatures ) and one exotherm at 201 . 9 ° c . ( onset temperature ). the tga curve showed a weight loss of 4 . 9 % before 150 ° c . scy - 078 hippurate type b : scy - 078 hippurate type b is produced from heating hippurate type a to 150 ° c . and then cooling the sample to room temperature . scy - 078 hippurate type b was characterized by xrpd , dsc , and tga ( fig1 - 14 ). the xrpd pattern showed that the sample is crystalline and a unique form compared to scy - 078 hippurate type a . the dsc curve displayed two endotherms at 39 . 6 ° c . and 166 . 4 ° c . ( onset temperatures ) and one exotherm at 201 . 4 ° c . ( onset temperature ). the tga curve demonstrated a weight loss of 1 . 8 % before 150 ° c . scy - 078 hippurate type c : cycle dsc and xrpd were performed to investigate the phase transition events during the heating - cooling process of scy - 078 hippurate type b ( fig1 - 16 ). the xrpd overlay and dsc curve suggested the melting point of scy - 078 hippurate type b at 163 . 9 ° c . followed by amorphous phase recrystallizing at 208 . 8 ° c . and a new anhydrate phase being formed . the new anhydrate phase is scy - 078 hippurate type c . scy - 078 fumarate type a ( molar equivalency counter ion / api 1 . 0 ): scy - 078 fumarate type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig1 - 18 ). the xrpd pattern indicated that the sample is crystalline and a unique form compared to the freebase meoh desolvate . the dsc curve of scy - 078 fumarate type a showed an endotherm at 33 . 1 ° c . and a melting point at 207 . 3 ° c . ( onset temperature ). the tga curve displayed a weight loss of 2 . 4 % before 120 ° c . a sample of scy - 078 fumarate type a was heated to 120 ° c . and then allowed to cool to room temperature . characterization by xrpd , dsc , and tga were then repeated . the xrpd pattern displayed no form change after heating and cooling . the dsc curve of heated - cooled scy - 078 fumarate type a exhibited two endotherms at 38 . 4 ° c . and 207 . 1 ° c . ( onset temperatures ). the tga curve of heated - cooled scy - 078 fumarate type a showed a weight loss of 2 . 0 % before 120 ° c . scy - 078 fumarate type b ( molar equivalency counter ion / api 0 . 8 ): scy - 078 fumarate type b prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig1 - 20 ). the xrpd pattern of scy - 078 fumarate type b indicated that the sample is weakly crystalline and that it is a unique form compared to the freebase meoh desolvate . the dsc curve of scy - 078 fumarate type b showed two endotherms at 37 . 9 ° c . and 178 . 5 ° c . ( onset temperature ). the tga curve demonstrated a weight loss of 13 . 4 % before 300 ° c . scy - 078 glycolate type a ( molar equivalency counter ion / api 2 . 0 ): scy - 078 glycolate type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig2 - 22 ). the xrpd pattern of scy - 078 glycolate type a indicated that the sample is crystalline and a unique form compared to the freebase meoh solvate . the dsc curve of the sample displayed two endotherms at 35 . 9 ° c . and 159 . 6 ° c . ( onset temperatures ). the tga curve showed a weight loss of 6 . 6 % before 100 ° c . scy - 078 mesylate type a ( molar equivalency counter ion / api 1 . 0 ): scy - 078 mesylate type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig2 - 24 ). the xrpd pattern indicated that the sample is crystalline and a unique form compared to the freebase meoh desolvate . the dsc curve displayed an endotherm at 44 . 2 ° c . and a melting point at 260 . 0 ° c . ( onset temperatures ). the tga showed a weight loss of 4 . 5 % before 120 ° c . next , a sample of scy - 078 mesylate type a was heated to 120 ° c . and then allowed to cool to room temperature . characterization by xrpd , dsc , and tga was then repeated . the xrpd pattern displayed no form change after heating and cooling . the dsc curve of the heated - cooled scy - 078 mesylate type a exhibited an endotherm at 59 . 7 ° c . and a melting point at 257 . 4 ° c . ( onset temperatures ). the tga curve of the heated - cooled scy - 078 mesylate type a showed a weight loss of 9 . 4 % before 120 ° c . scy - 078 calcium type a : scy - 078 calcium type a prepared from the salt study in example 6 was characterized by xrpd , dsc , and tga ( fig2 - 26 ). the xrpd pattern indicated that the sample is crystalline and a unique form compared to the freebase meoh desolvate . the dsc curve displayed two endotherms at 147 . 3 ° c . and 230 . 8 ° c . ( onset temperatures ). the tga curve showed a weight loss of 5 . 3 % before 170 ° c . preparation and characterization of scaled - up scy - 078 hippurate type b : to scale - up scy - 078 hippurate type b , a solution of hippuric acid ( 122 . 8 mg ) and scy - 078 meoh desolvate ( 500 . 3 mg ) in acn ( 5 . 0 ml ) was prepared . the suspension was then stirred ( 500 rpm ) at room temperature for 28 hours . following stirring , some slurry was filtered and the isolated solid was checked by xrpd to confirm scy - 078 hippurate type a . the suspension was filtered and dried at 150 ° c . for 1 hour before characterization . finally , the solid was check by xrpd to confirm to scy - 078 hippurate type b . the scaled - up scy - 078 hippurate type b was analyzed by xrpd , dsc , tga , and dvs ( fig2 - 30 ). the resulting xrpd pattern evidenced that scy - 078 hippurate type b was successfully scaled up . the 2 theta and d - spacing values are summarized in table 11 . the dsc curve showed two endotherms at 34 . 5 ° c . and 164 . 4 ° c . and one exotherm at 205 . 2 ° c . ( onset temperatures ). the tga curve showed a weight loss of 0 . 9 % before 130 ° c . the dvs curve showed that the sample is hygroscopic with a water uptake of - 3 . 5 % at 25 ° c . and 80 % rh . a second xrpd pattern performed after dvs showed scy - 078 hippurate type b converted to scy - 078 hippurate type a after dvs experiment . preparation and characterization of scaled - up scy - 078 fumarate type a : to scale - up scy - 078 fumarate type a , a solution of fumaric acid ( 79 . 8 mg ) and scy - 078 meoh desolvate ( 501 . 9 mg ) in acn ( 15 . 0 ml ) was prepared . the suspension was then stirred ( 500 rpm ) at room temperature for 28 hours . following stirring , some slurry was filtered and the isolated solid was checked by xrpd to confirm scy - 078 fumarate type a . finally , the suspension was filtered and dried at 30 ° c . for 4 hours in vacuum before characterization . characterization of scaled - up scy - 078 fumarate type a included xrpd , dsc , tga , and dvs ( fig3 - 33 ). the resulting xrpd pattern evidenced that scy - 078 fumarate type a was successfully scaled up . the 2 theta and d - spacing values are summarized in table 12 . the dsc curve showed an endotherm at 39 . 9 ° c . and a melting endotherm at 208 . 4 ° c . ( onset temperatures ). the tga curve showed a weight loss of 1 . 7 % before 150 ° c . the dvs curve showed that the sample is hygroscopic with a water uptake of 2 . 5 % at 80 % rh , 25 ° c . a second xrpd pattern performed after dvs showed scy - 078 fumarate type a had no form change . preparation and characterization of scaled - up scy - 078 mesylate type a : to scale up scy - 078 mesylate type a , a solution of methanesulfonic acid ( 66 . 7 mg ) and scy - 078 meoh desolvate ( 500 . 00 mg ) in acn ( 6 . 0 ml ) was prepared . the suspension was then stirred ( 500 rpm ) at room temperature for 28 hours . following stirring , some slurry was filtered and the isolated solid was checked by xrpd to confirm to scy - 078 mesylate type a . finally , the suspension was filtered and dried at 30 ° c . for 4 hours in vacuum before characterization . characterization of scaled - up scy - 078 mesylate type a included xrpd , dsc , tga , and dvs ( fig3 - 36 ). the resulting xrpd pattern evidenced that scy - 078 mesylate type a was successfully scaled up . the 2 theta and d - spacing values are summarized in table 13 . the dsc curve showed an endotherm at 45 . 1 ° c . and a melting endotherm at 252 . 5 ° c . ( onset temperatures ). the tga curve showed a weight loss of 5 . 5 % before 150 ° c . the dvs curve showed that the sample is hygroscopic with a water uptake of 11 . 5 % at 25 ° c . and 80 % rh . a second xrpd pattern performed after dvs showed scy - 078 mesylate type a had no form change . preparation and characterization of scaled - up scy - 078 phosphate type a : to scale up scy - 078 phosphate type a , a solution of phosphoric acid ( 87 . 2 mg ) and scy - 078 meoh desolvate ( 501 . 1 mg ) in etoh / etoac / acetic acid / h 2 o ( 6 . 0 ml , 5 : 3 : 0 . 15 : 0 . 1 ; v / v / v / v ) was prepared . the suspension was then stirred ( 500 rpm ) at room temperature for 28 hours . following stirring , some slurry was filtered and the isolated solid was checked by xrpd and named as scy - 078 phosphate type a . finally , the suspension was filtered and dried at 30 ° c . for 4 hours in vacuum before characterization . characterization of scaled - up scy - 078 phosphate type a included xrpd , dsc , tga , and dvs ( fig3 - 39 ). the xrpd pattern of the scaled - up scy - 078 phosphate type a was compared with another phosphate sample . the comparison xrpd pattern evidenced certain peak shifts , which are signaled with an asterisk . the 2 theta and d - spacing values of scy - 078 phosphate type a are summarized in table 14 . the dsc curve showed two endotherms at 43 . 5 ° c . and 261 . 6 ° c . ( onset temperatures ). the tga curve showed a weight loss of 5 . 7 % before 100 ° c . the dvs curve showed that the sample is hygroscopic with a water uptake of 12 . 5 % at 25 ° c . and 80 % rh . a second xrpd pattern performed after dvs showed scy - 078 phosphate type a had no form change . preparation and characterization of scaled - up scy - 078 citrate type a ( molar equivalency — counter ion / api 1 . 0 ): to scale up scy - 078 citrate type a , a solution of citric acid ( 130 . 7 mg ) and scy - 078 meoh desolvate ( 501 . 6 mg ) in acn ( 15 . 0 ml ) was prepared . the suspension was then stirred ( 500 rpm ) at room temperature for 30 hours . following stirring , some slurry was filtered and the isolated solid was checked by xrpd to confirm scy - 078 citrate type a . finally , the suspension was filtered and dried at 30 ° c . for 4 hours in vacuum before characterization . characterization of scaled - up scy - 078 citrate type a included xrpd , dsc , tga , and dvs ( fig4 - 42 ). xrpd pattern evidenced that scy - 078 citrate type a was successfully scaled up . the 2 theta and d - spacing values are summarized in table 15 . the dsc curve showed an endotherm at 38 . 5 ° c . and a melting endotherm at 183 . 7 ° c . ( onset temperatures ). the tga curve showed a weight loss of 4 . 1 % before 110 ° c . the dvs curve showed that the sample is hygroscopic with a water uptake of 6 . 4 % at 80 % rh , 25 ° c . a second xrpd pattern performed after dvs showed scy - 078 citrate type a had no form change . chemical characterization of scy - 078 salts : the chemical purity of each of the scaled - up salts of scy - 078 ( hippurate type b , fumarate type a , mesylate type a , phosphate type a , and citrate type a ) was tested using hplc chromatographs . the chromatographs of the five compounds indicated that each compound has purity greater than 99 % ( table 16 ). evaluation of the ph value of scy - 078 salts in water : the ph value for the saturated salt solutions of scy - 078 ( i . e ., hippurate type b , fumarate type a , mesylate type a , phosphate type a , and citrate type a ) was tested . to test the ph , a solution of each compound was equilibrated at room temperature using a rolling incubator ( 25 rpm ) for 1 hour and 24 hours before measurement . the results ( table 17 ) suggested that the ph values of each of the salts tested is in the range of 3 . 0 to 5 . 0 . evaluation of the kinetic solubility of scy - 078 salts : the kinetic solubilities of scy - 078 hippurate type b , scy - 078 fumarate type a , scy - 078 mesylate type a , scy - 078 phosphate type a , and scy - 078 citrate type a were measured in dextrose buffer at ph 5 . 5 , phosphate buffer at ph 6 . 0 , phosphate buffer at ph 7 . 5 , sgf media , fessif media , and fassif media according to the method described above . after filtration , 0 . 2 ml of supernatant was collected for hplc quantification . the remaining solution was collected for ph measurement . the remaining solid was collected for xrpd characterization . the results appear in table 18 . evaluation of the stability of scy - 078 salts : to test the chemical and physical stability of the salts , samples of the salts were placed under three different conditions for one week : ( 1 ) open dish at 25 ° c . with 60 % rh ; ( 2 ) open dish at 40 ° c . with 75 % rh ; and ( 3 ) closed dish at 60 ° c . with no humidity control . the chemical and physical stability of scy - 078 fumarate type a and scy - 078 citrate type a were tested as described above ( table 19 ). xrpd indicated that neither scy - 078 fumarate type a nor scy - 078 citrate type a experienced form change during assessment . scaled - up scy - 078 citrate type a : a second scale - up of scy - 078 citrate type a was carried out to obtain 2 . 5 g via reactive acn . to scale - up , scy - 078 meoh desolvate ( 2 . 5 g ) and citric acid ( 660 mg ) were dissolved in acn ( 80 ml ). the resulting solution was stirred at a rate of 1000 rpm at room temperature for 30 hours and then the solid was isolated . the solid obtained was dried at 50 ° c . under vacuum overnight . an xrpd pattern ( fig4 ) showed that scy - 078 citrate type a was successfully scaled up and that it is highly crystalline . the 2 theta and d - spacing values are summarized in table 20 . dsc curve ( fig4 ) exhibited two endothermic peaks at 56 . 7 ° c . and 187 . 1 ° c . ( onset temperatures ). tga curve ( fig4 ) showed 7 . 9 % weight loss before 150 ° c . approximate solubility of scy - 078 citrate type a : the approximate solubility of scy - 078 citrate type a from example 26 was determined in 19 solvents at room temperature ( 25 ± 3 ° c .) according to the procedure described above and is reported in table 21 below . kinetic solubility of scy - 078 citrate type a in water : the kinetic solubility of scy - 078 citrate type a from example 26 was evaluated according to the procedure described above . after the samples were centrifuged , the residual solids analyzed by xrpd and the supernatant concentration measured by hplc . results ( table 22 ) indicated that scy - 078 citrate type a partially converted to amorphous in water after 24 hours , and exhibited a slow rate of dissolution and increasing solubility in water from 1 hour to 24 hours . then the kinetic solubility of scy - 078 citrate type a was compared with a mixture of scy - 078 amorphous freebase / citric acid . the kinetic solubility comparison was conducted in water at room temperature and was measured at 1 hour , 4 hours , and 24 hours with a ratio of solute to solvent of 20 mg / ml and 50 mg / ml . results ( table 23 ) indicated that scy - 078 citrate type a shows higher dissolution rate and equilibrium solubility in water than the mixture of scy - 078 amorphous freebase / citric acid . the remaining solids from the solubility measurement of physical mixture of freebase : citric acid at 1 : 1 molar ratio in water were amorphous . to determine the form of the amorphous , liquid nmr was performed on a bruker 400m nmr spectrometer using cd 3 od . the spectrum showed the number of hydrogen atoms assigned to citric acid as 3 . 12 , corresponding to 0 . 78 equivalent of citric acid . this is less than 1 : 1 for mono - citrate and suggests it is a mixture that comprises a majority of amorphous citrate salt with a small quantity of amorphous freebase . equilibrium solubility of scy - 078 salts in water : equilibrium solubility of scy - 078 citrate type a from example 26 in water was determined using the method described above . results showed that scy - 078 citrate type a exhibits 38 . 1 mg / ml solubility in water with the undissolved material having become amorphous after stirring in water for 24 hours . then to further study the solubility of scy - 078 citrate type a in water , citrate type a was tested for 24 hours at three ratios of solute to solvent : 0 . 3 mg / ml , 2 . 0 mg / ml , and 50 . 6 mg / ml . each test used magnetic stirring and began with an initial ph of 8 . 0 . the results ( table 24 ) indicated that scy - 078 citrate type a exhibits a concentration - dependent solubility in water . kinetic solubility of scy - 078 citrate amorphous in water : scy - 078 citrate amorphous was prepared under various conditions , including lyophilization from phosphate buffer ( ph 6 . 0 ), lyophilization from water , and fast evaporation in thf . the results appear in table 25 . where the table indicates “ limited solid ,” there was not sufficient solid for xrpd analysis of the solid form . lyophilization in phosphate buffer ( ph 6 . 0 )— for lyophilization in phosphate buffer ( ph 6 . 0 ), scy - 078 citrate amorphous was prepared by first preparing 50 mm ph 6 . 0 buffer . then citrate type a ( 30 mg ) was weighed into a 20 - ml vial . then ph 6 . 0 buffer ( 20 ml ) was added to the vial and was stirred at room temperature for 24 hours . the samples were filtered and the supernatant was cooled to − 15 ° c . for 2 hours . finally , the frozen samples were lyophilized at − 50 ° c . for 12 hours . a larger batch ( 150 mg ) was prepared using the same procedure noted above . the kinetic solubility of the second batch of the lyophilized product in water was measured according to the above procedure except that ˜ 150 mg of solid and 1 . 0 ml of water were used . after the samples were centrifuged , the residual solids were analyzed by xrpd and the supernatant concentration was measured by hplc . lyophilization in water — for lyophilization in water , amorphous citrate was prepared by first weighing citrate type a (˜ 150 mg ) into a 20 - ml vial . then 10 ml of water was added to dissolve the solid completely . the solution was filtered and put in a condition of − 20 ° c . until it froze . finally , the sample was lyophilized under - 50 ° c . for 24 hours . the kinetic solubility of the lyophilized product in water was measured according to the above procedure except that ˜ 120 mg of solid and 1 . 5 ml of water were used . after the samples were centrifuged , the residual solids were analyzed by xrpd and the supernatant concentration was measured by hplc . fast evaporation in thf — for fast evaporation in thf , amorphous citrate was prepared by first weighing citrate type a from example 26 (˜ 150 mg ) into a 20 - ml vial . then thf ( 3 ml ) was added to dissolve the solid completely . the solution was filtered under a fume hood for performance of fast evaporation . the kinetic solubility in water of the product in water was measured according to the above procedure except that ˜ 120 mg of solid and 1 . 5 ml of water were used . after the samples were centrifuged , the residual solids were analyzed by xrpd and the supernatant concentration was measured by hplc . slow evaporation of scy - 078 citrate type a : slow evaporation experiments were performed in 12 different solvent systems . scy - 078 citrate type a from example 26 ( 10 mg ) was dissolved with solvent ( 0 . 05 ml − 0 . 25 ml ) for each sample in a 3 - ml glass vial . the visually clear solutions were subjected to slow evaporation at room temperature to dryness . the solids obtained were then isolated for xrpd analysis , which showed that no crystalline form was obtained . the results appear in table 26 . slurry conversion of scy - 078 citrate type a : slurry conversion experiments were conducted under 50 conditions . scy - 078 citrate type a from example 26 (˜ 10 mg ) was suspended in each solvent ( 0 . 5 ml ). the suspensions were stirred for 3 days at either room temperature ( table 27 ) or 50 ° c . ( table 28 ). after stirring , the solids were isolated for xrpd analysis . if the suspensions turned into clear solutions upon slurry , the clear solutions were subjected to slow evaporation at room temperature . the results revealed that scy - 078 citrate type b and mixtures of scy - 078 citrate type a and scy - 078 citrate type b were discovered . all scy - 078 citrate type c that was discovered was identified as freebase form . reverse anti - solvent addition of scy - 078 citrate type a : reverse anti - solvent addition experiments were conducted under 14 conditions . scy - 078 citrate type a from example 26 (˜ 10 mg ) was dissolved in each solvent ( 0 . 1 ml ) to obtain a clear solution . this solution was added drop - wise into a glass vial containing 2 . 0 ml of each anti - solvent at room temperature . the precipitate was isolated for xrpd analysis . slow evaporation experiments were conducted for the clear solutions . the results , which appear in table 29 , suggested that scy - 078 citrate type e and scy - 078 citrate type f were obtained . scy - 078 citrate type d and scy - 078 citrate type j were identified as freebase form . solid vapor diffusion of scy - 078 citrate type a : solid vapor diffusion experiments were conducted using four solvents at room temperature . scy - 078 citrate type a from example 26 (˜ 10 mg ) was placed into a 3 - ml glass vial . then the vial was sealed into a 20 - ml glass vial with a solvent ( 3 ml ). the system was kept at room temperature for six days , which was sufficient time for organic vapor to interact with the solids . the solids were characterized by xrpd to identify crystalline forms . the results ( table 30 ) indicated that scy - 078 citrate type a and scy - 078 citrate type b were generated . solution vapor diffusion of scy - 078 citrate type a : solution vapor diffusion experiments were conducted under 5 conditions at room temperature . scy - 078 citrate type a from example 26 (˜ 10 mg ) was dissolved in a solvent to obtain a clear solution in a 3 - ml glass vial . the vial was then sealed into a 20 - ml glass vial with a volatile anti - solvent ( 3 ml ). the system was kept at room temperature for six days , which allowed sufficient time for precipitation . as no precipitation was observed , the samples were evaporated slowly to dryness at room temperature . the solids were separated and analyzed by xrpd . the results ( table 31 ) indicated that no crystalline form was obtained . polymer induced crystallization of scy - 078 citrate type a : polymer induced crystallization experiments were performed under four conditions . scy - 078 citrate type a from example 26 (˜ 10 mg ) was dissolved in a solvent ( 0 . 1 ml - 0 . 8 ml ) in a 3 - ml glass vial . a mixed polymer (- 1 . 0 mg ) was added into the visually clear solutions . the “ mixed polymer ” was a mixture of six polymers ( polyvinyl alcohol , polyvinylchloride , polyvinyl pyrrolidone , polyvinyl acetate , hypromellose , and methyl cellulose ) at the mass ration of 1 . 0 . all the samples were then evaporated slowly at room temperature to dryness . the solids obtained were isolated for xrpd analysis . the results ( table 32 ) showed that no crystalline form was observed . slow cooling of scy - 078 citrate type a : slow cooling experiments were conducted under 10 conditions ( table 33 ). scy - 078 citrate type a from example 26 (˜ 10 mg ) was suspended in a solvent ( 0 . 1 ml - 0 . 2 ml ) at 50 ° c . suspensions were filtered at 50 ° c ., and the filtrates were collected and cooled from 50 ° c . to 5 ° c . at a rate of 0 . 1 ° c ./ min . all solutions were clear and subjected to slow evaporation at room temperature to induce precipitation . the solids were isolated for xrpd analysis . the results ( table 33 ) indicated that scy - 078 citrate type c and scy - 078 citrate type j were produced and that both scy - 078 citrate type c and scy - 078 citrate type j are freebase forms . scy - 078 citrate type a via reactive crystallization : scy - 078 citrate type a was obtained by reactive crystallization in acn . the xrpd pattern showed distinctive diffraction peaks ( fig4 ). dsc curve showed two endothermic peaks at 56 . 7 ° c . and 187 . 1 ° c . ( onset temperatures ) ( fig4 ). tga curve displayed a 7 . 9 % weight loss up to 150 ° c . ( fig4 ). dvs plot showed a water uptake of 7 . 0 % at 80 % rh ( fig4 ). there was no form change after dvs analysis . scy - 078 citrate type a was also tested with variable temperature xrpd analysis . no form change was observed upon heating scy - 078 citrate type a to 120 ° c . and then cooling back to 25 ° c ., indicating that scy - 078 citrate type a is an anhydrate . after crystallization process development , scy - 078 citrate type a exhibited higher crystallinity and less surface moisture adsorption was produced ( fig4 ). dsc curve showed two endothermic peaks at 41 . 7 ° c . and 194 . 8 ° c . ( onset temperatures ). tga curve displayed 2 . 9 % weight loss up to 150 ° c . dvs analysis showed a water uptake of 6 . 5 % at 25 ° c . and 80 % rh . no form change was observed after dvs analysis . 1 h - nmr spectrum in cd 3 od showed the molar ration of freebase and citric acid is 1 : 1 , indicating that scy - 078 citrate type a is mono - citrate . scy - 078 citrate type b : scy - 078 citrate type b was obtained by slurry conversion at room temperature in acn . scy - 078 citrate type b can also be obtained by slurrying scy - 078 citrate type a in various organic solvents such as etoh , acn , acetone , mibk , etoac , ipac , dcm , toluene , heptane , meoh / acetone ( 1 / 19 , v / v ), ipa / heptane ( 1 / 19 , v / v ), and thf / toluene ( 1 / 19 , v / v ). scy - 078 citrate type b converts to type a rapidly under vacuum or upon n 2 flow at room or elevated temperature . the xrpd pattern of scy - 078 citrate type b showed distinctive diffraction peaks ( fig5 ). dsc curve exhibited three endothermic peaks at 70 . 8 ° c ., 190 . 6 ° c ., and 202 . 9 ° c . ( peak temperatures ) ( fig5 ). tga curve displayed 10 . 3 % weight loss up to 150 ° c . ( fig5 ). scy - 078 citrate type e : scy - 078 citrate type e was obtained by drying a metastable solvate scy - 078 citrate type r from meoh / ipac . the xrpd pattern shows the crystalline form of the sample ( fig5 ). scy - 078 citrate type e is not stable at ambient conditions , since it rapidly converts to a new form ( scy - 078 citrate type m ) after exposing to air for 2 days ( fig5 ). scy - 078 citrate type f : scy - 078 citrate type f was obtained by reverse anti - solvent addition in ipa / toluene according to the process described in example 33 and table 29 . the xrpd pattern indicated that scy - 078 citrate type f is weakly crystalline ( fig5 ). dsc curve exhibited a wide endothermic peak at 37 . 3 ° c . ( onset temperature )( fig5 ). tga curve displayed a weight loss of 11 . 8 % up to 120 ° c . ( fig5 ). scy - 078 citrate type m : scy - 078 citrate type m was obtained by storing scy - 078 citrate type e in ambient conditions for 2 days . the xrpd pattern of scy - 078 citrate type m displayed distinctive diffraction peaks ( fig5 ). dsc curve exhibited two endothermic peaks at 125 . 8 ° c . and 193 . 3 ° c . ( onset temperatures ) ( fig5 ). tga curve displayed a 11 . 4 % weight loss up to 150 ° c . ( fig5 ). dvs plot showed 11 . 0 % water uptake at 25 ° c . and 80 % rh ( fig5 ). after dvs , scy - 078 citrate type m converts to partially amorphous . xrpd analysis was also performed at variable temperatures wherein xrpd patterns were produced at 25 ° c ., then at 150 ° c ., and finally , again at 25 ° c . ( fig6 ). a shift in diffraction peaks was observed , indicating that type m is probably a channel hydrate . scy - 078 citrate type n : scy - 078 citrate type n was obtained by slurrying scy - 078 citrate type b in etoh at room temperature for two weeks . scy - 078 citrate type n can also be obtained by exposing scy - 078 citrate type a in etoh vapor for 8 days or slurrying scy - 078 citrate type a in etoh for 2 hours . the xrpd pattern of scy - 078 citrate type n indicates that it is highly crystalline ( fig6 ). scy - 078 citrate type n converts to scy - 078 citrate type a after vacuum drying at room temperature ( fig6 ), indicating scy - 078 citrate type n is a metastable etoh solvate , which rapidly converts to scy - 078 citrate type a under vacuum or upon air / n 2 drying at ambient temperature or elevated temperature . scy - 078 citrate type o : scy - 078 citrate type o was obtained by slurrying scy - 078 citrate type m in acetone at room temperature for 19 hours . the xrpd pattern of scy - 078 citrate type o indicated that it is highly crystalline with distinctive diffraction peaks ( fig6 ). scy - 078 citrate type o converts to scy - 078 citrate type s under ambient or vacuum conditions . scy - 078 citrate type q : scy - 078 citrate type q was obtained when performing reactive crystallization of freebase and citric acid ( 1 : 1 ) in etoh without seeds . scy - 078 citrate type n was consistently obtained when the reactive crystallization was performed using scy - 078 citrate type n or scy - 078 citrate type a seeds . the xrpd pattern showed scy - 078 citrate type q is highly crystalline with distinctive diffraction peaks ( fig6 ). scy - 078 citrate type q can convert to scy - 078 citrate type a after vacuum drying at room temperature , indicating that scy - 078 citrate type q is a metastable etoh solvate ( fig6 ). the stability of the two etoh solvates , scy - 078 citrate type n and scy - 078 citrate type q , was evaluated by measuring their solubility at 5 ° c . and 20 ° c . ( table 34 ). the solubility was measured by slurrying scy - 078 citrate type n and scy - 078 citrate type q samples in etoh for 24 hours with a magnetic stirring rate of 1000 rpm . scy - 078 citrate type q exhibited lower solubility than scy - 078 citrate type n in etoh at 5 ° c . and 20 ° c ., indicating that scy - 078 citrate type q is thermodynamically more stable in etoh from 5 ° c . to 20 ° c . xrpd analysis of the remaining wet cakes from the solubility experiments showed no form change for both scy - 078 citrate type q and scy - 078 citrate type n . scy - 078 citrate type r : scy - 078 citrate type r was obtained by slurrying scy - 078 citrate type m in meoh / ipac ( 1 / 14 , v / v ) for 17 hours . scy - 078 citrate type r can also be obtained by reverse anti - solvent addition in meoh / ipac . the xrpd pattern indicated that scy - 078 citrate type r is weakly crystalline ( fig6 ). xrpd analysis also indicated that scy - 078 citrate type r is a metastable solvate that can easily convert to scy - 078 citrate type s upon air drying and to scy - 078 citrate type m after vacuum drying ( fig6 ). scy - 078 citrate type s : scy - 078 citrate type s can be obtained by drying scy - 078 citrate type o sample under ambient or vacuum condition . the xrpd patterns showed shift of diffraction peaks after conversion from scy - 078 citrate type o to scy - 078 citrate type s ( fig6 ). dsc curve exhibited two endothermic peaks at 35 . 7 ° c . and 188 . 0 ° c . ( onset temperatures ) ( fig6 ). tga curve displayed 6 . 6 % weight loss up to 100 ° c . ( fig6 ). dvs plot showed 8 . 2 % water uptake at 25 ° c . and 80 % rh for scy - 078 citrate type s ( fig7 ). xrpd analysis after dvs showed peak shifts . xrpd analysis was further performed at variable temperatures 30 ° c . to 120 ° c . and back to 40 ° c ., which showed a shift of diffraction peaks ( fig7 ). disproportionation of scy - 078 citrate salt : crystalline forms of scy - 078 citrate named type c , type i , type j , and type p were observed either during polymorph study or when investigating the inter - conversion relationship of different scy - 078 citrate forms . xrpd patterns of the four forms ( fig7 ) demonstrated that scy - 078 citrate type c and scy - 078 citrate type j are freebase forms and that scy - 078 citrate type i and scy - 078 citrate type p are likely freebase forms . scy - 078 citrate type i was obtained in dmso / etoh system . scy - 078 citrate type p was obtained by slurrying scy - 078 citrate type m in acetone / h 2 o system . scy - 078 citrate type a disproportionated to the freebase ( scy - 078 citrate type c , which converts to scy - 078 citrate type j upon drying ) when slurrying in etoh / h 2 o , acetone / h 2 o , and buoh / h 2 o systems . slurrying scy - 078 citrate type a or evaporating the citrate solution in dmso , dmac and dcm - related co - solvents also resulted in disproportionation . inter - conversion between scy - 078 citrate type a and citrate type b : slurry experiments were performed with scy - 078 citrate type a in different organic solvents in order to understand the inter - conversion between scy - 078 citrate type a and scy - 078 citrate type b . scy - 078 citrate type a (- 20 mg ) was suspended into a solvent ( 0 . 5 ml ) in a 1 . 5 - ml glass vial . after the suspensions were ultrasonicated for 1 hour or stirred for 6 hours at room temperature , the remaining solids were isolated for xrpd analysis . the results ( table 35 ) indicated that scy - 078 citrate type b can be obtained from various organic solvents . scy - 078 citrate type b was also prepared from scy - 078 citrate type a by slurry in etoh , acn , acetone , mibk , etoac , ipac , dcm , toluene , heptane , meoh / acetone ( 1 / 19 ), ipa / heptane ( 1 / 19 ), thf / toluene ( 1 / 19 ) or by solid vapor diffusion in etoac . scy - 078 citrate type b can convert to scy - 078 citrate type a via drying under n 2 or vacuum at room temperature . inter - conversion between scy - 078 citrate type a and scy - 078 citrate type n and scy - 078 citrate type q : scy - 078 citrate type n can be obtained by slurrying scy - 078 citrate type a ( or scy - 078 citrate type b ) in etoh with ultrasonication or at room temperature for 1 hour . scy - 078 citrate type n rapidly converts to scy - 078 citrate type a via vacuum filtration ( fig7 ). scy - 078 citrate type q was obtained by reactive crystallization of freebase meoh desolvate and citric acid ( 1 : 1 ) in etoh without seeds . after drying in vacuum at room temperature , scy - 078 citrate type q converts to scy - 078 citrate type a ( fig7 ). the study of the inter - conversion between scy - 078 citrate type a and scy - 078 citrate type n and scy - 078 citrate type q is summarized below in table 36 . inter - conversion relationship around channel hydrate scy - 078 citrate type m : metastable solvate scy - 078 citrate type r was obtained by reverse anti - solvent addition in meoh / ipac . scy - 078 citrate type r converted to scy - 078 citrate type e after drying in vacuum at room temperature , and then scy - 078 citrate type m was obtained by storing scy - 078 citrate type e under ambient conditions for 2 days ( fig7 ). scy - 078 citrate type r was found to convert to scy - 078 citrate type m directly upon vacuum drying at room temperature . slurry experiments were performed on scy - 078 citrate type m in selected organic solvents . the results ( table 37 ) indicated that scy - 078 citrate type m converted to scy - 078 citrate type 0 after slurrying in acetone for 17 hours , and scy - 078 citrate type 0 converted to scy - 078 citrate type s after air drying ( fig7 ). scy - 078 citrate type m converted to scy - 078 citrate type a when slurried in acn ( fig7 ), and converted to metastable solvate scy - 078 citrate type r in meoh / ipac co - solvent ( fig7 ). scy - 078 citrate type r converted to scy - 078 citrate type s upon air drying and converted back to scy - 078 citrate type m through vacuum drying at room temperature . no form change was observed by slurrying scy - 078 citrate type m in heptane ( fig7 ). stability study of scy - 078 citrate type a , scy - 078 citrate type m , and scy - 078 citrate type s : as described in example 25 and table 19 , scy - 078 citrate type a is physically / chemically stable at the tested conditions for at least 1 week . to test the physical and chemical stability of scy - 078 citrate type m and scy - 078 citrate type s , each was placed under three different conditions : ( 1 ) open dish at 25 ° c . with 60 % rh ; ( 2 ) open dish at 40 ° c . with 75 % rh ; and ( 3 ) closed dish at 60 ° c . with no humidity control . scy - 078 citrate type m was tested for 4 days and scy - 078 citrate type s was tested for 1 week ( fig8 - 81 ). the results ( table 38 ) showed that scy - 078 citrate type m was physically and chemically stable at 25 ° c . and 60 % rh for at least 4 days . one diffraction peak change and partial crystallinity loss was observed in the xrpd pattern of scy - 078 citrate type m after storage at 40 ° c . and 75 % rh . this is consistent with the previous observation in example 42 that scy - 078 citrate type m partially converts to amorphous after dvs analysis . the impurity of scy - 078 citrate type m increased under closed conditions at 60 ° c . for 4 days . scy - 078 citrate type s is physically and chemically stable under 60 ° c . closed conditions for one week . diffraction peak shifts were observed for the samples stored at 25 ° c . and 60 % rh and 40 ° c . and 75 % rh . alternative preparation of scy - 078 citrate type a : a 10 - l reactor was charged with scy - 078 phosphate ( 450 g ; freebase content in phosphate was 85 . 6 % by hplc ). 2 - methf ( 2 . 25 l ) was charged into the same reactor . a 10 % na 2 co 3 water solution ( 2 . 25 l ) at 20 ° c . was charged into the reaction in 25 min . the suspension was stirred at 20 ° c . for 20 min and then allowed to settle for 30 min . the organic layer was collected and washed with 1 . 8 l of saturated nacl water solution twice , and then further washed with 1 . 8 l deionized water once . the organic layer was transferred to a 4 - l crystallizer . the reactor was rinsed with 250 ml 2 - methf and the liquid was transferred into the crystallizer containing the organic layer . the solution was concentrated in the crystallizer to 900 ml at 50 ° c . the crystallizer was charged with 900 ml methanol and the mixture was cooled to 40 ° c . the mixture was stirred at 40 ° c . for 1 hour ( clear ). 4 . 5 g of seeds were added to the crystallizer and the suspension was aged at 40 ° c . for 1 hour . the mixture was then concentrated to 900 ml at 40 ° c . the crystallizer was then charged with 900 ml methanol and again concentrated to 900 ml at 40 ° c . this step was repeated twice more and the mother liquor was assayed by gas chromatography . the mixture was cooled to 10 ° c . in 2 hours and then aged at 10 ° c . for no less than three hours . the mother liquor was sampled for solution concentration by hplc . the suspension was filtered and the cake was dried in a vacuum over at 35 ° c . for 12 hours . to generate the citrate salt , a 10 - l jacketed crystallizer with a twin - impeller over - head agitator was used . the diameter of the impeller is 13 cm . first , etoh ( 500 ml ) was added into a 10 - l crystallizer ( crystallizer 1 ) and was agitated ( 300 rpm ). the temperature of crystallizer 1 was maintained at 25 ° c . the scy - 078 freebase ( 242 . 09 g ) was added to crystallizer 1 . another volume of etoh ( 500 ml ) was charged into crystallizer 1 . crystallizer 1 was heated to 50 ° c . a citric acid solution , prepared by dissolving citric acid ( 58 . 22 g ) into etoh ( 758 ml ), was charged into crystallizer 1 in 35 min . crystallizer 1 was heated to 55 ° c . and stirred for 20 minutes . then crystallizer 1 was cooled to 50 ° c . for 20 minutes . after cooling , the extraneous matter was filtered ( pore size of 30 ˜ 50 μm ) and the filtrate was transferred to another 10 - l crystallizer ( crystallizer 2 ). the filter was washed with etoh ( 5 ml ) and transferred into crystallizer 2 . the mixture in crystallizer 2 was stirred at 50 ° c . for 30 minutes . next a seed slurry , which was prepared from seeds ( 13 . 22 g ) that were sonicated and dispersed in 50 / 50 etoh / n - heptane ( 68 ml ), was rapidly charged into crystallizer 2 . the mixture in crystallizer 2 was aged at 50 ° c . for 2 hours . crystallizer 2 was then charged with n - heptane ( 1758 ml ) for 12 hours at 50 ° c . the mixture was again aged at 50 ° c . for 2 hours . from the resulting mixture , a sample was taken for xrpd analysis and microscopy . the mixture was cooled to 20 ° c . in 2 hours and then stirred at 20 ° c . for 3 hours . the batch was filtered and the cake was washed with a solution of 1 : 1 etoh / n - heptune ( 500 ml ). the cake was blown with n 2 for 60 minutes . finally , the cake was dried at 45 - 55 ° c . with n 2 blowing . ultimately 241 grams of product was obtained with a 86 . 4 % yield . xrpd analysis showed that the product was highly crystalline scy - 078 citrate type a ( fig8 ). tga curve showed a weight loss of 2 . 2 % before 150 ° c . ( fig8 ). the dsc curve showed a melting point of 197 . 8 ° c . ( onset temperature ) ( fig8 ). the resulting crystals were rod - like with an average size of 34 . 2 pm ( fig8 ). preparation and characterization of scy - 078 trifluoroacetate type a : scy - 078 amorphous freebase ( 994 . 3 mg ) and trifluoroacetic acid ( freebase / acid molar ratio — 1 / 1 ) were weighted into a 5 - ml vial , followed by addition of 5 ml acetonitrile . the mixture was slurried at rt with a magnetic stirring rate of 1000 rpm for 4 days . the suspension was centrifuged and vacuum dried at rt overnight . scy - 078 trifluoroacetate type a is highly crystalline as shown in the xrpd ( fig8 ). a weight loss of 1 . 1 % is observed up to 120 ° c . in the tga curve ( fig8 ). the dsc ( fig8 ) shows two endothermic peaks , one at 65 . 8 ° c . and 229 . 8 ° c . trifluoroacetate type a converted to type b after stored under ambient conditions for 2 days ( fig8 ). the molar ratio of trifluoroacetate type a ( acid : freebase ) was determined to be 1 : 1 via hplc - ic confirmation . preparation and characterization of scy - 078 trifluoroacetate type b : trifluoroacetic acid ( 331 . 5 mg ) was added into acetonitrile ( 8 ml ) in a 20 - ml glass vial , followed by addition of amorphous scy - 078 freebase type a ( freebase / acid molar ratio = 1 / 1 ). the mixture was stirred at rt with a magnetic stirring rate of 600 rpm for 24 hours . the suspension was vacuum filtered and dried at rt for 20 hours . trifluoroacetate type a was obtained ( 2 . 18 g ), which converted to trifluoroacetate type b after storage at ambient conditions for almost 1 month . scy - 078 trifluoroacetate type b is highly crystalline as shown in the xrpd ( fig8 ). a weight loss of 4 . 7 % is observed up to 120 ° c . in the tga curve ( fig8 ). the dsc ( fig8 ) shows two endothermic peaks , one at 92 . 8 ° c . and 230 . 0 ° c . due to the reversible conversation of trifluoroacetate type a and type b , the molar ratio of trifluoroacetate type b ( acid : freebase ) is postulated to be 1 : 1 , same as type a . from the dvs ( fig9 ), 3 . 4 wt % of water uptake was observed at 25 ° c . 80 % rh , indicating that type b is moderately hygroscopic . the dvs revealed potential form change with respect to rh , estimated to be between 30 % rh and 40 % rh . scy - 078 trifluoroacetate type b converted to type a after dvs as shown in fig9 . to investigate transition relationship of trifluoroacetate type a and type b , both samples were stored in chambers with varying relative humidity to monitor any form change . summary of trifluoroacetate type b stored at varying relative humidity is listed in table 39 , and xrpd patterns overlay is displayed in fig9 . trifluoroacetate type b converted to type a only at high relative humidity ( 97 % rh ) while type b is stable at low relative humidity (& lt ; 22 % rh ). varying temperature ( vt )- xrpd of trifluoroacetate type a was performed . vt - xrpd patterns overlay is displayed in fig9 . type a converted to type b after heated to 120 ° c . preparation and characterization of scy - 078 hcl type i : 342 . 7 μl of concentrated hcl ( 37 . 5 %) was dispersed in 40 ml of acetone . 2 . 0 mg of scy - 078 freebase type a ( freebase / acid molar ratio = 1 / 1 . 5 ) was added . the suspension was settled in a biochemical incubator to perform heat - cooling cycles ( 50 ° c .˜ 20 ° c .) with a magnetic stirring rate of 600 rpm . the suspension was cooled to 5 ° c . at a rate of 0 . 1 ° c ./ min and aged at 5 ° c . for 17 hours . the wet cake was vacuum filtered and dried at rt for 20 hours . scy - 078 hcl type i ( 2 . 06 g ) was obtained . scy - 078 hcl type i is highly crystalline as shown in the xrpd ( fig9 ). a weight loss of 4 . 2 % is observed up to 120 ° c . in the tga curve ( fig9 ). the dsc ( fig9 ) shows three endothermic peaks , one at 46 . 2 ° c ., one at 115 . 5 ° c . and one at 274 . 3 ° c . the molar ratio of scy - 078 hcl type i ( acid : freebase ) was determined to be 1 . 5 : 1 via hplc - ic . from the dvs ( fig9 ), 6 . 1 wt % of water uptake was observed at 25 ° c ./ 80 % rh , indicating hcl type i is moderately hygroscopic . no form change was observed after dvs characterization as shown in fig9 . preparation and characterization of scy - 078 hcl type ii : scy - 078 hcl type ii was obtained by suspending hcl type i in acetate buffer ( ph 5 . 5 ) for 4 hours . the xrpd pattern ( fig9 ) indicates type ii is highly crystalline . the tga shows that hcl type ii exhibits a weigh loss of 6 . 9 % up to 150 ° c . and the dsc shows an endothermic peak at 48 . 3 ° c . ( onset temperature ), as shown in fig9 . the solubility of trifluoroacetate type a , type b and hcl type i was measured in sgf at ambient temperature . approximately 90 mg of solid sample was weighted into a 4 - ml centrifuge tube , and 3 ml of sgf buffer was added before leaving the suspension on a rolling incubator ( 25 r / min ). 1 . 0 ml aliquot of the suspension was sampled for centrifugation ( 10000 rpm , 3 mins ) the supernatant was analyzed by hplc and ph measurement and solid by xrpd characterization at 1 hr , 4 hr and 24 hrs , respectively . the results are summarized in table 40 and the solubility curves are displayed in fig1 . all three salts exhibit high solubility in sgf (& gt ; 20 mg / ml at 24 hrs ). trifluoroacetate type b converted to type a in sgf after an hour . however , no form change was observed of trifluoroacetate type a and hcl type i in sgf . the xrpd patterns of residual solid are shown in fig1 , fig1 , and fig1 . the solubility of trifluoroacetate type a , type b and hydrochloride type i was measured in the fassif alternative media at ambient temperature . approximately 15 mg of solid sample was weighted into a 4 - ml plastic tube , and 3 ml of the media was added before leaving the suspension on a rolling incubator ( 25 r / min ). 1 . 0 ml aliquot of the suspension was sampled for centrifugation with the supernatant submitted for hplc and ph measurement and solid for xrpd characterization at 1 hr , 4 hr and 24 hrs , respectively . the results are summarized in table 41 and the solubility curves are displayed in fig1 . all three salts exhibit poor solubility in the fassif alternative media (& lt ; 0 . 01 mg / ml at 24the kinetic hrs ). trifluoroacetate type b converted to type a after an hour . however , no form change was observed of trifluoroacetate type a and hcl type i . the xrpd patterns of residual solid are shown in fig1 , fig1 , and fig1 . the solubility of trifluoroacetate type a , type b and hcl type i was measured in the fessif alternative media at ambient temperature . approximately 36 mg of solid sample was weighted into a 4 - ml plastic tube , and 3 ml of the media was added before leaving the suspension on a rolling incubator ( 25 r / min ). 1 . 0 ml aliquot of the suspension was sampled for centrifugation with the supernatant submitted for hplc and ph measurement and solid for xrpd characterization at 1 hr , 4 hr and 24 hrs , respectively . the results are summarized in table 42 and the solubility curves are displayed in fig1 . all three salts exhibit a solubility of ˜ 3 mg / ml at first one hour . hcl type i exhibits an equilibrium solubility of 3 . 5 mg / ml at 24 hrs , while trifluoroacetate ( both type a and type b ) exhibit a decreasing solubility after an hour . trifluoroacetate type a converted to type b after an hour . however , no form change was observed of trifluoroacetate type b and hydrochloride type i . the xrpd patterns of residual solid were included in fig1 , fig1 , and fig1 . the solubility of trifluoroacetate type a , type b and hcl type i was measured in acetate buffer ( ph 5 . 5 ) at ambient temperature . approximately 15 mg of solid sample was weighted into a 4 - ml plastic tube , and 3 ml of acetate ph 5 . 5 buffer was added before leaving the suspension on a rolling incubator ( 25 r / min ). 1 . 0 ml aliquot of the suspension was sampled for centrifugation with the supernatant submitted for hplc and ph measurement and solid for xrpd characterization at 4 hr and 24 hrs , respectively . the results are summarized in table 43 and the solubility curves are displayed in fig1 . trifluoroacetate type a exhibits higher solubility in acetate ph 5 . 5 buffer , and no form change was observed . however , type b converted to type a in acetate ph 5 . 5 buffer . while hcl type i exhibits lower solubility in acetate ph 5 . 5 buffer comparing with trifluoroacetate , and hcl type i converted to type ii in acetate ph 5 . 5 buffer . the xrpd patterns of residual solid were included in fig1 , fig1 , and fig1 . the solubility of trifluoroacetate type a , type b and hcl type i was measured in the phosphate ( ph 6 . 0 ) alternative media at ambient temperature . approximately 15 mg of solid sample was weighted into a 4 - ml plastic tube , and 3 ml of media was added before leaving the suspension on a rolling incubator ( 25 r / min ). 1 . 0 ml aliquot of the suspension was sampled for centrifugation with the supernatant for hplc and ph measurement and solid for xrpd characterization at 4 hr and 24 hrs , respectively . the results are summarized in table 44 , and the solubility curves are displayed in fig1 . hcl type i exhibits higher solubility , while trifluoroacetate type a exhibits lower solubility . trifluoroacetate type a firstly converted to type b at 4 hrs and back to type a at 24 hrs , while type b converted to type a at 24 hrs . no form change was observed of hcl type i . the xrpd patterns of residual solid were included in fig1 , fig1 , and fig1 . physical and chemical stability evaluation of trifluoroacetate type a , trifluoroacetate type b , and hcl type i was performed at 25 ° c ./ 60 % rh , 40 ° c ./ 75 % rh and 60 ° c . for 1 , 2 , 4 and 8 weeks . in the experiments , approximately 20 mg of solid was placed into a 1 . 5 - ml glass vial . the vials were stored under 25 ° c ./ 60 % rh ( uncapped ), 40 ° c ./ 75 % rh ( uncapped ) and 60 ° c . ( capped ) conditions for 8 weeks . xrpd analysis was then employed to check the crystalline form of the solid , and hplc was utilized to determine the purity profile at 1 , 2 , 4 and 8 weeks . from the stability results summarized in table 45 , both trifluoroacetate type a and hcl type i are physically and chemically stable under 25 ° c ./ 60 % rh , 40 ° c ./ 75 % rh and 60 ° c . conditions for 8 weeks . the solid form change of trifluoroacetate type a at 2 and 4 weeks was postulated to the air - exposure when the sample was taken out for xrpd characterization . trifluoroacetate type b is chemically stable , however , physically unstable evidenced by conversion to type a under these conditions . xrpd patterns overlay of trifluoroacetate types a and b and hcl type i at stressed conditions are displayed from fig1 to fig1 . | 2 |
as conducive to a full understanding of the novelty and utility of the present invention , one example of a conventional valve device will first be briefly described with reference to fig1 . throughout the following description of the known valve device and the valve device according to the present invention , directions indicated by terms such as &# 34 ; upper &# 34 ;, &# 34 ; lower &# 34 ;, &# 34 ; above &# 34 ;, and &# 34 ; below &# 34 ; are those as viewed in the figures of the accompanying drawings . this known valve device 10 , which is a gate valve of the so - called outside screw yoke type , has a housing structure comprising a valve casing or body 11 and bonnet 12 fixed together , with a gasket 13 interposed therebetween , by screws 14 . centrally disposed partly within the body 11 and extending and beyond the bonnet 12 is a valve stem 15 . this stem 15 has a lower sliding part with a smooth outer surface and an upper screw - threaded part 20 . an annular gland packing 16 is fitted between the sliding part of the stem 15 and the upper part of the bonnet 12 in order to prevent leakage therebetween . the gland packing 16 is held in place by an annular packing retainer 17 , which in turn is pressed downward against the gland packing 16 by fixing bolts 18 . the stem 15 is connected at its inner end to a valve element , which in the example shown , is a gate 21 . a handle or handwheel 19 is screw engaged with the upper threaded part 20 of the stem 15 . by rotating the handwheel 19 the stem 15 can be raised or lowered together with the gate 21 thereby to open or shut the valve . in the valve device 10 of the above described construction , exchanging of the packing 16 is possible without removing the bonnet 12 , that is , with the valve in opened state , by loosening the fixing bolts 18 , swinging the same outward , and moving the packing retainer 17 upward . however , in order to replace the gasket 13 , it is necessary to remove the bonnet 12 . consequently , it is necessary to stop the flow of the fluid in the piping by shutting separate shut - off valves ( not shown ) provided in the piping on the upstream and downstream sides of the valve device 10 . as a result , at the time of replacement of the sealing members , it is necessary to temporarily stop the operation of the equipment in which the valve device 10 is installed , whereby this valve device 10 cannot be applied in equipment of continuous operation the interruption of which is undesirable . furthermore , in the above described valve device 10 , the assembly and attachment of the various parts with respect to the body 12 is complicated . moreover , the packing retainer 17 and related parts cannot be drawn out from the stem 15 , and an ample working space cannot be obtained . for this reason , the work of replacing the sealing members is troublesome and requires excessive time . thus , this valve device 10 is unsuitable for use in equipment handling fluids contaminated with radiation as , for example , the aforementioned equipment in a nuclear power plant . accordingly , it is contemplated in the present invention to provide a valve of a construction such that the work of periodically replacing its sealing members can be carried out with the rest of the equipment in continuous operation and , moreover , in a short time . in a first embodiment of the invention as illustrated in fig2 and 3 , a valve device 30 , which is of the inside screw type construction , comprises essentially a valve body 31 , a bonnet 32 fixed to the body 31 , a valve stem 33 , and a stem holding member 34 constituting an essential element of the present invention for holding the stem 33 in a screw - engaged manner . the body 31 is provided therein with a fluid flow passage 35 comprising a inflow passage 35a and an outflow passage 35b and a stem insertion bore 36 having a bottom and formed with a centerline axis intersecting substantially perpendicularly that of the flow passage 35 at the middle part thereof . a cylindrical valve seat 37 is provided at the part where the stem insertion bore 36 intersects the flow passage 35 . a valve element 38 , which is a wedge - shaped gate connected to the lower end of the stem 33 , is moved up or down together with the stem 33 to be separated from or seated against the valve seat 37 thereby to open or shut the flow passage 35 . the stem 33 can be rotated about its axis by turning a handwheel 39 fixed to its outer or upper end . the stem 33 is provided around a portion thereof somewhat above its lower end with square screw threads 33a . the aforementioned stem holding member 34 is generally of the shape of a hollow cylinder coaxially disposed around the stem 33 and having at its upper portion internal screw threads 34c meshed with the above mentioned screw threads 33a of the stem 33 . the lower portion of this stem holding member 34 is provided around its outer surface with external screw threads 34c , which are meshed with internal screw threads 36a formed on the wall surface of the above mentioned stem insertion bore 36 at the upper open part of the body 31 . thus the stem holding member 34 is fixed to the body 31 . this screw connection and fixing of the stem holding member 34 is adopted with consideration of work such as replacement of parts such as the valve gate 38 . the stem holding member 34 has at its lower end an annular contact surface 34b which , when this member 34 is fixed in place as described above , is pressed with a specific pressure in abutting state against an annular ledge 36b formed in the wall of the bore 36 , thereby being in a metal - contact state . in this case , the annular contact surface 34b and the annular ledge 36b are both precision finished to exact planar surfaces and thereby constitute a first metal - contact seal 40 . this first metal - contact seal 40 is continually in sealing state while the stem holding member 34 is fixed in position . the inner wall surface of the stem holding member 34 at the lower end of the internal screw threads 34c is increased in inner diameter , whereby a downwardly facing ledge is formed . the inner rim of this ledge is chamfered to form a bevel seat surface 34d to function as described hereinafter . the lower surface of the bonnet 32 is fixed by screws 42 to the upper surface of the body 31 with a spiral gasket 41 interposed therebetween . at the upper part of the bonnet 32 , a packing 43 of the shape of a hollow cylinder is fitted between the inner wall of the bonnet and the stem 33 and is held in place by a packing retainer 45 , which in turn is pressed downward against the packing 43 by a cap nut 44 screw engaged with the upper part of the bonnet 32 . when the handwheel 39 of the valve device 30 of the above described construction is turned , and the valve gate 38 is lifted off from the valve seat 37 to its fully - opened state , the fluid ( not shown ) in the piping flows into the flow passage 35 . in this valve device 30 , the bonnet 32 is of a double - seal construction afforded by the first metal - contact seal 40 serving as a first - stage barrier and the gasket 41 and the packing 43 serving as a second - stage barrier . in addition , the passage of infiltration of the fluid into a space 46 in the interior of the bonnet 32 and around the stem 33 is limited to only the meshing part 47 between the screw threads 33a and 34c , and the rate of infiltration of the fluid into the space 46 is very low . moreover , the pressure of the fluid infiltrating into the space 46 becomes low . for these reasons , the capability of the valve device 30 to prevent leakage of the fluid to the outside is markedly superior to that of the known valve device 10 . accordingly , this valve device 30 of the invention is highly suitable for use in places where fluids in piping must positively be prevented from leaking to the outside . furthermore , when the meshing part 47 of the screw threads 33a and 34c is made to be a very narrow flow passage , it acts to cushion the transmission of pressure therethrough . for this reason , the pressure of the fluid within the flow passage 35 does not act directly on the gasket 41 . as a result , the serviceable life of the gasket 41 is prolonged , and the period between replacements is lengthened . next , the procedure of replacing the packing 43 and the gasket 41 of this valve device 30 will be described with reference to fig3 . this replacement of exchanging of these sealing members is carried out as described below with the valve device 30 in its opened state without shutting off the flow of the fluid through the piping including the valve device 30 . first , the handwheel 39 is turned in the valve opening direction to cause the stem 33 to reach the upper limiting position of its movement . when the stem 33 thus reaches this limiting position , the rotation of the handwheel 39 is limited . at this instant , however , the handwheel 39 is not immediately released from the turning manipulation , but a specific torque in the valve opening direction is further applied thereto , after which the handwheel manipulation is stopped . by this handwheel manipulation , the annular edge part 33b - 1 of a flange part 33b of the stem 33 near the lower end thereof is brought into a state wherein it is pressed with a specific pressure into contact against the aforementioned chamfered seat surface 34d of the stem holding member 34 . these parts thus form a second metal - contact seal 48 , which seals the screw meshing part 47 . as a result of the functioning of the first and second metal - contact seals 40 and 48 , the space 46 is placed in a state wherein it is completely sealed off from the flow passage 35 , and the fluid in the flow passage 35 cannot leak out even when the bonnet 32 is disconnected and removed from the body 31 . to replace the replaceable sealing members , the handwheel 39 is first detached from the stem 33 , this detaching being possible because this valve device 30 is of the inside - screw type . next , the nut 44 is unscrewed off , and the packing 43 is extracted upward . the screws 42 are then unscrewed and removed , and the bonnet 32 is lifted straight upward , away from the body 31 , until it is free of the stem 33 . with the valve parts in this disassembled state , the gasket 41 and the packing 43 can be readily replaced . the disassembled valve parts are thereafter reassembled in the sequence which is reverse to that described above for disassembly . in this case , the work of replacing the sealing members can be carried out efficiently in a short time because the bonnet 32 can be handled as a single unitary structure . this feature is highly important in positively protecting the human body from harmful effects in hazardous environments such as that involving nuclear radiation . furthermore , this valve device 30 affords great safety because there is little possibility of leakage of the fluid to the outside at the time of replacement of the sealing members . since , as described above , the work of replacing the sealing members can be carried out while the valve device 30 is opened , that is , with the equipment in which the valve is installed in operation , the valve device 30 is highly suitable for use in the equipment of such facilities as nuclear power plants , facilities handling petroleum products , and city gas supplying facilities . if , in the machining of the stem 33 , the above described annular edge 33b - 1 of the flange part 33b is rounded with a radius of curvature of the order of 0 . 1 mm ., galling or scoring of the chamfered surface 34d of stem holding member 34 and damaging of the annular edge can be effectively prevented , and the metal - contact seal 48 will function with a positive sealing effect . furthermore , even when the valve device 30 is in its fully shut state , the space 46 is in a state wherein it is positively sealed from the flow passage 35 . for this reason , replacement of the sealing members can be carried out also in the fully - shut state of the valve . a second embodiment of the valve of the invention will now be described with reference to fig4 . in fig4 those structural parts which are essentially the same as corresponding parts in fig2 are designated by like reference numerals . detailed description of such parts will be omitted . a valve device 50 of the invention has a construction which is fundamentally the same as that of the aforedescribed valve device 30 and employs o - rings for its replaceable sealing members . this valve device 50 is suitabe for use in equipment handling fluids at lower temperatures than those in the case of the aforedescribed valve device 30 . in this valve device 50 , an o - ring 51 is interposed between the bonnet 32 and the body 31 . in the bonnet 32 , a ring 52 comprising a combination of an o - ring and a back - up ring is fitted in an annular recess formed in the inner surface of a through bore 32a through which the stem 33 is passed at the upper part of the bonnet . the replacement of the o - ring 51 and the ring 52 can be carried out rapidly , similarly as in the case of the aforedescribed valve device 30 . because of this sealing arrangement wherein use is made of the combined ring 52 as the sealing member in the through bore 32a of the bonnet 32 in this valve device 50 , the force needed to turn the handwheel 39 is less than that in the case of the valve device 30 in which a gland packing is used . the reason for this is that the gland packing is being pressed by the packing retainer in order to assure its sealing performance , and consequently this increases the resistance to rotation of the handwheel . in the valve device 50 , furthermore , there is little possibility of rusting of the stem 33 which tends to occur when a gland packing is used because of the halogen compounds contained in the asbestos , which is the principal constituent of the gland packing . in the case where the above described valve devices 30 and 50 are to used in nuclear power equipment , both the stem 33 and the stem holding member 34 are made of austenitic stainless steel in consideration of their corrosion resistance . for this reason , the screw meshing part 47 becomes a combination of parts of the same material , whereby galling or scoring would readily occur . accordingly , in the present embodiment of the invention , the threaded part 33a of the stem is roll threaded thereby to increase the surface hardness thereof ( for example , to a surface hardness of h r c 50 ). by this measure , a difference in hardness is established between the meshing screw thread parts 33a and 34c , and galling is suppressed . examples of modification of the second metal - contact seal 48 in the above described valve devices 30 and 50 will now be described with reference to fig5 , and 7 . in these figures , those constituent parts which are the same or equivalently similar to corresponding parts in fig3 are designated by like reference numerals . referring first to fig5 showing a first modification , the flange part 61 of this metal - contact seal 60 has a stellite - filled construction comprising a main body part 61a and a peripheral stellite - filled part 61b . the stellite - filled part 61b in the flange part 61 has an annular edge part 61b - 1 which is pressed against the chamfered seat surface 34d of the stem holding member 34 thereby to form the metal - contact seal 60 . in this case , since there is a difference between the hardnesses of the stellite - filled part 61b and the seat surface 34d , galling does not readily occur . furthermore , if the annular edge part 61b - 1 is rounded , galling and chipping of the contacting parts can be prevented with even greater effectiveness . a second modification of the second metal - contact seal 48 is illustrated in fig6 . in this metal - contact seal 70 , the stem holding member 34 has a ledge - like annular planar surface 34e formed therein instead of the annular chamfered seat surface 34d . an upwardly facing planar surface 33b - 2 of the flange part 33b of the stem 33 is adapted to be abuttingly pressed against this downwardly facing annular planar surface 34e . in this construction , the tendency for galling to occur is less , and , moreover , the machining is easier , than in the case of the metal - contact seal 48 shown in fig3 . fig7 illustrates a third modification . in this metal - contact seal 80 , a downwardly directed annular projection 34f is formed in the stem holding member 34 in place of the annular chamfered seat surface 34d , and the upwardly facing planar surface 33b - 2 of the flange part 33b of the stem 33 is adapted to be abuttingly pressed against the lower planar surface 34f - 1 of this annular projection 34f with a margin of a width d left around the periphery . by this construction , a metal - contact seal can be obtained with a uniform width around the entire periphery thereof even when the centerline axes of the stem 33 and its flange part 33c are out of alinement . | 5 |
the following description provides embodiments of apparatus that provide protection for building subject to events that increase the load on conduit hangers . specifically , methods and apparatuses for supporting conduits using frangible hanger assemblies are described . such methods and apparatus allow the conduit hanger to fail before the buildings to which they are attached . fig2 a is an elevational view of a first embodiment conduit hanger assembly 30 installed to support conduit 12 from concrete deck 14 . conduit hanger assembly 30 includes anchor 16 which may be placed within concrete deck 14 . anchor 16 can , in general , be a drill - in , shoot - in or glue - in type anchor for attaching to poured concrete or a cast - in - place type anchorage that is set into the concrete during pouring . anchor 16 is attached to a first threaded rod 21 that extends downwards from the anchor , and a connector assembly 32 attached to the first threaded rod and which supports bracket 18 . more specifically , connector assembly 32 includes a connector link assembly 40 threadable into first threaded rod 21 and threaded rod 22 and threaded nuts 26 which are used to support bracket 18 . connector link assembly 40 and the various embodiments and combinations described here function as a tension component for supporting conduits up to some maximum load . when the maximum load is exceeded , the connector link assembly 40 , which is frangible breaks . in certain embodiments , the connector link assembly 40 breaks by a ductile fracture . this invention facilitates the design of utility hanger assemblies and the like so that in the serial chain of components supporting a load , the link assembly will meet the load requirements and be the first to fail in an overload condition . connector link assembly 40 , as discussed subsequently in greater detail , includes a connector piece 42 having a first end 421 and a second end 423 , and a pair of connector links shown as an upper link 44 a having a first end 441 a and a second end 443 a , and a lower link 44 b having a first end 441 b and a second end 443 b . first end 441 a has internal threads and is threadably connected to threaded rod 21 and second end 443 a is attached to first end 421 using fastener ( s ) 53 . first end 441 b has internal threads and is threadably connected to threaded rod 22 and second end 443 b is attached to second end 423 using fastener ( s ) 51 , as discussed subsequently . conduit hanger assembly 30 is designed to be able to hold the load of conduit 12 from concrete deck 14 and , in the case of a sufficiently large tensile force , fail before the concrete fails . in this way , conduit hanger assembly 30 does not damage the integrity of concrete deck 14 . in certain embodiments , connector link assembly 40 undergoes testing to determine the maximum load that it may support in a seismic event . the actual tests may vary according to local building codes . in general , one may determine a maximum permissible load for any configuration of connector link assembly 40 by , for example , seismic testing . thus , in one embodiment , connector piece 42 is frangible and , specifically , is designed to be the weakest part of conduit hanger assembly 30 under tension . fig2 b is the view of fig2 a , where connector piece 42 is subjected to a sufficient force to fail before the concrete deck fails . the inventive conduit hanger assembly 30 thus fails with a break in connector piece 42 , leaving anchor 16 , threaded rod 21 , and upper link 44 a attached to concrete deck 14 . this is in contrast to the prior art conduit hanger assembly , as shown in prior art fig1 b . the failure of connector piece 42 near upper connector link 44 a is illustrative , and the failure mode of conduit hanger assembly 30 may be at some other place in the conduit hanger assembly , such as in connector piece 42 near lower connect link 44 b , some other location in the connector piece , or some other location within the conduit hanger assembly that does not result in damage to concrete deck 14 . in certain embodiments , connector links 44 a and 44 b are identical , and are shown in fig3 a through 3e as one embodiment of a connector link 44 , where fig3 a is a perspective view , fig3 b is a front elevational view , fig3 c is a side elevational view of the connector link of fig3 a , fig3 d is a top plan view , and fig3 e is a bottom plan view . connector link 44 has a first end 4401 , which is generally similar to first ends 441 a and 441 b of fig2 a and a second end 4403 , which is generally similar to second ends 443 a and 443 b of fig2 a . first end 4401 has a bore 49 that is threaded to accept a male threaded rod , stud or bolt , such as a threaded rod 21 or 22 , and two legs 45 defining a narrow gap 46 ( as , for example , second ends 443 a and 443 b of fig2 a ) between the two legs , and transverse holes 47 through legs 45 that align on either side of the gap 46 . while fig3 a , 3b , and 3c show two holes 47 , various embodiments may have one hole or may have three or more holes . first end 4401 also includes an upper portion 48 which is hexagonally shaped along a longitudinal axis to facilitate cooperation with wrenches and tools for engagement and tightening a threaded connection . alternatively , upper portion 48 may be cylindrical , square or other shape depending on the type of connection method . the gap 46 is designed to accept a connector piece , such as connector piece 42 . in certain embodiments , an end of gap 46 provides a seat against which connector piece 42 rests when the connector piece is fully inserted into gap 46 . a pin placed through transverse hole 47 can also pass through a hole in the connector piece 42 , as discussed subsequently , for retaining connector piece 42 . fastener ( s ) 51 and 53 and transverse hole 47 may , in alternative embodiments , be unthreaded , partially threaded , or threaded throughout . in a second embodiment conduit hanger assembly , connector link 44 a and first threaded rod 21 of conduit hanger assembly 30 are replaced with a second embodiment connector link 54 , which combines the function of connector link 44 a and the first threaded rod 21 . fig4 a is a front elevational view of second embodiment connector link 54 , and fig4 b is a side elevational view of the connector link of fig4 b . connector link 54 is generally similar to connector link 44 and first threaded rod 21 , except as explicitly stated . connector link 54 has a first end 5401 and a second end 5403 . first end 5401 includes an integral or attached threaded stud 56 that is threadable into anchor 16 . second end 5403 is generally similar to second end 4403 and supports connector piece 42 . fig6 a is a side elevational view of the connector link of fig4 a and 4b attached to a drill - in type anchor 16 . in a third embodiment conduit hanger assembly , connector link 44 a , first threaded rod 21 , and anchor 16 of conduit hanger assembly 30 are replaced with a third embodiment connector link 64 , which combines the function of connector link 44 a , the first connector rod , and the anchor . fig5 a is a front elevational view of a third embodiment connector link 64 , and fig5 b is a side elevational view of the connector link . connector link 64 is generally similar to connector link 54 and / or 44 , except as explicitly stated . connector link 64 includes an anchor 66 , at a first connector link end 6401 , and two legs 45 defining a narrow gap 46 at a second connector link end 6403 . anchor 66 of first connector link end 6401 can be anchored directly in the concrete pour of concrete deck 14 , and second connector link end 6403 can support connector piece 42 . fig6 b is a side elevational view of the connector link of fig5 a and 5b cast into a concrete deck 14 . a wide variety of geometries may be used for connector piece 42 . thus , for example and without limitation , fig7 a is a sectional view 7 a - 7 a of fig2 a , where connector piece 42 , is a length of electrical conduit disposed in the gap 46 of the legs 45 legs 45 may which may be , for example and without limitation , the legs of connector link 44 , 54 , or 64 . as further examples of connector piece 42 : fig7 b is similar to fig7 a , where connector piece 42 is a length of pipe 72 ; fig7 c is similar to fig7 a , where connector piece 42 is a length of rectangular tubing 74 ; fig7 d is similar to fig7 a , where connector piece 42 is a length of strut channel 76 ; and fig7 e is similar to fig7 a , where connector piece 42 is a length of an angle piece 78 . fig8 a , 8b , and 8c are illustrative of one method of assembling the pieces of connector assembly 40 using connector piece 42 . fig8 c is a side view of connector piece 42 , and fig8 a and 8c are a front elevation view and side elevational view , respectively , of connector assembly 40 . it will be appreciated that the following description applies , for example and without limitation , to any of the other connector pieces , such as connector piece 42 , 74 , 76 , or 78 . as shown in fig8 c , connector piece 42 has , or is provided with , one or more holes 52 and , as shown in fig8 a and 8b , connector piece 42 is attached to links 44 a and 44 b by placing each end of connector piece 42 is positioned all of the way into gap 46 of each connector link 44 . next , fastener ( s ) 51 and 53 , which may be , for example , one or more fasteners 50 which are self - drilling , self - tapping , standard threaded , pins or rivets . in any case , hole or holes 52 in connector piece 42 are provide to will align with holes 47 in the connector links 44 a / 44 b . in certain embodiments , hole 52 is positioned at a predetermined distance d from first end 421 by pre - drilling the hole . in the embodiments , where hole 52 is not pre - drilled , connection piece 42 may be inserted into gap 46 such that a desired distance d is achieved by advancing the fastener into the connection piece . in certain embodiments , the distance d determines when connection piece 42 fails , as shown in fig2 b . since larger distances d correspond to a higher load before failure , a user may select a distance d that determines when conduit hanger assembly 30 will fail under a tensile load . one example of the desired structural failure of frangible connector piece 42 , which is not meant to limit the scope of the present invention , is illustrated in fig8 c , 9a , and 9b , where fig8 c is a side view of connector piece 42 prior to failure , and fig9 a and 9b are a front elevation view and side elevational view , respectively , of connector assembly 40 after the structural failure of connector piece 42 . regardless of how hole 52 is formed , under a sufficient tensile load , the hole may first elongate as it undergoes ductile fracture , as shown in fig8 d . as the load increases , connector assembly 40 will ultimately fail when the strength of the connector assembly is exceeded , as shown in fig9 a and 9b . in certain embodiments , the maximum load which connector assembly 40 may support is determined by several parameters , which may be , for example , the thickness t of connector piece 40 ( see fig7 a - 7 e ), the material of the connector piece , the distance d between hole 52 and first end 421 , and details of fastener 50 , such as the fastener size and material . thus , as described above , failure loads for specific connector assembly 40 may be determined as a function of the various parameters noted in the previous paragraph ( fastener type , thickness , materials , hole locations and diameters , etc .). the selection of parameters thus provides a calibration indicating the failure of the connector assembly and a user can be provided with configurations which may fail at certain loadings . fig1 a - 10c illustrate a first alternative embodiment of connector link 44 of fig3 a including aperture 82 at upper portion 48 , where fig1 a is a perspective view , fig1 b is a front elevational view , and fig1 c is a side elevational view of the connector link as upper connector link 44 a attached to a concrete anchor 16 . first alternative connector link 44 may , in general , be used as upper link 44 a or lower link 44 b . aperture 82 intersects the bore 49 , and may alternatively continue through the opposite side of upper portion 48 . aperture 82 permits visual inspection of the engagement of anchor 16 threads , as shown in fig1 c . fig1 a - 11c illustrate a second alternative embodiment of connector link 44 of fig3 a including a threaded aperture 82 a , where fig1 a is front elevational view , fig1 b is a top plan view , and fig1 c is a side elevational view of the connector link as upper connector link 44 a attached to concrete anchor 16 . second alternative connector link 44 may , in general , be used as upper link 44 a or lower link 44 b . connector link 44 of fig1 a - 11c is useful for further securing the connector link to anchor 16 . threaded aperture 82 a can accept a threaded fastener 86 that can act as a set - bolt when tightened against a rod inserted into a bore 49 a , which may be threaded or non - threaded . as in the second alternative embodiment link 44 , aperture 82 a may pass through upper portion 48 to bore 49 a , or may pass through the opposite wall . the set - screw arrangement will work well securing non - threaded rods . fig1 a - 12c illustrate the second alternative embodiment connector link 44 of fig1 a with a clevis - type attachment , where fig1 a is a front elevational view , fig1 b is a side elevational view , and fig1 c is a front elevational view of the connector link attached to concrete anchor 16 . fig1 a - 12c show the second alternative embodiment connector link 44 a of fig1 a and a clevis 94 , formed by the combination of a u - shaped bracket 90 , a bolt 88 and a nut 89 pivotally attached to the connector link at aperture 82 . the top of bracket 90 includes an aperture 92 to allow connection to anchor 16 or other components in a hanger assembly . fig1 a , 13b , and 13c are front elevational views of a first , second , and third alternative embodiment of connector assembly 40 . from either calculations or from trial - and - error , the amount of tensile load required for connector piece 42 to fail at that location can be determined , and can be considered to be a calibrated strength of conduit hanger assembly 30 . in the embodiment of fig1 a , there are two fasteners 53 near first end 421 and one fastener 51 located a distance d 1 from second end 423 . with this embodiment , the weakest part of connector piece 42 is between second end 423 and the hole that is at the distance d 1 from the second end . in the embodiment of fig1 b , there is one fasteners 53 located a distance d 2 from first end 421 and two fasteners 51 located near second end 423 . with this embodiment , the weakest part of connector piece 42 is between first end 421 and the hole that is at the distance d 2 from the first end . in the embodiment of fig1 c , there is one fasteners 53 located a distance d 2 from near first end 421 and one fastener 51 located a distance d 3 from second end 423 . for this embodiment , the distances d 2 and d 3 determine the load factor at each end of the connector piece . fig1 a is a side elevational view of any of the connector link assemblies described herein with indicia 100 . thus , for example , connector link assembly 40 of fig1 b is shown with indicia 100 on connector piece 42 . a user may user indicia 100 to align connector piece 42 with end 4403 of upper link 44 a , prior to inserting one fastener 53 . this allows the user to be sure that the proper spacing is provided for fastener 53 . another advantage of indicia 100 is shown in fig1 b , which shows connector link assembly 40 after a seismic event that did not result in the complete failure of connector piece 42 . thus , for example , if there is partial tearing of connector piece 42 , connector link assembly 40 may stretch without breaking . thus , upper link 44 a and lower link 44 b may , as a result of the stretching or tearing of connector piece 42 , move apart by a distance 102 , as a user would clearly see by inspection of the connector piece as shown in fig1 b . an alternative indicia 106 is shown in fig1 a , which is a side elevational view of the connector link assembly 40 with alternative indicia as a sprayed - on contrast such as paint or dye . indicia 106 has the similar benefits as indicia 100 , in that it can be used to align connector link assembly 40 , as in fig1 a . further , as shown in fig1 b , which is a side elevational view of the connector link assembly of fig1 a after a seismic event ( as in fig1 b ), a gap 108 in indicia 106 is easily seen to indicate structural damage to connector piece 42 . the conduit hanger assembly component described herein are easily arranged and adapted to support conduits in a building . typically , the location and run of utilities in a building are only generally specified by the building designers , and installers came decide how to make each hanger for each location . thus , for example , the connector links described herein could be provided to a job site in bulk , and connector link assemblies could be entirely made on - site with commonly available material for connector pieces . as a result , frangible conduit hanger assemblies could be easily constructed in most circumstances for a variety of applications and situations . fig1 , 17 , 18 , 19 , and 20 illustrate a few of the many examples of applications of the inventive frangible members . fig1 is an elevational view of an installed alternative conduit hanger assembly 120 with two connector link assemblies 40 in series . fig1 is an elevational view of an installed other alternative conduit hanger assembly 140 with one link 44 . conduit hanger assembly 130 includes a connector piece 42 that is attached directly to bracket 18 without an intervening lower bracket . fig1 is an elevational view of an installed version of yet another conduit hanger 150 with inventive links 40 as used for supporting ducting 152 . fig1 is an elevational view of an installed version of another conduit hanger 160 as used for supporting a trapeze 152 including several conduits . the following examples are results of tests on several embodiments described herein . specifically , conduit hanger assembly 30 , as in fig2 a and 2b was tested with a ½ inch anchor 16 and for various dimensions of connector piece 42 . it was previously determined that , for a bolt 16 comprising a ½ inch diameter , a trubolt + carbon steel seismic wedge type anchor ( itw commercial construction , glendale heights , ill .) will fail under tension with a load of 8 , 925 lbs . when the bolt has an embedment of 3½ inches into a minimum concrete thickness of 6 inches , the concrete surrounding an embedded bolt will fail at a cracked concrete strength of 5 , 455 lbs . including a factor of safety , which are required by building codes , the maximum load on such an anchor must be less than 2 , 659 lbs . tests were performed on by placing threaded rods 21 and threaded rod 22 of conduit hanger assembly 30 in tension of increasing amounts until the assembly failed . if the conduit hanger assembly 30 fails under a load less than 2 , 659 lbs ., then the conduit hanger assembly can safely be used to support loads without causing failure of the concrete . a number of conduit hanger assemblies 30 , similar to that of fig2 a and 2b were assembled . in each conduit hanger assembly , connector piece 42 was formed from electrical metallic tubing ( emt ) conduit , which is a commonly available thin - walled steel tube having a circular cross section . specifically , tests were conducted with emt conduit sizes of ¾ ″, 1 ″, 1¼ ″, 1½ ″ and 2 ″, with one fastener 53 , which was a ¼ inch screw that was screwed through the conduit wall at a location , d , ⅜ ″ from center of screw hole to cut end of conduit ( see fig8 c ). the test results are presented in table 1 . table 1 shows that each of the assemblies failed with loads less than 2 , 659 lbs ., thus ensuring that the conduit hanger assembly will fail before the concrete near the anchor fails . table 1 also shows that failure load increases with wall thickness , as the 1¼ ″, 1½ ″ and 2 ″ connector pieces all have the same wall thickness and the same load for ductile failure of the connector piece . reference throughout this specification to “ one embodiment ” or “ an embodiment ” means that a particular feature , structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention . thus , appearances of the phrases “ in one embodiment ” or “ in an embodiment ” in various places throughout this specification are not necessarily all referring to the same embodiment . furthermore , the particular features , structures or characteristics may be combined in any suitable manner , as would be apparent to one of ordinary skill in the art from this disclosure , in one or more embodiments . similarly , it should be appreciated that in the above description of exemplary embodiments of the invention , various features of the invention are sometimes grouped together in a single embodiment , figure , or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various inventive aspects . this method of disclosure , however , is not to be interpreted as reflecting an intention that the claimed invention requires more features than are expressly recited in each claim . rather , as the following claims reflect , inventive aspects lie in less than all features of a single foregoing disclosed embodiment . thus , the claims following the detailed description are hereby expressly incorporated into this detailed description , with each claim standing on its own as a separate embodiment of this invention . further , those skilled in the art will recognize that other and further modifications may be made thereto without departing from the spirit of the invention , and it is intended to claim all such changes and modifications as fall within the scope of the invention . | 5 |
referring to fig1 through 5 for illustrating one preferred embodiment , there is shown a tool rack organizer 10 mounted on a vertical support surface 12 , such as a garage or storage wall , and supporting and organizing various articles 14 typically housed therein such as lawn and garden implement , tools and the like . the organizer 10 includes a support bracket assembly 20 supporting an inner or rear arm 22 , a middle arm 24 and an outer or front arm 26 aligned in horizontal rows parallel to the surface 12 . as shown in fig1 and 2 , the organizer has a closed storage position whereat the arms are in vertically aligned , uniformly horizontally transversely spaced relationship . as shown in fig3 the outer arm 26 may be pivoted outwardly to a partially opened position to gain access to the middle arm 24 . as shown in fig4 thereafter the middle arm 24 may pivoted outwardly to a fully opened position to gain access to the articles on the inner arm 22 . the support bracket assembly 20 is attached to the support surface 12 and typically the studs therebehind by suitable threaded fasteners 28 . referring additionally to fig5 the support bracket assembly 20 includes a support plate 30 having a triangular base leg 32 fastened to the surface 12 and a triangular front leg 34 integrally connected and transversely disposed with respect thereto . both legs are provided with mounting holes 36 for attachment to adjacent support surfaces with the fasteners 28 . it will be appreciated that the support bracket assembly 20 may also be corner mounted or along a side wall using the front leg 34 as the mounting surface . moreover , the organizer may be assembled and mounted as a mirror image of the orientation shown in fig1 . a u - shaped mounting bracket 40 is centrally attached to the support plate 30 by suitable means such as weldments . the bracket 40 includes a rectangular horizontal top plate 42 interconnected with a rectangular bottom plate 44 by a rectangular vertical center plate 46 . the inner side of the center plate 46 is forwardly spaced from the base leg 32 to establish therebetween a rectangular slot for receiving the inner end of the rear arm 22 . the outer side of the center plate 46 is spaced inwardly from the outer sides of the plates 42 and 44 for receiving the inner ends of the middle arm 24 and outer arm 26 . the arms 22 , 24 and 26 are formed of rectangular tubing and include a longitudinal series of hook mounting holes 50 on the front and rear walls for supporting conventional peg - board type mounting hooks 51 . the rear arm 22 is formed of a single length of tubing and includes vertically aligned cylindrical bushing 52 at the inner end having a sliding fit within the inner slot in the mounting bracket 40 . a bolt 54 extends through apertures in the plates 42 , 44 and bushings 52 and threaded to nut 56 to fixedly capture the inner end of the rear arm 22 fixedly locating the arm adjacent the surface 12 . the middle arm 24 is formed of a single length of tubing and includes vertically aligned cylindrical bushing 60 at the inner end having a sliding fit within the outer slot in the mounting bracket 30 . a bolt 62 extends through apertures in the outer front edges of the plates 42 , 44 and the bushing 60 and threaded to nut 64 to pivotally support the inner end of the middle arm 24 . the upper end of the bushing 60 includes a detent sector 66 having a series of indents that cooperate with an upper detent ball assembly 68 threaded in a nut in the upper plate 42 to establish detented positions for the middle arm as shown in fig3 and 4 . accordingly , the middle arm is pivotal about a vertical axis 69 ( fig3 and located at the various detent positions the outer arm 26 is generally l - shaped having an outer portion 70 and an inner portion 72 transverse thereto , both formed of rectangular tubing . the outer portion 70 is comparable to the rear and middle arms including the aligned mounting holes 50 . the inner portion 72 includes vertically aligned cylindrical bushing 74 at the inner end having a sliding fit within the outer slot in the mounting bracket 30 . a bolt 76 extends through apertures in the outer front edges of the plates 42 , 44 , aligned with and outward of the apertures for the middle arm , and bushing 74 and threaded to nut 78 to pivotally support the inner end of the middle leg 24 . the lower end of the bushing 74 includes a detent sector 80 having a series of indents that cooperate with an upper detent ball assembly 82 threaded into a nut on the lower plate 44 to establish detented positions for the outer arm as shown in fig3 and 4 . the outer or front arm 26 is thus pivotable about a vertical axis 83 ( fig3 ) through the detented positions . in use , the organizer may be mounted at a convenient location with the arms horizontally aligned . the organizer may be selectively assembled in either left hand or right hand orientations . the mounting hooks may be arrayed on the arms to receive associated articles for storage . the outer and middle arms may be selectively pivoted to separately and selectively present the arm carrying a desired article for storage or removal . after completion , the arms may be returned to the compact closed position . a further embodiment of the invention is shown in fig6 through 12 . therein , fig6 illustrates a tool rack organizer 110 mounted on a vertical surface 112 , such as a garage storage wall , for the compact storage and easy accessibility of a variety of tools and implements of the type commonly used in the maintenance of a household and grounds . for example , the organizer 110 may hold various handled lawn tools , such as hoes and rakes , and home tools , such as hammers and hand tools . it will also be appreciated that the organizer may be beneficially used in connection with businesses and trades in a commercial setting for the storage of equipment used in such pursuits . more particularly , the organizer 110 comprises a rack assembly 120 attached to the wall 112 at a rectangular mounting plate 122 and vertically reinforced by triangulated leg assemblies 124 ( fig8 ). the rack assembly 120 includes a fixed inner support arm 126 , a pair of pivotal middle support arms 134 , and a pair of outer support arms 136 . the arms 134 and 136 are pivotable between the closed position shown in solid lines and the open position shown by dashed lines . the inner arm 126 is an elongated rectangular tube that is attached by suitable means , such as welds , at a rear surface to the front surface of the mounting plate 122 . the rack assembly 120 includes a pair of longitudinally spaced , frontally and outwardly diverging support brackets 128 attached at rear ends to the outer ends of the base arm 126 . each support bracket 128 includes in spaced relation a middle support plate assembly 130 and an outer support plate assembly 132 , respectively pivotally carrying in transversely aligned and parallel spaced relationship arms 134 , 136 . the arms 134 , 136 are connected at inner ends to the support brackets 128 by vertical pin connections 138 and 139 , respectively , with the pin connection 139 lying longitudinally and frontally outward of the pin connection 138 . the rack arms 134 , 136 are disposed in pivotal in non - overlapping , phase opposition for movement between the closed storage position shown in solid lines and the open handling position shown in dashed lines . the side brackets 128 are outwardly inclined with respect to the base arm 126 in the range of about 30 ° to 70 °, to allow full non - interfering pivotal movement between storage and open positions . a divergence around 45 ° to 60 ° is preferred . for compactness , a spacing of about 4 to 12 inches is preferred . the arms 126 , 134 and 136 , and the side brackets 128 are formed of rectangular galvanized steel tubing , or like construction components suitable for the application . the inner arm 126 is attached to the mounting plate 122 by welds 140 . the ends of the inner arm 126 are beveled for attachment to the inner sidewalls of the side brackets 128 . the mounting plate 122 is provided with a longitudinal series of apertures 140 for receiving conventional and suitable fasteners 142 for attaching the organizer 110 at a desired and convenient location on the vertical surface 112 . the front vertical surface of the inner arm 126 is provided with a longitudinal series of attachment holes 144 for receiving conventional mounting hooks 146 for suspending the tools and equipment . suitable hooks may be of the two - leg type used for pegboard applications , in which instance the hole spacing is appropriate for selective , variable location on the inner arm 126 . referring to fig9 and 10 , the side brackets 130 include support arm holder 130 , 132 for pivotally supporting the arms 136 , 136 . each support arm holder includes an upper support plate assembly 150 including a a top plate 152 attached to the top surface of the side bracket 128 and a bottom plate 154 attached to the bottom surface of the side bracket 128 . the top plate 152 and the bottom plate 154 are interconnected at the rear margins by a vertical rear sidewall 156 . the plates 152 , 154 and the sidewall 156 form inwardly and frontally opening pockets for slidably receiving the inner ends of the arms . the plates 152 , 154 and the inner ends of the arms are provided with aligned vertical apertures for receiving the shanks of the pivotal connectors 138 . a suitable connector is an appropriately sized threaded fastener 158 ( fig1 ). to maintain the arms in the desired storage or handling position , as shown in fig9 and 10 , a detent 160 is provided in the bottom plate 154 having a detent head 162 at the top surface thereof . in the closed storage position , the detent head 162 engages the front wall of the arms to resist outer pivoting . in the open handling positions , the detent head 162 engages the rear wall the arms to maintain the extended position . as illustrated , a threaded fastener is a suitable mechanism . the position of the detents may vary to prescribe the desired angularity of the rack arms in the handling position . the inner opposed ends of the arms 134 , 136 are slightly spaced in the closed positions and may be covered with suitable end caps , if desired . the front walls of the arms are provided with a longitudinal series of holes for receiving the aforementioned mounting hooks . referring to fig8 the leg assemblies 124 includes a support strut 170 connected at a lower end to a base plate 172 at bracket 174 and connected at an upper end to the front lower wall of the side bracket 128 at bracket 176 . the base plate 172 is fixedly connected to the support surface 112 by threaded fasteners 178 . the length of the strut 170 may be provided with axial adjustability , for horizontally orienting and structurally supporting the legs 128 in operative position . in use , with the organizer attached at a desired location on the surface 112 , the hooks 144 are attached at desired locations on the support arms for the convenient mounting of the user &# 39 ; s equipment . thereafter , the arms are folded to the closed storage position and disposed in parallel rows . when a desired item is required , the arms are opened as required to gain access and removal , and the opened arms returned to storage positions . the sequence is reversed for return storage of the items . having thus described a presently preferred embodiment of the present invention , it will now be appreciated that the objects of the invention have been fully achieved , and it will be understood by those skilled in the art that many changes in construction and widely differing embodiments and applications of the invention will suggest themselves without departing from the sprit and scope of the present invention . the disclosures and description herein are intended to be illustrative and are not in any sense limiting of the invention , which is defined solely in accordance with the following claims . | 1 |
referring now to fig1 - 4 , the interconnection arrangement of the present invention is generally referred to at 10 and is illustrated as installed with pad - mounted gear 12 including an enclosure 14 . in the illustrative configurations of fig1 - 3 , the enclosure 14 of the pad - mounted gear 12 has affixed thereto illustrative modules or assemblies 16 , 18 , 20 , and 22 . in a specific example for purposes of illustrating the application and utility of the present invention , the modules or assemblies 18 , 20 and 22 are switch operators for power operation of switches ( not shown ) within the enclosure 14 . further , the module or assembly 16 is an auxiliary enclosure that houses a communication and control unit ( not shown ) having , for example , a remote terminal unit ( rtu ) and a radio transceiver . in an illustrative arrangement to provide remote supervisory control , the pad - mounted gear 12 , the interconnection arrangement 10 , the switch operators 18 , 20 and 22 , and the rtu in the module 16 provide a self - contained arrangement for an automated distribution system that is responsive to signals from a remote location , such as a master station computer , to operate the switches of the pad - mounted gear 12 . additionally , the arrangement permits monitoring of circuit conditions at the location . the interconnection arrangement 10 defines enclosed cable pathways for the routing of the electrical conductors to accomplish the interconnection of the various modules or assemblies 16 , 18 , 20 and 22 so as to provide control paths between the switch operators and the communication and control unit and to route operating power between the switch operators and the communication and control unit . the defined cable pathways of the interconnection arrangement 10 not only provide efficient routing of the various conductors for the interconnection between the predetermined points , but also provide shielding of the low - voltage interconnection conductors from the medium voltage present within the pad - mounted gear 12 . in accordance with important aspects of the present invention , the interconnection arrangement 10 is capable of installation with the pad - mounted gear 12 either during manufacture of the pad - mounted gear 12 in a manufacturing environment , or as a field retrofit installation to existing installed pad - mounted gear . that is , if the pad - mounted gear 12 is either already , presently installed at a location or otherwise available in the field , the modules or assemblies 16 , 18 , 20 and 22 may be affixed to the enclosure 14 and the interconnection arrangement 10 may be assembled with the pad - mounted gear 12 , the interconnection arrangement 10 being positioned below and supporting the pad - mounted gear 12 . interconnections are then made between the modules and assemblies by the connection of the routed conductors to the appropriate points of the modules and assemblies via preassembled and routed cable harnesses within the cable pathways , as will be explained in more detail hereinafter . further , the interconnection arrangement 10 , when assembled , has no externally accessible fasteners . of course , it should be understood that the field retrofit is performed with the pad - mounted gear 12 de - energized . further , as to an installed pad - mounted gear 12 , the cable terminations to the power system need to be disconnected and the pad - mounted gear 12 lifted off the pad to attach the interconnection arrangement 10 . referring now additionally to fig2 - 6 , the interconnection arrangement 10 includes a base member 24 defined by upstanding wall members and having a periphery essentially congruent to the pad - mounted gear 12 . in the illustrative configuration , the enclosure 14 of the pad - mounted gear 12 includes a generally rectangular base and thus the interconnection arrangement 10 also includes a base 24 that is of similar dimensions as defined by upstanding wall members 26 , 28 , 30 , and 32 . the wall members 26 , 28 , 30 and 32 include turned edges or flanges 34 , 35 at the top and bottom , respectively , of each of the wall members . the wall members 26 , 28 , 30 and 32 are appropriately affixed to each other by the use of fasteners or the like . a structural support member 36 , best seen in fig5 is affixed to and spans the wall members 26 , 30 for providing additional rigidity and strength to the base 24 . four structural members 38 , best seen in fig6 are affixed to the structural support member 36 , span the wall members 28 , 32 , and are of approximately the same height as the wall members and the structural support member 36 . the structural members 38 each include upper and lower flanges 39 , 41 respectively . additionally , covers 40 and 46 are affixed to the tops of the members 38 and covers 42 , 44 are affixed to the bottoms of the members 38 so as to define an enclosed cable pathway or duct 48 within the central section of the base 24 of the interconnection arrangement 10 . the structural support member 36 includes an appropriate central opening 37 for the continuation of the cable pathway 48 . the members 36 and 38 also divide the base 24 into compartments corresponding to the predetermined compartments of the enclosure 14 of the pad - mounted gear 12 . internal duct members 52 , best seen in fig7 - 8 , are provided at the ends of the cable pathway 48 adjacent the walls members 28 , 32 and are each respectively affixed to one of the structural members 38 and one of the wall members 28 , 32 so as to span an opening 54 provided in the structural members 38 to continue the cable pathway 48 into the internal ducts 52 . specifically , a flange 53 of the internal duct 52 is affixed to the member 38 and a flange 55 is affixed to the wall 28 or 32 . cableway openings at 56 , 57 , 58 and 59 are provided through the wall members 28 and 32 at the appropriate locations of the modules and assemblies 16 , 18 , 20 , and 22 . referring now to fig9 external ducts 60 are affixed to the exterior of the wall members 28 , 32 of the base 24 over the cableway openings 56 , 57 , 58 , and 59 . the external ducts 60 are dimensioned to extend upward to the bottom of the respective modules and assemblies 16 , 18 , 20 , and 22 . in this manner , the external ducts 60 provide an extension of the cable pathway 48 into and through appropriate openings in the bottom of the enclosures of the respective modules and assemblies 16 , 18 , 20 and 22 via the open top portions 62 of the external ducts 60 . for example , an opening 64 is provided in the bottom of the module 22 , as seen in fig3 . in accordance with the features of the present invention , it should be noted that the cable pathway 48 extends between all the modules and assemblies 16 , 18 , 20 , and 22 via the external ducts 60 , the internal ducts 52 , and the central enclosed portion of the base 24 defined by the members 38 and the covers 40 , 42 , 44 , and 46 . thus , whatever interconnections are needed for particular configurations can be readily accomplished via the provision of predetermined , preassembled cable harnesses of conductors . for example , as shown in fig4 the cable harnesses 66 , 68 , and 70 are provided for the necessary interconnection of control paths between the communication and control unit 16 and the respective switch operators 18 , 20 , and 22 . appropriate strain relief and protection for the cable harnesses 66 , 68 , and 70 are provided at the cableway openings 56 , 57 , 58 , and 59 via suitable strain - relief members , bushings , grommets , or the like . the cable harnesses 66 , 68 , and 70 include appropriate connectors , e . g ., connectors 72 , 74 for the cable harness 70 , which are arranged to interfit with respective connectors or the like 76 in the switch operator 22 and 78 in the communication and control unit 16 . additionally , power control interconnections are provided via cable harnesses 80 and 82 between the respective switch operators 20 and 22 and the switch operator 18 . in a specific configuration , the switch operators 20 , 22 receive operating power from the switch operator 18 such that the switch operators 20 , 22 are designated as companion operators . considering now in more detail the field retrofit installation of the interconnection arrangement 10 , after the pad - mounted gear 12 has been de - energized and the cable terminations to the power conductors disconnected , the modules and assemblies 16 , 18 , 20 , and 22 are attached to the enclosure 14 of the pad - mounted gear 12 and suitably connected to the switch - operating shafts . of course , the modules and assemblies may optionally have already been attached to the pad - mounted gear 12 prior to the time of installation of the interconnection arrangement 10 . next , the pad - mounted gear 12 is physically and structurally disconnected from the pad or other mounting structure . at this point , the pad - mounted gear 12 is lifted off the pad so that the interconnection arrangement 10 may be attached to the mounting pad . prior to the attachment of the interconnection arrangement 10 to the pad - mounted gear 12 , the interconnection arrangement 10 is prepared in the field . this entails applying appropriate gasketing to various parts , feeding and extending the cable harnesses 66 , 68 , 70 , 80 and 82 through the holes 56 , 57 , 58 , and 59 in the base 24 , affixing the external ducts 60 to the base 24 , and also attaching the internal ducts 52 . for example , the external ducts 60 are affixed to the base 24 via bolts 61 ( fig4 ) that are inserted from the inside of the base and threaded into clip nuts 63 ( fig9 ) carried by the external ducts 60 . at this point in the installation , bottom access plates of the modules and assemblies 16 , 18 , 20 , and 22 , such as an access plate 67 ( fig3 ) overlying the opening 64 of module 22 , are removed and the pad - mounted gear 12 lowered onto the base 24 which has been positioned on the pad . the base 24 is attached to the enclosure 14 of the pad - mounted gear 12 via suitable fasteners or the like that are assembled through holes 88 in the base 24 and the enclosure 14 . as the enclosure 14 is lowered onto the base 24 , the various cable harnesses are passed through the openings 64 of the modules and assemblies 16 , 18 , 20 , and 22 . the ground bus connector 84 of the base 24 is connected to the respective ground bus connector of the enclosure 14 . the connectors of the cable harnesses are then connected into the mating connectors of the modules and assemblies . after these steps , the external ducts 60 are affixed to the modules and assemblies and the external ducts 60 are also now firmly affixed to the base 24 ; e . g ., the external ducts 60 are affixed to the modules via bolts 90 ( fig9 ) that are inserted from the inside of the module 20 and threaded into clip nuts 92 ( fig4 and 9 ) carried by the external ducts 60 . next , the internal ducts 52 are positioned for final affixing and then tightened into place , the internal ducts 52 having been loosely attached previously but oriented so as to provide access to the interior for any necessary cable harness manipulation . finally , the pad - mounted gear 12 with attached interconnection arrangement 10 is physically secured to the pad . the desired current and / or voltage sensors are installed , and suitable interconnections accomplished . for example , the cable harnesses 66 , 68 , and 70 are provided with appropriate cable conductors and connectors , for example , connector 86 on cable harness 70 for interconnection to a mating connector of the various installed sensors . it should be noted that there are no externally accessible fasteners . regarding the different configurations of the interconnection arrangement 10 that are possible for the same or different configurations of pad - mounted gear 12 and to illustrate the flexibility of the invention to accommodate different configurations , the interconnection arrangement 10 in one specific illustration is arranged to accommodate from one to four locations of switch operators . where only one switch operator is provided , at the location of assembly 18 , only the cable harness 66 is provided and the internal and external ducts 52 and 60 and the covers 44 , 46 on the right - hand side of the base 24 in fig4 are deleted . referring now additionally to fig1 , a cover plate 90 may be provided that can be affixed over either selected ones of the openings 54 of the structural members 38 or the central opening 37 of the structural support member 36 as desired to form a particular configuration . this illustrates that in the various configurations , the cable pathway 48 is totally closed within the base 24 . thus , where two switch operators are provided , at locations 18 , 20 , the cable harness 70 is omitted , the internal and external ducts are omitted at the location for the operator 22 , and the cover plate 90 is installed at the opening 54 of the structural member 38 at the upper right in fig4 . considering other structural details , it should be noted that the internal ducts 52 are not of identical sizes , as can be seen from fig4 . additionally , for the module 16 , the external duct 60 is not the same size as the remaining ducts due to the dimensions of the enclosure of the module 16 . for example , if four switch operators are provided at the locations 16 , 18 , 20 , and 22 , the external ducts 60 would all be identical . as will be apparent to those familiar with the underground distribution art , sufficient cable termination length must be available to accommodate the interconnection arrangement 10 . for example , the interconnection arrangement could replace an existing base spacer or be added to the height of the pad - mounted gear 12 above the pad , assuming sufficient extra length of cable is available . turning now to a discussion of the assembly of the interconnection arrangement 10 in a manufacturing environment , the kit of components can be identical to the field retrofit kit or may be slightly different . for example , for manufacturing assembly , the internal duct 52 may be omitted and the routing of cable harnesses performed by direct entry from the central duct between the structural members 38 and into the external duct 60 , which is then positioned to 60 &# 39 ; from the position as shown in fig4 ( i . e ., in a downward direction in fig4 ). while there have been illustrated and described various embodiments of the present invention , it will be apparent that various changes and modifications will occur to those skilled in the art . accordingly , it is intended in the appended claims to cover all such changes and modifications that fall within the true spirit and scope of the present invention . | 7 |
referring to fig1 there is shown a preferred embodiment of a phase - difference detecting circuit 11 in accordance with the present invention . the phase - difference detecting circuit 11 comprises a phase - difference detecting part 12 for detecting a phase difference between a first signal ina with a first frequency and a second signal inb with a second frequency , and a latching part 13 for latching an output of the phase - difference detecting part 12 and outputting it as an output &# 34 ; out &# 34 ; of the phase - difference detecting circuit 11 . the phase - difference detecting part 12 is constituted by a first d flip - flop ( dff1 ) 14 , a second d flip - flop ( dff2 ) 15 , a delay circuit ( delay means ) 18 comprising inverters 16 and 17 , and a 3 - input nand gate ( logic means ) 19 . the first d flip - flop ( dff1 ) 14 has a data terminal d to which the first signal ina different in frequency from the second signal inb is input , a clock terminal ck to which the second signal inb is input , a reset terminal to which a reset signal res is input , and an output terminal xq1 connected to an input terminal of the 3 - input nand gate 19 . likewise , the second d flip - flop ( dff2 ) 15 has a data terminal d into which the first signal ina is input , a clock terminal ck to which a third signal inc delayed from the second signal inb by a predetermined time ( phase ) difference dt by the delay circuit 18 is input , a reset terminal to which the reset signal res is input , and an output terminal q2 connected to an input terminal of the 3 - input nand gate 19 . the first signal ina with a first frequency is also input to the 3 - input nand gate 19 . the output x of the 3 - input nand gate 19 is output to the latching part 13 , which is constituted by cross - coupled nand gates 20 , 21 and an inverter 22 . the nand gate 20 has an input terminal to which the output x of the 3 - input nand gate 19 is input , while the nand gate 21 has an input terminal to which the reset signal res is input . accordingly , the same first signal ina is input to both the first flip - flop 14 and the second flip - flop 15 , and the clock of the second flip - flop 15 is delayed from the clock of the first flip - flop 14 by the time difference dt between the signals inb and inc . fig2 schematically illustrates a pll frequency synthesizer to which the phase - difference detecting circuit 11 is applied . the parts substantially identical to corresponding parts of fig1 are designated by the same reference numerals and therefore a detailed description of the identical parts will not be given . in fig2 a pll integrated circuit ( ic ) 31 comprises a first and gate 32 to which a signal osc in and a power save control signal ps respectively corresponding to the signals ina and res of fig1 are input , a second and gate 33 to which the power save control signal ps and a signal f in ( corresponding to the signal inb of fig1 ) output from a vco are input , a programmable reference frequency divider 2 to which the output of the first and gate 32 is input , and a programmable comparison frequency divider 4 to which the output of the second and gate 33 is input . the outputs of the and gates 32 and 33 and the power save control signal ps are input to a phase - difference detecting circuit 11 , which detects the phase difference between the two signals osc in and f in and outputs a control signal ps1 corresponding to the output ( out ) of the phase - difference detecting circuit 11 of fig1 to the reference frequency divider 2 and the comparison frequency divider 4 . the output f r of the reference frequency divider 2 , the output f v of the comparison frequency divider 4 , the power save control signal ps , and the control signal ps1 are input to a phase comparator 3 . the phase comparator 3 is connected to a charge pump 5 , which outputs the pll ic output d o to a low - pass filter 6 connected to the vco 7 . note that the standby control of the phase comparator 3 may be performed by the power save control signal ps instead of the control signal ps1 , as shown by the broken line in fig2 . in that case , the phase comparator 3 becomes active earlier than the frequency dividers 2 and 4 , but there is no problem because the frequency dividers 2 and 4 do not become active until the phases of the signals osc in and f in become small . fig3 schematically illustrates the structure of the divide - by - n frequency divider 4 , which is substantially the same as that of the divide - by - r frequency divider 2 . the output control signal ps1 from the phase - difference detecting circuit 11 goes low in the standby mode ( when ps = 0 ). if the set terminals of a first flip - flop fl and a second flip - flop f2 are low and the clear terminal of a third flip - flop is low , then the q1 output of the first flip - flop f1 and the q2 output of the second flip - flop f2 go high , and the q3 output of the third flip - flop f3 goes low . the q3 output of the third flip - flop f3 is connected to the load terminals of flip - flops f1 through fn and a nor gate 34 . the q outputs of the flip - flops f1 through fn are connected through inverters to the inputs of a detecting circuit det for detecting a digital value 4 . the output of the circuit det is connected to the d input of the first flip - flop f1 . at the time of the load state ( load = low ), the flip - flops f1 through fn is in the dividing - ratio data reading state , and do no go to the counting state even if the clock signal f in is input . since the two inputs of the nor gate 34 are low and high at that time , the output f v of the frequency divider 4 goes to low . if in the active mode ( when ps = 1 ) the input signals to the frequency dividers 2 and 4 rise at the same time , the control signal ps1 will go high . as a result , the output f v goes high because the two inputs of the nor gate 34 are both low at the time the control signal ps1 goes high , and therefore the output f v is output . if the control signal ps1 is high , the flip - flops f1 , f2 and f3 are all reset , and the count will start when the clock signal f in makes a low - to - high transition . if the load terminals of the flip - flops f1 through fn go to high level , the flip - flops f1 through fn are all reset and the dividing operation will start thereafter , the dividing operation is performed according to a predetermined dividing ratio . fig4 schematically illustrates the structure of the phase comparator 3 and the charge pump 5 . in the standby mode ( when ps = 0 ), the flip - flops fa and fb of the phase comparator 3 go to the clear state because the control signal ps1 is low . the q output of the flip - flop fa goes low , and the xq output of the flip - flop fb goes high . at this time , the p - channel and n - channel mos transistors of the charge pump are both cut off , and the pll ic output d o goes to the high impedance state . if the control signal ps1 goes high , then flip - flops fa and fb are reset ( because one of the two inputs of a nand gate 35 goes high ), and the normal phase comparison operation for detecting the phase difference between the reference signal f r and the variation signal f v is performed . note that the pll ic output d o is held to the high impedance state until the phase comparison operation starts . fig5 and 6 are timing diagrams showing how the phase - difference detecting circuit 11 is operated . fig5 shows waveforms when the phase difference t1 between the input signals ina and inb is greater that the phase difference dt between the input signals inb and inc , while fig6 shows waveforms when the phase difference t2 between the input signals ina and inb is less than the phase difference dt between the input signals inb and inc . suppose that the signals ina and inb are different signals which are not the same in frequency and phase . if , with such a condition , the res input is not asserted and the two signals ina and inb are input , the relationship between the two signals will go to the state shown in fig5 and 6 . since in fig5 the phase difference t1 between the two signals ina and inb is above the phase difference dt between the signals inb and inc , the xq1 output of the d flip - flop 14 or dff1 is low and the q output of the d flip - flop 15 or dff2 is high , so that the output ( out ) of the phase - difference detecting circuit 11 remains low . if , as shown in fig6 the rising edge of the signal inb leads the rising edge of the signal ina and the phase difference t2 between the two signals ina and inb is within the phase difference dt between the signals inb and inc , the xq1 output of the dff1 will go high because the dff1 reads the level of the signal ina before the rising edge of the signal ina , and the q2 output of the dff2 will go high because the dff2 reads the level of the signal ina after the rising edge of the signal ina . since at this time the signal ina is high , the output x of the nand gate 19 goes low and the output ( out ) of the detecting circuit 11 thus goes low . in this way , the state where the phase difference between the two signals ina and inb is within the phase difference dt between the signals inb and inc is detected . if , as shown in fig7 ( a ), the frequencies of the input signals ina and inb both do not vary and the phase difference t1 is greater than dt , the pll will not be operated because the phase difference is always above a predetermined time difference dt . in order to avoid this condition , the signals ina and inb are not the same in frequency and phase , and therefore there is a moment that a phase difference t6 becomes less than dt , as shown in fig7 ( b ). in fact , in the intermittent operation of a pll , the charge pump output goes to the high impedance state at the standby time , and the low - pass filter can hold the output voltage when the loop is locked , by the capacity . however , the condition of fig7 ( a ) that the phase difference is always above the predetermined time difference dt cannot occur because the output voltage slightly varies due to the leak current and thus the frequency slightly varies . note that the phase difference dt between the signals inb and inc can be easily varied by simply increasing and decreasing the number of the inverters 16 and 17 of the delay circuit 18 . the phase difference dt between the signals inb and inc is set so that the two low - to - high transitions or high - to - low transitions can quickly match depending on the frequencies of the two signals . for example , when the low - to - high transition of the signal ina does not match with the low - to - high transition of the signal inb , a larger phase difference dt is set . in the phase - difference detecting circuit 11 , the low - to - high transitions of the signals ina and inb are detected at the same time . if the output ( out ) of the phase - difference detecting circuit 11 changes , it will be necessary to reset the circuit to detect the low - to - high transition after that time . the reset signal res is therefore input to the dff1 , dff2 and the latching part 13 , as shown in fig1 . in the embodiment of fig1 in addition to the xq1 output of the dff1 and the q2 output of the dff2 , the signal ina is input to the 3 - input nand gate 19 . the reasons are as follows . that is , if the signal ina is left unconnected and only the xq1 and q2 outputs are connected , the output x of the circuit 11 will go low regardless of the phase difference between the signals ina and inb , as shown in the point a of fig8 . consequently , the output ( out ) of the circuit 11 that is to change at the point b of fig8 will change . the reason is that , when the q2 output of the dff2 goes high at the point ( a ) of fig8 and at the point a the xq1 output of the dff1 goes high and the q2 output goes low , the q2 output is delayed by the phase difference dt between the signals inb and inc and therefore the output x of the nand gate 19 goes to a low level . in the embodiment of fig1 the signal ina is input to the nand gate 19 to eliminate this incorrect operation , and the above described problem is thus overcome . fig9 shows a timing diagram when the phase - difference detecting circuit 11 is applied to the pll ic 31 . in the figure , suppose now that the pll ic 31 is in the standby mode ( ps = low ). with this state , each counter goes to the reset state , the charge pump output goes to the high impedance state . therefore , since the voltage at the time of lock is held by the cr time constant of the low - pass filter 6 , the external vco 7 ideally oscillates at a frequency f in of the lock time , but in fact the vco oscillating frequency slightly changes due to leak . if the standby mode is switched to the operating mode , each input gate is then opened , the oscillating output of the external osc is input by the osc in signal and enters the phase - difference detecting circuit 11 . the vco oscillating output is also input by the f in signal and enters the phase - difference detecting circuit 11 . if the rising edges of the two signals become the relationship of fig6 then the control signal ps1 is output from the circuit 11 to the frequency dividers 2 and 4 . if the frequency dividers 2 and 4 are operated at the same time as the input of the control signal ps1 to the frequency dividers 2 and 4 to output the signals f r and f v to the phase comparator 3 , an error signal will become very small and thus the lock - up time can be greatly quickened . thus , in the present invention , the transition state where two different frequency signals go high or low at the same time with a predetermined range is detected , and at the same time the counters of the reference frequency divider 2 and comparator frequency divider 4 are operated . therefore , if the phase - difference detecting circuit 11 according to the present invention is used , for example , in an intermittently operated pll ic , the reference signal f r and the comparison signal f v which are the same in phase can be produced for a very short time . consequently , the error signal can be made very small and the lock - up time is thus greatly shortened , so that the performance of the pll synthesizer is greatly enhanced . the invention has been described with reference to the preferred embodiment . obviously modifications and alternations will occur to others upon a reading and understanding of this application . it is intended to include all such modifications and alternations insofar as they come within the scope of the appended claims or the equivalents thereof . | 7 |
fig1 illustrates an exploded view of a targeted eye drop dispenser 10 including a reservoir assembly 12 and a cap 14 . the reservoir assembly 12 includes a flexible plastic reservoir bottle 16 , a neck 18 extending vertically from the top surface 20 of the reservoir bottle 16 , a threaded surface 22 encompassing the neck 18 , tubular extension member 24 extending from the neck 18 , and a tubular passage 25 having a dispensing orifice 27 aligned in the tubular extension member 24 . the tubular extension member 24 includes a target tip 26 , which can be radiused as illustrated , and having a plurality of highly visible targets , such as rings 28a - 28n aligned coaxially on the target tip 26 . the target rings 28a - 28n are of highly visible colors such as phosphorescent orange , lime or other suitable highly visible colors . alternatively , the target tip 26 can include a flat surface or any other shaped surface suitable for bearing of a highly visible color , whether the colors are displayed in the form of concentric rings , a solid color , or any other suitable design which would lend itself toward visual capture during the process of eye drop application by an individual . the target tip 26 can also have target rings or surfaces which contain glow - in - the - dark visual surfaces for application in low light or complete darkness situations where a person &# 39 ; s eyes cannot tolerate bright lights . fig2 illustrates a top view of the reservoir assembly 12 along line 2 -- 2 of fig1 where all numerals correspond to those elements previously described . illustrated in particular is the target tip 26 including the highly visible target rings 28a - 28n . fig3 an alternative embodiment , illustrates an exploded cross - sectional view of a targeted eye drop dispenser 50 having at least one or more lighted targets 52 . the targeted eye drop dispenser 50 includes a reservoir assembly 54 and a cap 56 . the reservoir assembly 54 includes a flexible plastic reservoir bottle 58 , a neck 60 extending vertically from the top surface 62 of the reservoir bottle 58 , a threaded surface 64 encompassing the neck 60 , and a tubular extension member 66 extending from the neck 60 . a tubular passage 68 in the neck 60 connects the interior of the reservoir bottle 58 and a target tip 70 to allow for dispensing of eye drop medication from the reservoir assembly 54 . the lighted target 52 , in the form of a light emitting diode ( led ), aligns in the upper portion of the tubular extension member 66 at the target tip 70 in very close proximity to the dispensing orifice 72 at one end of the tubular passageway 68 . the lighted target 52 aligns in a passageway 74 in the tubular extension member 66 . wires 75 and 77 from the lighted target 52 also align in the passageway 74 and connect to a switch assembly 76 actuated by a push button 78 and to a small battery 80 aligned in the structure of the reservoir bottle 58 . the lighted target 52 can be in the form of a steady or pulsating led of any desirable eye attracting color such as , but not limited to , white , red , green , yellow , or other desirable colors . in the alternative , the lighted target could be a lighted crystal display ( lcd ) which could be steady or pulsating . it is appreciated that an lcd could be applied in place of the plurality of target rings 28a - 28n of fig1 and flash sequentially from the outside ring to the inside ring , thus providing an eye catching target . in another embodiment , the energy source , such as a battery for activating the lighted target , is placed in a separate carrier configured to receive at least a portion of the eye drop dispenser . specifically , the battery is placed in the carrier with its leads exposed so that upon placing the dispenser in the carrier , the battery leads contact opposite leads on the dispenser that are in electrical communication with the light source . preferably the carrier does not extend completely about the dispenser , in order that the reservoir remain partially exposed to enable squeezing of the same so as to dispense the eye drop solution . the carrier / dispenser combination can be constructed so that the light source always illuminates upon placing the dispenser in the carrier , or an additional switching mechanism such as that described previously can be used so that the dispenser can remain in the carrier without discharging the battery . fig4 illustrates the mode of operation of the targeted eye drop dispenser where all numerals correspond to those elements previously described . the cap 14 of fig1 is first removed and then the reservoir assembly 12 is inverted by the user . the user then tilts their head back and the reservoir assembly 12 is placed in the region over the user &# 39 ; s eye 82 . the user then visually acquires the plurality of target rings 28a - 28n and focuses upon them . after visual capture of the target rings , as portrayed by lines 82 - 88 , the reservoir bottle is gently squeezed causing the desired eye wash solution 92 to be dispensed into the user &# 39 ; s eye 82 from the aligned dispensing orifice 27 . various modifications can be made to the present invention without departing from the apparent scope hereof . | 0 |
in low power circuit applications , it is very important to reduce a gate bias voltage of the mos transistors which are employed by the current mirror circuit . that &# 39 ; s because that once the gate bias voltage is reduced , the operating power will also be automatically reduced . thus , the present invention set forth a current mirror circuit which can reduce the threshold voltage through providing a substrate bias voltage higher than the source bias voltage . please refer to fig2 a which illustrates a schematic view of a current mirror circuit in a preferred embodiment according to the present invention . the current mirror circuit is employed to receive an input current i in so as to produce an output current identical to the input current and includes a first transistor n 1 , a second transistor n 2 , a third transistor n 3 , a fourth transistor n 4 , a resistor r , an input current source i in , a first power supply vss and a second power supply vdd . a first end of the resistor r is employed to receive the input current source i in . the gate electrode of the first transistor n 1 is coupled to the second end of the resistor r to receive a first bias voltage , the drain electrode thereof id coupled to the first power supply vss and the substrate electrode thereof is coupled to the drain electrode thereof . the gate electrode of the second transistor n 2 is coupled to the gate electrode of the first transistor n 1 , the source electrode thereof is coupled to the first power supply vss and the substrate thereof is coupled to the substrate electrode of the first transistor n 1 . the gate electrode of the third transistor n 3 is coupled to the first end of the resistor r to receive a second bias voltage , the source electrode thereof is coupled to the drain electrode of the first transistor n 1 , the substrate electrode thereof is coupled to the substrate electrode of the first transistor n 1 and the drain electrode is coupled to the second end of the resistor r . the gate electrode of the fourth transistor n 4 is coupled to the gate electrode of the third transistor n 3 , the source electrode thereof is coupled to the drain electrode of the second transistor n 2 , the substrate electrode thereof is coupled to the source electrode thereof and the output current i out is generated from the drain electrode thereof . meanwhile , the first power supply vss is coupled to the ground , and the first transistor n 1 , the second transistor n 2 , the third transistor n 3 and the fourth transistor n 4 are n - type metal - oxide semiconductor transistors . according to the circuit described above and further based on the body effect , the threshold voltage is equal to : v th = v th0 γ ({ square root }{ square root over ( v sb +| 2φ f |)}−{ square root }{ square root over ( 2φ f )}) furthermore , because the substrate electrode of the third transistor n 3 is coupled to the drain electrode thereof in the present invention , the threshold voltage of the third transistor n 3 is equal to v th0 . identically , the substrate electrode of the fourth transistor n 4 is coupled to the drain electrode thereof , and thus the threshold voltage of the fourth transistor n 4 is also equal to v th0 . as to the threshold voltage of the first transistor n 1 , it is equal to : v th , n1 = v th - 0 + γ ({ square root }{ square root over ( v sd , n1 + 2φ f )}−{ square root }{ square root over ( 2φ f )}) since the voltage v sd , n1 of the first transistor n 1 is negative , the threshold v th , n1 thereof is lower than v th0 , which is generally equal to 0 . 7 v ). depending on the same theory , the v sd , n1 of the second transistor n 2 is also negative , and thus the threshold v th , n2 thereof is lower than v th0 . furthermore , both the threshold voltages of the first transistor n 1 and the second transistor n 2 are the same . consequently , the gate bias voltage of the first transistor n 1 and the second transistor n 2 is equal to : v g , n1 = v g , n2 = v th0 + γ ( v sd , n1 + 2 φ f - 2 φ f ) + 2 i i n μ n c ox ( l w ) n1 based on the formula described above , because v sd , n1 & lt ; 0 , γ ({ square root }{ square root over ( v sd , n1 +| 2φ f |)}−{ square root }{ square root over ( 2φ f )} is also negative . therefore , the gate bias voltage of the first transistor n 1 and the second transistor n 2 can be reduced so as to reduce the operating power of the whole system . another embodiment according to the present invention is shown in fig2 b . a current mirror circuit includes a first transistor pt , a second transistor p 2 , a third transistor p 3 , a fourth transistor p 4 , a resistor r , an input current source i in , a first power supply vss and a second power supply vdd . the difference from that in fig2 a is the first transistor p 1 , the second transistor p 2 , the third transistor p 3 and the fourth transistor p 4 are p - type metal - oxide semiconductor transistors . now , if each element in both fig1 b and fig2 a is adjusted to suit the input current i n equal to 10 μa and r is supposed as 40 kω , the result of voltage variation is shown in fig3 . the simulation method is to vary the input current from 0 μa to 40 μa . as shown in fig3 the node voltage of v 1a is restricted under the threshold voltage ( 0 . 7 v ) of the mos transistor and when the input current i in is larger than 1 . 8 ma , because the first transistor n 1 and the second transistor n 2 shown in fig2 a can not maintain a normal function , the current will flow through the drain electrode to the substrate electrode so as to cause a latch - up . however , when in the present invention , the desired input current is equal to 10 μa , v 1a is equal to 0 . 3 v , and thus the first transistor n 1 and the second transistor n 2 will not lose efficiency . moreover , the voltage variations of v 2b and v 2a respectively in fig1 b and fig1 a are shoves in fig4 . as shown in fig4 when the input current i in is equal to 10 μa , v 2a will 150 mv lower than v 1a . that means , if v sb of the mos transistor is set as − 0 . 3v , the original threshold voltage will be reduced from 0 . 75 v to 0 . 6 v so as to reduce 0 . 15 v of the operating voltage due to the body effect . a low power operating system like this should be very practical . please refer to fig5 which is a comparison plot of the input current and the output current in fig1 b and fig2 a . as shown in fig5 when the input current i in is larger than 18 μa , part of the current is already flow into the substrate electrode . in view of the aforesaid , the circuit structure according to the present invention can be employed as the input current is lees variable so that the gate bias voltage of the transistor can be reduced through reducing the threshold voltage thereof so as to reduce the operating voltage of the system . thus , the present invention can effectively overcome the defects in the prior arts . consequently , the present invention conforms to the demand of the industry and is industrial valuable . while the invention has been described in terms of what is presently considered to be the most practical and preferred embodiments , it is to be understood that the invention needs not be limited to the disclosed embodiment . on the contrary , it is intended to cover various modifications and similar arrangements included within the spirit and scope of the appended claims which are to be accorded with the broadest interpretation so as to encompass all such modifications and similar structures . | 6 |
the fig1 shows a diagrammatic sketch of an internal combustion engine having turbocharging and having low - pressure exhaust - gas recirculation . although the exemplary embodiment relates to a diesel engine , the description may however also be applied to other types of internal combustion engine . a schematically illustrated multi - cylinder diesel engine 2 has inlet ducts 4 and outlet ducts 6 . the outlet ducts 6 open out via a collector 8 into an exhaust line 10 , which opens out into a turbine 12 of a turbocharger 14 . the turbine 12 is coupled by means of a shaft 16 to a compressor 18 of the turbocharger 14 . the turbocharger 14 may be a turbocharger with fixed geometry ( fgt ) or a turbocharger with variable geometry ( vgt ). the outlet of the turbine 12 is adjoined by an exhaust section 20 in which are arranged , in this sequence , a diesel oxidation catalytic converter 22 , a diesel particle filter 24 , a control system for controlling the exhaust - gas back pressure , which control system comprises a throttle flap 26 and a bypass 28 , which leads past the throttle flap 26 , with an integrated valve , and a silencer 30 . a low - pressure egr line 32 is connected to the exhaust section 20 downstream of the turbine 12 and upstream of the diesel oxidation catalytic converter 22 , which low - pressure egr line 32 opens out via an egr valve 34 into a fresh - air line 36 that conducts fresh air from an air filter 38 into the compressor 18 of the turbocharger 14 . the mixture of fresh air and recirculated exhaust gas that is compressed by the compressor 18 passes via an air inlet line 40 into a combined inlet air cooler and distributor 42 , where said mixture is cooled and distributed between the inlet ducts 4 . the inlet air cooler and distributor 42 comprises a bypass ( not shown ), with the inlet air mixture being conducted , as required , either through the inlet air cooler and distributor 42 or through the bypass and past the inlet air cooler and distributor 42 . a throttle flap 44 may also be provided in the inlet line 40 in order to close the inlet line 40 when the diesel engine 2 is shut down . the low - pressure egr line 32 comprises a heatable particle filter 46 that is traversed by the recirculated exhaust gas . the particle filter 46 comprises an electric heater , for example in the form of grids , which are integrated into the filter matrix , composed of heating or glow wires 47 , by means of which any soot and oil particles in the recirculated exhaust gas are burned . the low - pressure egr line 32 may also comprise , downstream of the particle filter 46 and upstream of the egr valve 34 , a heat exchanger 48 that dissipates the heat contained in the exhaust gas to an arbitrary heat sink — such as for example the inlet air collector and cooler 40 . the heat exchanger 48 comprises a bypass ( not shown ), with the inlet air mixture being conducted selectively either through the heat exchanger 48 or through the bypass and past the heat exchanger 48 . referring now to fig2 , a method to control egr for an internal combustion engine is shown . routine 200 begins at 202 where engine operating conditions are determined . engine operating conditions are determined from sensors and actuators . in one example , routine 200 determines engine temperature , ambient temperature , the pressure drop across a particulate filter in the high pressure egr loop , the pressure drop across a particulate filter in the exhaust system , time since engine start , engine load , engine torque demand , engine speed , and amount of air inducted to the engine . in other example embodiments , additional or fewer operating conditions may be determined based on specific objectives . at 204 , the routine judges whether or not to flow egr . the decision to flow egr may be based on the operating conditions determined at 202 . in one example , egr is activated after the engine has been operating for a threshold amount of time and after engine coolant temperature reaches a threshold level . in addition , other conditions may be used to activate or enable the egr system . for example , egr may be enabled after engine load is greater than a threshold or after engine speed exceeds a threshold . routine 200 then proceeds to 206 if egr is activated . otherwise , routine 200 proceeds to exit . at 206 , the egr valve is controlled in response to engine operating conditions . in one example , the egr valve position is related to engine speed and driver demand torque . the egr valve positions may be stored in a table or function indexed by engine speed and driver demand torque . the egr valve positions correspond to an empirically determined egr flow rate . the egr valve position may be controlled by a vacuum actuator or by a stepper motor , for example . at 208 , routine 200 judges whether or not to regenerate a particulate filter in the egr loop . in one embodiment , routine 200 makes a decision based on the pressure drop across a particulate filter . in another embodiment , routine 200 may decide to regenerate the particulate filter in response to a model . for example , a soot accumulation model that estimates the amount of soot produced by an engine may be the basis for regenerating a particulate filter . if the estimated amount of soot exceeds a threshold , particulate filter regeneration is initiated . on the other hand , if a pressure across the particulate filter is determined from a sensor or an estimating model , particulate filter regeneration may be initiated after the observed or estimated pressure exceeds a threshold . in addition , other conditions may be included that determine when to regenerate the particulate filter . for example , filter regeneration may not proceed if engine temperature is above a threshold temperature or if engine temperature is below a threshold temperature . in one embodiment an electrically heated particulate filter is activated after egr begins flowing in the egr tube so that oxidized particulate matter may be oxidized and released from the filter and then flow back into the engine before being exhausted . further , in one embodiment , the temperature of the particulate filter may be elevated by flowing egr into the engine for a predetermined amount of time before the electrical heater is activated to heat the particulate filter . in other words , current is not supplied to the particulate filter heater until exhaust gases have flowed from the exhaust system to the intake system for a threshold amount of time or until the particulate filter reaches a threshold temperature . by elevating the particulate filter temperature with exhaust gases , it is possible to lower the thermal gradient that the filter is exposed to and therefore degradation of the particulate filter and particulate filter heater may be reduced . in one example , the rate that current is applied to the particulate filter heater may be related to the temperature of the particulate filter at a time when regeneration is requested . for example , as the temperature of the particulate filter increases , the amount of current supplied to the particulate filter over a period of time can be increased . if particulate filter regeneration is desired and conditions are met , routine 200 proceeds to 210 . otherwise , routine 200 proceeds to exit . at 210 , current is ramped to the electrical particulate filter heater that is in the egr loop . for example , current may be applied at a low level and increased over a period of time . in one example , the heater current is ramped when the engine is relatively cold . for example , if the engine is started at 20 ° c . the particulate filter heater current may be slowly ramped so that heater or particulate filter performance does not degrade . at higher temperatures , the particulate filter heater current may be ramped at a higher rate of current per second . thus , under a first condition of a particulate filter heater current is ramped at a first rate of current , and under a second condition of a particulate filter heater current is ramped at a second rate . at 212 , routine 200 judges whether or not particulate filter regeneration is complete or if conditions for regeneration are no longer present . in one embodiment , regeneration is determined complete when the pressure difference across the particulate filter is less than a predetermined amount . if routine 200 judges that regeneration is complete , routine 200 proceeds to exit . otherwise , routine continues to loop back . it will be appreciated that the configurations disclosed herein are exemplary in nature , and that these specific embodiments are not to be considered in a limiting sense , because numerous variations are possible . for example , the above systems can be applied to v - 6 , i - 4 , i - 6 , v - 12 , opposed 4 , and other engine types . the subject matter of the present disclosure includes all novel and nonobvious combinations and subcombinations of the various systems and configurations , and other features , functions , and / or properties disclosed herein . the following claims particularly point out certain combinations and subcombinations regarded as novel and nonobvious . these claims may refer to “ an ” element or “ a first ” element or the equivalent thereof . such claims should be understood to include incorporation of one or more such elements , neither requiring nor excluding two or more such elements . other combinations and subcombinations of the disclosed features , functions , elements , and / or properties may be claimed through amendment of the present claims or through presentation of new claims in this or a related application . such claims , whether broader , narrower , equal , or different in scope to the original claims , also are regarded as included within the subject matter of the present disclosure . | 5 |
referring to fig3 an improved a / d converter in accordance with principles of the present invention is described . a / d converter 50 includes analog chopper 12 ′, buffer amplifier 14 , quantizer 52 , digital filter and decimator 1 54 , fir filter 56 and decimator 2 58 . analog chopper 12 ′ chops analog input signal v in with a square wave of frequency f chop , which successively reverses the polarity of v in . analog chopper 121 may be implemented using any well - known analog chopping circuitry . for example , as shown in fig4 if input signal v in is a differential signal v in =( v in + − v in − , analog chopper 12 ′ may be implemented using cross - coupled switches 24 , 25 , 26 , and 27 . switch 24 is controlled by chop signal q , and is coupled between v in + and v cout + . switch 25 is controlled by chop signal q , and is coupled between v in − and v cout − . switch 26 is controlled by complementary chop signal { overscore ( q )}, and is coupled between v in + and v cout − . switch 27 is controlled by complementary chop signal { overscore ( q )}. and is coupled between v in − and v cout + . chop signals q and { overscore ( q )} are complementary logic signals of frequency f chop . for example , when q is high and { overscore ( q )} is low , v cout + = v in + , and v cout − = v in − . when { overscore ( q )} is high and q is low , v cout + = v in − and v cout − = v in + . analog chopper 12 ′ alternatively may be implemented using multiplexer circuitry as described by mccartney , analog multiplier circuitry , or any other suitable analog chopper circuitry . buffer amplifier 14 couples the output of analog chopper 12 ′ to quantizer 52 , which may be any conventional oversampling quantizer , such as a single or multi - bit δ - σ modulator , successive approximation quantizer , flash quantizer , pipelined quantizer , or other suitable oversampling quantizer . quantizer 52 provides a digital output at a rate f quant that is substantially higher than f chop . the digital output of quantizer 52 is the input to digital filter and decimator 1 54 , which includes a digital filter and a decimator that reduces the output data rate by a factor of m . for example , digital filter and decimator 1 54 may be implemented using sinc 3 filter and decimator 20 ( fig1 ), in which m equals the oversampling ratio n of quantizer 52 . alternatively , digital filter and decimator 1 54 may be any other suitable digital filter and decimator . digital filter and decimator 1 54 provide an output sequence x ′( n ) at a rate f quant / m . if control frequency f chop to analog chopper 12 ′ equals f quant /( 2 × m ) then successive output samples x ′( n ) of digital filter and decimator 1 54 are digital representations of the analog signals ( v in + v os ) and −( v in − v os ), where v os is the input - referred offset of buffer amplifier 14 and quantizer 52 . for example , x ′( n ) for n = 0 , − 1 , − 2 , 3 , − 4 may be expressed as : comparing equations ( 1 ) and ( 7 ), sequence x ′( n ) may be expressed as : x ′ ( n )=(− 1 ) n x ( n ), n = 0 , − 1 , − 2 , ( 8 ) fir filter 56 removes v os from sequence x ( n ) if fir filter 56 has l coefficients h ′( n ), n = 0 , 1 , 2 , . . . , l − 1 , output z ′( n ) of fir filter 56 may be expressed as : z ′ ( n ) = ∑ k = 0 l - 1 h ′ ( k ) × ′ ( n - k ) ( 9 ) combining equations ( 8 ) and ( 9 ), output z ′( n ) may be expressed as : z ′ ( n ) = ( - 1 ) n ∑ k = 0 l - 1 ( - 1 ) - k h ′ ( k ) × ( n - k ) ( 10 ) decimator 2 58 reduces the data rate by a factor p , which is an even integer greater than or equal to 2 . that is , from every block of p successive samples z ′( n ), decimator 2 58 provides the first sample at its output y ′( n ), and discards the remaining p − 1 samples . output y ′( n ) is at a rate f quant /( m × p ). for example , if p = 2 , output y ′( n ) is at a rate f chop . because p is an even integer , the phase relation between analog chopper 12 ′ and decimator 2 58 may be set so that y ′( n ) is chosen for n always even or n always odd . if n is even , output y ′( n ) may be expressed as : y ′ ( n ) = ∑ k = 0 l - 1 ( - 1 ) - k h ′ ( k ) × ( n - k ) ( 11 ) from equations ( 2 ), ( 6 ), ( 11 ) and ( 12 ), therefore , ∑ k = 0 l - 1 h ( k ) × ( n - k ) = ∑ k = 0 l - 1 ( - 1 ) - k h ′ ( k ) × ( n - k ) ( 13 ) h ′ ( n )=(− 1 ) n h ( n ), n = 0 , 1 , 2 , . . . , l − 1 ( 14 ) thus , for n even , coefficients h ′( n ) of fir filter 56 equal coefficients h ( n ) of prior art fir filter 22 , but with the sign reversed for all odd coefficients . alternatively , if n is odd , output y ′( n ) may be expressed as : y ′ ( n ) = ∑ k = 0 l - 1 ( - 1 ) - ( k - 1 ) h ′ ( k ) × ( n - k ) ( 15 ) from equations ( 2 ), ( 6 ), ( 15 ) and ( 16 ), therefore , ∑ k = 0 l - 1 h ( k ) × ( n - k ) = ∑ k = 0 l - 1 ( - 1 ) - ( k - 1 ) h ′ ( k ) × ( n - k ) ( 17 ) h ′ ( n )=(− 1 ) ( n 1 ) h ( n ), n = 0 , 1 , 2 , . . . , l − 1 ( 18 ) thus , for n odd , coefficients h ′( n ) of fir filter 56 equal coefficients h ( n ) of prior art fir filter 22 , but with the sign reversed for all even coefficients . fig5 illustrates another converter circuit of this invention that includes a sensor within the chopped conversion chain . circuit 60 includes excitation source 32 , analog chopper 34 ′ and sensor 36 , and a / d converter 62 . a / d converter 62 includes chop synch 40 ( as in fig2 ), and includes buffer amplifier 14 , quantizer 52 , digital filter and decimator 1 54 , fir filter 56 and decimator 2 58 ( as in fig3 ). converter 60 reduces thermal emf errors due to sensor interconnects and also reduces offset , offset drift and 1 / f noise errors produced by buffer amplifier 14 and quantizer 52 . in another aspect of the invention , a method of attenuating a converted digital signal over a wide null band — e . g ., from 48 hz to 62 hz — is provided . using conventional methods to produce a wide null band requires complex filter circuitry that is difficult to fabricate and occupies a substantial amount of die space . in a method for producing a wide null band according to the invention , the band is produced using substantially fewer components and less complex circuitry than by conventional methods . two examples of circuits which can be used to implement the method according to the invention are shown in fig1 and 3 . to produce the desired null band , this method requires only a cascade connection of the two digital filters / decimators . therefore , the method of the invention can operate with or without the second digital chopper 18 ( as in the circuit shown in fig1 ) or by modifying the sign of the coefficients of the second digital filter / decimator ( as in the circuit in fig3 ). more specifically , the circuit shown in fig1 can be used in a method according to the invention by implementing fir filter 22 with two equal coefficients of ½ { h ( 0 )= h ( 1 )= 0 . 5 } and , filter 20 as a sinc 4 filter . alternatively , the method can be implemented using the circuit shown in fig3 . to accomplish this , the digital filter / decimator 54 can be implemented as a sinc 4 with an impulse response of total length 4 * k and a decimation factor m = 4 * k ( f 1 = fs /( 4 * k )) and the digital filter / decimator 58 can be implemented as an fir of length 2 with coefficients h ( 0 )=− h ( 1 )= 0 . 5 or h ( 0 )=− h ( 1 )=− 0 . 5 and decimation factor p = 2 ( fout = fs /( 8 * k )). the actual value of k typically has little influence over the described invention . nevertheless , a common value selected in such configurations is k = 256 . the notch , or center , frequency fo can again be defined as fo = fs / k . the attenuation of the input signal magnitude around the notch frequency , fo , due to such an implementation can be written as : h ( f ) = 20 × log 10 ( sin ( π × f / fo ) k × sin ( π × f / k × fo ) ) 4 × sin ( 8 × π × f / fo ) 2 × sin ( 4 × π × f / fo ) ( 19 ) it should be noted that the method according to invention is not limited to these particular circuit configurations but , rather , these are only exemplary configurations of circuits that produce the results required by the method of the invention . fig6 shows one preferable frequency response that is obtainable according to the method of the invention . in this particular response , an fclk signal is selected such that fs = 55 * k hz , which provides a corner frequency of fo = fs / k = 55 hz . it is shown in fig6 that an implementation according to the invention provides better than about 87 db of input perturbation rejection in a frequency range of 48 hz (= 50 hz − 4 %) to 62 . 5 hz (= 60 hz + 4 %), or about +− 14 % of the corner frequency . for many applications , this level of rejection is sufficient . furthermore , in this particular embodiment , attenuation that extends about +− 14 % around a center frequency of about 55 hz , or other center frequency chosen to provide coverage of the 50 hz and 60 hz power line frequencies , also provides a substantial advantage . it should be noted that the invention is not limited to this particular range . persons skilled in the art further will recognize that the circuitry of the present invention may be implemented using circuit configurations other than those shown and discussed above . all such modifications are within the scope of the present invention , which is limited only by the claims that follow . | 7 |
the present principles are directed to determining the span of the user profiles of a single account based on binary feedback . embodiments of the present invention identify composite accounts within , e . g ., a movie delivery system , and furthermore identify the individuals sharing such an account to learn accurate profiles of different users &# 39 ; behaviors . the present description illustrates the present principles . it will thus be appreciated that those skilled in the art will be able to devise various arrangements that , although not explicitly described or shown herein , embody the present principles and are included within its spirit and scope . all examples and conditional language recited herein are intended for pedagogical purposes to aid the reader in understanding the present principles and the concepts contributed by the inventor ( s ) to furthering the art , and are to be construed as being without limitation to such specifically recited examples and conditions . moreover , all statements herein reciting principles , aspects , and embodiments of the present principles , as well as specific examples thereof , are intended to encompass both structural and functional equivalents thereof . additionally , it is intended that such equivalents include both currently known equivalents as well as equivalents developed in the future , i . e ., any elements developed that perform the same function , regardless of structure . thus , for example , it will be appreciated by those skilled in the art that the block diagrams presented herein represent conceptual views of illustrative circuitry embodying the present principles . similarly , it will be appreciated that any flow charts , flow diagrams , state transition diagrams , pseudocode , and the like represent various processes which may be substantially represented in computer readable media and so executed by a computer or processor , whether or not such computer or processor is explicitly shown . the functions of the various elements shown in the figures may be provided through the use of dedicated hardware as well as hardware capable of executing software in association with appropriate software . when provided by a processor , the functions may be provided by a single dedicated processor , by a single shared processor , or by a plurality of individual processors , some of which may be shared . moreover , explicit use of the term “ processor ” or “ controller ” should not be construed to refer exclusively to hardware capable of executing software , and may implicitly include , without limitation , digital signal processor (“ dsp ”) hardware , read - only memory (“ rom ”) for storing software , random access memory (“ ram ”), and non - volatile storage . other hardware , conventional and / or custom , may also be included . similarly , any switches shown in the figures are conceptual only . their function may be carried out through the operation of program logic , through dedicated logic , through the interaction of program control and dedicated logic , or even manually , the particular technique being selectable by the implementer as more specifically understood from the context . in the claims hereof , any element expressed as a means for performing a specified function is intended to encompass any way of performing that function including , for example , a ) a combination of circuit elements that performs that function or b ) software in any form , including , therefore , firmware , microcode or the like , combined with appropriate circuitry for executing that software to perform the function . the present principles as defined by such claims reside in the fact that the functionalities provided by the various recited means are combined and brought together in the manner which the claims call for . it is thus regarded that any means that can provide those functionalities are equivalent to those shown herein . reference in the specification to “ one embodiment ” or “ an embodiment ” of the present principles , as well as other variations thereof , means that a particular feature , structure , characteristic , and so forth described in connection with the embodiment is included in at least one embodiment of the present principles . thus , the appearances of the phrase “ in one embodiment ” or “ in an embodiment ”, as well any other variations , appearing in various places throughout the specification are not necessarily all referring to the same embodiment . referring now to fig1 , a block diagram is shown of a system 100 for delivering content to a home or end user in connection with determining user information and profiles . the content originates from a content source 102 , such as a movie studio or production house . the content may be supplied in at least one of two forms . one form may be a broadcast form of content . the broadcast content is provided to the broadcast affiliate manager 104 , which is typically a national broadcast service . the broadcast affiliate manager may collect and store the content , and may schedule delivery of the content over a deliver network , shown as a first delivery network 106 . the first delivery network 106 may include satellite link transmissions from a national center to one or more regional or local centers . the first delivery network 106 may also include local content delivery using local delivery systems such as over - the - air broadcast , satellite broadcast , or cable broadcast . the locally delivered content is provided to a receiving device 108 in a user &# 39 ; s home , where the content will subsequently be searched by the user . it is to be appreciated that the receiving device 108 can take many forms and may be embodied as a set top box / digital video recorder ( dvr ), a gateway , a modem , etc . further , the receiving device 108 may act as entry point , or gateway , for a home network system that includes additional devices configured as either client or peer devices in the home network . a second form of content is referred to as special content . special content may include content delivered as premium viewing , pay - per - view , or other content not otherwise provided to the broadcast affiliate manager such as , e . g ., movies , video games or other video elements . in many cases , the special content may be content requested by the user . the special content may be delivered to a content manager 110 . the content manager 110 may be a service provider , such as an internet website , affiliated , for instance , with a content provider , broadcast service , or delivery network service . the content manager 110 may also incorporate internet content into the delivery system . the content manager 110 may deliver the content to the user &# 39 ; s receiving device 108 over a separate delivery network , second delivery network 112 . the second delivery network 112 may include high - speed broadband internet type communications systems . it is important to note that the content from the broadcast affiliate manager 104 may also be delivered using all or parts of the second delivery network 112 and content from the content manager 110 may be delivered using all or parts of the first delivery network 106 . in addition , the user may also obtain content directly from the internet via the second delivery network 112 without necessarily having the content managed by the content manager 110 . several adaptations for utilizing the separately delivered content may be possible . in one possible approach , the special content is provided as an augmentation to the broadcast content , providing alternative displays , purchase and merchandising options , enhancement material , etc . in another embodiment , the special content may completely replace some programming content provided as broadcast content . finally , the special content may be completely separate from the broadcast content , and may simply be a media alternative that the user may choose to utilize . for instance , the special content may be a library of movies that are not yet available as broadcast content . the receiving device 108 may receive different types of content from one or both of the delivery networks . the receiving device 108 processes the content , and provides a separation of the content based on user preferences and commands . the receiving device 108 may also include a storage device , such as a hard drive or optical disk drive , for recording and playing back audio and video content . further details of the operation of the receiving device 108 and features associated with playing back stored content will be described below in relation to fig2 . the processed content is provided to a display device 114 . the display device 114 may be a conventional 2 - d type display or may alternatively be an advanced 3 - d display . the receiving device 108 may also be interfaced to a second screen such as a touch screen control device 116 . the touch screen control device 116 may be adapted to provide user control for the receiving device 108 and / or the display device 114 . the touch screen device 116 may also be capable of displaying video content . the video content may be graphics entries , such as user interface entries , or may be a portion of the video content that is delivered to the display device 114 the touch screen control device 116 may interface to receiving device 108 using any well - known signal transmission system , such as infra - red ( ir ) or radio frequency ( rf ) communications and may include standard protocols such as infra - red data association ( irda ) standard , wi - fi , bluetooth and the like , or any other proprietary protocols . in the example of fig1 , the system 100 also includes a back end server 118 and a usage database 120 . the back end server 118 includes a personalization engine that analyzes the usage habits of a user and makes recommendations based on those usage habits . the usage database 120 is where the usage habits for a user are stored . in some cases , the usage database 120 may be part of the back end server 118 . in the present example , the back end server 118 ( as well as the usage database 120 ) is connected to the system the system 100 and accessed through the second delivery network 112 . referring now to fig2 , a block diagram of an embodiment of a receiving device 200 is shown . receiving device 200 may operate similar to the receiving device described in fig1 and may be included as part of a gateway device , modem , set - top box , or other similar communications device . the device 200 shown may also be incorporated into other systems including an audio device or a display device . in either case , several components necessary for complete operation of the system are not shown in the interest of conciseness , as they are well known to those skilled in the art . in the device 200 shown in fig2 , the content is received by an input signal receiver 202 . the input signal receiver 202 may be one of several known receiver circuits used for receiving , demodulation , and decoding signals provided over one of the several possible networks including over the air , cable , satellite , ethernet , fiber and phone line networks . the desired input signal may be selected and retrieved by the input signal receiver 202 based on user input provided through a control interface or touch panel interface 222 . touch panel interface 222 may include an interface for a touch screen device . touch panel interface 222 may also be adapted to interface to a cellular phone , a tablet , a mouse , a high end remote or the like . the decoded output signal is provided to an input stream processor 204 . the input stream processor 204 performs the final signal selection and processing , and includes separation of video content from audio content for the content stream . the audio content is provided to an audio processor 206 for conversion from the received format , such as compressed digital signal , to an analog waveform signal . the analog waveform signal is provided to an audio interface 208 and further to the display device or audio amplifier . alternatively , the audio interface 208 may provide a digital signal to an audio output device or display device using a high - definition multimedia interface ( hdmi ) cable or alternate audio interface such as via a sony / philips digital interconnect format ( spdif ). the audio interface may also include amplifiers for driving one more sets of speakers . the audio processor 206 also performs any necessary conversion for the storage of the audio signals . the video output from the input stream processor 204 is provided to a video processor 210 . the video signal may be one of several formats . the video processor 210 provides , as necessary , a conversion of the video content based on the input signal format . the video processor 210 also performs any necessary conversion for the storage of the video signals . a storage device 212 stores audio and video content received at the input . the storage device 212 allows later retrieval and playback of the content under the control of a controller 214 and also based on commands , e . g ., navigation instructions such as fast - forward ( ff ) and rewind ( rew ), received from a user interface 216 and / or touch panel interface 222 . the storage device 212 may be a hard disk drive , one or more large capacity integrated electronic memories , such as static ram ( sram ), or dynamic ram ( dram ), or may be an interchangeable optical disk storage system such as a compact disk ( cd ) drive or digital video disk ( dvd ) drive . the converted video signal , from the video processor 210 , originating either from the input or from the storage device 212 , is provided to the display interface 218 . the display interface 218 further provides the display signal to a display device of the type described above . the display interface 218 may be an analog signal interface such as red - green - blue ( rgb ) or may be a digital interface such as hdmi . it is to be appreciated that the display interface 218 can generate the various screens for presenting the search results in a three dimensional gird as will be described in more detail below . the controller 214 is interconnected via a bus to several of the components of the device 200 , including the input stream processor 202 , audio processor 206 , video processor 210 , storage device 212 , and a user interface 216 . the controller 214 manages the conversion process for converting the input stream signal into a signal for storage on the storage device or for display . the controller 214 also manages the retrieval and playback of stored content . furthermore , as will be described below , the controller 214 performs searching of content and the creation and adjusting of the gird display representing the content , either stored or to be delivered via the delivery networks , described above . the controller 214 is further coupled to control memory 220 ( e . g ., volatile or non - volatile memory , including ram , sram , dram , rom , programmable rom ( prom ), flash memory , electronically programmable rom ( eprom ), electronically erasable programmable rom ( eeprom ), etc .) for storing information and instruction code for controller 214 . control memory 220 may store instructions for controller 214 . control memory may also store a database of elements , such as graphic elements containing content . the database may be stored as a pattern of graphic elements . alternatively , the memory may store the graphic elements in identified or grouped memory locations and use an access or location table to identify the memory locations for the various portions of information related to the graphic elements . further , the implementation of the control memory 220 may include several possible embodiments , such as a single memory device or , alternatively , more than one memory circuit communicatively connected or coupled together to form a shared or common memory . still further , the memory may be included with other circuitry , such as portions of bus communications circuitry , in a larger circuit . referring now to fig3 , the user interface process of the present disclosure employs an input device that can be used to express functions , such as fast forward , rewind , etc . to allow for this , a tablet or touch panel device 300 ( which is the same as the touch screen device 116 shown in fig1 ) may be interfaced via the user interface 216 and / or touch panel interface 222 of the receiving device 200 . the touch panel device 300 allows operation of the receiving device or set top box based on hand movements , or gestures , and actions translated through the panel into commands for the set top box or other control device . in one embodiment , the touch panel 300 may simply serve as a navigational tool to navigate the grid display . in other embodiments , the touch panel 300 will additionally serve as the display device allowing the user to interact directly with the navigation through the grid display of content . the touch panel device may be included as part of a remote control device containing more conventional control functions such as activator buttons . the touch panel 300 can also include at least one camera element . as described in further detail below , content displayed on the touch panel device 300 may be zapped or thrown to the main screen ( e . g ., display device 114 shown in fig1 ). referring now to fig4 , the use of a gesture sensing controller or touch screen , such as that shown above , provides for a number of types of user interaction . the inputs from the controller are used to define gestures and the gestures , in turn , define specific contextual commands . the configuration of the sensors may permit defining movement of a user &# 39 ; s fingers on a touch screen or may even permit defining the movement of the controller itself in either one dimension or two dimensions . two - dimensional motion , such as a diagonal , and a combination of yaw , pitch and roll can be used to define any 4 - dimensional motion , such as a swing . a number of gestures are illustrated in fig4 . gestures are interpreted in context and are identified by defined movements made by the user . bumping 420 is defined by a two - stroke drawing indicating pointing in one direction , either up , down , left or right . the bumping gesture is associated with specific commands in context . for example , in a time shifting mode , a left - bump gesture 420 indicates rewinding , and a right - bump gesture indicates fast - forwarding . in other contexts , a bump gesture 420 is interpreted to increment a particular value in the direction designated by the bump . checking 440 is defined as in drawing a checkmark . it is similar to a downward bump gesture 420 . checking is identified in context to designate a reminder , user tag or to select an item or element . circling 440 is defined as drawing a circle in either direction . it is possible that both directions could be distinguished . however , to avoid confusion , a circle is identified as a single command regardless of direction . dragging 450 is defined as an angular movement of the controller ( a change in pitch and / or yaw ) while pressing a button ( virtual or physical ) on the tablet 300 ( i . e ., a “ trigger drag ”). the dragging gesture 450 may be used for navigation , speed , distance , time - shifting , rewinding , and forwarding . dragging 450 can be used to move a cursor , a virtual cursor , or a change of state , such as highlighting outlining or selecting on the display . dragging 450 can be in any direction and is generally used to navigate in two dimensions . however , in certain interfaces , it is preferred to modify the response to the dragging command . for example , in some interfaces , operation in one dimension or direction is favored with respect to other dimensions or directions depending upon the position of the virtual cursor or the direction of movement . nodding 460 is defined by two fast trigger - drag up - and - down vertical movements . nodding 460 is used to indicate “ yes ” or “ accept .” x - ing 470 is defined as in drawing the letter “ x .” x - ing 470 is used for “ delete ” or “ block ” commands . wagging 480 is defined by two trigger - drag fast back - and - forth horizontal movements . the wagging gesture 480 is used to indicate “ no ” or “ cancel .” depending on the complexity of the sensor system , only simple one - dimensional motions or gestures may be allowed . for instance , a simple right or left movement on the sensor as shown here may produce a fast forward or rewind function . in addition , multiple sensors could be included and placed at different locations on the touch screen . for instance , a horizontal sensor for left right movement may be placed in one spot and used for volume u / down , while a vertical sensor for up down movement may be place in a different spot and used for channel up / down . in this way , specific gesture mappings may be used . as discussed in further detail below , a two finger swipe gesture may be utilized to initiate the throwing or moving of content from the tablet 300 to the main screen or display device 114 . referring now to fig5 , a method is shown that may be implemented by , e . g ., a content distribution service , an online market service , etc . ( e . g ., content manager 110 or the broadcast affiliate manager 104 ) to ascertain information about multiple users associated with a single account using binary feedback information . block 502 receives a set of binary labels as an input . these labels are provided by one or more users sharing an account and are associated with a set of items . for example , the items in question may be movies , and the labels can indicate whether the account has viewed these movies or not . alternatively , the items could be products advertised to the account and the labels may indicate whether the account purchased the products or not . the label for an item i is denoted herein as y i . block 504 receives a set of item descriptors , one of each of labeled item . these descriptors could be , e . g ., vectors describing the genre or actors participating in a movie or other features of the product advertised . this feature descriptor may be represented as a vector of real - valued numbers of dimension d ( where d is the number of features ). the descriptor of item i will be shown herein as x i . using this information , block 506 estimates the mean and covariance of the underlying features x i . to do this , block 506 constructs estimates of the feature mean and covariance over the features and labels . a standard gaussian version of the features may then be constructed as { circumflex over ( σ )} − 1 / 2 ( x i −{ circumflex over ( μ )}), where { circumflex over ( σ )} is the covariance and { circumflex over ( μ )} is the feature mean . using the calculated estimates , block 508 identifies a vector r that belongs to a convex code spanned by the vectors profiling each user . the vector may be calculated as where n is the number of labels , and this vector lies in the interior of the convex cone spanned by the parameter profiles . the vector r may then be used to perform a mirroring operation , where all labels lying in the negative half space determined by r are flipped , for example by changing + 1 to − 1 and − 1 to + 1 in block 510 . the flipped labels are denoted herein by z i . block 512 computes a weighted covariance matrix q over all x i , where each point &# 39 ; s contribution is weighed by the mirrored labels . the matrix q is determined as the spectrum of q has a specific structure that reveals the span of the users . in particular , q converges to a matrix that contains an eigenvalue with multiplicity n - k , where n is the number of labels and k is a number of remaining eigenvalues . block 514 calculates eigenvectors and eigenvalues of the matrix q . most eigenvalues of q will be equal to each other ( i . e ., a number of eigenvalues having multiplicity n - k ), but a small number of eigenvalues will differ . the standout eigenvalues are calculated by finding the median value of all the eigenvalues and identifying the k values furthest from the median . the number of eigenvalues that “ stand out ” in this respect is interpreted as being a number of users associated with the account . the eigenvectors corresponding to the stand - out eigenvalues yield the span of the user profiles . block 516 rotates the eigenvectors by multiplying by to obtain the span and outputs these quantities . the resulting span is a set of vectors that are in the subspace defined by all linear combinations of the vectors . the span output by block 516 can be used for several tasks . for example , the span may be used to predict a label for an item given a new feature vector ( in other words , predicting whether a user would watch this movie ). the span may also be used for clustering , allowing the content provider to identify which user associated with an account generated a particular label . any algorithm that does either clustering or prediction will run with improved accuracy if one first projects the features to the span defined by profiles . using such information allows the content provider to make a recommendation using well known techniques . for example , if a user choose a movie with a certain actor , the content provider could recommend other movies with that actor . these and other features and advantages of the present principles may be readily ascertained by one of ordinary skill in the pertinent art based on the teachings herein . it is to be understood that the teachings of the present principles may be implemented in various forms of hardware , software , firmware , special purpose processors , or combinations thereof . most preferably , the teachings of the present principles are implemented as a combination of hardware and software . moreover , the software may be implemented as an application program tangibly embodied on a program storage unit . the application program may be uploaded to , and executed by , a machine comprising any suitable architecture . preferably , the machine is implemented on a computer platform having hardware such as one or more central processing units (“ cpu ”), a random access memory (“ ram ”), and input / output (“ i / o ”) interfaces . the computer platform may also include an operating system and microinstruction code . the various processes and functions described herein may be either part of the microinstruction code or part of the application program , or any combination thereof , which may be executed by a cpu . in addition , various other peripheral units may be connected to the computer platform such as an additional data storage unit and a printing unit . it is to be further understood that , because some of the constituent system components and methods depicted in the accompanying drawings are preferably implemented in software , the actual connections between the system components or the process function blocks may differ depending upon the manner in which the present principles are programmed . given the teachings herein , one of ordinary skill in the pertinent art will be able to contemplate these and similar implementations or configurations of the present principles . although the illustrative embodiments have been described herein with reference to the accompanying drawings , it is to be understood that the present principles is not limited to those precise embodiments , and that various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the scope or spirit of the present principles . all such changes and modifications are intended to be included within the scope of the present principles as set forth in the appended claims . | 6 |
referring now to the drawings , and particularly to fig1 - 4 , a concrete discharge chute employing a preferred embodiment of the concrete chute apparatus of the present invention is shown and generally designated by the reference numeral 10 . in fig1 , a concrete discharge chute 10 is shown concrete discharge chute 10 is arranged in cooperation with a conventional cement truck ( not shown ) and includes a main chute section 12 to which is hingeably coupled to over - chute section 14 . main chute section 12 and over - chute section 14 form an elongated chute having a concave interior through which cement can be dispensed when over - chute section 14 is in the down position . main chute section 12 has a distal end 22 and a proximal end 20 , where the proximal end is that end closest to the cement truck . similarly , over - chute section 14 has a distal end 26 and a proximal end 24 , where the distal end is that end furthest from the truck when over - chute section 14 is in its down position . the chute sections further include distal end surfaces substantially orthogonally oriented relative to a chute axis . in fig1 , over - chute section 14 is shown in its up position . this position is used when the concrete truck is traveling on roads and highways . to place the discharge chute 10 in this position , over - chute section 14 rotates counter - clockwise about chute hinge 16 and comes to rest on the main chute section 12 as shown . in an embodiment , the discharge chute 10 may have oversized hinge portions of the chute sections such that the length of the chute section sidewalls are not in contact with one another . when over - chute section 14 is in this up position , a circular opening is formed between the over - chute section 14 and the main chute section 12 . the new and improved concrete chute apparatus 18 , located at the distal end of the main chute 22 , is shown obscuring the aforementioned opening . such apparatus may also be referred to as abutment plate 18 , as the apparatus abuts an inner surface of main chute section 12 to prevent the discharge of cement or cement debris . consequently , plate 18 is shown in fig1 in its “ in use ” position . that is , abutment plate 18 is shown in that position that prevents concrete debris from falling from concrete discharge chute 10 . by positioning the abutment plate 18 within the main chute 12 , cement debris and residue in concrete discharge chute 10 is prevented from accidentally discharging from the truck . abutment plate 18 is mounted to over - chute section 14 such that abutment plate 18 remains stationary with respect to over - chute section 14 . abutment plate 18 is mounted to a chute first edge 36 spaced from and parallel to a chute second edge 38 . abutment plate 18 may be welded or riveted or otherwise directly mounted onto over - chute section 14 using any metal fastening method . alternately , abutment plate 18 may be mounted via plate - mounting bracket 28 and plate - mounting means 30 . in the preferred embodiment shown , plate - mounting means 30 may be a bolt . plate 18 is mounted to the proximal end 24 of over - chute section 14 such that abutment plate 18 is arranged within the distal end 22 of main chute 12 when over - chute section 14 is in the up , or traveling , position . placement at the distal end 22 of main chute 12 allows abutment plate 18 to accommodate a larger volume of concrete debris within the main chute section 12 than would be possible if abutment plate 18 were arranged at , for example , the proximal end 20 of main chute 12 . referring to fig2 , the over - chute section 14 is shown in the down , or dispensing , position . chute handle 32 would be used to rotate the over - chute section 14 about the chute hinge 16 , thus positioning over - chute section 14 in either the up or down position . as noted above , plate 18 remains stationary with respect to over - chute section 14 . consequently , abutment plate 18 is arranged above the concrete discharge chute 10 when the over - chute section is in the down position more particularly , abutment plate 18 is arranged above over - chute section 14 . abutment plate 18 includes an arcuate bottom wall orthogonally oriented between the front and rear parallel walls of the plate . it is noted that the arcuate abutment plate bottom wall is arranged to form complementary reception within the concave interior surface of the main chute section 12 . abutment plate 18 may have an arcuate top wall 42 configured to allow the material dispensed from the discharge chute 10 to extend somewhat above the level of the sidewall extents of the chute sections . in an embodiment , abutment plate 18 may include a straight top wall . in yet another embodiment , abutment plate 18 may include an arcuate portion coupled with at least one linear portion , as shown . fig3 is a cross sectional view taken on line 3 of fig1 . shown in fig3 is the abutment plate 18 in use . that is , abutment plate 18 is in the down position , and is preventing discharge of cement 40 located within main chute section 12 . abutment plate 18 may retain cement 40 unless the level of cement 40 exceeds the height of arcuate top wall 42 . abutment plate 18 is therefore constructed of a rigid material having sufficient strength to hold material dispensed from discharge chute 10 . in an embodiment , abutment plate may be of the same material as the discharge chute 10 . in an embodiment , abutment plate may be metal , metal alloy , rigid plastic , or composite . also shown in fig3 by way of example is plate - mounting means 30 in a position offset from abutment plate 18 . in an alternate embodiment , plate - mounting means 30 may be commensurate with abutment plate 18 . plate mounting means 30 may be any means known in the art to attach abutment plate 18 to over - chute 14 . fig4 is a cross - sectional view of fig2 along line 4 . fig4 illustrates dispense of cement from concrete discharge chute 10 while abutment plate 18 is in use . as shown , abutment plate 18 is arranged above over - chute chute section 14 . the material dispensed may pass unaffected by the presence of abutment plate 18 . this may also be true in those cases in which a large volume of material is discharged , such that the discharge chute is completely full and material extends above the sidewalls in those areas of the chute closest to the chute axis . for example , arcuate top wall 42 of abutment plate 18 will allow dispense of cement , for example , to pass beneath , even if the level of the cement rises above the sidewalls of the chute . in use , it can now be understood that the concrete chute apparatus described herein would provide a substantially maintenance free apparatus which would in function provide a means to prevent debris from falling from the chute of a cement truck or similar vehicle having an articulated chute . the abutment plate 18 would not require independent adjustment , and would therefore always be in the correct position . the abutment plate 18 has no moving parts which could malfunction or which would require servicing . further , the abutment plate 18 is attached to the discharge chute 10 and therefore could not become lost . while a preferred embodiment of the concrete chute apparatus inline water treatment system has been described in detail , it should be apparent that modifications and variations thereto are possible , all of which fall within the true spirit and scope of the invention . with respect to the above description then , it is to be realized that the optimum dimensional relationships for the parts of the invention , to include variations in size , materials , shape , form , function and manner of operation , assembly and use , are deemed readily apparent and obvious to one skilled in the art , and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention . for example , any suitably rigid material may be used for the concrete chute apparatus . further , the apparatus may be attached to the over - chute using any metal fastening means known in the art . therefore , the foregoing is considered as illustrative only of the principles of the invention . further , since numerous modifications and changes will readily occur to those skilled in the art , it is not desired to limit the invention to the exact construction and operation shown and described , and accordingly , all suitable modifications and equivalents may be resorted to , falling within the scope of the invention . | 1 |
the following detailed description and appended drawings describe and illustrate various exemplary embodiments of the invention . the description and drawings serve to enable one skilled in the art to make and use the invention , and are not intended to limit the scope of the invention in any manner . in respect of the methods disclosed , the steps presented are exemplary in nature , and thus , the order of the steps is not necessary or critical . one possible overall arrangement of an elevator installation is illustrated in fig1 and fig1 a . fig1 shows the elevator installation 1 in a schematic side view and fig1 a shows the same elevator installation 1 in a schematic plan view . the illustrated elevator installation 1 comprises an elevator car 3 which moves in a vertical direction in a shaft 2 along guide tracks 7 . the elevator car 3 is supported by support means 5 and is connected with a counterweight 4 . the counterweight 4 and the elevator car 2 are driven by a drive 6 by way of the support means 5 and move in opposite sense in the elevator shaft 2 . the elevator car 3 is provided with braking equipment 11 which brakes the elevator car or keeps it at standstill . the braking equipment 11 comprises at least two brake units 12 which each act on a respective one of the guide tracks 7 . the brake units 12 co - operate as a single braking equipment 11 , wherein the braking equipment 11 can optionally define the braking force requirement for a single individual brake unit 12 . the brake units 12 are , in the illustrated example , attached below the car body 3 . however , attachment laterally and / or above the elevator car 3 is also possible . obviously , combinations of these attachment locations are also conceivable . this would be useful above all if , for extending the braking performance , several brake units 12 are used . the elevator car is provided with guide shoes which guide the car 2 along the guide track 7 . in the illustrated example the guide track 7 is formed by a t - shaped guide rail , which at the same time is also a brake track 8 . other forms of elevator installations are obviously possible . an automotive elevator car , for example with a linear motor , can be used and the elevator shaft can be partly open , or separate tracks for guiding ( guide track 9 ) and braking ( brake track 8 ) can be used . fig2 shows the elevator brake unit 12 as used in correspondence with the present invention in the elevator installation 1 according to fig1 . the brake unit 12 is attached to the car 3 . the brake unit 12 comprises a brake housing 13 , a brake plate 14 movable with respect to the brake housing 13 and a brake plate 15 fixed with respect to the brake housing 13 . the brake plates 14 and 15 are , in the case of need , brought by means of an advance device 19 into contact with the brake track 8 . the brake plates 14 and 15 are connected by means of fastening plates 16 with the brake housing 13 and the advance device 19 , respectively . the brake track 8 in the illustrated example is at the same time the guide track 7 , wherein a conventional t - shaped guide rail is used . the brake unit 12 further comprises a guide support 17 . the guide support 17 serves for fastening or connecting the brake housing 13 with the car 3 . it is fixedly connected with the car 3 . a wear - compensating device 30 is , in the illustrated example , arranged between the guide supports 17 and the brake housing 13 . the guide support 17 at the same time comprises the guide shoe 9 which guides the elevator car 3 along the guide track 7 . the guide shoe 9 is resiliently mounted with respect to the car 3 . this enables insulation from guidance vibrations . a resilient intermediate element 10 allows the car 3 oscillatory deviations ( distance “ a ”) relative to the guide track 7 . a clearance “ if ”, “ ib ” of the brake unit is in this case set to be of such a size that even in the case of outward oscillation of the car within the scope of the guidance resilience “ a ” and possible guidance plays “ f ” as well as offsets in the meeting of guide track parts no contact of the brake plates 14 , 15 with the guide track 7 or brake track 8 takes place . the wear - compensating device 30 now keeps the fixed clearance “ if ”, during release of the brake 12 , substantially constant on the side of the fixed brake plate 15 . the illustrated brake unit 12 further consists of electromechanical components . it comprises advance regulating means 21 which keeps a predetermined total clearance “ it ” constant by actuating the advance device 19 . the total clearance “ it ” is formed by the sum of the fixed clearance “ if ” and the movable clearance “ ib ”, wherein the fixed clearance “ if ” corresponds with the side of the fixed brake plate 15 and the movable clearance “ ib ” corresponds with the side of the movable brake plate 14 . the terms “ fixed ” and “ movable ” are used in this connection merely for definition . the advance regulating means 21 moves the movable brake plate 14 directly perpendicularly to the brake or guide surface 7 , 8 . as a rule , several wear - compensating devices 30 are arranged in parallel , preferably one above the other . the brake unit 12 is an electromechanical brake unit in which the movable brake lining 14 is advanced by means of an electromechanical drive , such as , for example , a spindle drive . in the case of need the advance spindle is actuated by way of a gear stage . the brake unit 12 preferably comprises advance checking means in the advance regulating means 21 . by means of this advance checking means a brake plate wear and / or deviations from a normal behavior of the brake unit 12 can be ascertained and a signal generated on an advance checking signal line 24 so that the overall wear can be checked by this method . as a rule the wear - compensating device 30 is set in such a manner that the clearance “ if ” of the side of the fixed brake plate 15 is equal to the clearance “ ib ” of the movable brake plate 14 . it thus corresponds with half the total clearance “ it ”. this setting is advantageous when centrally suspended or centrally guided elevator cars 3 are concerned . however , the wear - compensating device 30 also enables asymmetric settings , whereby an uneven division of the clearances ( if , ib ) can be achieved . this is useful particularly in the case of asymmetrically suspended elevator cars , where a possible wear of the guide shoes 9 makes itself noticeable on one side . the guide support 17 further comprises a holder 18 . the holder 18 supports the brake plates 14 , 15 or the fastening plates 16 and conducts braking forces directly into the guide support 17 and further into the car 3 . the brake housing 13 itself is thereby relieved of the actual braking force ; merely the normal force acting in one direction and generating the braking force by way of friction has to be accepted . fig3 illustrates the settable wear - compensating device 30 in detail . the wear - compensating device 30 consists of a positioning part 31 , a restoring unit 32 , a first abutment 33 and a second abutment 34 . the wear - compensating device 30 produces a connection of the brake housing 13 with the guide support 17 . in this embodiment the positioning part 31 is connected by a slip connection 35 with the guide support 17 . the positioning part 31 is preferably produced from a plastic material . it can be displaced relative to the guide support 17 only by a substantial force of , for example , approximately 25 n to 50 n . the positioning part 31 itself is slidably arranged in the brake housing 13 to be easy - running . the brake housing 13 can thereby displace relative to the guide support 17 in two stages . the direction of displacement is in that case oriented in the direction of the normal force . in a first displacement stage the brake housing 13 can be displaced by a small force slidingly relative to the positioning part 31 and thus also slidingly relative to the guide support 17 . this sliding displacement is limited by the first abutment 33 and the second abutment 34 . this first displacement stage corresponds with the desired clearance “ if ” of the fixed brake plate side . in the example , this first displacement stage or the clearance “ if ” is settable by means of a clearance play setting screw 36 . the restoring unit 32 , which is arranged between the brake housing 13 and the positioning part 31 , in the form of a spring in this connection displaces the brake housing 13 up to the boundary mark of the first abutment 33 . in a second displacement stage the brake housing 13 together with the positioning part 31 can be displaced in slipping manner relative to the guide support 17 . the fig4 series — comprising fig4 . 1 to 4 . 4 a - now explain by way of example the functional sequence for compensation of wear . fig4 . 1 , 4 . 2 , 4 . 3 and 4 . 4 each show a working setting , by way of example , of the brake unit and the details according to fig4 . 1 a , 4 . 2 a , 4 . 3 a and 4 . 4 a show the respectively associated setting of the wear compensation device . fig4 . 1 and fig4 . 1 a show the brake unit 12 in the working setting , i . e . the brake is open . the brake linings 14 , 15 are spaced on both sides of the brake track 8 by the clearance ( if , ib ). the positioning part 31 of the wear compensating unit 30 is pressed against the first abutment 33 defined by the clearance play setting screw 36 . the possible free displacement path or slide path of the positioning part 31 is set in correspondence with the desired fixed clearance “ if ”. in the case of actuation of the brake unit 12 there thus takes place in a first step ( s 1 ) advance of the movable brake plate 14 by means of the advance device 19 until the movable plate 14 contacts the brake track 8 , and then , by further actuation of the advance device 19 , the brake housing 13 together with the fixed brake plate 15 is urged towards the opposite side of the brake track 8 ( s 2 ) until the fixed brake plate 15 contacts the opposite side of the brake track 8 . tightening of the brake plates 14 , 15 relative to the brake track 8 now takes place by a further advance movement , whereby braking is carried out . this work setting is illustrated in fig4 . 2 and 4 . 2 a . it is illustrated in the following how now compensation is provided for the clearance in the wear compensating unit 30 . the positioning part 31 stands against the second abutment 34 . compensation for abrasion or wear of the movable brake plate 14 is now , as illustrated in fig4 . 3 and 4 . 3 a , provided directly by a further advance of the movable brake plate 14 by the advance device 19 . compensation of wear “ v ” of the fixed brake plate 15 is carried out indirectly in that the advance device 19 further advances the brake housing 13 together with the fixed brake plate 15 ( s 3 ) or pulls this tight and this advance of the brake housing 13 produces in the wear - compensating device 30 a slipping in the slip connection 35 between the brake housing 13 and the guide support 17 , since the slide path of the positioning part 31 is already applied . the advanced position of the brake housing 13 together with the fixed brake plate 15 thus now achieved forms the final working position of the fixed brake lining 15 in this braking sequence . this final working position now necessarily forms the basis for resetting of the brake housing 13 together with the fixed brake plate 15 . on opening of the brake unit 12 the reverse sequence takes place analogously , which leads to the state according to fig4 . 4 and 4 . 4 a . the advance device 19 relieves the brake plates 14 , 15 , and thereafter the brake housing 13 together with the fixed brake plate 15 , beginning from the final working position , is reset in correspondence with the set clearance “ if ” of the fixed brake plate 15 ( s 4 ). this resetting is produced by the restoring unit 32 which , acting against the positioning part 31 , displaces the brake housing 13 in acting in correspondence with the set clearance path “ if ” back to the first abutment 33 . as is apparent in fig4 . 4 a , the positioning part 31 now slips relative to the guide support 17 by the wear amount “ v ”. the fixed brake plate 15 has reached its clearance “ if ” and the movable brake plate 14 can now be drawn back by the residual amount of the total clearance ( ib = it − if ). the brake unit is ready for the next braking action and the advance travels correspond with the new state . thus , actuating times , which were applicable to the new brake , can also be maintained for a worn brake . fig5 shows a schematic view of a second embodiment brake unit 12 a with a wear - compensating device and an elevator car guide integrated in the brake unit . the guide support 17 is guided along the brake and guide track 7 , 8 directly by the guide shoe 9 , whilst the car 3 is fastened relative to the guide support 17 by way of a resilient element 10 a , for example a rubber spring , a damper or an active vibration damping means . the function of the braking equipment 12 a itself corresponds with the foregoing illustrations . the advantage of this solution results from the fact that the clearance “ if ” can be executed to be smaller , since an oscillatory path of the car does not have to be taken into consideration . obviously the coupling of the guide support 17 is designed in such a manner that vertical braking and retaining forces can be transmitted . fig6 shows a schematic view of a third embodiment brake unit 12 b with a wear - compensating device and a separate guidance for the brake unit and the elevator car . the guide support 17 b is guided along the brake and guide track 7 , 8 directly by the guide shoe 9 and the car 3 is guided by own guide elements ( not illustrated ). the function of the brake equipment 12 b itself corresponds with the preceding illustrations . the advantage of this solution results from the fact that the clearance “ if ” can similarly be formed to be small , since an oscillatory path of the car 3 does not have to be taken into consideration and a design of the guide shoe 9 of the brake can be undertaken independently of the car 3 . fig7 shows a fourth of embodiment of a brake unit 12 c with wear - compensating device . the guide support 17 is fastened relative to the car 3 . the brake housing 13 is connected with the guide support 17 by way of the positioning part 31 c and a support pin 37 . the support pin 37 is analogously a part of the guide support 17 . the brake housing 13 is slidingly displaceable on the sleeve - shaped positioning part 31 c , wherein the displaceability on the positioning part 31 c is limited by a slide limitation , which can be set by means of clearance play setting screw or clearance play setting nut 36 in correspondence with the desired clearance “ if ”. the restoring unit 32 urges the brake housing 13 , when the advance device 19 is relieved , into the release position with respect to the first abutment 33 . when the wear “ v ” occurs , the positioning part 31 c can slip on the support pin 37 , which leads to a wear compensation , as analogously explained in the fig4 series . two support pin arrangements of that kind are preferably arranged one above the other , whereby braking forces are also directly transmissible . the slip connection 35 in this example of embodiment is solved in particularly economic manner . o - rings 38 are inserted in the positioning part 31 c and the positioning part 31 c is pushed by light pressure onto the support pin 37 , which is advantageously produced from metal or steel . this slip connection 38 is preferably lubricated . the definition of the required slip force takes place in co - ordination with the definition of the restoring unit . the force required for slipping lies by more than approximately 40 % above the force able to be applied by the restoring unit . instead of the illustrated slip connection 35 on a friction basis , use could also be made of detent connections . detent connections re - adjust in steps . fig8 shows the brake unit according to fig7 with an integrated holder . the guide support 17 already illustrated in fig7 is provided with the holder 18 , which directly supports the brake plates 14 , 15 during braking and thus introduces braking and holding forces into the guide support 17 . the brake housing 13 together with the wear - compensating device 30 and the entire advance device 19 is thereby loaded merely by normal forces . fig9 shows another embodiment of a brake unit with a wear - compensating device and a support pin according to the present invention . the brake housing 13 is , similarly to that shown in fig7 , connected with the guide support 17 by way of the positioning part 31 and a support pin 37 d . the support pin 37 d is analogously a part of the guide support 17 . the brake housing 13 is arranged on the sleeve - shaped positioning part 31 d to be slidingly displaceable . the displaceability on the positioning part 31 d is limited by a slide limitation , which can be set by means of clearance play setting screw or clearance play setting nut 36 in correspondence with the desired clearance “ if ”. the functionality of the slide limitation in this example is integrated in the support pin 37 d and the functionality of the slipping is integrated between brake housing 13 and the positioning part 31 d . the restoring unit 32 urges the brake housing 13 , when the advance device 19 is relieved , towards the first abutment 33 into the clearance position . when the wear “ v ” occurs , the brake housing 13 can slip on the positioning part 31 d , which leads to a wear compensation as explained analogously in the fig4 series . here , too , two support pin arrangements of that kind are preferably arranged one above the other , whereby the braking forces were transmitted directly to the guide support . with knowledge of the present invention and the illustrated variants of embodiment the elevator expert can change and combine the set forms and arrangements as desired . for example , the illustrated use of o - rings , the solution of the support pin and also the arrangement of guide elements or the use of a holder can be combined with the illustrated arrangements of wear - compensating devices . similarly , the guide shoe can be formed with use of known technologies . in particular , use can be made of a sliding guide shoe or a roller guide shoe 9 a in fig5 . the guide shoe 9 a can comprise a measuring system on the basis of which a travel speed of the braking equipment or of the car can be ascertained to generate a signal on a line 25 . this information can be used , for example , by a regulating unit of the braking equipment . in addition , a regulated clearance play setting with use of a servomotor is possible . in that case , for example , a clearance play “ if ” of the fixed brake plate side would be changed in dependence on the operational state of the elevator installation in that the clearance play setting screw 36 would be screwed in or out by means of the servomotor . in accordance with the provisions of the patent statutes , the present invention has been described in what is considered to represent its preferred embodiment . however , it should be noted that the invention can be practiced otherwise than as specifically illustrated and described without departing from its spirit or scope . | 1 |
referring to fig1 an engine 7 has a throttle body 1 having a throttle valve 2 communicated with an intake pipe 3 . in the intake system , an air cleaner 4 and intake air temperature sensor 5 are provided . the throttle body 1 is further communicated with an intake manifold 6 which is communicated with a combustion chamber of each cylinder ( not shown ) in the engine 7 . in an exhaust pipe 17 , an o 2 - sensor 13 is provided . fuel is supplied to fuel injectors 8 from a fuel tank 9 by a fuel pump 10 , and returned to the tank 9 through a passage 12 and a pressure regulator 11 which is opened by intake manifold pressure applied through a pipe 12a . an intake manifold pressure sensor 14 is provided in the throttle body 1 for detecting intake manifold pressure p . a coolant temperature sensor 16 is provided in the engine 7 for detecting of temperature of the coolant . the coolant temperature sensor 16 produces an output signal , the voltage of which is dependent on the temperature . output signals of the sensors 5 , 13 , 14 and 16 are applied to a control unit 15 for controlling fuel injectors 8 . the control unit 15 is further applied with a pulse signal from crank angle sensor ( engine speed sensor ) 18 representing engine speed n and with a signal from an idle switch 19 which is turned on when an accelerator pedal of the vehicle is released . referring to fig2 showing the control unit 15 , a fuel injection pulse width calculator 20 is applied with output signals of the intake air temperature sensor 5 , intake manifold pressure sensor 14 , coolant temperature sensor 16 , o 2 - sensor 13 and crank angle sensor 18 . the fuel injection pulse width calculator 20 calculates a basic pulse width dependent on the intake manifold pressure p and the engine speed n from sensors 14 and 18 , respectively . the basic pulse width is corrected in accordance with output signals of the coolant temperature sensor 16 intake air temperature sensor 5 and o . sub . 2 - sensor 13 to obtain an appropriate fuel injection pulse width in the engine operating condition . a fuel injection pulse width signal from the fuel injection pulse width calculator 20 is applied to fuel injectors 8 through a driver 21 to inject the fuel to operate the engine . in order to cut off the fuel at idling of the engine , a fuel cutoff control section 22 is provided in the control unit 15 . the fuel cutoff control section 22 has a fuel cutoff deciding section 23 to which output signals of the coolant temperature sensor 16 , crank angle sensor 18 and idle switch 19 are applied . the fuel cutoff deciding section 23 determines that the vehicle is under a fuel cutoff condition when an engine speed n exceeds a predetermined cutoff engine speed n c ( n ≧ n c ) while the accelerator pedal is released in the engine warmed - up state . the engine speed n and the output signal of the idle switch 19 are also supplied to an engine speed increase calculator 24 where increment δn or increasing rate of the engine speed is obtained by either of the following equations . where n e is the engine speed after a predetermined time from closing of idle switch 19 , n id is the engine speed when the idle switch is turned on , t is the elapsed time and θ is the crank angle . the output signals of the deciding section 23 and the calculator 24 are fed both to an immediate cutoff deciding section 25 and a delayed cutoff deciding section 26 to which a set delay time signal is applied from a timer 27 . an output signal from the cutoff deciding sections 25 or 26 is applied to the injection pulse width calculator 20 in order to compulsively cutoff the fuel injection . the operation of the system will be described hereinafter with reference to a flowchart shown in fig3 and to graphs shown in fig4 a to 4d . referring to fig3 at a step s101 , it is determined whether the idle switch is on or off . when the accelerator pedal is depressed for the acceleration of the vehicle , the idle switch 19 is off so that the program proceeds to a step s106 . thus , the fuel cutoff deciding section 23 determines that the engine is not under a condition for the fuel cutoff so that a fuel signal is applied to the fuel injection pulse width calculator 20 . accordingly , the injection pulse width obtained in dependence on the intake manifold pressure p and engine speed n and others is fed to the injector 8 so as to provide an appropriate air - fuel ratio in relation to the amount of intake air , in any engine operating conditions . when the accelerator pedal is released while the vehicle is driven or at a stop , idle switch is turned on . therefore , the program proceeds to a step s102 where it is determined whether engine speed n is larger than the predetermined cutoff speed n c . when the engine speed n is smaller than the speed n c ( n & lt ; n c ), the program goes to the step s106 , so that fuel injection is continued . when the acceleration pedal is suddenly released to close the throttle valve at a time t o ( fig4 a ), while the engine speed n is larger than the fuel cutoff speed n c ( n ≧ n c ) fig4 c ), the fuel cutoff deciding section 23 determines that the vehicle is under the fuel cutoff condition , thereby applying a signal to the immediate cutoff deciding section 25 and delayed cutoff deciding section 26 . in the electronic fuel injection system for an engine having a large intake manifold volume , engine torque gradually decreases as shown in fig4 b . at a step s103 , the engine speed increment δn is calculated at the engine speed increase calculator 24 and the increment δn is compared with a predetermined reference value k . the output of the calculator 24 is applied to the deciding sections 25 and 26 . when the clutch is engaged during the release of the accelerator pedal , the load of a transmission system exerted on the engine restrains the increase of the engine speed as shown in fig4 c . when the increment δn is smaller than the reference value k ( δn & lt ; k ), counting of the delay time set in the timer 27 is started . when the set time has elapsed , the program proceeds to a step 105 where a fuel cut flag fcut is set . therefore , a cutoff signal from the delayed cutoff deciding section 26 is applied to the fuel injection pulse width calculator 20 to stop the injection as shown by a dotted line in fig4 c . if the clutch is disengaged at a time t 1 immediately after the release of the accelerator pedal in order to shift the change speed gear , the remaining torque of the engine speeds up the engine as shown in fig4 d . when the engine speed increment δn becomes larger than the predetermined value k , the program proceeds directly to the step s105 . accordingly , the fuel is cutoff at a time t 2 as shown by a dotted line in fig4 d . thus , the engine speed decreases until the gear shift operation is completed at a time t 3 . when the accelerator pedal is depressed , the idle switch 19 is turned off , thereby injecting the fuel ( steps s101 , s106 ). thus , the engine speed increases in accordance with the depression of the accelerator pedal . during the cutoff of the fuel while coasting , if the engine speed n becomes lower than the predetermined cutoff speed n c , the fuel injection is restored by the signal from the fuel cutoff deciding section 23 ( steps s102 , s106 ). the system of the present invention may also be applied to an engine provided with a carburetor . in accordance with the present invention , when the clutch is disengaged in order to shift gears of the manual transmission , the speed up of the engine is prevented without fail . while the presently preferred embodiment of the present invention has been shown and described , it is to be understood that this disclosure is for the purpose of illustration and that various changes and modifications may be made without departing from the scope of the invention as set forth in the appended claims . | 5 |
the block diagram of a system for generating a periodic sequence y n is illustrated in fig1 . register 10 , in its most general form , is a parallel - in - parallel - out analog register of k stages . this is the memory of the system . the output signal of register 10 is an x n vector signal whose components denote the stages of the register at time n . the periodic sequence y . sub . n is produced by a transversal operation h ( in general , nonlinear ) on x n in h network 30 . the next state of the memory , x n + 1 , is generated in f network 20 by operating on the signal vector x n with a vector function f , and by substituting x n + 1 for x n in register 10 . the equations that mathematically describe the system of fig1 are the operator f of equation ( 1 ) may be nonlinear , although for purposes of this invention , it is restricted to have a fixed point at 0 ( i . e . f ( 0 ) = 0 ) and to be analytic in the neighborhood of 0 . for the sequence x n to be periodic , there must exist a smallest integer p such that x n + p = x n . this , of course , is one definition of periodicity . since x n + 1 = f ( x n ) by equation ( 1 ), x n + p may be rewritten as x n + p = f p ( x n ), where f p is a p - fold composition of f . this implies that x n + p = x n = f p ( x n ), or that f p = i , where i is the identity map . it can be said , therefore , that f p is p periodic , where periodicity is defined as the smallest integer p which renders f p equal to the identify map i . the linear term in the taylor expansion of f , designated l , is called the linear part of f . it can be shown that replacing f by l does not change the period of recursion , and that accordingly , nonlinearities in f cannot increase the period , or for a given period , nonlinearities in f cannot reduce the required memory . for convenience and ease of implementation , therefore , f is restricted to be a linear map l . it can also be shown that for any desired period p ( which can be represented by the canonical prime number decomposition ## equ1 ## the minimum required memory , k , is ## equ2 ## where δ = 1 if the greatest common divisor of p and 4 is equal to 2 ( designated ( p , 4 )= 2 ), and where δ = 0 otherwise . equation ( 3 ) can also be expressed as k = σk i - δ , where k i = φ ( p i . sup . α . sbsp . i ). the euler function φ ( p i . sup . α . sbsp . i ) has a value equal to the number of positive integers which are less than and relatively prime to p i . sup . α . sbsp . i . in close form , it is known that φ ( p i . sup . α . sbsp . i ) is equal to ( p i . sup .. sup . α . sbsp . i - 1 )( p - 1 ). from the above , given a period p , the minimum memory required for the implementation of the system of fig1 can be computed . table 1 depicts the required memory for periods ranging from 1 through 61 . table 2 depicts the maximum period obtainable for given memory size , ranging from k = 1 to k = 50 . table 2 is generated by searching through an expanded table 1 for the maximum period at each given memory size . for example , k = 8 in table 1 corresponds to periods 16 , 21 , 28 , 36 , 40 , 42 , and 60 . in fact , 60 is the maximum period achievable with memory k = 8 . table 1______________________________________period memory period memory1 1 31 302 1 32 163 2 33 124 2 34 165 4 35 106 2 36 87 6 37 368 4 38 189 6 39 1410 4 40 811 10 41 4012 4 42 813 12 43 4214 6 44 1215 6 45 1016 8 46 2217 16 47 4618 6 48 1019 18 49 4220 6 50 2021 8 51 1822 10 52 1423 22 53 5224 6 54 1825 20 55 1426 12 56 1027 18 57 2028 8 58 2829 28 59 5830 6 60 8 61 60______________________________________ table 2______________________________________ memory maximum period 1 2 2 6 4 12 6 30 8 60 10 120 12 210 14 420 16 840 18 1260 20 2520 24 5040 26 9240 28 13860 30 27720 32 32760 34 55440 36 65520 38 120120 40 180180 42 360360 46 720720 50 942480______________________________________ in accordance with the principles of this invention , for the generation of sequences having a period ## equ3 ## r independent subperiods must be generated and combined to form the period p ( with the only exception that r - 1 subperiods are generated when ( p , 4 )= 2 ). each subperiod i is generated with an independant register i of memory k i and an independent linear feedback network l i . if l i is chosen to have the form 0 1 . . . 0 0 0 . . . . . . . . . . . . . . . . l . sub . i = 0 0 . . . 1 0 0 ( 4 ) 0 0 . . . 0 1 0 0 0 . . . 0 0 1 β . sub . k . sbsb . i . sup . i α . sub . k . sbsb . i . sbsb . 1 . sup . i . . . β . sub . 3 . sup . i β . sub . 2 . sup . i β . sub . 1 . sup . i where x i n + 1 = l i x i n , and x i n + 1 and x i n are column vectors starting with the terms ( x i n + 1 ) k . sbsb . i and ( x i n ) k . sbsb . i and decrementing to ( x i n + 1 ) 1 and ( x i n ) 1 , respectively , the following observations can be made . a . l i represents the mapping of an x i n vector ( of a sequence of period p i . sup . α . sbsp . i ) onto an x i n + 1 vector wherein each component of x i n + 1 , except the last component , is derived from a single component of x i n . more specifically , ( x i n + 1 ) j = ( x i n ) j - 1 for all k i & gt ; j & gt ; 1 , while ( x . sup . i . sub . n . sub .+ 1 ). sub . 1 = β . sup . i . sub . 1 ( x . sup . i . sub . n ). sub . 1 + β . sup . i . sub . 2 ( x . sup . i . sub . n ). sub . 2 + β . sup . i . sub . 3 ( x . sup . i . sub . n ). sub . 3 + . . . β . sup . i . sub . k . sbsb . i ( x . sup . i . sub . n ). sub . k . sbsb . i ( 5 ) b . this choice of l i greatly simplifies the circuitry since the parallel register of fig1 can be substituted with a shift register which inherently provides the function ( x i n + 1 ) j = ( x i n ) j - 1 6 c . the ( x i n + 1 ) 1 vector component can be implemented in an l i feedback network connected to each shift register stage via a multiplication network multiplying each ( x i n ) j by a constant β i j and an addition network performing the sum in accordance with equation ( 5 ). this arrangement is illustrated in fig2 wherein the product signals β 1 j ( x 1 n ) j are summed in accordance with equation ( 5 ) and inserted into the first shift register &# 39 ; s first stage , and the product signals β i j ( x i n ) j are summed in accordance with equation ( 5 ) and inserted into the ith register &# 39 ; s first stage . it can further be shown that if the coefficients β i j are restricted to be integers then , necessary requirements on the roots of ψ ( λ ) cause the determinant l i - λi to be equal to the cyclotomic polynomial of order p i . sup . αi , i . e ., ## equ4 ## since all the coefficients of a cyclotomic polynomial of power - of - prime order are 0 or 1 , all the β &# 39 ; s are either 0 or - 1 . in fact , it can be shown that every ( p i . sup .. sup . α . sbsp . i - 1 ) th tap , viewing the shift register in the direction of signal transfer , ( left to right in fig2 ), has a multiplicative factor - 1 , or a polarity reversal , and all other taps have a multiplicative factor 0 . the above is correct for all p such that ( p , 4 )≠ 2 . if ( p , 4 ) = 2 , the canonical prime number decomposition of p must contain the factor 2 1 , in which case p can be written ## equ5 ## and only r - 1 registers are necessary for implementing the period p . the lone factor 2 may be combined with any one of the p i . sup . α . sbsp . i terms and be implemented via an l i matrix whose characteristic polynomial is a cyclotomic polynomial of order 2p . sup . α . the coefficients of a cyclotomic polynomial of order 2p . sup . α are ± 1 or 0 . as related to the hardware implementation , the particular p i . sup . α . sbsp . i chosen to be combined with the factor 2 is constructed in exactly the same manner as if it were not combined , except that in the feedback path the signal of every odd nonzero tap is multiplied by + 1 instead of - 1 . the above derived cyclotomic polynomials and the resultant cyclotomic circuits are merely a specie of a class of circuits whose characteristic functions are cyclotomic polynomials . these circuits , herein called cyclotomic circuits are circuits having a shift register of a specified number of stages , integer feedback coefficients associated with each stage and multiplying the output signal of each stage , and a nonmodulo summer responsive to the integer multiplied signals impressing its output signal onto the first stage of the shift register . cyclotomic circuits , in general , do not utilize minimum memory in their sequence generation without the above described power - of - prime decomposition . these circuits , however , have the distinct advantage over prior art circuits in that they always utilize integer coefficient factors . this allows for easy implementation and error free operation . a cyclotomic (&# 34 ; circle - dividing &# 34 ;) polynomial of order m , denoted f m ( λ ), is defined as a polynomial with integer coefficients , all of whose roots are primitive m th roots of unity ( that is , r m = 1 , and r n ≠ 1 for 0 & lt ; n & lt ; m ). from this definition , it can be explicitly determined that ## equ6 ## where the product is taken over all d &# 39 ; s occurring in the range 1 ≦ d & lt ; m , such that d and m are relatively prime . the number of d &# 39 ; s determines the degree of the f m ( λ ) polynomial . the number of d &# 39 ; s within the range is found by evaluating the euler function φ ( m ) and adding 1 to the result . the euler function φ ( m ) is defined , in fact , as an integer equal to the number of positive integers less than or equal to m and having no integer factors , other than 1 , common to m ( such integers are said to be relatively prime to m ). when m is written as a product of powers of prime ## equ7 ## it can be shown that ## equ8 ## for example , if m = 30 , φ ( m ) = 7 and thus , the number of numbers relatively prime to 30 is 7 + 1 , or 8 . indeed , the numbers that are relatively prime to 30 are 1 , 7 , 11 , 13 , 17 , 19 , 23 , and 29 . this list in fact contains exactly eight numbers . in view of equation ( 9 ), the function f m ( λ ) of equation ( 7 ) can be rewritten as ## equ9 ## for m = 30 , equation ( 11 ) can be rewritten as , ## equ10 ## note that all roots appear in complex conjugate pairs , i . e . ## equ11 ## which is the complex conjugate of ## equ12 ## conversion of equation ( 12 ) to cartesian coordinates yield f . sub . 30 ( λ ) = λ . sup . 8 + λ . sup . 7 - λ . sup . 5 - λ . sup . 4 - λ . sup . 3 + λ + 1 ( 13 ) with the expected real integer coefficients . interestingly , all the nonzero coefficients of f ( λ ) in equation ( 13 ) are either + 1 , - 1 , or zero . these coefficients correspond to the β j coefficients of equations ( 5 ) and ( 7 ). thus , an order 30 cyclotomic circuit , though not of minimum memory , can be implemented with a single shift register ( of length 8 ) and a single l i network of the type shown in fig2 . specifically , correlating equations ( 7 ) and ( 13 ), in the l 1 network of fig2 β 1 = - 1 , β 2 = 0 , β 3 = 1 , β 4 = 1 , β 5 = 1 , β 6 = 0 , β 7 = 1 and β 8 = - 1 . as illustrated by the above example , cyclotomic polynomials , happily , make very desirable characteristic polynomials because of their extreme simplicity . for example , for k & lt ; 105 , or for a k that is a product of two prime numbers , the coefficients of f ( λ ) are all 0 or ± 1 . for a k that is a power of a single prime , the coefficients are all 0 and + 1 ; and for k & lt ; 385 , the coefficients do not exceed 2 in absolute value . this means , of course , that in all cases of practical interest , the feedback coefficients of network 20 in fig1 will be 0 and ± 1 ; which means that there is either no connection , a direct connection or a negative connection . equation ( 2 ), supra , defines the operation h which transforms the multilevel vector signal x n to a multilevel scalar signal y n . the use of the h operator also allows for the shaping of nonlinearities into the output signal y n in order to satisfy other conditions , such as the fit of y n to a desired norm , the spreading of the energy of the output signal in the frequency domain , etc . periodicity of the output signal is guaranteed , of course , independent of h , by the periodicity of the sequence x n . the only requirement on h , therefore , is that it not decrease the period of the recursion . it can be shown that a sufficient condition on h for preserving the period p is that the linear part of h preserves the period of x n . it can further be shown that this condition is satisfied if h is made a function of a single output from each of the shift registers which generate the sequences of relatively prime periods . since the sequences generated by the shift registers of fig2 are relatively prime , having been designed in accordance with the prime number decomposition of the period p , the h function of fig2 need be responsive to only single outputs of each of the shift registers of fig2 to produce no reduction in the output signal &# 39 ; s period . fig3 illustrates the sequence generator of this invention for a period p = 90 . shift register 11 generates the period ( 2 )( 5 ), while shift register 12 generates the period 3 2 . the h function chosen is simply the sum function of a single output of the registers 11 and 12 . as has been indicated , supra , the utilization of only a single output from each register assures that the transversal network h will not reduce the period p . in accordance with this invention , the number of stages required for shift register 11 is ( 5 1 - 1 )( 5 - 1 ), or 4 . every 5 1 - 1 , or 1 th , tap is nonzero , and since the period has a multiplicative factor 2 , every odd nonzero tap ( counting in the direction of signal flow ) has a + 1 multiplicative factor , while every even nonzero tap has a - 1 multiplicative factor . this feedback arrangement is illustrated in fig3 with two summers ; an inverting ( polarity reversing ) summer 14 connected to taps 2 and 4 of register 11 and a noninverting summer 15 connected to taps 1 and 3 of register 11 and to the output port of summer 14 . the output signal of summer 15 is applied to the input port of register 11 . the number of stages in shift register 12 is ( 3 2 - 1 )( 3 - 1 ), or 6 , and every 3 2 - 1 , or 3 rd , tap has a - 1 multiplicative factor . accordingly , in the illustration of fig3 an inverting ( polarity reversing ) summer 16 is connected and made responsive to taps 3 and 6 of register 12 , and the output signal of summer 16 is applied to the input port of register 12 . the output signals of registers 11 and 12 are connected to analog adder 13 which combines the output signals of register 11 and 12 to develop the desired sequence of period 90 . in addition to the displayed capability of generating a signal sequence of any desirable period , it can also be shown that the apparatus of this invention may be arranged to provide both a desirable sequence period and a specific amplitude sequence . in concept , this capability is easily realizable via the h function , because with any chosen initial state for the generator , a particular sequence of period p is developed ; and from the developed sequence , the desired sequence can be derived from an h network comprising a read - only memory of large enough storage . in practice , however this brute force technique is unattractive because the resultant h network would be extremely complex , large , and expensive , and because any changes in the desired sequence would entail drastic changes in the h network . it can be shown , that even with a restricted h function which simply comprises the sum of single outputs of the independent registers in the sequence generator , an innumerable number of sequences can be generated by judiciously controlling the initial state of the sequence generator . not all possible sequences are generatable in this manner because in order to generate all sequences of length p , p ° of freedom are necessary , whereas the available memory in the sequence generator of this invention offers only k degrees of freedom . however , it can shown that for a given desired sequence w of length p , a best approximation w ( in the least square sense ) can be realized by controlling the initial conditions in the following manner . 1 . having a memory of length k , generate a set of k orthonormal unit vectors , d u , forming an orthonormal basis and defining a linear space . 2 . compute the projection of w on the space defined by the set of d u vectors by computing the normal inner products of w with each of the d u vectors , i . e ., compute & lt ; w , d u & gt ; for u = 1 , 2 . . . k . for purposes of clarity , the immediately following description depicting the generation of an orthonormal basis is limited to a period p which is a single power of a prime number , i . e ., p = q v . it has been shown , supra , that when p = q v , the l matrix has k distinct roots ρ n , where k =( q v - 1 )( q - 1 ), and that these roots are the primitive roots of unity of the cyclotomic polynomial of order q v . it can be shown that vectors generated from powers of different roots are orthogonal , i . e ., ( ρ 1 i , ρ 2 i , ρ 3 i . . . ρ p i ) is orthogonal to ( ρ 1 j , ρ 2 j , ρ 3 j . . . ρ p j ) when i ≠ j , and that the set of vectors 1 / p ( ρ 1 n , ρ 2 n , ρ 3 n . . . ρ p n ) for n = 1 , 2 , 3 , . . . k forms a valid orthonormal basis . another orthonormal basis can be derived from sequences of length p generated by inserting the following set of initial conditions in the shift register of the sequence generatorvector shiftno reg . 1 2 3 . . . k loc . ______________________________________1 1 0 0 . . . 02 0 1 0 . . . 03 0 0 1 . . . 0k 0 0 0 . . . 1______________________________________ it can be shown that this generated set of k sequences can be orthonormalized by the graham - schmitt orthonormalization procedure and that the resultant orthonormal basis b n defines the same linear space defined by the d u basis . since b n and d n define the same linear space , it can be shown that for a given desired sequence w , the best approximation sequence w can be generated by computing ## equ14 ## for purposes of illustration , the use of the above method is described for a sequence generator having a period 5 where the desired sequence is (- 5 , 0 , 4 , 2 , - 1 ). in accordance with the principles of this invention , the sequence generator of period 5 has 4 stages . the 4 initial conditions are the initial conditions , therefore , are the first k components of w , in this instance (- 5 , 0 , 4 , 2 ,). these initial conditions yield the sequence w = (- 5 , 0 , 4 , 2 , - 1 ), which in this case is exactly equal to w . the above procedure for p = q v may be generalized ## equ16 ## when it is realized that the orthonormal basis for one register generated by its ρ vectors ( which are the ( p i . sup . α . sbsp . i ) th roots of unity ) is orthogonal to the orthonormal basis for another register generated by its ρ vectors ( which are the ( p j . sup . α . sbsp . j ) th roots of unity ). similar results can be shown to be true for orthonormal bases composed of b u vectors generated in the same manner as in the p = q v case . thus , when ## equ17 ## each of the r ( or r - 1 ) registers has k i stages of memory , and r ( or r - 1 ) independent orthonormal bases must be generated , with each basis having k i vectors . the remainder of the procedure is the same as for p = q v cases . namely , compute the factors & lt ; w , b u & gt ; and construct the approximated function ## equ18 ## for example , if a sequence generator is constructed to provide a period of 12 , and if it is further desired that the output sequence be it can be shown that the generator will comprise two registers of length 2 , one ( register a ) connected to develop a period 3 and the other ( register b ) connected to develop a period 4 . the orthonormal basis of register a may be derived from the initial conditions 10 and 01 which yield the sequences from the above , the inner products & lt ; w , b u & gt ; can be computed , which when carried out , results in the above indicates that the initial condition for register a is + 2 and - 1 and the initial condition for register b is - 1 and 0 . carrying out the computation , it can be seen that in this example w is exactly equal to w . the above discussion has been limited , until now , to ideal analog shift registers , in the sense that no errors have been assumed to exist . in a physical implementation of the sequence generator of this invention , errors will be introduced by interstage transmission losses within the shift register and by gain variations in the feedback amplifier . the problems raised by the nonidealness of such practical systems are not critical in many applications , but in applications where idealness is critical a skilled artisan can easily resolve the problems associated therewith . however , for the sake of completeness , fig4 is presented to illustrate one way of overcoming the loss problem . therein , a quantizer 22 is interposed between the summing gain unit 23 and register 24 . the quantizer must be a staircase quantizer which is sensitized to resolve and quantize all the levels that are expected to be encountered in the operation of the generator . quantizer 22 may comprise , for example a plurality of voltage comparators which one input of each connected to summing unit 23 and the other input of each connected to the various desired quantizer threshold voltages . the output currents of the voltage comparators may be summed and applied to a resistor to provide the necessary staircase quantization function . it is understood , of course that the embodiments shown and disclosed herein are only illustrative of the principles of this invention , and that modifications may be implemented by those skilled in the art without departing from the spirit and scope of the invention . for example , although the virtues and advantages of the subject apparatus have been associated with analog shift registers , in any particular application where , subject to known initial conditions , the maximum value for the output sequence is known , a bank of shift registers , somewhat akin to those used by the aforementioned nakamura patent , may be used , thereby eliminating the need for a quantizer . also , although a particular signal of the disclosed embodiments has been described , it is to be understood that any avilable signal in the disclosed embodiments can serve as the output signals , since that signal would differ from the described signal only be a time delay and , possibly , by a multiplicative constant . | 7 |
referring now to the drawings , and more particularly , to fig1 and 2 , one embodiment of a collapsable table 10 , made according to the present invention is disclosed . table 10 includes a table top 20 , a pair of interlocking legs 30 and 40 , and a leg receiving block 50 , see fig2 . table top 20 includes substantially planar top surface 22 and bottom surface 24 . in the preferred embodiment , table top 20 includes a downwardly depending flange 21 about the perimeter of the table top . the depth of the flange below the undersurface of the table top is preferably equal to the combined thicknesses of the essentially flat legs 30 and 40 for storing purposes , as will hereinafter be explained . the table may be made of any of the common materials such as wood , plastics , or metals . it is also contemplated that the top surface 22 of table top 20 may be venerred , as in standard table tops . referring now to fig2 , and 4 , the leg receiving block of one preferred embodiment of the present invention may be seen to advantage . leg receiving block 50 may be round in configuration , in which case the diameter of block 50 must be slightly smaller than the central openings 31 and 41 of legs 30 and 40 , respectively , as shown in fig1 . it is an essential element of the present invention that the receiving block 50 be of lesser width than the openings in the legs for proper storage of the legs on the undersurface of the table top . block 50 includes two notches 51 which extend the complete diameter of the block and intersect one another at substantially right angles . depth of the notches should be sufficient to prevent any rotation or lateral movement of the legs in respect to the block . block 50 may be mounted to the undersurface 24 of table top 20 in the center of the undersurface by means of glue , screws , or other conventional fastening means . leg receiving block 50 may be made of any suitable material . as may be seen in fig1 and 3 legs 30 and 40 of collapsable table 10 are essentially plate like , having vertical coplanar opposing surfaces . each of the legs 30 and 40 , contain at their uppermost edge a pair of horizontally extending , rectilinear , table top contacting surfaces separated by a recede portion 32 and 42 , respectively . the recede portions are flat and extend horizontally parallel with the table top contacting surfaces . leg 30 includes a pair of oppositely disposed grooves 33 extending vertically from the center of recede portion 32 to an opening 31 located in the center of the leg . leg 30 also contains a vertical slit 35 , in alignment with grooves 33 , extending from opening 31 to a second recede portion 34 which defines two floor contacting shoes 36 and 37 . leg 40 has the same general configuration and the same dimensions as leg 30 . leg 40 includes a vertical slit 45 extending from first recede portion 42 to a centrally located opening 41 , and a pair of oppositely disposed grooves 43 extending from opening 41 to a second recede portion 44 which defines a pair of floor contacting shoes 46 and 47 . in assembling collapsable table 10 , leg 30 is lowered onto leg 40 so that the edges of the leg which define slit 35 interlockingly engage the grooves 43 of leg 40 . in the process , the edges of leg 40 defining slit 45 interlockingly engage grooves 33 of leg 30 . it will therefore be seen that legs 30 and 40 are locked together at right angles one to the other in an immovable relationship . table top 20 is then lowered onto the uppermost surfaces of legs 30 and 40 so that the horizontally extending , rectilinear , top surfaces of recede portion 32 and 42 mate with and interlockingly engage notches 51 of leg receiving block 50 . the rectilinear top edges of the legs protruding above the recede portions concurrently make flush contact with bottom surface 24 of table top 20 . the process is simply reversed for dismanteling . for storage , or for carrying , legs 30 and 40 are placed flat against one another with the planar side surfaces of the legs laying flush against one another and against the bottom surface 24 of table top 20 as may be seen to advantage in fig4 . the centrally located circular openings 31 and 41 of legs 30 and 40 respectively , encase leg receiving block 51 in a snug relationship . the uppermost surface of the outermost leg is flush with the top surface of leg receiving block 51 and depending flange 21 of table top 20 while in this stored position . referring now to fig5 and 6 , a second preferred embodiment of the present invention may be seen . the second embodiment differs from the above described embodiment primarily in the square shapes of top and legs and in the configuration of leg receiving block 50 &# 39 ; and central openings 31 &# 39 ; and 41 &# 39 ; of legs 30 &# 39 ; and 40 &# 39 ;, respectively . in the second embodiment the central leg openings and the leg receiving block are both square , the openings being slightly larger than the block for convenient storage as previously mentioned . the square configuration of the block and openings , while lacking the advantage found in the circular block and openings as previously described of storage of the legs at any angle relative to the block , does have the particular advantage of holding the legs in a secure and non rotatable position relative to the block and to the undersurface of the table top . in either embodiment , the table may include a first locking means , locking flanges 70 located on the bottom surface of receiving blocks 50 or 50 &# 39 ; as may be seen in fig4 and 6 . flanges 70 are horizontally rotatable about pins 71 , and in operation are rotated so that the undersurface of the flange comes in contact with the uppersurface of the side of a leg to hold the legs flush against the undersurface of the table top for storage and for carrying . the table may also contain a second locking means to lock the legs to the undersurface of the table top and leg receiving block to maintain the table in an assembled position . for this purpose , a flange 80 is mounted on the bottom surface of the receiving block adjacent the intersecting notches 51 as may be seen in fig2 and 6 . flange 80 is rotated to engage flange receiving slots 84 which are located adjacent to and parallel with the top surface of the first recede portion of the legs and transverse to the vertical grooves and slits of the legs as may best be seen in fig1 and 5 . having thus described in detail a preferred selection of embodiments of the present invention , it is to be appreciated and will be apparent to those skilled in the art that many physical changes could be made in the apparatus without altering the inventive concepts and principles embodied therein . the present embodiments are therefore to be considered in all respects as illustrative and not restrictive , the scope of the invention being indicated by the appended claims rather than by the foregoing description , and all changes which come within the meaning and range of equivalency of the claims are therefore to be embraced therein . | 0 |
referring now to the drawings , and more particularly to fig1 one embodiment of the line storage device in accordance with the present invention is shown and referenced generally by numeral 10 . by way of example , line storage device 10 will be described for its use with a rocket - deployed line charge system , the basic elements of which are illustrated in fig1 . however , it is to be understood that line storage device 10 can be used with any similar line charge or other deployment system having a propulsion unit tethered to a distributed and tethered set of individual masses . more generally , the present invention will also be of use in any system requiring the storage of excess line and tangle - free payout of the line as is the case with a parachute system . in terms of the illustrated line charge system , a rocket 100 has a line 102 coupled on one end thereof to an aft end of rocket 100 . the other end of line 102 is coupled to the forward end of distributed line charge 104 . briefly , line charge 104 includes a fuze or detonator 106 coupled to a plurality of distributed explosive charges 108 by means a detonating cord 110 . a substantial amount of line 102 ( e . g ., eight feet or more ) extends between rocket 100 and fuze 106 . for proper operation of line charge 104 , rocket 100 must travel down range with line 102 being paid out thereafter . payout of line 102 must be tangle - free in order to assure proper placement of line charge 104 and activation of fuze 106 . that is , if line 102 becomes entangled with itself during payout , line charge 104 may not be placed in its anticipated location . if line 102 becomes entangled with line charge 104 , failure of fuze 106 as well as inaccurate placement of line charge 104 can result . accordingly , it is necessary to store line 102 in a tangle - free fashion as well as provide for its payout in a tangle - free fashion . to achieve tangle - free storage and payout of line 102 , line storage device 10 is provided . in the embodiment illustrated in fig1 line storage device 10 is a piece or block 12 of material having a channel 14 formed in a surface 16 thereof . channel 14 is laid out in a non - overlapping zigzag pattern over the length of block 12 . laid into channel 14 is the excess amount of line 102 between rocket 100 and fuze 106 . the width w of channel 14 can be formed so that line 102 and channel 14 are in press - fit engagement . alteratively or additionally , line 102 can be secured in channel 14 by , for example , a light tacking glue ( not shown ) or by tape covering channel 14 and adhered to surface 16 . such tape can be wrapped about block 12 . the optional tape feature is illustrated in fig1 by dashed lines 18 which indicate the edges of the wrapped tape . channel 14 is accessed from either end of block 12 so that line 102 can extend from either end of block 12 . the zigzag pattern presented by channel 14 can be any nonoverlapping zigzag pattern into which line 102 can be nondestructively formed . block 12 is made from a material that supports line 102 prior to the deployment of line charge 104 and that fails or ruptures during the deployment of line charge 104 . by doing so , the present invention provides a means to absorb and release launch energy that produces a standing wave in line 102 as discussed above in the background of the invention . more specifically , when rocket 100 begins to travel down range , line 102 between rocket 100 and line storage device 10 is placed in tension by the forward momentum of rocket 100 and the resting weight of line charge 104 . as line 102 is pulled taut at block 12 by rocket 100 at one end and by line charge 104 at the other end , line 102 exerts force on each successive “ loop ” formed by channel 14 in block 12 . due to the extreme tensile force , block 12 ruptures sequentially from both ends thereof at each successive loop of channel 14 effectively paying out line 102 while insuring against entanglement and absorbing / releasing launch energy to reduce the loading imparted by the standing wave . the energy is released during the sequential rupturing of block 12 . to support line 102 prior to deployment and failure at time of deployment as described above , block 12 is made from a solid material that will rupture as line 102 achieves a threshold tension . one suitable material is polystyrene which is lightweight , inexpensive , easily formed in terms of both overall shape and channel 14 , and is readily ruptured when line 102 achieves its threshold tension . other suitable materials include plaster and low density frangible plastics such as polypropylene , acrylic , vinyl , polyvinyl chloride and cellulose acetate just to name a few . block 12 can be formed from a piece of the selected stock material or could be molded into its specific shape and size . block 12 could also be formed or molded about a pre - shaped zigzag pattern of line 102 to thereby fully encase line 102 in block 12 . if there is a substantial amount of line 102 that must be stored or if the overall size of block 12 is of concern , the present invention can be extended to store parallel layers of line 102 . for example , line storage device 20 shown in top and bottom plan view in fig2 a and 2b , respectively , creates two layers of channels for storing line 102 . however , as will be appreciated by one of ordinary skill in the art , the following two - layer description can easily be extended to three or more layers . referring simultaneously to fig2 a and 2b , block 22 has zigzag channel 24 formed in top surface 26 as illustrated in fig2 a . channel 24 terminates at a feed through hole 28 that passes through to bottom surface 27 into which zigzag channel 25 is formed as illustrated in fig2 b . since line 102 must still extend from opposing ends of block 20 , line 102 is led across block 20 by a straight channel 29 in bottom surface 27 . by using feed through hole 28 to carry line 102 to its next layer of channel , all of line 102 is kept within and protected by block 102 . alternatively , line 102 can be led outside of block 102 to the next layer . the advantages of the present invention are numerous . as purely a line storage device , the present invention provides for ease of handling excess line . as a line payout control device , the present invention ensures that no slack develops during payout of the line by holding the line in a frangible package that ruptures in accordance with the sequential storing / payout of the line . thus , line snags or entanglement during deployment of a line charge system are eliminated thereby providing a high degree of confidence in terms of line charge placement and detonation . although the invention has been described relative to a specific embodiment thereof , there are numerous variations and modifications that will be readily apparent to those skilled in the art in light of the above teachings . it is therefore to be understood that , within the scope of the appended claims , the invention may be practiced other than as specifically described . | 1 |
inbred corn line lh185 is a yellow dent corn with superior characteristics , and provides an excellent parental line in crosses for producing first generation ( f 1 hybrid corn . lh185 was developed from the single cross lh59 × lh123ht by selfing and using the pedigree system of plant breeding . selfing and selection were practiced within the above f 1 cross for seven generations in the development of lh185 . some of the criteria used to select ears in various generations include : yield , stalk quality , root quality , disease tolerance , late plant greenness , late season plant intactness , ear retention , pollen shedding ability , silking ability , and corn borer tolerance . during the development of the line , crosses were made to inbred testers for the purpose of estimating the line &# 39 ; s general and specific combining ability , and evaluations were run by the williamsburg , iowa research station . the inbred was evaluated further as a line and in numerous crosses by the williamsburg and other research stations across the corn belt . the inbred has proven to have a very good combining ability in hybrid combinations . the inbred has shown uniformity and stability for all traits , as described in the following variety description information . it has been self - pollinated and ear - rowed a sufficient number of generations , with careful attention to uniformity of plant type to ensure homozygosity and phenotypic stability . the line has been increased both by hand and sibbed in isolated fields with continued observation for uniformity . no variant traits have been observed or are expected in lh185 . inbred corn line lh185 has the following morphologic and other characteristics ( based primarily on data collected at williamsburg , iowa ): lh185 is a line developed from the parents lh59 and lh123 . lh185 as a plant resembles more closely the lh123 parent except lh185 is a shorter plant with a very low ear placement . lh185 is earlier flowering than lh123 . in hybrid combination , the ear type is somewhat like lh123 ( relatively short and girthy ). lh185 has a much greater area of adaptability than lh123 had when lh123 was used commercially . one particular agronomic trait that increases lh185 &# 39 ; s area of adaptation over lh 123 is lh 185 &# 39 ; s improved resistance to summer stalk brittling . this was a particularly limiting problem that was characteristic of lh123 in a number of hybrids . lh185 has very good general combining ability . lh185 &# 39 ; s yield to moisture ratio is improved over either parent . in the tables that follow , the traits and characteristics of inbred corn line lh185 are given in hybrid combination . the data collected on inbred corn line lh185 is presented for the key characteristics and traits . the tables present yield test information about lh185 . lh185 was tested in several hybrid combinations at numerous locations , with two or three replications per location . information about these hybrids , as compared to several check hybrids , is presented . the first pedigree listed in the comparison group is the hybrid containing lh185 . information for the pedigree includes : 2 . a mean for the percentage moisture (% m ) for the hybrid across all locations . 3 . a mean of the yield divided by the percentage moisture ( y / m ) for the hybrid across all locations . 4 . a mean of the percentage of plants with stalk lodging (% sl ) across all locations . 5 . a mean of the percentage of plants with root lodging (% rl ) across all locations . 6 . a mean of the percentage of plants with dropped ears (% de ). 7 . the number of locations indicates the locations where these hybrids were tested together . the series of hybrids listed under the hybrid containing lh185 are considered check hybrids . the check hybrids are compared to hybrids containing the inbred lh 185 . the (+) or (-) sign in front of each number in each of the columns indicates how the mean values across plots of the hybrid containing inbred lh185 compare to the check crosses . a (+) or (-) sign in front of the number indicates that the mean of the hybrid containing inbred lh185 was greater or lesser , respectively , than the mean of the check hybrid . for example , a + 4 in yield signifies that the hybrid containing inbred lh185 produced 4 bushels more corn than the check hybrid . if the value of the stalks has a (-) in front of the number 2 , for example , then the hybrid containing the inbred lh185 had 2 % less stalk lodging than the check hybrid . table 1______________________________________overall comparisons oflh185 × lh195 hybrid vs . check hybrid mean % hybrid yield % m y / m % sl % rl de______________________________________lh185 × lh195 227 20 . 95 10 . 82 1 6 0 ( at 16 loc &# 39 ; s ) as compared to : lh195 × lh212 + 7 -. 67 +. 64 - 3 + 1 0lh132 × lh212 + 16 -. 43 +. 53 - 3 + 1 0lh195 × lh59 + 14 +. 64 +. 36 - 1 + 3 0lh195 × lh184 + 14 +. 67 +. 34 - 1 + 3 0______________________________________ table 2______________________________________overall comparisons oflh185 × lh198 hybrid vs . check hybrid mean % hybrid yield % m y / m % sl % rl de______________________________________lh185 × lh198 221 20 . 54 10 . 78 1 7 0 ( at 21 loc &# 39 ; s ) as compared to : lh132 × lh82 + 29 - 1 . 34 + 2 . 02 - 1 + 1 0lh204 × lh212 + 7 -. 63 +. 65 - 2 + 2 0lh132 × lh59 + 15 -. 37 +. 92 - 1 + 2 0lh205 × lh216 + 21 -. 34 + 1 . 17 0 + 1 0lh198 × lh59 + 12 -. 04 +. 59 0 + 1 0lh198 × lh82 + 27 +. 09 + 1 . 29 - 1 - 4 0______________________________________ table 3______________________________________overall comparisons oflh185 × lh132 hybrid vs . check hybrid mean % hybrid yield % m y / m % sl % rl de______________________________________lh185 × lh132 211 21 . 42 9 . 85 1 6 0 ( at 17 loc &# 39 ; s ) as compared tolh132 × lh212 + 3 -. 86 +. 51 - 1 + 3 0lhe136 × lh82 + 22 -. 03 + 1 . 05 - 1 + 3 0lh132 × lh59 + 17 +. 44 +. 61 - 1 + 1 0lh204 × lh212 + 2 +. 91 -. 37 - 2 + 1 0______________________________________ table 4______________________________________overall comparisons oflh185 × lh74 hybrid vs . check hybrid mean % hybrid yield % m y / m % sl % rl de______________________________________lh185 × lh74 189 20 . 91 9 . 03 3 4 0 ( at 21 loc &# 39 ; s ) as compared tolh74 × lh51 + 1 - 2 . 31 +. 95 - 1 - 1 0lh216 × lh206 + 1 - 1 . 84 +. 76 + 2 0 0lh132 × lh165 + 11 - 1 . 09 +. 96 0 - 1 0lh132 × lh167 + 1 -. 34 +. 18 - 1 - 1 0lh202 × lh82 + 14 -. 08 +. 64 - 4 - 2 0______________________________________ inbred seeds of lh185 have been placed on deposit with the american type culture collection ( atcc ), rockville , md . 20852 , under deposit accession number 75618 on dec . 3 , 1993 . a plant variety protection certificate is being applied for with the united states department of agriculture . although the foregoing invention has been described in some detail by way of illustration and example for purposes of clarity and understanding , it will be obvious that certain changes and modifications may be practiced within the scope of the invention , as limited only by the scope of the appended claims . | 8 |
as hereinbefore set forth , the present invention is concerned with a process for the hydration of olefinic hydrocarbons to prepare the corresponding alcohols . the process is effected by treating an olefinic hydrocarbon containing from about 2 to about 6 carbon atoms with water in the presence of certain catalytic compositions of matter of the type hereinafter set forth in greater detail . examples of olefinic hydrocarbons which may be employed as the starting materials in the process of this invention will include ethylene , propylene , butene - 1 , butene - 2 , pentene - 1 , pentene - 2 , hexene - 1 , hexene - 2 , hexene - 3 , etc . it is also contemplated within the scope of this invention that mixtures of the aforesaid olefins such as mixtures of ethylene and propylene , propylene and butene , etc . may also be used as the starting materials . in the preferred embodiment of this invention , the olefins will comprise the off - gases from refinery operations and may include mixtures of olefins and paraffins such as ethylene / ethane or propylene / propane . the hydration of the olefins by treatment with water is effected at hydration conditions which will include operating parameters such as temperatures in the range of from about 100 ° to about 300 ° c ., pressures ranging from about 10 to about 500 pounds per square inch gauge ( psig ), liquid hourly space velocities ranging from about 0 . 1 to about 10 . 0 hrs . - 1 based upon the olefin charged , and water to hydrocarbon ratios ranging from about 10 : 1 to about 50 : 1 moles of water per mole of hydrocarbon . the catalytic composition of matter which is used to effect the hydration of the olefin will comprise an alpha - zirconium phosphate , some specific examples of these compounds including alpha - zirconium orthophosphate , alpha - zirconium metaphosphate , alpha - zirconium pyrophosphate , ortho - zirconium hypophosphate , etc . the catalytic compositions of matter comprise solids which possess a layered or sheet - type structure in which the distance between the layers may be varied depending upon the preparative techniques which are employed in forming the catalyst . various methods of preparing the catalyst may be employed including those which are well known in the art . by forming the catalyst in a layered structure and by utilizing a cross - linking agent , it is possible to obtain a catalytic composition of matter which possesses excellent thermal stability and thus may be employed to effect the desired hydration reaction at temperatures well in excess of those which have heretofore been used in hydration reactions . the process of the present invention may be effected in any suitable manner and may comprise either a batch or continuous type of operation . for example , when a batch type operation is employed , a quantity of the catalyst is placed in an appropriate apparatus such as an autoclave of the rotating , mixing or stirring type along with water in an amount sufficient to afford the desired ratio of water to hydrocarbon . the autoclave is sealed and the hydrocarbon charge comprising an olefin containing from 2 to about 6 carbon atoms along with , if so desired , a paraffin which acts as a diluent , is charged to the reactor until the desired operating pressure has been attained . in the preferred embodiment of the invention , the operating pressure is afforded by the autogeneous pressure of the olefin , if in gaseous form . however , it is also contemplated within the scope of this invention that the olefinic charge stock may afford only a partial operating pressure , the remainder being produced by the introduction of a substantially inert gas such as nitrogen , helium , argon , etc . upon attaining the desired operating pressure , the apparatus is heated to a predetermined operating temperature within the range hereinbefore set forth , higher operating temperatures being possible due to the heretofore stated thermal stability of the catalytic compositions of matter . after allowing the hydration reaction to proceed for a predetermined period of time which may range from about 0 . 5 up to about 10 hours or more in duration , the reaction time being dependent upon the operating parameters chosen , heating is discontinued . after the apparatus has returned to room temperature , the excess pressure is vented , the apparatus is opened and the reaction mixture is recovered therefrom . the liquid reaction mixture is separated from the catalyst by conventional means such as filtration , decantation , centrifugation , etc ., and subjected to conventional means of separation such as fractional distillation , whereby the desired alcohol is separated from unreacted water and / or undesirable side products which may have been formed , and recovered . it is also contemplated that the hydration reaction of the present invention may be effected in a continuous manner of operation . when such a type of operation is employed , a quantity of the catalyst is placed in an appropriate reaction apparatus which is maintained at the desired operating conditions of temperature and pressure . the olefinic charge stock and the water are continuously charged to the reactor through separate means and , after passage through the reactor for a predetermined period of time , the reactor effluent is continuously withdrawn . the effluent is then subjected to conventional means of separation whereby unreacted starting materials comprising the olefinic hydrocarbon and water are separated from the alcohol product and recycled to the reaction zone to form a portion of the feedstock , while the desired product is recovered . a continuous type of operation may be effected in any suitable manner , one type of operation comprising a fixed bed mode in which the catalytic composition of matter is positioned in the reactor as a fixed bed and the reactants are passed through said bed in either an upward or downward flow . alternatively , a moving bed type of operation may be employed in which the catalyst and the reactants are passed through the reaction zone either concurrently or countercurrently to each other . a third method of operation which may be employed comprises the slurry type of operation in which the catalytic composition of matter is charged to the reactor as a slurry in either the water or the olefinic hydrocarbon . examples of alcohols which may be produced by utilizing the process of this invention will include ethanol , isopropanol , sec - butanol , sec - pentanol and sec - hexanol . the following examples are given for purposes of illustrating the process of this invention . however , it is to be understood that these examples are given merely for purposes of illustration and that the present process is not necessarily limited thereto . isopropanol may be prepared by placing the catalytic composition of matter comprising alpha - zirconium orthophosphate in a rotating autoclave along with a sufficient amount of water necessary to maintain a ratio of 25 : 1 moles of water per mole of hydrocarbon . the autoclave may then be sealed at a 65 / 35 mixture of propylene / propane charged thereto until a pressure of 100 psig is attained . the autoclave may then be heated to a temperature of 200 ° c . and maintained thereat for a period of four hours . at the end of this period , heating may be discontinued and after the autoclave has returned to room temperature , the excess pressure may be vented . the autoclave may then be opened and the reaction mixture recovered therefrom . after separating the liquid mixture from the catalyst , the former may then be subjected to fractional distillation and the desired isopropanol may be recovered therefrom . in this example , a catalyst comprising alpha - zirconium metaphosphate may be placed in an autoclave along with water in an amount sufficient so as to maintain a mole ratio of 50 moles of water per mole of hydrocarbon which may be charged to the reactor . the autoclave may then be sealed and a mixture of butene - 2 and butane may be charged to the reactor until an initial operating pressure of 250 psig has been reached . the autoclave may then be heated to a temperature of 300 ° c . and maintained thereat for a period of four hours . at the end of this time , heating may be discontinued and , after the autoclave has reached room temperature , the excess pressure may be vented . the autoclave may then be opened and the reaction mixture recovered therefrom . after separation from the catalyst , the liquid reaction mixture may again be subjected to fractional distillation and the desired sec - butanol may be separated from water and recovered . in a manner similar to that hereinbefore set forth , alpha - zirconium pyrophosphate may be used to catalyze the hydration of pentene - 2 and hexene - 1 by treating these compounds at an elevated temperature of about 250 ° c . and a pressure of 500 psig for a period of four hours . after recovery of the liquid product and separation from the catalyst , the product may be subjected to fractional distillation and the desired sec - pentanol and sec - hexanol recovered therefrom . | 2 |
the present invention relates generally to database systems and more particularly to deletion of data from child tables with multiple parents . the following description is presented to enable one of ordinary skill in the art to make and use the invention and is provided in the context of a patent application and its requirements . various modifications to the preferred implementations and the generic principles and features described herein will be readily apparent to those skilled in the art . thus , the present invention is not intended to be limited to the implementations shown , but is to be accorded the widest scope consistent with the principles and features described herein . when running applications against data in database environments , data is oftentimes operated on as groups of related data . these groups are typically defined by how tables containing the data are related to one another . in groups of related tables , there are parent tables and child tables . parent tables are tables that are related to another table where the relationship extends from the parent to the child . fig1 illustrates a system 100 with an application 102 , a database management system ( dbms ) 104 , and a database 106 . stored in database 106 is a plurality of tables . dbms 104 is operable to control access to and manipulation of data stored in database 106 . as seen in fig1 , application 102 is in communication with dbms 104 and is submitting a query 108 against one or more of the plurality of tables stored in database 106 . query 108 may be seeking to retrieve , modify , and / or delete one or more rows from a table in database 106 . query 108 may be written in structured query language ( sql ) or other database query languages . some applications , such as archiving applications , use a parent table to qualify data in a child table in order to copy the qualified data to another storage location , then delete the archived data from the parent and child tables . in one implementation , a row of a child table is qualified by a parent table when a column in the row of the child table and a related column in a row of the parent table have the same value and the row of the parent table satisfies a query on the parent table . the query may be from an application , such as an archiving application . depicted in fig2 is an example concerning three tables , table - a 202 , table - b 204 , and table - c 206 . as seen from fig2 , table - c 206 has two parent tables , table - a 202 and table - b 204 , assume , for instance , each of the tables in fig2 includes two columns — c 1 and c 2 . assume also that column c 1 in table - a 202 is related to column c 1 in table - c 206 and that column c 2 in table - b 204 is related to column c 2 in table - c 206 . if a query requests every row in table - a 202 where c 1 = x , then each row in table - c 206 where c 1 = x is a row qualified by table - a 202 and will be returned along with each row in table - a 202 where c 1 = x . when a child table has multiple parent tables , as with table - c 206 in fig2 , a special situation arises when deleting data from the child table because the child table is qualified by different parents , i . e ., each parent qualifies a set of data in the child . data sought to be deleted by an application can be defined as the intersection of all qualified sets plus the data qualified by each parent that does not exist in the intersection . to put it another way , the data subject to deletion can be thought of as the union of all qualified sets minus any duplicates in the intersection . when deleting qualified sets of data from a child table with multiple parents , special considerations have to be made not to delete data related to one parent if the data is also related to data in another parent that is not being deleted by the application . deleting the data could lead to inconsistencies in the overall data . in addition , other applications may not be able to locate data that have been improperly deleted and consequently , inaccurate results may be returned . fig3 shows a process 300 for deleting data in a child table with a plurality of parent tables according to an implementation of the invention . at 302 , data from the child table that is qualified by each parent table is deleted . data from the child table that is qualified by only one parent table and is not related to data from any other parent table is deleted at 304 . to help illustrate , four tables , table - a 402 , table - b 404 , table - c 406 , and table - d 408 , are depicted in fig4 . as seen in fig4 , table - d 408 is a child table with three parent tables . in order to find out whether any data in child table - d 408 , which is qualified by data in at least one of the parent tables 402 - 406 that an application seeks to delete , can be safely deleted by the application without breaking any relationship to data in one of the parent tables 402 - 406 that is not sought by the application , a determination is made as to whether a set of data in child table - d 408 that is qualified by data in at least one of the parent tables 402 - 406 sought by the application , which is denoted as d ′ in fig4 , includes a subset of data qualified by each of the parent tables , table - a 402 , table - b 404 , and table - c 406 . a subset - 1 410 representing the intersection of data in child table - d 408 qualified by parent table - a 402 ( ad ′), data in child table - d 408 qualified by parent table - b 404 ( bd ′), and data in child table - d 408 qualified by parent table - c 406 ( cd ′) is depicted in fig4 . thus , subset - 1 410 includes data in child table - d 408 qualified by each of the parent tables 402 - 406 . this subset of data can be deleted from child table - d 408 because none of the data in the subset has a relationship to data in a parent table that the application is not seeking to delete . fig4 also depicts a subset - 2 412 , which represents data in child table - d 408 qualified solely by parent table - a 402 , a subset - 3 414 , which represents data in child table - d 408 qualified solely by parent table - b 404 , and a subset - 4 416 , which represents data in child table - d 408 qualified solely by parent table - c 406 . before deleting data in one of the subsets 412 - 416 , a determination is made as to whether data in the subset is related to data in one of the other parent tables not qualifying the data in the subset . in one implementation , a row in a child table is related to a row in a parent table when a column in the row of the child table and a related column in the row of the parent table have the same value . for instance , assume that each of tables 402 - 408 has three columns , c 1 , c 2 , and c 3 , and that parent table - a 402 and child table - d 408 are related by column c 1 , parent table - b 404 and child table - d 408 are related by column c 2 , and parent table - c 406 and child table - d 408 are related by column c 3 . hence , with respect to subset - 2 412 , to determine whether a row in subset - 2 412 of child table - d 408 is related to a row in parent table - b 404 or parent table - c 406 , the value in column c 2 of the row in subset - 2 412 can be compared to column c 2 values in table - b 404 to determine if there is a match , and the value in column c 3 of the row in subset - 2 412 can be compared to column c 3 values in table - c 406 to determine if there is a match . a row in subset - 2 412 can be deleted from child table - d 408 if it is not related to a row in parent table - b 404 or parent table - c 406 . a row in subset - 3 414 can be deleted from child table - d 408 if it is not related to a row in parent table - a 402 or parent table - c 406 . a row in subset - 4 416 can be deleted from child table - d 408 if it is not related to a row in parent table - a 402 or parent table - b 404 . this ensures that the data deleted from child table - d 408 data will not include data that may be accessed by another application . child table - d 408 may also have additional subsets of data ( not shown ) that are qualified by two of the parent tables 402 - 406 . these subsets of data , however , cannot be safely deleted from child table - d 408 because a row in one of these subsets of data may be related to a row in a qualifying parent table that is not being sought by the application , i . e ., the row in child table - d 408 is , for instance , qualified by a row in parent table - a 402 and a row in parent table - b 404 , and related to another row in parent table - a 402 that is a non - qualifying row ( i . e ., a row that the application is not seeking to delete ). the above methodology can be generalized to a case where a child table c ahs a set of data c ′ sought by an application and parent tables a to n . to delete data from child table c : determine ac ′, . . . , nc ′ in c ′ determine whether ac ′, . . . , nc ′ exists in c ′ delete data in ac ′, . . . , nc ′ from c delete data in nc ′ from c if it is not related to data in parent tables of c other than parent table n data is represented in tables as rows of data with columns of information . as discussed above , tables may be related to one another by specifying a column in one table and relating it to a column in another table . the relationship can be described as a tuple and represented as { a . c 1 , b . c 1 }, where a . c 1 is a column ‘ c 1 ’ in a table ‘ a ’ that is related to b . c 1 , which is a column ‘ c 1 ’ in a table ‘ b ’. fig5 illustrates an exmaple of a child table - c 506 with a parent table - a 502 and a parent table - b 504 . in the example of fig5 , a relationship exists between column ‘ a ’ in table - a 502 and column ‘ a ’ in table - c 506 , depicted as { a . a , c . a } in fig5 . a relationship also exists between column ‘ b ’ in table - b 504 and column ‘ b ’ in table - c 506 , depicted as { b . b , c . b } in fig5 . using the examples and relationship principles described above , a delete methodology can be expressed as the following : { c . a , c . b } is an element of c ′ if an only if ( a . a = c . a ) or ( b . b = c . b ) { c ′. a , c ′. b } is an element of ac ′ intersection bc ′ if an only if { ac ′. a , ac ′. b }={ bc ′. a , bc ′. b } if { c ′. a , c ′. b } is an element of ac ′ intersection bc ′, delete { c ′. a , c ′. b } from c if ({ c ′. a , c ′. b } is an element of c ′) and ({ c ′. a , c ′. b } is not an element of ac ′ intersection bc ′) and ( for every c ′. b where { a . a , c ′. a } is not an element of a or for every c ′. a where { b . b , c ′. b } is not an element of b ), delete { c ′. a , c ′. b } from c . c ′ is a set of data in child table - c 506 sought by an application . the set of data in table - c 506 sought by the application may be less than all of the data in child table - c 506 . the invention can take the form of an entirely hardware implementation , an entirely software implementation , or an implementation containing both hardware and software elements . in one aspect , the invention is implemented in software , which includes , but is not limited to , firmware , resident software , microcode , etc . furthermore , the invention can take the form of a computer program product accessible from a computer - usable or computer - readable medium providing program code for use by or in connection with a computer or any instruction execution system . for the purposes of this description , a computer - usable or computer - readable medium can be any apparatus that can contain , store , communicate , propagate , or transport the program for use by or in connection with the instruction execution system , apparatus , or device . the medium can be an electronic , magnetic , optical , electromagnetic , infrared , or semiconductor system ( or apparatus or device ) or a propagation medium . examples of a computer - readable medium include a semiconductor or solid state memory , magnetic tape , a removable computer diskette , a random access memory ( ram ), a read - only memory ( rom ), a rigid magnetic disk , and an optical disk . current examples of optical disks include dvd , compact disk — read - only memory ( cd - rom ), and compact disk — read / write ( cd - r / w ). shown in fig6 is a data processing system 600 suitable for storing and / or executing program code . data processing system 600 includes a processor 602 coupled to memory elements 604 a - b through a system bus 606 . in other implementations , data processing system 600 may include more than one processor and each processor may be coupled directly or indirectly to one or more memory elements through a system bus . memory elements 604 a - b can include local memory employed during actual execution of the program code , bulk storage , and cache memories that provide temporary storage of at least some program code in order to reduce the number of times the code must be retrieved from bulk storage during execution . as shown , input / output or i / o devices 608 a - b ( including , but not limited to , keyboards , displays , pointing devices , etc .) are coupled to data processing system 600 . i / o devices 608 a - b may be coupled to data processing system 600 directly or indirectly through intervening i / o controllers ( not shown ). in the implementation , a network adapter 610 is coupled to data processing system 600 to enable data processing system 600 to become coupled to other data processing systems or remote printers or storage devices through communication link 612 , communication link 612 can be a private or public network . modems , cable modems , and ethernet cards are just a few of the currently available types of network adapters . by performing an existence check for relationships to a parent table before deleting a row in a child table , integrity of data in the child table can be assured without having to implement rules or constraints in a database management system . in addition , the methodologies described above can be implemented independent of the database management system and only in those applications that require data consistency to be maintained . hence , all applications are not impacted as with the rules approach . further , there is no need for complex error checking , nor is there a dependency on rollback to restore previously deleted data . while various implementations for deleting data from child tables with multiple parents have been described , the technical scope of the present invention is not limited thereto . it is to be understood by those skilled in the art that various modifications or improvements can be added to the above implementations . it is apparent from the appended claims that such modified or improved implementations fall within the technical scope of the present invention | 6 |
a preferred embodiment of the present invention will be described with reference to the accompanying drawings . fig1 is a cigarette manufacturing machine comprising tobacco content control devices according to an embodiment of the present invention . in the cigarette manufacturing machine shown in fig1 cut tobacco is sucked upward through chimney 100 and adhered by suction to the lower side of perforated cigarette conveyor 103 which is located beneath suction chamber 102 . the adhered tobacco layer is transferred to the left in the drawing toward trimmer 104 . the density of the tobacco layer is measured by first radiometric density detector 106 located in the upstream side of trimmer 104 . the thickness of the cut tobacco layer is adjusted to a proper thickness by trimmer 104 . the cut tobacco layer having the proper thickness is transferred onto and rolled in cigarette paper which is fed from paper roll 108 and stacked on cloth tape 110 . the cigarette paper is glued by glue applicator 112 and the glued portions are dried by heater 114 to form a stick - like cigarette . the thus formed stick - like cigarette is transferred to the left and passed through second radiometric density detector 116 to check its density and to cut the cigarettes into the required length with cutter 118 . the cigarettes from cutter 118 are transferred to a tray by a conveyor ( not shown ). fig2 shows the construction of first radiometric density detector 106 . detector 106 mainly comprises radiation source 106a which emits radiant rays , and ionization box 106b which receives the radiant ray from radiation source 106a . radiation source 106a and ionization box 106b are spaced apart from each other by a predetermined distance . aperture windows 106c and 106d are located between ionization box 106b and radiation source 106a and serve as a radiation path . aperture windows 106c and 106d oppose each other and are spaced apart from each other by a predetermined distance . metal films 106e and 106f , preferably consisting of titanium foils , are adhered to aperture windows 106c and 106d , respectively . a channel for passing trimmed tobacco t on perforated conveyor 103 is provided between thin metal films 106e and 106f . shutter 106g is provided between radiation source 106a and aperture window 106c to prevent leakage of radiation . the operation of first radiometric density detector 106 will be described below . when shutter 106g is open , the radiant rays emitted from radiation source 106a is transmitted through thin metal film 106e of aperture window 106c and is incident on trimmed tobacco t . the radiation rays are transmitted through trimmed tobacco t in accordance with the density of tobacco t and are incident on ionization box 106b through metal film 106f of aperture window 106d . the outer periphery of ionization box 106b is maintained at a high potential by high voltage power supply 106h , so that an ionization current corresponding to the measured density of trimmed tobacco t is generated , and this current is supplied to amplifier 106i . a trimmer ( not shown ) is controlled and driven by this signal current . a detection output from first radiometric density detector 106 represents a density signal representing the density of the tobacco layer prior to formation of cigarettes . fig3 shows the construction of second radiometric density detector 116 . detector 116 is similar to that which is used on known cigarette manufacturing machines as described above and mainly comprises radiation source 116a and ionization box 116b which oppose each other and are spaced apart from each other by a predetermined distance . stick - like cigarette s is located between radiation source 116a and ionization box 116b . shutter 116c for shielding radiation rays are provided between radiation source 116a and stick - like cigarette s . in addition to radiation source 116a and ionization box 116b which are used to detect the density of stick - like cigarette s , detector 116 also includes reference object 116e , radiation source 116d , and ionization box 116f , which are used to provide a target value of the cigarette density . radiation source 116d and ionization box 116f oppose each other through reference object 116e . ionization box 116f detects the density of reference object 116e and is electrically connected through lead wires to ionization box 116b for detecting the cigarette density . the operation of the second radiometric density detector will be described below . radiation rays emitted from detector 116 are incident on stick - like cigarette s and is transmitted therethrough according to the cigarette density . the transmitted rays are incident on ionization box 116b . a negative voltage is applied by high voltage power supply to the outer periphery of ionization box 116b . when the radiation rays are incident on ionization box 116b , an ionization current is generated according to an intensity of the incident ray . the radiation rays from reference radiation source 116d are transmitted through reference object 116e and incident on ionization box 116f . a positive voltage is applied from the high voltage power supply to the outer periphery of ionization box 116f . upon reception of a radiant ray , ionization box 116f generates an ionization current corresponding to the target value . the ionization current generated upon application of the negative voltage to ionization box 116b and the ionization current generated upon application of the positive voltage to ionization box 116f are electrically coupled by the lead wires connected to the rear portions of ionization boxes 116b and 116f . a composite current is then supplied to amplifier 116g located in the upper portion of the detector . if stick - like cigarette s has the reference density , an output signal from amplifier 116g is set to zero . however , if the density of stick - like cigarette s is higher than the reference density , an output signal from amplifier 116g has a negative level ; and if the density of stick - like cigarette s is lower than the reference density , an output signal from amplifier 116g has a positive level . therefore , the output signal from amplifier 116g corresponds to a deviation in density of stick - like cigarette s from the reference density . fig4 shows a control circuit of the tobacco content control device of this embodiment . the same reference numerals as in fig1 to 3 denote the same parts in fig4 . as described above , cut tobacco t is sucked upward through chimney 100 and adhered in a stratiform on the lower side of perforated cigarette conveyor 103 which is located beneath suction chamber 102 . tobacco t is transferred in the allowed direction , and the density of the tobacco layer is detected by first radiometric density detector 106 . the radiation rays emitted from radiation source 106a provided in first radiometric density detector 106 are transmitted through tobacco t and incident on ionization box 106b . since a high voltage is applied to ionization box 106b , a small ionization current is generated thereby . the small current signal is amplified by amplifier 106i and the amplified signal is added to the reference signal from standard signal generator 200 . the sum signal is supplied to amplifier 202 . an output signal as an amplified signal from amplifier 202 is a voltage signal having a polarity and a magnitude , both of which correspond to the deviation of the density of the tobacco layer from the reference density . the cut tobacco , the density of which is detected by first radiometric density detector 106 , is transferred to the left and excessive tobacco is shaved off by trimming disc 104a . thereafter the tobacco is rolled in cigarette paper and glue is applied to the paper to form the stick - like cigarette . the density of the stick - like cigarette is measured by second radiometric density detector 116 . as described above , in second radiometric density detector 116 , radiation rays emitted from radiation source 116a are transmitted through stick - like cigarette s and incident on ionization box 116b . radiation rays emitted from radiation source 116d are transmitted through reference object 116e and are incident on ionization box 106f . the voltages having opposite polarities are applied to the outer peripheries of ionization boxes 106b and 106f , and the rear portions of these ionization boxes are electrically connected to each other . an amplified output signal from amplifier 116g serves as a voltage signal having a polarity and a magnitude , both of which represent a deviation of the measured density of stick - like cigarette s from the density of the reference object . an output signal from amplifier 116g is amplified by amplifier 204 and is integrated by integrator 222 . the integrated output signal from integrator 222 represents a sum of signals corresponding to a deviation of the measured density of the stick - like cigarette from the reference density , i . e ., the average deviation of the tobacco density . the operation terminal in the latter stage is driven such that the sum becomes zero , thereby always maintaining the density of the cigarette constant . the output signal from integrator 222 is amplified by amplifier 224 and is supplied as a second detection signal to adder 226 . the output signal from amplifier 202 is supplied to a high pass filter constituted by capacitor 251 , resistor 252 , and voltage follower 253 . the filter is provided for allowing a high frequency component of the output signal to pass therethrough and preventing a low frequency component of the output signal , which is also contained in the output signal from amplifier 204 , from passing therethrough . thus , the instantaneous change of the output signal is delivered from the high pass filter . the time constant of this filter is preferably about one minute . switch 205 is provided to inhibit the filter function during calibration . the deviation detection signal free from the dc component is amplified by amplifiers 254 and 255 , and the amplified signal is supplied to adder 226 as a first detection signal in the same manner as in the second detection signal . a sum output from adder 226 is amplified by amplifier 228 , and the amplified signal is further amplified by amplifier 230 . the output from amplifier 230 is supplied to electrohydraulic servo valve 232 . electrohydraulic servo valve 232 selectively supplies the pressurized oil from gear pump 234 to the upper and lower chambers of cylinder 236 according to the applied voltage , thereby displacing piston 238 upward or downward within cylinder 236 . the upward or downward movement of piston 238 is transmitted to trimming disc 104a of trimmer 104 through link 240 , shaft 242 , link 244 , and connecting rod 246 to move trimming disc 104a upward or downward . the position of trimming disc 104a is detected by differential transformer 248 having a primary coil , which is applied with a reference alternative voltage signal of several khz from oscillator 250 and has its center core connected to piston 238 through shaft 242 and link 240 . therefore , in response to the upward and downward movement of piston 238 , a corresponding signal appears in the secondary coil of differential transformer 248 by a mutual induction coupling , and this signal is amplified by amplifier 257 . half - wave portions of the output from amplifier 257 are dropped off to ground by switch 259 which is operate by the output signal of amplifier 250 , and the remaining half - wave portions are flattened by low pass filter 256 . an output from amplifier 258 is applied to adder 226 as a third input signal . with the above arrangement , when the sum of the first and second input signals of adder 226 is positive , that is to say , when the tobacco contents are deficient , a voltage appears at the output terminal of adder 226 . as a result , the output from amplifier 230 is increased in a positive direction , so that electrohydraulic servo valve 232 slowly changes the flow of oil to push up piston 238 , lowering trimming disk 104a through link 240 , shaft 242 , link 244 , and connecting rod 246 to increase the tobacco content . trimming disc 104a is lowered until the third signal becomes equal to the sum of the signal ( i . e ., the first signal ) from the first radiometric density detector and the signal ( i . e ., the second signal ) from the second radiometric density detector . when the tobacco contents are excessive , the polarities in the foregoing operation are inverted . the second signal generated by the above arrangement , i . e ., the signal generated by second radiometric density detector 116 is obtained by integrating a signal corresponding to the density deviation by integrator 222 . the first signal , i . e ., the signal generated by first radiometric density detector 106 is a signal corresponding to the density deviation . accordingly , when there is a difference between the first and second signals , the first signal may be dominant during a short time period , but the second signal is gradually increased by integration to a value which overwhelms the first signal . therefore , the tobacco content can be determined and controlled according to the first signal with respect to variations of a short period and according to the second signal with respect to variations of a long period . in this embodiment , first radiometric density detector 106 is arranged in the upstream side of trimmer 104 due to the following reason . in the practical control device , delay ( delay time ) td occurs from the detection by the first radiometric density detector to driving of the trimmer o the basis of the detection signal . it is therefore difficult to accurately control the tobacco content of the cigarettes due to the delay time td . in particular , in order to eliminate variations in higher frequencies , the delay time td cannot be neglected . in the cigarette manufacturing machine , the first radiometric density detector is located in the upstream side of the trimmer , so that the first detection signal can be feed forwarded and the tobacco contents of cigarettes can be controlled . however , in the feed forward control system mentioned with reference to fig1 and 4 , the tobacco content is transferred along conveyor 103 from first radiometric density detector 106 to trimming device 104 . therefore , transfer time tt is required between the tobacco content density detection performed by first radiometric density detector 106 and the trimming performed by trimming device 104 . that is , transfer time tt is the time required from the tobacco content to be transferred from detector 106 to trimming device 104 . in the case where a trimming device operates at a high speed , as in the case of this embodiment , transfer time tt is long in comparison with delay time td . transfer time tt and delay time td can be controlled by adjusting the response speed of amplifier 254 of the feed forward control system . in this case , however , amplifier 254 cannot be set at the maximum response speed , so that the frequency response characteristics are not satisfactory . in the control device of the present invention , delay circuit 400 delays the detection signal output from first radiometric density detector 106 by difference time δt such that difference time δt corresponds to the difference between transfer time tt ( i . e ., a mechanical delay ) and delay time td ( i . e ., an electrical delay ). in this manner , the transfer time required for the tobacco content to be transferred from first radiometric density detector 106 to trimming device 104 is compensated for . as a result of this compensation , only high frequency components , which are picked up from the detection signal supplied from the first radiometric density detector by use of the high pass filter and correspond to an instantaneous variation in the density of the tobacco content , are delayed by difference time δt , so that the response speed of the feed forward control system is prevented from lowering . fig5 shows an example of the construction of delay circuit 400 shown in fig4 . as is shown in fig5 delay circuit 400 operates on the basis of reference power source voltage vref and can delay a signal by maximum transfer time tt ( td = 0 ). in delay circuit 400 , the high frequency signal picked up by the high pass filter is input through input terminal 401 and its amplitude is adjusted by amplifier 402 . the amplitude - adjusted signal is supplied to analog delaying element 403 , which is a charge transfer element such as a bbd , and is then output from output terminal 404 after predetermined difference time δt . analog delaying element 403 is connected to clock 405 , and this clock 405 is connected to variable resistor circuit 406 for adjusting the signal transmitting frequency of clock 405 . therefore , the signal transmitting frequency of clock 405 is adjusted by varying the resistor of variable resistor circuit 406 , and the transfer speed controlled by analog delaying element 403 is adjusted by the clock signal supplied from clock 405 . as a result , difference time δt is adjusted . in delay circuit 400 shown in fig5 the analog signal is delayed and output as it is . however , the present invention is not limited to this . for example , the analog signal may be converted into a digital signal by means of an a / d converter before it is delayed , and the delayed digital signal may be converted again into an analog signal by means of a d / a converter . fig6 shows a drive unit for driving trimming disc 104a for controlling the thickness of the tobacco layer . referring to fig . s , piston 238 is vertically slidable in cylinder 236 which is mounted on outer casing 306 . piston 238 is pushed down when pressurized oil is introduced into cylinder chamber 236a through pipe 300 , so that the oil in cylinder chamber 236b is drained into the tank through pipe 302 and return pipe 304 . similarly , when pressurized oil is introduced into cylinder chamber 236b to push piston 238 up , the oil in opposite cylinder chamber 236a is drained into the tank through pipe 300 and return pipe 304 . the hydraulic system is kept at a predetermined oil pressure . when an oil pressure exceeding the preset pressure is applied from the gear pump , the oil pressure acts on relief valve 314 through pipe 312 , connected midway along pipe 310 between gear pump 234 and electrohydraulic servo valve 232 , and is drained through return pipe 316 and filter 308 . the pressure in the hydraulic system is controlled by pressure adjusting screw 318 . the upward and downward movement of piston 238 moves connecting rod 320 which is pivotally connected to piston 238 . the other end of connecting rod 320 is pivotally connected to link 240 , so that upward and downward movement of piston 238 causes link 240 to vertically rock along with shaft 242 . shaft 242 is axially supported by outer casing 306 . the rocking movement is transmitted by shaft 242 through link 244 which is fixed to the end of shaft 242 to vertically move connecting rod 246 which is pivotally supported at the other end of the arm . trimming disc 104a is vertically moved by the upward and downward movement of connecting rod 246 . link 330 is axially supported at the other end of shaft 242 and is rockable upon rotation of shaft 242 . link 332 is attached to link 330 and is moved vertically upward or downward by the rocking movement of link 330 . the center core of differential transformer 248 is fixed to link 332 so that the core can be vertically moved the same manner as in link 332 . for example , differential transformer 248 is adapted to produce a positive voltage when the core is moved upward and a negative voltage when the core is moved downward , in proportion to the distance of movement . in other words , differential transformer 248 generates a positive voltage when connecting rod 246 is moved upward and a negative voltage when connecting rod 246 is moved downward . motor 336 is connected to gear pump 234 through universal joint 338 . as described above , unlike the density detector utilizing air - permeability properties or an electrostatic capacitance change , the second radiometric density detector according to the present invention can generate an accurate detection signal and performs very stable measurement . a deviation of the measured value from the target value is integrated , and the integrated value is fed back to accurately control the average density of the produced cigarettes . delay ( delay time ) occurs until the trimmer is started in response to the detection signal after the signal is measured by the radiographic density detector . this delay time degrades control performance because the control system undesirably oscillates when the response time is shortened to 1 / 5 or less of the idle time as the reference for the response of the control system as a whole is increased . a device disclosed by u . s . ser . no . 705 , 877 ( japanese patent disclosure ( kokai ) no . 60 - 234574 and epc laid open publication no . 160 , 799 ) serves to improve response characteristics so as to minimize the delay time . feedforward control in the present invention is open loop control . the deviation from the target value cannot be integrated . however , the response time of the control system can be shortened to a time required for feeding the cut tobacco between the radiometric density detector as the detection terminal and the trimmer as the operation terminal . an arrangement of feedforward control is described in japanese patent publication no . 40 - 14560 , wherein pressure variations in the air chamber are converted by a bellows into variations in position , and the variations are feed forwarded by a hydraulic unit . however , precision of the signal is poor , and a satisfactory effect cannot be obtained . according to the present invention , the advantages of feedback control of the radiometric density detector , the electrohydraulic servo mechanism operated as an operation terminal with a short response time , and feed - forward control are combined to obtain an ideal control system operated at high speed in response to the detection signal . further , in the feed forward control system , the transfer time , i . e ., the time required for the density - detected tobacco content to be transferred to the trimming device is compensated for in consideration of both the mechanical and electrical time delays . as a result , the control system of the present invention operates at a high speed and with high accuracy . as a result of the above - mentioned control , the response speed of the control device is ten times as high as the control speed of the prior art control device . in addition , the irregularities of the tobacco content of cigarettes can be reduced from 2 . 5 % ( prior art ) to 1 . 8 %. in the control device shown in fig4 no delay circuit is incorporated in the feed forward control system . in this case , the irregularities of the tobacco content of cigarettes is reduced to 2 . 0 %. in view of this value , it can be understood that the present invention can remarkably reduce the irregularities of the tobacco content . therefore , the tobacco contents can be reduced by about 1 . 7 % in the present invention . as described above , a very high - speed control system can be arranged according to the present invention , and the irregularities of the tobacco content of cigarettes can also be minimized . | 8 |
in the following description , like reference characters designate like or corresponding parts throughout the several views shown in the figures . it is also understood that terms such as “ top ,” “ bottom ,” “ outward ,” “ inward ,” and the like are words of convenience and are not to be construed as limiting terms . referring to the drawings in general and fig1 in particular , it will be understood that the illustrations are for the purpose of describing the preferred embodiment of the invention and are not intended to limit the invention thereto . an infiltrated polycrystalline diamond composite tool 10 of the prior art is shown in fig1 . the infiltrated polycrystalline diamond composite tool 10 includes a plurality of uncoated diamonds 2 with an infiltrant 4 disposed between the diamonds 2 . free space 16 may exist between the uncoated diamond particles 2 . the infiltrated polycrystalline diamond composite tool 10 has a working surface 18 . depending on the intended application of the infiltrated polycrystalline diamond composite tool 10 , the working surface may be a cutting edge , an abrasive surface , or the like . the infiltrated polycrystalline diamond composite tool 10 may also include a support 6 , which generally comprises the infiltrant material . the support 6 may also include a hard material 8 , such as a carbide . the support 6 serves as a backing layer and ultimately provides a degree of support and rigidity to the infiltrated polycrystalline diamond composite tool 10 . in the prior - art infiltrated polycrystalline diamond composite tool 10 , the infiltrant 4 has partially in , filtrated most of the free space 16 between the diamonds 2 . during the formation of the infiltrated polycrystalline diamond composite tool 10 , the diamonds 2 are partially dissolved by the infiltrant 8 and subsequently precipitated , resulting in diamond - to - diamond bonding 12 and grain growth , which in turn forms a continuous polycrystalline diamond matrix 13 . because the matrix material 4 does not wet the surface of the diamonds 2 well , infiltration of the pre - form is incomplete . as a result , diamond - to - diamond bonding 12 within the infiltrated polycrystalline diamond composite tool 10 is incomplete and the polycrystalline diamond matrix 13 does not completely form . in addition , some free space 16 remains within the infiltrated polycrystalline diamond composite tool 10 . consequently , the durability of the infiltrated polycrystalline diamond composite tool 10 is limited . fig2 is a schematic representation of a coated diamond particle 20 of the present invention . the coated diamond particle 20 comprises a diamond 22 having a palladium - free wetting - enhancement coating 24 disposed on and substantially covering the outer surface of the diamond 22 . the wetting enhancement coating 24 may comprise the same material as that is later used as the infiltrant in the tool . the wetting enhancement coating 24 is preferably formed from either nickel , cobalt , iron , or combinations thereof , with cobalt being the most preferred material . the palladium - free wetting - enhancement coating 24 can be deposited directly onto the surface of the diamond 22 using vapor deposition techniques such as , but not limited to , chemical vapor deposition , physical vapor deposition , plasma assisted chemical vapor deposition , and combinations thereof . a schematic view of another coated diamond particle 30 of the present invention is shown in fig3 . the diamond 22 is coated with a palladium - free activation layer 34 and a palladium - free wetting - enhancement coating 24 to form the coated diamond particle 30 . the surface of the diamond 22 is a sensitized surface 32 , formed by treating the diamond 22 with a sensitizing agent . the sensitizing agent typically has two stable valence states , is capable of reacting with the activation layer 34 , and is stable in water . in the present invention , the surface of the diamond 22 is preferably sensitized by immersing the diamond 22 in a solution of tin dichloride ( sncl 2 ) and hydrochloric acid ( hcl ) at room temperature for approximately five minutes . other metals having two stable valence states , including manganese , iron , cobalt , nickel , copper , and cadmium , may be used as sensitizing agents as well . during sensitization , sncl 2 is physically absorbed onto the surface of the diamond 22 . following immersion , the diamond is then washed with distilled water and dried . following sensitization , the palladium - free activation layer 24 is deposited onto the sensitized surface 32 of the diamond 22 . the palladium - free activation layer 34 is preferably formed from silver , although other metals , such as copper , gold , cobalt , and platinum , may be used to form the palladium - free activation layer 34 . when silver is used to form the palladium - free activation layer 34 , the sensitized diamond 22 is immersed in a silver nitrate ( agno 3 ) solution at room temperature for approximately five minutes . tin dichloride ( sncl 2 ), which is the preferred sensitizer of the present invention , forms the species sn ( iv ) on the sensitized surface 32 of the diamond 22 , thereby preventing the oxidation of the metal activator species in the palladium - free activation layer 34 . the palladium - free activation layer 34 comprising silver is precipitated onto the diamond surface according to the reaction . to form elemental silver on the sensitized surface 32 of the diamond 22 . the palladium - free activation layer 34 comprising silver may be alternatively deposited from a colloidal suspension of silver . following precipitation of the palladium - free activation layer 34 , the diamond 22 is again washed with distilled water and dried . the palladium - free activation layer 34 formed from silver may comprise between about 0 . 01 and about 10 weight percent of the diamond particle . following deposition of the palladium - free activation layer 34 on the diamond 22 , the palladium - free wetting - enhancement coating 24 is deposited over the palladium - free activation layer 34 . the palladium - free wetting - enhancement coating 24 is preferably deposited by an electroless plating process . as described above , the palladium - free wetting - enhancement coating 24 may be comprised of the same material as the metallic infiltrant that will ultimately be used to form an infiltrated tool . the palladium - free wetting - enhancement coating 24 may be formed from either nickel , cobalt , iron , or combinations thereof , with cobalt being the preferred material . the electroless plating procedure is a simple reduction reaction , in which the cobalt ( ii ) ion from cobalt ( ii ) sulfate is reduced to elemental cobalt while dimethylamineborane ( dmab ) is oxidized to ( ch 3 ) 2 nh 2 + and b ( oh ) 3 : 3co 2 + + 3 ( ch 3 ) 2 nhbh 3 + 6h 2 o → 3co o + b + 3 ( ch 3 ) 2 nh 2 + + 2b ( oh ) 3 + 9 / 2h 2 + 3h + the reduction of cobalt continues in the presence of the reducing agent as long as the catalytic reduction of the metal is possible . in the present invention , the catalytic sites at which the electroless plating takes place are provided by first depositing the palladium - free activation layer 34 . in the absence of such catalytic sites , little if any coverage of the diamond 22 by the palladium - free wetting - enhancement coating 24 could be achieved by electroless plating . the palladium - free wetting - enhancement coating 24 may further include either phosphorus or boron . in the present invention , the palladium - free wetting - enhancement coating 24 preferably comprises cobalt and boron . boron , which is produced by the reduction of co ( ii ) by dmab , may comprise up to 30 weight percent of the palladium - free wetting - enhancement coating 24 . to achieve the optimum abrasion resistance , a palladium - free wetting - enhancement coating 24 comprising up to about 5 weight percent boron is preferred . the palladium - free wetting - enhancement coating 24 preferably has a thickness of between about 0 . 01 microns and about 5 microns . the coated diamond particles 20 , 30 of the present invention have an average diameter in the range of between about 0 . 0001 and about 1 millimeter . for use in a cutting tool , the average diameter of the coated diamond particles 20 , 30 is preferably greater than about 10 microns and less than about 100 microns , as coated diamond particles 20 , 30 in this size range provide optimal abrasion resistance for the tool . in addition to use in a cutting tool application , the coated diamond particles 20 , 30 of the present invention may be used for mesh products , such as grit for abrasives , which utilize diamond particles having an average diameter between about 10 microns and about 1 millimeter . infiltrated polycrystalline diamond composite tools of the present invention include cutting tool blanks , wire dies , drill blanks , and the like . these infiltrated polycrystalline diamond composite tools are formed from a preform that is prepared using the coated diamond particles 20 , 30 described above and a metallic infiltrant source that infiltrates the : free space 16 between the coated diamond particles 20 , 30 under the application of ; high temperature and pressure . fig4 is a schematic representation of a preform 40 of the present invention . a plurality of coated diamond particles 20 are placed in a refractory container 52 to form a bed 53 . coated diamond particles 30 , having a sensitized surface 32 , palladium - free activation layer 34 , and palladium - free wetting - enhancement coating 24 can be substituted for part or all of the coated diamond particles 20 . the refractory container 52 is formed from a refractory material , such as a ceramic or metal , having a melting temperature above that of the metallic infiltrant 44 and the temperatures used in the infiltration process . a metallic infiltrant source 54 , comprising the metallic infiltrant 44 , is placed in the refractory container 52 , such that the metallic infiltrant source 54 contacts the bed 53 of coated diamond particles 20 . preferably , the metallic infiltrant source 54 , is placed in the refractory container 52 such that the metallic infiltrant source 54 is positioned on top of and in contact with the bed 53 of coated diamond particles 20 . the metallic infiltrant 44 is substantially palladium - free and preferably comprises cobalt , although iron , nickel , and combinations of iron , nickel , and cobalt may also be used . the pre - form 40 is then heated to a temperature above the melting point of the metallic infiltrant 44 and pressure is applied to the metallic infiltrant source 54 , thereby forcing the molten metallic infiltrant 44 into the free space 16 between the coated diamond particles 20 . the preform 40 is preferably heated to a temperature between about 1300 ° c . and about 1700 ° c . pressures in the range of between about 40 kbar to about 70 kbar are applied to the preform 40 in order to achieve infiltration by the metallic infiltrant 44 . during the infiltration process , the palladium - free wetting - enhancement coating 24 melts and combines with the molten metallic infiltrant 44 . the presence of the palladium - free wetting - enhancement coating 24 on the diamonds 22 permits the molten metallic infiltrant 44 to completely wet the diamonds 22 . at the same time , the combination of molten metallic 44 and palladium - free wetting - enhancement coating 24 acts as a liquid - state sintering aid , dissolving some of the diamonds 22 . the diamonds 22 then ; re - crystallize to form a continuous polycrystalline diamond matrix 56 in which diamond - to - diamond bonding 58 between individual diamonds 22 is present . upon cooling , the combined molten metallic infiltrant 44 and palladium - free wetting - enhancement coating 24 materials resolidify to form a contiguous , fully dense metallic phase 62 ! that interpenetrates the continuous polycrystalline diamond matrix 56 , as shown in fig5 to form a fully infiltrated polycrystalline diamond composite tool blank 59 . a working surface 68 , such as a cutting edge or an abrasive surface , can then be provided to form the infiltrated polycrystalline diamond composite tool 60 . the continuous polycrystalline diamond matrix 56 formed from the diamonds 22 comprises between about 85 and about 95 volume percent of the infiltrated polycrystalline diamond composite tool 60 . the infiltrated polycrystalline diamond composite tool 60 is preferably a supported infiltrated polycrystalline diamond composite tool 60 , having an infiltrated support layer 46 , as shown in fig5 . the infiltrated support layer 46 comprises a continuous matrix formed by a plurality of hard particles 48 that is interpenetrated by the metallic infiltrant 44 . the hard material 48 is preferably tungsten carbide , although other carbides , such as silicon carbide , titanium carbide , zirconium carbide , niobium carbide , combinations thereof , and the like may be used . the supported infiltrated polycrystalline diamond composite tool 60 is formed by including particles of the hard material 48 in the metallic infiltrant source 54 that is used to assemble the preform 40 . during the infiltration process , the infiltrated support layer 46 fuses to the remainder of the infiltrated polycrystalline diamond composite tool 60 . the features of the present invention are illustrated by the following example . an activated layer of palladium was precipitated onto a first group of diamond particles . a second group of diamond particles was provided with a silver activation layer precipitated from solution . both the first and second groups of diamond particles were then electrolessly plated with a cobalt / boron coating . scanning electron microscopy ( sem ) was used to study the integrity of the cobalt / boron coatings on the two groups of particles . similarly , auger spectroscopy scans were used to investigate the continuity of the cobalt / boron coatings . a representative sem micrograph and auger spectroscopy scan obtained for the palladium - activated diamond particles are shown in fig5 and 6 , respectively . fig7 and 8 are a sem micrograph and auger spectroscopy scan , respectively , obtained for silver - activated diamond particles . there was no discernible difference in the contiguity of the cobalt / boron coatings deposited on the silver - activated particles and the contiguity of the cobalt / boron coatings deposited on the , palladium - activated particles . the integrity of the coating appears to be the same , or perhaps superior for the silver activated material . the experiment also showed no distinct difference in the apparent continuity of the coatings . polycrystalline diamond composite tools were also produced using these coated diamond particles , with no adverse sintering affects noted . abrasion tests were then conducted on these polycrystalline diamond composite tools . the tests indicated that the polycrystalline diamond composite tools of the present invention had abrasion resistances that were at least as good as those of tools made using uncoated diamond particles . while various embodiments are described herein , it will be appreciated from the specification that various combinations of elements , variations or improvements therein may be made by those skilled in the art , and are within the scope of the invention . | 8 |
the waveguide holographic telltale display 50 shown in fig1 embodies the present invention . the windshield 50 comprises bottom and top windshield singlets 52 and 54 , sandwiching the other elements , including a solar coating or holographic solar control film 64 adjacent the top singlet 54 , which is preferably a tinted singlet . a layer of polyvinyl butyral ( pvb ) 70 is adjacent the film 64 . a halfwave layer 66 is disposed adjacent the bottom singlet 52 . a hologram 62 is in turn disposed next to the layer 66 . the hologram 62 has several sections . section 62a is the telltale hologram , providing a predetermined telltale image when illuminated by the light source 56 . the telltale image conveys some predetermined message , such as a low fuel indication , a seatbelt warning , or the like . section 62b is a mirror hologram . the hologram in section 62c can be a solar control reflection hologram , or an inert film which tapers from full - thickness adjacent to hologram 62a down to zero thickness one to two inches away from hologram 62a . this tapering is to avoid any abrupt discontinuities in thickness within the two singlets that will result in objectionable seethrough distortion . hologram layer 62 can be made of one single piece of film , as described below ; otherwise , sections 62a , 62b and 62c can be made separately . the bottom windshield glass singlet 52 comprising the vehicle windshield is made of clear glass instead of the conventional tinted glass . the top glass singlet 54 can either be tinted or clear ; however , if it is clear , then some other means for blocking ir light from entering the passenger cabin , such as a dielectric or holographic ir reflecting layer , will be employed in a typical application . the light source 56 can be an incandescent bulb ( halogen or non - halogen ), a high - intensity discharge bulb , or the fiber optic output of a remotely - located incandescent or high - intensity discharge bulb . light from the source 56 is collimated by a collimating lens , a parabolic reflector , or a non - imaging reflecting concentrator cavity . the use of a non - imaging reflector is described in commonly assigned , co - pending application ser . no . 07 / 994 , 816 , filed dec . 22 , 1992 , entitled &# 34 ; linear lamp holographic trapped beam chmsl ,&# 34 ; by r . t . smith and a . daiber . this application is incorporated herein in its entirety by this reference . see also &# 34 ; the optics of non - imaging concentrators ,&# 34 ; w . t . welford and r . winston , academic , new york , 1978 , for more information on non - imaging concentrators . the collimated light is injected into the lower windshield singlet 52 by a wedged prism 60 attached to the lower singlet , or alternatively by a prismatic notch cut in the lower singlet , or by an input coupling hologram located directly above the lower singlet . fig8 shows the prism 60 in further detail . the prism 60 is a right angle prism characterized by a length dimension l , a height dimension h and a prism angle θ . if the windshield inner singlet 52 has a thickness dimension w , the prism parameters are determined as follows : light from the light source 56 is trapped inside the windshield by total internal reflection from the air / glass interface for singlet 52 . a majority of the internally trapped collimated light is confined within the clear lower glass singlet 52 by the photopolymer zero - degree reflection hologram 62b . this is mainly to avoid the light from being absorbed by the tinted upper singlet 54 and / or the dielectric / metal solar control film 64 . the zero - degree reflection hologram 62b is a mirror reflection hologram whose fringes are parallel to the hologram surface . the reflection hologram 62b need not extend across the full width of the windshield , but rather need only extend across the lateral extent of the telltale hologram layer 62a between that layer and the light source . the reflection hologram 62b is designed to reflect very efficiently ( greater than 90 %) the light incident on it at a highly off - axis angle , e . g ., in this exemplary embodiment , 48 degrees . the hologram spectral bandwidth is tailored to cover the spectral range of the desired telltale image or the spectral bandwidth of the lamp , whichever is smaller . this reflection hologram 62b reflects very strongly over the wavelength range of the telltale hologram 62a for s - polarized light , but is not as effective a reflector for p - polarized light . therefore , the s - polarized light will essentially be confined to the inner glass singlet 52 ( assuming for the moment there is no halfwave film 66 ). however , the p - polarized light will partially transmit beyond the hologram 62 , through the polyvinyl butyral ( pvb ) 70 , and be reflected either by the dielectric or holographic solar control film 64 or the outer glass / air singlet back through the telltale and / or mirror hologram layer 62 into the lower singlet 52 . in this manner , the p - polarized light is allowed to bounce back and forth on both sides of the hologram layer 62 as it propagates up the windshield glass . the s - polarized light is diffracted strongly by the telltale hologram 62a as seen in fig2 which illustrates the path of light from the light source 56 through the system of fig1 under the assumption there is no halfwave film 66 installed therein . the foregoing configuration , assuming again there is no halfwave film 66 , would cause two problems . first of all , the strongly diffracted s - polarized light from the telltale hologram 62a which is headed for the driver would reflect fairly strongly off the inner and outer glass / air interfaces ( or solar control film 64 ), creating an objectionable ghost image . secondly , since the telltale image arriving at the driver would be primarily s - polarized , when the driver puts on his s - polarized sunglasses , the telltale image will be virtually extinguished . these problems are partially solved by placing the polyvinyl alcohol ( pva ) halfwave film layer 66 between the inner glass singlet 52 and the telltale / mirror hologram layer 62 . referring now to fig3 a and 3b , and starting at the point where the light is injected into the lower singlet 52 , the p - polarized light incident on the halfwave layer 66 is flipped to s - polarization , is reflected strongly by the mirror hologram 62b , and is flipped back to p - polarized light as it passes back through the halfwave layer 66 into the lower singlet 52 . the s - polarized light ( fig3 b ) entering the lower singlet 52 gets flipped to p - polarized light as it passes through the halfwave layer 66 , and partially transmits through the telltale hologram layer 62a , where it reflects off the solar control film 64 and / or the outer glass / air interface and passes back through the hologram 62 and halfwave 66 layers where it re - enters the lower singlet 52 as s - polarized light again . s - polarized light incident on the telltale hologram 62a gets diffracted strongly toward the driver , but is flipped to p - polarization as it passes through the halfwave layer 66 . the p - polarized light reflects weakly off the inner glass / air singlet . the weakly reflected p - light gets flipped back to s - polarization before reflecting fairly strongly off the outer glass / air interface and to the driver . the net effect is to reduce the ghost image brightness . therefore , the result is a bright p - polarized image at the driver with a very weak p - polarized ghost image ( fig3 a ). the p - polarized light incident on the hologram 62a from the bottom is diffracted weakly by the hologram 62a , gets flipped back to s , reflects fairly strongly off the inner glass 52 / air interface , gets flipped back to p - polarization , reflects weakly off the outer glass / air interface , gets flipped back to s - polarization , and finally reaches the driver . the result is a weak s - polarized image with a much weaker ghost image ( fig3 b ). the halfwave film layer 66 is only a partial solution because even an ideal halfwave layer will rotate the s - polarized light totally to p - polarized light from one incident angle and one wavelength only . for a range of wavelengths , such as are generated by the light sources referred to above , the majority of light will be rotated to p but it will not be 100 %. therefore , there will be some residual s - polarized light to cause ghosting and reduced brightness with polarized sunglasses . furthermore , the lamp light incident on the halfwave layer covers a range of angles , not just one . finally there may uncertainties in the production fabrication of these halfwave layers that will cause their retardance to deviate from a perfect halfwave . the exact wavelength at which the halfwave film layer 66 is designed will depend on what lamp is used . if it is an incandescent bulb , the limiting bandwidth is the telltale bandwidth . if a telltale image covers 600 - 630 nm , then the midband wavelength would be at 615 nm , and this is the wavelength for which the halfwave layer will be designed . if an led source with a peak brightness at 660 nm is used as the light source 56 , then the halfwave layer &# 39 ; s midband wavelength is at 660 nm . fig3 a , 3b , 4a and 4b and tables 1 and 2 show a comparison in image brightness results , respectively including , and not including a halfwave layer for the example of light incident on the windshield at 72 . 8 ° in air and a telltale hologram 62a which diffracts 100 % of s - polarized light and 50 % of p - polarized light . clearly the halfwave layer improves the situation . it even slightly improves the image brightness . table 1______________________________________ s - polarization p - polarization average pol______________________________________main image 0 . 928 0 . 32 1 . 248ghost image 0 . 024 0 . 008 0 . 032main / ghost ratio 38 . 7 40 39______________________________________ table 2______________________________________ s - polarization p - polarization average pol______________________________________main image 0 . 64 0 . 464 1 . 104ghost image 0 . 083 0 . 0024 0 . 0854main / ghost ratio 7 . 71 193 . 3 12 . 9______________________________________ the p - polarized light that is incident on the telltale hologram 62a from its top side ( adjacent the outer singlet 54 ) is weakly diffracted by the hologram , is weakly reflected off the upper glass / air interface , is flipped back to s - polarization , and arrives at the driver as an extra ghost image . for the example of fig4 a and 4b , if the value of light incident on the hologram from the top side is one , then the value of light reaching the driver is 0 . 023 . this is a non - negligible ghost image . however , by the time the p - polarized light reaches the top surface of the telltale 62a it has been appreciably attenuated by the tinted upper singlet 54 and / or the solar control film 64 and the pvb 70 . therefore , there is no need for a polarizer in the light source 56 lamp to eliminate this component . fig9 is a top view of a telltale hologram exposure system 200 suitable for fabricating the telltale hologram 62a . the collimated reference beam 202 illuminates the film plate 208 ( illustrated in fig1 ), and is provided via a collimating lens 204 and spatial filter 206 . the reference beam illuminates the holographic film layer 212 through a prism liquid gate comprising prism 210 . the hologram film 212 is mounted on plate 208 which is immersed in an index matching liquid 214 within layer 216 . the object beam 210 is provided via a spatial filter 220 , a focusing lens 222 , a high gain diffusing screen 224 , an image reticle 226 , and plano - convex spherical lenses 228 and 232 . the focusing lens 222 takes the spherically diverging wave from the spatial filter 220 and focuses it to a point at the center of the aperture mask 230 , i . e ., if the high gain screen is not present . this ensures that maximum illumination is arriving at the eyebox 234 . the high gain screen 224 diffuses the light , and the image reticle 226 is a transparency mask with clear openings and opaque areas that define a telltale image . the diffuse light from the screen that exits this reticle mask 226 is focused by the two lenses 228 and 232 so that an image of the reticle mask bisects the film 212 plane . an aperture mask 230 is placed on the exiting face of the first lens 228 , and defines the size of the eyebox 234 . the outline of the aperture mask 230 is focused by the second lens 232 through the film plate to a point in space far away from the film plate ( thirty inches or more ), where the image of the aperture mask is located . this image defines the eyebox for the playback of the hologram . fig1 is a side view of the exposure system 200 of fig9 . fig1 is an expanded side view of a portion of the exposure system of fig1 . fig1 shows an expanded view of the prism 210 and film plate 208 . the object beam 218 creates an evenly illuminated image 236 that bisects the hologram film plane which can be seen from a well - defined eyebox 234 behind the hologram . when this hologram is played back in reverse in the system of fig1 the light is diffracted by the telltale hologram 62a so that a viewer located inside a well - defined eyebox in the driver &# 39 ; s head area sees a vertical telltale image 236 bisecting the plane of the windshield . outside of the hologram &# 39 ; s eyebox the driver sees nothing . dielectric / metal solar control coatings of windshields suitable for the film 64 are made by libbey owens ford ( lof ) and others . one exemplary lof coating is marketed as the &# 34 ; ez - kool &# 34 ; brand of solar control glass , lof automotive center , 35715 stanley drive , sterling heights , mich . 48312 . the mirror hologram 62b is exposed merely by roll - laminating a piece of photopolymer film onto a metal mirror ( the film has some self - adhesion ) and illuminating the film / mirror with a collimated laser beam incident at the angle which will yield the correct peak wavelength for playback . a layer of pva may need to be placed between the hologram layer and pvb to avoid plasticizers from the pvb from entering the hologram layer 62 and causing undesirable peak wavelength and spectral bandwidth changes . it makes sense that the halfwave pva layer 66 below the hologram layer 62 should also serve as the barrier layer between the hologram 62 and the pvb 70 . therefore , it might be advantageous to place the hologram layer 62 next to the underside of the upper glass singlet 54 . however , it may be difficult to bond the hologram layer 62 directly to a dielectric solar control coating 64 on the underside of the singlet 54 . a preferred alternative approach is to use a broadband ir reflective photopolymer holographic mirror to reject ir light instead of the dielectric coating , as shown in fig5 . the display 100 of fig5 comprises the inner and outer windshield singlets 102 and 104 , with the outer singlet 104 comprising tinted glass , and the inner singlet 102 of clear glass . light from the light source 106 is collimated by reflector 108 and fed into the inner singlet 102 by prism 110 , as in the embodiment of fig1 . a halfwave pva layer 114 is disposed between the hologram layer 116 and the pvb layer 112 disposed adjacent the inner singlet 102 . in fig5 the mirror hologram 116b , telltale hologram 116a , and holographic solar control mirror hologram 116c are all incorporated in one single hologram 116 layer which is attached to the inner surface of the outer glass singlet 104 by any one of a variety of adhesives and / or primers . each hologram comprising layer 116 can be fabricated by contact printing , i . e ., roll - laminating the hologram film against a rigid hologram master and illuminating with a collimated laser beam . the laser beam passes through the film , reflectively diffracts off the master and back onto the film to create the replicated hologram . in the case of the mirror reflection hologram and the solar control hologram , the master plate is a zero - degree mirror hologram , or else it can be replaced by a simple aluminum mirror . in the case of the telltale hologram , the master plate incorporates the telltale holograms in it . the holographic film is threaded onto a replication system that has three contact - copy exposure modules , one for each hologram type . once the film passes through the three exposure modules , it is uv cured and rolled onto an output spool . as an option , the roll of exposed film can be oven heated to enhance the hologram efficiency . fig6 is a graph illustrating a typical type of performance achievable with a solar control ir reflection hologram of fig5 as used in the embodiment and its advantages over a tinted windshield . as an added benefit the outer glass singlet can be made tinted if desired to increase the blockage of ir light . a cross - sectional view of the system mounted in a vehicle is shown in fig7 . the windshield 150 includes inner and outer singlets 152 and 154 . a hologram layer 156 disposed between the singlets comprises a mirror hologram 156b except in the vicinity of the telltale holograms 156a . a light source 160 , reflector 162 and prism 164 provide a means for injecting light into the windshield singlet 152 . if one desires the road glare to arrive at the driver in s - polarization instead of in p - polarization , then an additional halfwave layer would need to be placed between the hologram layer and the inner surface of the outer singlet . normally road glare is s - polarized ; therefore , polarized sunglasses are designed to absorb s and pass p . if a halfwave layer in the windshield causes the road glare to be flipped to p - polarization , it will pass through the polarized sunglasses virtually unattenuated . therefore , an additional halfwave layer could flip the polarization sense back to p - polarized light . this layer would also serve to modify the ghost image brightnesses as shown in table 3 for the example of fig4 . table 3______________________________________ s - polarization p - polarization average pol______________________________________main image 0 . 32 0 . 928 1 . 248ghost image 0 . 0415 0 . 0048 0 . 0463main / ghost ratio 7 . 71 193 . 3 27______________________________________ in either case , the thickness of the halfwave layer or layers can be gradually tapered down to zero outside of the hologram area to avoid any appreciable see - through distortion when looking through the windshield from the driver &# 39 ; s vantage point . another embodiment of the invention is shown in fig1 . in this case the layer 252 in which the light propagates toward the telltale hologram is physically separated from the windshield by an air gap g . in this case , once the light is injected into this layer 252 , it propagates up the layer by total internal reflection , and does not need a mirror reflection hologram to confine it . this greatly simplifies the design for customers who do not mind a physically separated layer from the windshield . fig1 shows the waveguide telltale hologram assembly 250 , separated by the air gap g from the inside surface of the conventional windshield 280 . the assembly 250 thus comprises a plastic light guide 252 , into which collimated light is injected from a light source 254 , reflector 256 and plastic prism 258 , in a manner similar to the light source arrangement of fig1 . the halfwave layer 260 is disposed on the surface 252a of the light guide facing the windshield 280 . the telltale hologram 262 is in turn disposed on the exterior surface of the halfwave layer 260 , between the air gap and the halfwave layer . as shown in fig1 , light from the light source propagates up the light guide by total internal reflection , until it reaches the telltale hologram and is diffracted from the hologram toward the viewer . the assembly could be secured in the position shown by various convention means , e . g ., by use of spacers and adhesives . it is understood that the above - described embodiments are merely illustrative of the possible specific embodiments which may represent principles of the present invention . for example , some applications may not require the half - wave plate , and in this case the half - wave plate may be omitted , thereby providing a simpler and cheaper display . other arrangements may readily be devised in accordance with these principles by those skilled in the art without departing from the scope and spirit of the invention . | 6 |
please refer to fig1 to fig6 , which are a structural view showing a preferred embodiment according to the present invention ; views showing states of use under a scan mode and a normal mode ; a view showing a state of use when a through - silicon - via ( tsv ) fails ; and views showing an area size and a wire length for a test tsv used as a redundant tsv . as shown in the figures , the present invention is an apparatus of three - dimensional integrated - circuit ( 3d - ic ) chip using a fault - tolerant test tsv , where a test tsv for a 3d - ic test structure is used as a redundant tsv for repairing signals of a 3d - ic chip . the present invention comprises a 3d - ic chip 1 , a tsv part 2 , two normal logic function circuits 3 and two 3d - ic test logic circuits 4 . the 3d - ic chip 1 comprises a first sub - chip 11 and a second sub - chip 12 , where the second sub - chip 12 is stacked on the first sub - chip 11 . the tsv part 2 is set between the first sub - chip 11 and the second sub - chip 12 to transfer signals between the first sub - chip 11 and the second sub - chip 12 . the tsv part 2 comprises a plurality of tsvs 21 ˜ 24 and a test tsv 25 . each of a second to a fourth tsvs 22 ˜ 24 is set with a first multiplexer 212 ˜ 214 at an input terminal . the first multiplexer 212 ˜ 214 is coupled to the input terminals of the second to the fourth tsvs 22 ˜ 24 through a shared terminal . each of a first to the fourth tsvs 21 ˜ 24 is set with a second multiplexer 221 ˜ 224 at an output terminal . the second multiplexer 221 ˜ 224 is coupled to the output terminals of the first to the fourth tsvs 21 ˜ 24 through a selecting terminal . the test tsv 25 has a third multiplexer 215 at an input terminal and a demultiplexer 225 at an output terminal . the third multiplexer 215 is coupled to the input terminal of the test tsv 25 through the shared terminal . the demultiplexer 225 is coupled to the output terminal of the test tsv 25 through the shared terminal . the test tsv 25 is used as a redundant tsv to repair signal of one of the first to the fourth tsvs 21 ˜ 24 when the one of the first to the fourth tsvs 21 ˜ 24 fails . the normal logic function circuits 3 are set in the first and the second sub - chips 11 , 12 and are connected to the first to the fourth tsvs 21 ˜ 24 , the first multiplexers 212 ˜ 214 and the second multiplexers 221 ˜ 224 , where signals are transferred through the first to the fourth tsvs 21 ˜ 24 . the 3d - ic test logic circuits 4 are set in the first and the second sub - chips 11 , 12 and are connected to the test tsv 25 with the third multiplexer 215 and the demultiplexer 225 for transferring test data between the first and the second sub - chips 11 , 12 and outputting test results through the test tsv 25 . thus , a novel apparatus of 3d - ic chip using a fault - tolerant test tsv is obtained . in fig2 , on using the present invention , the test tvs 25 provides circuit test for the 3d - ic chip 1 under a scan mode by adjusting selecting signals of the third multiplexer 215 and the demultiplexer 225 to 0 ; transferring test data between the first sub - chip 11 and the second sub - chip 12 ; and outputting test result . in fig3 , when none of the tsvs fails , the selecting signals of the first multiplexers 212 ˜ 214 and the second multiplexers 221 ˜ 224 are adjusted to 0 with the third multiplexer 215 and the demultiplexer 225 un - activated . thus , all the signals between the first and the second sub - chips 11 , 12 are normally transferred along the original paths of the tsvs 21 ˜ 24 . in fig4 , when one of the tsvs fails , such as the first tsv 21 , the selecting signals of the first multiplexers 212 ˜ 214 , the second multiplexers 221 ˜ 224 , the third multiplexer 215 and the demultiplexer 225 are adjusted to 1 so that all the signals between the first and the second sub - chips 11 , 12 are shifted to neighboring tsvs , where the signal of the failed first tsv 21 is shifted to the second tsv 22 . the test tsv 25 is used as a redundant tsv for shifting the signal of the neighboring tsv . in another word , the signal of the fourth tsv 24 is transferred through the redundant tsv so that all signals are normally transferred as are repaired . in fig5 , the present invention uses different test bandwidth ( 32 - bits , 48 - bits and 64 - bits ); and , by using the test tsv in a two - layer structure and a four - layer structure , 3 . 4 % and 4 . 1 % of the chip area can be reduced , respectively , due to no extra area occupied by redundant tsvs . traditionally , in order to achieve a certain yield of tsv , redundant tsvs are used so that the test tsv is placed at a worse position in the test wiring design ; but , in fig6 , the present invention achieves an average reduction of 21 . 8 % of the total length of the test wiring by using the test tsv . the present invention uses a test tsv , which will transfer test data for a 3d - ic chip when being operated under a scan mode , to repair another failed tsv when being operated under a normal mode . since the test tsv does not transfer signal under the normal mode , the present invention provides a structure for repairing the failed tsv without increasing the chip area . the test tsv is functioned as a redundant tsv for repairing signal . through replacing the failed tsv with the test tsv used for testing the 3d - ic chip , the chip area is not increased and the yield is improved as well . besides , the number of redundant tsvs used is apparently reduced with lowered production cost . to sum up , the present invention is an apparatus of 3d - ic chip using a fault - tolerant test tsv , where a failed tsv is repaired without increasing chip area ; a test tsv is functioned as a redundant tsv for repairing signal ; through replacing the failed tsv with the test tsv , the chip area is not increased and yield is improved as well ; and the number of redundant tsvs used is apparently reduced with lowered production cost . the preferred embodiment herein disclosed is not intended to unnecessarily limit the scope of the invention . therefore , simple modifications or variations belonging to the equivalent of the scope of the claims and the instructions disclosed herein for a patent are all within the scope of the present invention . | 6 |
the present invention relates to methods and devices for inhibition of overgrowth of vascular tissue , e . g ., fibrointimal proliferation or neointimal hyperplasia , in transplanted vascular tissue . the treatments described in the present invention occur during the surgical grafting procedure , but their effect is often not detected clinically for many months after successful completion of the surgery . the present invention also relates to revascularization procedures such as bypass grafting of the femoral artery to the popliteal artery , aortofemoral bypass grafting procedures utilizing transplanted autologous vascular tissues , such as the autologous saphenous vein . the present invention relates to a method of reducing overgrowth of vascular repair tissue , e . g ., fibrointimal proliferation or neointimal hyperplasia , in autologous coronary bypass conduit grafts , comprising the steps of : ( b ) subjecting the graft to irradiation with a dose effective for reducing fibrointimal proliferation or neointimal hyperplasia , to give a treated graft ; and in one embodiment of the method of the present invention , the coronary bypass conduit graft is removed from the long saphenous vein , the short saphenous vein , the cephalic vein , the brachiocephalic vein , or radial artery . in another embodiment of the method of the present invention , the irradiation is beta irradiation from within the lumen of the graft . in another embodiment of the method of the present invention , the irradiation is x irradiation from a micro x - ray source within the lumen of the graft . in another embodiment of the method of the present invention , the irradiation is from the gamma emitting radionuclide 125 i . in another embodiment of the method of the present invention , the mammal is a human . in another embodiment of the method of the present invention , the dose is limited to a range of between about 1 . 0 gy and about 60 . 0 gy . in another embodiment of the method of the present invention , the dose is limited to a range of between about 3 . 0 gy and about 30 . 0 gy . in another embodiment of the method of the present invention , the dose is limited to a range of between about 6 . 0 gy and about 20 . 0 gy . in another embodiment of the method of the present invention , the radiation source is 90 sr . one specific embodiment of the present invention is a method of reducing fibrointimal proliferation or neointimal hyperplasia in autologous coronary bypass vein grafts , comprising the steps of : ( a ) providing a vein harvested ex vivo from a human , said vein selected from the long saphenous vein and the short saphenous vein ; ( b ) subjecting the vein to beta irradiation from within the lumen of the vein , with a dose effective for reducing fibrointimal proliferation or neointimal hyperplasia , said dose ranging from between about 6 . 0 gy and about 20 . 0 gy of 90 sr , to give a treated vein ; and the present invention also relates to a device for irradiating ex vivo autologous coronary bypass conduit grafts of a mammal , comprising ( a ) a sterile sleeve insertable ex vivo into the lumen of the graft ; and ( b ) a radiation source capable of delivering a dose effective for reducing fibrointimal proliferation or neointimal hyperplasia in the graft , said source insertable into said sleeve for endovascular delivery of the radiation dose to the graft . in one embodiment of the device of the present invention , the coronary bypass conduit graft is removed from the long saphenous vein , the short saphenous vein , the cephalic vein , the brachiocephalic vein , or radial artery . in another embodiment of the device of the present invention , the radiation source produces beta irradiation . in another embodiment of the device of the present invention , the radiation is x rays from a micro x - ray source . in another embodiment of the device of the present invention , the radiation source is the gamma emitting radionuclide 125 i . in another embodiment of the device of the present invention , the mammal is a human . in another embodiment of the device of the present invention , the radiation source delivers a dose of between about 1 . 0 gy and about 60 . 0 gy . in another embodiment of the device of the present invention , the radiation source delivers a dose of between about 3 . 0 gy and about 30 . 0 gy . in another embodiment of the device of the present invention , the radiation source delivers a dose of between about 6 . 0 gy and about 20 . 0 gy . in another embodiment of the device of the present invention , the radiation source is 90 sr . the present invention also relates to a device for irradiating ex vivo an autologous coronary bypass vein graft in a human , comprising ( a ) a sterile sleeve insertable ex vivo into the lumen of the vein graft ; and ( b ) a radiation source capable of delivering a dose effective for reducing fibrointimal proliferation or neointimal hyperplasia in the vein graft , said source comprising radiation seeds of 90 sr , said source insertable into said sleeve for endovascular delivery of the radiation dose to the vein graft , said dose ranging from between about 6 . 0 gy and about 20 . 0 gy . the present invention also relates to a second device for irradiating ex vivo an autologous coronary bypass conduit graft of a mammal , comprising ( a ) a sterile sleeve for holding ex vivo the graft during its irradiation , wherein the sleeve is insertable ex vivo into the graft lumen ; ( b ) a radiation seed safe module attached , with or without fixed or detachable adaptor means , to the sleeve with locking or screwing means , said module containing a radiation source capable of being driven into and through the lumen of the sterile sleeve to provide endovascular delivery of a radiation dose to the graft , said radiation dose suitable for reducing fibrointimal proliferation or neointimal hyperplasia in the graft ; and ( c ) a radiation shield attached at or near the junction of the sleeve and the radiation seed safe module . in one embodiment of the second device of the present invention , the coronary bypass conduit graft is removed from the long saphenous vein , the short saphenous vein , the cephalic vein , the brachiocephalic vein , or radial artery . in another embodiment of the second device of the present invention , the radiation source produces beta irradiation . in another embodiment of the second device of the present invention , the radiation is x - rays from a micro x - ray source . in another embodiment of the second device of the present invention , the radiation comes from the gamma emitting radionuclide 125 i . in another embodiment of the second device of the present invention , the mammal is human . in another embodiment of the second device of the present invention , the radiation source comprises radiation seeds of 90 sr . in another embodiment of the second device of the present invention , the radiation dose is limited to the range between about 1 . 0 gy and about 60 . 0 gy . in another embodiment of the second device of the present invention , the radiation dose is limited to the range between about 3 . 0 gy and about 30 . 0 gy . in another embodiment of the second device of the present invention , the radiation dose is limited to the range between about 6 . 0 gy and about 20 . 0 gy . the present invention also relates to a device for beta irradiating ex vivo an autologous vein graft of a human , comprising ( a ) a sterile sleeve for holding ex vivo the graft during its irradiation , wherein the sleeve is insertable ex vivo into the graft lumen ; ( b ) a radiation seed safe module attached , with or without fixed or detachable adaptor means , to the sleeve with locking or screwing means , said module containing a radiation source comprising one or more radiation seeds of 90 sr capable of being driven into and through the lumen of the sleeve to provide endovascular delivery of a radiation dose to the graft , said radiation dose suitable for reducing fibrointimal proliferation or neointimal hyperplasia in the graft , said radiation dose between about 8 . 0 gy and about 20 . 0 gy ; and ( c ) a radiation shield attached at or near the junction of the sleeve and the radiation seed safe module . the present invention also relates to a third device for irradiating ex vivo autologous coronary bypass conduit grafts of a mammal , comprising ( a ) a sterile slender elongated means insertable ex vivo into the lumen of the graft , for the purpose of mounting and positioning the graft ; ( b ) a cylinder with one or more attached radiation sources , said elongated means with mounted graft insertable into the inside of the cylinder for exovascular delivery of the radiation dose to the graft , said radiation sources capable of delivering a dose effective for reducing fibrointimal proliferation or neointimal hyperplasia in the graft . fig1 shows schematically a sterile disposable sleeve 1 , according to a preferred embodiment of the present invention . sleeve 1 may be formed of any desired material , including plastic or other polymeric material , preferably plastic . the sleeve 1 is optionally covered with balloon 4 . the sleeve 1 without balloon varies between about 1 and about 8 mm in outer diameter . it may be inserted by the surgeon into the coronary bypass conduit , e . g ., the saphenous vein segment . the balloon 4 is placed to account for varying inner diameters of the bypass conduit lumen , in order to enhance uniform irradiation of the graft . the balloon 4 can be inflated according to the size of the graft lumen , and the pressure within the balloon can optionally be monitored with a conventional manometer . the sleeve 1 is sealed closed at one end and is open at the other so that the shielded radiation , e . g ., strontium , source can be inserted into the sleeve after the bypass conduit graft is placed upon it . the sleeve 1 can be screw - locked ( luer lok type ) if desired into a sterile 1 . 2 cm thick clear plastic “ test - tube ” structure that protects the vein during the procedure , and attenuates any beta particles that pass through the vein segment during the radiation treatment ( not shown ). optionally , the irradiation procedure can be performed with a hinged clear plastic hood 29 that attenuates beta rays , such as that exemplified in fig8 . the clear plastic hood 29 is typically at least about 1 . 2 cm thick . lumen 2 of the sleeve 1 is a hollow cavity inside of the sleeve 1 , with the purpose of providing a way to insert , inside the vein , a radiation source , such as radiation seeds , for endovascular delivery of radiation . typically lumen 2 is a cavity with a uniform inner diameter , formed , for example , by drilling at one end of an elongated means to form the sleeve 1 . placement of a graft 5 on the plastic sleeve 1 is shown schematically in fig2 a , according to a preferred embodiment of the invention . the graft is shown in cross - section . a pressure measuring device , e . g ., a manometer , is also shown for balloon 4 . it will be understood from this and other figures that the size and pressure of the balloon are adaptable to the size of the particular graft about to be reimplanted into its autologous host . alternatively , the balloon 4 may be manufactured to inflate to a predetermined external diameter and length . in some cases , a balloon is not necessary to the method and procedure of the present invention , e . g ., a solid plastic rod with lumen or cavity for radiation source may be sufficient . instead of a balloon , appropriate placement of mesh or filaments are readily employed to position the vein to receive a substantially uniform radiation dose . for example , fig2 b schematically shows , according to one embodiment of the present invention , a sterile sleeve 1 with mesh 36 bounded by a fixed collar 37 and a slidable collar 38 . to expand the mesh 36 , the slidable collar 38 is moved toward the fixed collar 37 . an illustration of an expanded mesh is schematically shown in fig2 c , according to one preferred embodiment of the present invention , with slidable collar 38 moved away from the distal end of sterile sleeve 1 . to give an example of the filaments , fig2 c schematically shows , according to one embodiment of the present invention , a sterile sleeve 1 . a radiation seed safe module 34 , depicted schematically in fig3 houses radiation seeds 8 in a detachable safe 6 , prior to endovascular delivery of the radiation seeds 8 into the lumen 2 of the sleeve 1 . see also fig2 . an end cap 7 , which can be metallic or formed of other desired material , protects handlers from unwanted irradiation when the adaptor 3 or other attachment means is removed . an internal source stop 9 prevents retraction of the radiation source , e . g ., seeds , beyond and outside of the detachable safe 6 . within the lumen 2 of the detachable safe 6 , is an outer cable sleeving 11 , and an inner cable 10 , typically epoxied . the adaptor 3 when present , may have a threaded fitting 33 for attachment to the sterile sleeve 1 , or it may lock onto the sterile sleeve 1 . there are a variety of ways to attach sleeve 1 to the detachable safe 6 . the sleeve 1 can be directly attached to the detachable safe 6 as illustrated schematically in fig7 and 8 . alternatively , the sleeve 1 can be attached to the base and pedestal 30 , to which is attached the detachable safe 6 , such that a lumen 2 forms a continuous passageway to allow insertion of radiation seeds into the lumen 2 of the sleeve 1 , as illustrated in fig4 . another means of attachment is with an adaptor 3 that is fixed or detachable , as illustrated in fig1 - 3 . the attachment means in each such situation includes , but is not limited to , any permanent or detachable fitting , such as a threaded fitting , screw lock , luer lok , luer slip , john guest ® quick disconnect fitting , keck ® connector , a barbed fitting , a flared fitting , a combination of a flared female end and male end , an asti teflon ® connector , a loose collar capable of tightening the junction when screwed tight , a keyed fitting with one or more pins , a snap lock , and the like . the radiation shield 12 can serve several other uses during the procedure . the radiation shield 12 can contain niches for thermolucent dosimeter diodes or for scintillation dosimeters ( not shown ) for the measurement of dose at the surface to provide a measure of irradiation that is transmitted through the vein . such an arrangement provides an indirect measure of the dose absorbed by the vein fig4 schematically shows a cross - section of an assembled device 13 , according to a preferred embodiment of the present invention , with its component parts . the sleeve 1 with graft 5 is shown attached to a base and pedestal 30 , with housing 12 serving as a radiation shield . base and pedestal 30 is made of any desired material . housing 12 is made of any desired material , preferably clear plastic . a tube 15 to an air inflator ( not shown ) provides means to inflate balloon 4 . on the outside of the housing 12 is the radiation safe seed module 34 with detachable safe 6 , end cap 7 , outer cable sleeving 11 , inner cable 10 and exemplary radiation seed 8 . the lumen 2 forms a continuous passageway from the distal end of the detachable safe 6 , which connects to the driver ( not shown ), through the base and pedestal 30 and into the sleeve 1 . the inner cable 10 with radiation seeds 8 at or near its tip is driven into the lumen 2 of the sleeve 1 , to deliver a radiation dose to graft 5 . typically , appropriate dosing can be achieved by one pass of the inner cable 10 with radiation seeds 8 into and out of the lumen 2 of the sleeve 1 . when dosing is complete , the inner cable 10 is withdrawn from the lumen 2 of the sleeve 1 into the lumen 2 of the detachable safe 6 . the graft at this point has been suitably irradiated and is ready for removal by the surgical staff for reimplanting in the patient . the beta source control device 16 of fig5 exemplifies an electronic apparatus for automating the methods and devices of the present invention . related afterloading devices suitable for different uses are disclosed and claimed in u . s . pat . no . 5 , 103 , 395 , herein incorporated by reference . the device 16 has the detachable safe 6 with attached cable and sheathing 20 wound around a drive cable capstand 21 , which is rotatably driven by a drive stepping motor 22 for insertion and withdrawal of radiation source ( not shown ) into the sleeve 1 with graft 5 ( not shown ). an emergency retract handle 19 provides manual control of the endovascular delivery system of the present invention . a liquid crystal display readout 17 with data entry and control panel 18 are also set forth in fig5 . the control box for driving or inserting radiation seeds into the lumen of the sleeve is set forth in fig6 . the inner cable 10 , which contains radiation seeds 8 ( shown , for example , in fig3 and 4 ) is driven by a cable driver pinion 24 and motor , into and out of the lumen 2 of the sleeve 1 ( not shown ). inner cable 10 is secured by outer cable sleeving 11 . inner cable 10 is held in place against the cable driver pinion 24 by a pinch idler 23 . pinch idler 23 rotates freely as the inner cable 10 is moved . encoder 25 monitors the position of the inner cable 10 and is part of the position control circuit . using the radiation seed safe module attached to a computer - controlled stepping motor for the purpose of pushing or driving via cable , cam or high precision gear - driven telescoping device , such as is used to telescope a cameral lens , the source train of 90 sr seeds , wire , or a single high - intensity source delivers the dose of irradiation in a more precisely controlled and more accurate manner than by manual manipulation . one illustration of this apparatus is schematically shown in fig5 and 6 . the computer - controlled stepping motor prevents undesirable irradiation occurring during extrusion and retraction of the source train , which would add a small level of dose inhomogeniety along the length of the treated vessel graft . the stepping motor may be connected to the push - rod by a cam or a inner cable 10 . the inner cable 10 is on a spool within the unit containing the drive stepping motor 12 . the outer cable sleeving 11 is uncoiled out of the motor module to be attached to the radiation seed safe module . ( the radiation seed safe module may also be kept within the central unit with only a connector at the end of the outer cable sleeving 11 ). the drive stepping motor is a high speed , high precision device to deliver the radiation dose , by driving a spool of hard metal wound about which the inner cable is coiled . the inner cable extends into the outer cable sleeving and can be optionally attached to the end of the radiation source train ( not shown ) within the radiation seed safe module . the radiation seed safe module can be made so that the inner cable connects to the source train by screw lock or permanently fixed , or other conventional attachment means . a variety of safety features are readily added to the devices of the present invention . in one model with a permanently attached radiation seed safe module , the radiation seed safe module can be machined so that the exit is smaller than the strontium seed casing so it cannot be retracted beyond the safe , e . g ., an internal source stop 9 of fig3 . an encoder monitors the position of the inner cable and is part of the position control circuit . a screw clamp at each end of the radiation seed safe module prevents the radiation source from leaving the radiation seed safe module between treatments . another interlock within the radiation seed safe module prevents accidental extrusion of the seeds until correctly connected . the drive stepping motor has a key that must be turned to the “ on ” position before it will drive the inner cable into and through the lumen of the sterile sleeve . the control panel also has a mechanical key control to prevent accidental activation of the drive stepping motor . an optional second channel in the radiation seed safe module allows the manual or automated advancement of a check cable prior to advancing the radiation seeds into and through the lumen of the sleeve . an illustration of manual control of radiation treatment in the methods and devices of the present invention is set forth in fig7 and 8 . a knob 29 for manual grasping terminates a removable plunger 26 for insertion and removal of radiation seeds 8 . detent plunger 27 and grooves 28 for distance detents locks the radiation seeds 8 at the desired position . the plunger may be removed by releasing the spring - loaded detent plunger 27 . the assembled apparatus of fig9 shows attachment of a housing 29 , and a base and pedestal 30 suitable for a desk top procedure . care in preventing overstretching of the vessel graft on the sleeve 1 with balloon 4 is readily accomplished by appropriate selection of one or more balloons from a series of graduated diameter balloons of fixed size when inflated . the selected balloon or balloons can be either a single balloon or a series of balloons . an alternative arrangement is one or more spiral balloons of appropriate size that wind around the sleeve . the balloons preferably range in size from about 15 mm maximum outer diameter to about 90 mm outer diameter , in 0 . 5 mm increments . the surgeon measures the vessel graft diameter , selects the correct size balloon , places the balloon on the sleeve 1 and then places the vessel graft on the balloon . the balloon is inflated after complete placement within the lumen or cavity of the vessel graft . thereafter the vessel graft is ready for irradiation . the goal of selecting the appropriate balloon is to distend the vessel graft to almost but no more than its normal diameter . another embodiment of the present invention covers a different class of devices that utilize radiation administered external to and outside of the vessel graft , as schematically illustrated by fig9 a , 9 b and 10 . this apparatus is a cylinder 32 , with radiation wire or linear arrays 34 of seeds placed longitudinally and in parallel to the inner central pin 31 . a cross section of cylinder 32 is set forth in fig9 b . during irradiation treatment , the vessel graft mounted on the sleeve 1 is placed inside of the cylinder 32 . in this fashion , beta or gamma irradiation can be administered from outside the vessel graft , i . e ., an exovascular delivery of a radiation dose . the vessel graft ( not shown ) is mounted on a sleeve 1 and is then protected with a sterile thin - walled plastic cylinder ( not shown ) by inserting thereon the sleeve 1 with already mounted vessel graft . once sealed in a sterile fashion within the cylinder and placed within the cylinder 32 , an optional retractable shield ( not shown ) is removed to expose the radiation source . administration of the dose to the vessel graft is achieved by a number of approaches , e . g ., 90 sr in the form of seeds , wire or foil , or transmuted red phosphorus ( 32 p ) combined with malleable thermoplastic material . several long linear sources ( wires or seeds in a row ) in the inner wall of the cylinder 32 are arranged so that a homogeneous dose distribution is achieved where the vessel graft is treated . besides the cylinder 32 with linear rows of radiation sources , other configurations for radiation delivery in the present invention readily occur to the skilled artisan . for example , a variety of chambers lined with fabricated 90 sr foil are suitable ( not shown ), including containers such as a cylinder , tube , or a box . these liners may be installed in a configuration to achieve multiple treatments , e . g ., a beta dose distribution to allow treatment of one to six vein segments . the vessel graft 5 mounted on a sleeve 1 is placed within the inside of the chamber , a sterile plastic liner placed therebetween to protect the mounted vessel graft from microbiological contamination of the chamber . the chamber , be it a cylinder , tube , or box may be hinged and the “ clam - shell or “ lid ” closed to administer the dose of therapeutic irradiation . the simplest design is a 90 sr foil - lined cylinder , sealed at one end with a thin center - post ( not shown ). thin 0 . 5 mm sterile plastic liners can be inserted onto the sleeve and over the post . over the post , the vessel graft on a sleeve with optional balloon is inserted and left in place for the length of time required to administer the desired dose . in one embodiment , a strontium source is utilized to administer a therapeutic dose of beta irradiation between about 6 . 0 to about 18 . 00 gy , preferably between about 10 . 0 to about 14 . 0 gy . a segment of saphenous vein ( usually 15 cm long but sometimes longer ) is irradiated from within the lumen of the vein via an apparatus that houses and provides endovascular delivery of 90 sr radiation sources . the sources are uncovered by a retractable shield or are protruded from a housing that serves as a radiation shield . the methods and devices of the present invention are adaptable to a variety of beta and gamma irradation sources , including , but not limited to , 90 sr , 90 y , 106 ru , 32 p , 192 ir , 125 i , 198 au , or 103 pd . one preferred radiation source is 90 sr . preferred dosage ranges are between about 1 . 0 gy and about 60 . 0 gy , preferably between about 3 . 0 gy and about 30 . 0 gy , most preferably between about 6 . 0 gy and about 20 . 0 gy . selecting the appropriate isotope and dosage is within the skill of the art . the desired exposure time is readily calculated for a given graft diameter , radioisotope , and sleeve geometry and size . the outward configuration of the radiation source is typically in the form of a seed , a piece of foil , a ring , a pin , or a rod . the selected radioactive material may be contained within glass , foil , or ceramics , or , alternatively , within a powder or liquid medium , such as microparticles in liquid suspension . when solid materials are used , the preferred outer diameter of the material is approximately 0 . 5 mm , allowing it to be inserted into the central lumen of the vein sleeve . such radioactive materials may be formed into pellets , spheres , and / or rods in order to be placed into the chamber of the treating element . various alternative treating elements may also be used to contain the radioactive material without departing from the present invention . for example , the treating elements may be toroidal , spherical , or in the form of elongated rings , and in such configurations , the radioactive material may be actually impregnated in a metal and formed into the desired shape . alternatively , a radioactive powder may be fired to fuse the material so that it may be formed into the desired shape , which may then be encapsulated in metal , such as titanium , stainless steel or silver , or in plastic , as by dipping in molten or uncured plastic . in still another embodiment , the treating elements may be formed from a ceramic material which has been dipped in a radioactive solution in a still further alternative , the treating elements may be constructed in the form of two piece hollow cylindrical capsules having a larger - diameter half with a central cavity and a smaller - diameter half also having a central cavity , the smaller half slidably received within the larger half and bonded or welded to form the capsule structure . the methods and devices of the present invention are suitable for any autologous coronary bypass conduit , provided that the bypass conduit is large enough . suitable veins and arteries include , but are not limited to the long saphenous vein , the short saphenous vein , the cephalic vein , the brachiocephalic vein , or radial artery . ex vivo irradiation of saphenous vein graft during coronary artery bypass surgery the technique of ex vivo irradiation requires few modifications from the conventional bypass coronary artery procedure . the patient is brought into the surgery room . monitors are attached and intravenous lines are started . the patient is put to sleep . once the patient is asleep , the surgeon performs a median sternotomy or in some cases a lateral mini - thoractomy . the pericardium is incised and the beating heart is exposed . canulas are positioned into the right atrium and into the aorta . the heart is stopped with cardioplege solution and the bypass perfusion pump is started to circulate blood through the body in the place of the beating heart . incisions are made on the inner aspect of one or both legs . the saphenous vein is dissected from the fatty tissues of the medial leg . the vein is checked for leaks by distending with saline or thereafter sterile fluid under pressure . branching venules are ligated and leaks are repaired . the vein is cut to a 15 cm length . after the vein is resected , inspected , and repaired , a radiation treatment sleeve is selected by the surgeon based upon the diameter of the saphenous vein when it was filled with blood when still in the patient &# 39 ; s leg . after the correct sleeve is selected , it is placed into the lumen of the graft so that the vein is “ impaled ” upon the sleeve . then , the sleeve mounted with saphenous vein is attached via adaptor to the base and pedestal with clear plastic hood . then , a detachable safe ( containing radiation seeds ) with mechanical or automated control units is attached via adaptor to the sleeve mounted with saphenous vein . a treatment time and treatment plan are selected from an atlas or devised upon a miniature treatment planning computer for a treatment upon the size of the treatment sleeve . then , after the clear plastic hood is lowered , radiation seeds of 90 sr are placed by remote control into the sleeve mounted with saphenous vein , and thus in effect into the lumen of the saphenous vein graft segment . a dose of 20 . 0 gy is administered . the radiation seeds are then withdrawn by remote control from the lumen of the saphenous vein graft segment . the vein is removed from the sleeve and handed to the surgeon . then , one end of the vein is sewn to an incision into the aorta and the other end is sewn to the coronary artery just beyond an angiographically detected blockage of the artery . this procedure is repeated until all coronary arteries with significant blockages are bypassed , so that blood coming through the saphenous vein graft from the aorta to the coronary artery bypasses the blocked or occluded areas to perfuse the heart muscle . then , the heart beat is restarted , the perfusion pump is removed , the patient &# 39 ; s heart begins to circulate his own blood . chest tubes are placed through the chest wall to drain any blood into the thoracic cavity to a sealed collecting system outside of the patient . the chest incision is then closed with sternal wires and with sutures . the patient is taken the cardiovascular intensive care unit and allowed to awaken . while the foregoing specification teaches the principles of the present invention , with examples provided for the purpose of illustration , it will be understood that the practice of the invention encompasses all of the usual variations , adaptations , modifications or deletions as come within the scope of the following claims and its equivalents . | 0 |
in a rabbit model of chf obtained by rapid ventricular pacing , we previously demonstrated that caspase - 3 activation is associated with a reduction in contractile force of failing myocytes . using in vivo transcoronary adenovirus - mediated gene delivery of the potent caspase inhibitor p35 , we could correct caspase - 3 activation in failing myocardium with a positive impact on sarcomeric organization and contractile performance ( laugwitz et al ., 2001 ). the beneficial effect was observed at the level of the intact heart in vivo , but also at the level of single cells isolated from in vivo ad - p35 - infected myocardium . therefore , extranuclear , cytosolic mechanisms independent of the execution of nuclear apoptosis must have mainly accounted for the negative effects of caspase - 3 activation in heart failure . to better understand the mechanism that may cause cytosolic caspase - 3 - mediated sarcomeric disarray , we performed a screening for caspase - 3 interacting proteins expressed in the heart . we employed a modified yeast two - hybrid system utilizing , as bait vector , the plasmid pbtm - casp3 - p12p17 m , which has already been succesfully used to identify gelsolin as a substrate for caspase - 3 ( kamada et al ., 1998 ). both large ( p17 ) and small ( p12 ) subunits of active caspase - 3 were separately expressed in yeast at equimolar ratios under adh1 promoters . the small subunit was fused to the lexa dna - binding domain , and a point mutation in the active site of the enzyme ( cys - 163 to ser ) prevented proteolytic cleavage of interacting substrates . the bait plasmid was cotransfected into yeast with a human heart cdna expression library fused to the gal4 activation domain . by screening 30 millions transformants , we obtained 125 positive clones which were divided into 22 groups on the base of inserted fragment size and restriction enzyme digestion pattern . dna sequencing analysis showed that six of the positive clones encoded overlapping c - terminal parts ( clone # 7 , # 12 , and # 20 ) or the complete sequence ( clones # 3 , # 9 , and # 17 ) of vmlc1 . mlc1 is one of the six polypeptide chains of the myosin molecule , and is proposed to function as an actin / myosin tether regulating cross - bridge cycling events ( morano , 1999 ). in this study we further analysed the vmlc1 clones , and the others will be described elsewhere . to examine cleavage of vmlc1 candidates by caspase - 3 in vitro , proteins encoded by the cdnas were produced by in vitro transcription / translation - reaction . as shown in fig1 a , clones # 3 , # 9 and # 17 , which contained the complete sequence of human vmlc1 , were cleaved by human recombinant active caspase - 3 , and this cleavage was blocked in the presence of its tetrapeptide inhibitor devd - fmk , suggesting that vmlc1 is a substrate for caspase - 3 . immunoblot analysis of protein extracts from left ventricle , incubated with active caspase - 3 , confirmed this result ( fig1 b ). a ˜ 20 kd cleavage product for vmlc1 was already evident with 5 ng / μl active caspase - 3 . indeed , other structurally related sarcomeric proteins , ventricular regulatory myosin light chain ( vmlc2 ), or β myosin heavy chain , were not cleaved , demonstrating that cleavage of vmlc1 was not due to a generalized degradation of proteins ( fig1 c ). to determine caspase - 3 cleavage site of vmlc1 , purified human vmlc1 was incubated with recombinant active enzyme ( fig2 a ). cleavage of purified vmlc1 resulted in two fragments at ˜ 20 kd and ˜ 5 kd . edman sequence analysis of the cleavage products revealed that caspase - 3 cleaved vmlc1 at e 135 of the c - terminal motif dfve 135 g , which is highly conserved ( fig2 b ). this result was confirmed by immunoblot analysis , using a monoclonal antibody for vmlc1 ( clone f 109 . 16 a 12 ) directed against the sequence v 134 eglrv 139 at the caspase - 3 cleavage site . the antibody detected the intact vmlc1 protein but did not detect either of the two cleavage fragments ( data not shown ). the mapped cleavage site corresponds to the caspase - 3 consensus sequence dxxd ( cohen , 1997 ) with exception of substituting the last aspartate residue for the similar acidic glutamate residue at position 135 . recently , cleavage of lens connexin 45 . 6 by caspase - 3 has also been identified at the e 367 residue of deve 367 g ( yin et al ., 2001 ). an extensive screening of several databases did not , however , show any other known substrate of caspase - 3 to be cleaved at the same , atypical cleavage site ( motif dfve ). to determine the functional relevance of vmlc1 cleavage by caspase - 3 in the heart in vivo , we investigated the evidence of vmlc1 cleavage products in extracts from rabbit failing ventricular myocardium , where we have previously documented a ˜ 6 - fold increase in caspase - 3 activity ( laugwitz et al ., 2001 ). as shown in fig3 a , the intact vmlc1 protein of ˜ 27 kd was relatively stable in healthy control hearts . in contrast , a main ˜ 20 kd fragment , corresponding to the n - terminal cleavage product , was present in failing myocardium . myosin is the major component of the thick filaments of sarcomeres , and consists of two heavy chains ( α and β ), each associated with two types of light chains , the essential ( mlc1 ) and the regulatory ( mlc2 ). x - ray crystallographic analyses demonstrated that essential and regulatory myosin light chains are spatially close , and are both associated with the neck region of the myosin heavy chain globular head ( rayment et al ., 1993 ). to examine whether in failing myocytes a morphological disruption of the organized vmlc1 staining of a - bands in sarcomeres occurred and whether it correlated with caspase - 3 activation , single cardiomyocytes from control and chf hearts were isolated . fig3 b shows confocal laser scanning microscopy of isolated ventricular myocytes after staining for activated caspase - 3 and immunostaining for vmlc1 or vmlc2 . in cardiomyocytes isolated from control hearts , there was no evidence of caspase - 3 activation , and both myosin light chains appeared organized in the sarcomeric units ( fig3 b , panels a - b and e - f ). in contrast , failing myocytes with activated caspase - 3 presented a loss of the characteristic localization of vmlc1 in sarcomeres , and the a - band vmlc2 staining , which was maintained , showed a reduced sarcomeric organization compared to that of control cells ( fig3 b , panels c - d and g - h ). sarcomeric disarray in failing cells presenting caspase - 3 activation was confirmed by phalloidin staining , which visualizes actin filaments ( fig3 b , panels k - l ). single - cell shortening experiments in failing cardiomyocytes showed a reduction of basal and isoproterenol - stimulated contraction correlated to the amount of caspase - 3 activation in the cytosol of the failing cells ( fig3 c ). a lot of data suggests that myosin light chains play an important role in cardiac and skeletal muscle function . removing mlcs from chicken skeletal muscle myosin reduces the velocity of actin filament movement by 90 % without significant loss of the myosin atpase activity in an in vitro motility assay ( lowey et al ., 1993 ). furthermore , mlc2 removal has little effect on isometric force , whereas mlc1 removal reduces the isometric force by over 50 % ( vanburen et al ., 1994 ). mutations in the human essential light chain ( met149val ) or regulatory light chain ( glu22lys , pro94arg ) of myosin are associated with rare variants of inherited cardiac hypertrophy , characterized by midventricular cavity obstruction , and correlate with disruption of the stretch activation response of the cardiac papillary muscles ( potter et al ., 1996 ). transgenic mice expressing the human mutant mlc1 met149val faithfully replicate the cardiac disease of the patients with this mutant allele ( vemuri et al ., 1999 ). in the human heart , two different essential myosin light chain isoforms exist : ( a ) an atrial specific isoform ( amlc1 ), which is expressed in the fetal heart and decreases to undetectable levels during early postnatal development in the ventricle , but persists in the atrium for the whole life , and ( b ) a ventricular specific isoform ( vmlc1 ), which is the same isoform present in adult slow skeletal muscle ( price et al ., 1980 ). the reexpression of amlc1 in adult human ventricles has been reported in patients with ischemic or dilative cardiomyopathy and valvular heart disease ( schaub et al ., 1987 ; sutsch et al ., 1992 ). interestingly , in such patients with end - stage heart failure caspase - 3 activation has also been documented ( narula et al . 1999 ). the isoform shift of vmlc1 to amlc1 correlates with an increase in cross - bridge cycling kinetics as measured in skinned fibers derived from the diseased muscle ( morano et al ., 1997 ). postsurgical return to a normal hemodynamic state decreases amlc1 expression in these patients ( sütsch et al ., 1992 ). the functional significance of this isoform switch is not completely clear , but may be a direct compensatory mechanism to caspase - 3 induced vmlc1 cleavage , triggered when the heart attempts to maintain normal cardiac function . the molecular mechanism for mlc1 to affect the cross - bridge kinetics seems to reside in its ala - pro - rich extended n - terminus , which has been shown to interact with the c - terminus of actin ( trayer et al ., 1987 ; milligan et al ., 1990 ). the extended mlc1 n - terminus may provide a tether between the myosin and actin filaments , serving to position the two filament systems for cross - bridge interaction and to amplify small movements of the myosin globular head ( sweeney 1995 ). the mlc1 c - terminus anchors the protein to the myosin globular head . destruction of vmlc1 at the c - terminal motif dfve 135 g by activated caspase - 3 could alter myosin / actin cross - bridge interactions by modifying myosin head stability and thereby lead to reduced force transmission . taken together , this data clearly illustrates that minute changes in vmlc1 structure or composition , particularly in the c terminal anchoring moiety of vmlc1 , can have a dramatic impact on myocyte function and heart contractility . we have therefore demonstrated that vmlc1 is a cellular target for activated caspase - 3 . vmlc1 is cleaved , and its localization in sarcomeres is partially lost in failing cardiomyocytes , presenting caspase - 3 activation and reduced contractile performance . it is plausible that vmlc1 disruption could alter the stiffness of the myosin neck region and therefore reduce the full range of myosin movement during contraction . our findings suggest that caspase - 3 - mediated cleavage of vmlc1 may represent a molecular mechanism contributing to the deterioration of cardiac function prior to myocyte cell death ( summarized in fig4 ). as we had found that the atypical vmlc1 cleavage site dfve did not occur in any other known substrate of caspase - 3 , we intended to identify specific mlc protectants for the treatment of heart failure . the atypical novel cleavage site was therefore used to establish a high throughput - scaleable in vitro assay to differentially screen for caspase - 3 inhibitors which do not inhibit the physiological execution of cell death , but can protect vmlc1 from destruction in heart failure ( summarized in fig5 ). compounds identified in such a screen could be used to treat heart failure and other cardiac diseases , without having a pro - oncogenic potential . to this end , fluorimetric in vitro assays using the specific cleavage sites coupled to indicator dyes were established . caspase - 3 and the structurally almost identical caspase - 7 ( wei et al ., 2000 ) cleaved both substrates , devd and dfve , with a highly reproducible michaelis - menten kinetic . fig6 shows an example of the kinetic course and a lineweaver - burk plot for the substrate dfve cleaved by caspase - 3 . to our surprise , we found that the k m - values for caspase - 3 induced cleavage of both substrates differed markedly . we measured a k m - value for devd which compared well to existing literature data ( table 1 ), whereas the k m - value for dfve was in the range of some other rare substrates of caspase - 3 ( table 1 ). this differential substrate affinity allows to screen for specific inhibitors of vmlc1 cleavage , which would , however , not affect the cleavage of most other known substrates of caspase - 3 and 7 . in such a screen , every compound would be tested at identical concentrations for the inhibition of both reactions ( first assay ), and compounds which specifically inhibit dfve , but not devd cleavage would be selected and tested in cardiomyocytes ex vivo upon coinjection of active caspase - 3 for their capacity to protect against vmlc1 cleavage ( 2nd assay ). as p35 inhibits all effector caspases ( subtypes 1 , 3 , 6 , 7 , 8 and 10 ; e . g ., zhou et al ., biochemistry 1998 ; 37 : 10757 ), our concern was whether the observed beneficial effects of p35 in heart failure were really due to inhibition of caspase - 3 and of the structurally almost identical caspase - 7 . especially , we sought to exclude that the decrease in vmlc1 cleavage in the presence of p35 was due to predominant inhibition of a different caspase , and to exclude that the cleavage of vmlc1 was induced by caspase - 3 only indirectly acting via other effector caspases . therefore , we tested all these enzymes for their capacity to cleave ac - dfve - amc . we found that only caspase - 3 and 7 , which are structurally very similar , can specifically cleave this substrate , whereas no cleavage was detectable with other caspases nor with the related protease calpain - i at physiological substrate concentrations . however , the highly homologous caspase - 7 cleaved the new substrate dfve with almost 1 log scale lower affinity compared to caspase - 3 . table i kinetic constants for chromogenic peptide substrates ( j biol chem . 1997 apr 11 ; 272 ( 15 ): 9677 - 82 ) substrate km ( μm ) ac - devd - pna 11 ac - dqmd - pna 44 ac - vdvad - pna 67 ac - veid - pna 250 ac - yevd - pna 370 ac - vqvd - pna 510 yeast two - hybrid screening using pbtm - casp3 - p12p17 m as bait vector was performed with a human heart cdna library , fused to the gal4 activation domain in the pact2 plasmid ( clontech , heidelberg , germany ), following the hybrid hunter two - hybrid system protocol ( invitrogen , groningen , the netherlands ) in l40 yeast cells ( mata trp1 lue2 his3 ade2 lys2 :: 4lexaop - his3 ura3 :: 81exaop - lacz ). a total of 30 × 10 6 independent clones were screened by selective growth on trp − / leu − / his − / ura − / lys − / ade + synthetic dropout medium plates and expression of β - galactosidase activity . to construct expression plasmids for positive clones obtained from the two - hybrid screening , ecori - xhol fragments of positive clones were inserted into the ecori - xhol cloning sites of pyes2 / nt - a plasmid ( invitrogen ), in which the sequences were under control of the t7 promoter . biotinylated lysine - labeled proteins were prepared from expression plasmids using a tnt t7 quick coupled transcription / translation system ( promega , mannheim , germany ), according to the manufacturer &# 39 ; s instructions . five μl of biotinylated lysine - labeled protein were incubated for 1 h at 37 ° c . with 15 ng / μl recombinant active caspase - 3 ( bd pharmingen , heidelberg , germany ) and optionally with 25 μm tetrapeptide caspase - 3 inhibitor devd - fmk , in a tris - cl reaction buffer , ph 7 . 5 ( 6 mm tris - cl , ph 7 . 5 , 1 . 2 mm cacl 2 , 5 mm dtt , 1 . 5 mm mgcl 2 and 1 mm kcl ). the reaction was stopped by addition of sds - page sample buffer , and cleaved products were size fractionated by sds - 15 % page and blotted to a nitrocellulose membrane . colorimetric detection of biotinylated products was performed on blots with transcend colorimetric translation detection system ( promega ). rabbit ventricle protein extracts were prepared by homogenization in tris - cl reaction buffer , ph 7 . 5 . to examine the cleavage by caspase - 3 , 150 μg protein from control heart extracts were incubated for 1 hr at 37 ° c . with different amounts of recombinant human caspase - 3 , in presence or absence of the caspase - 3 inhibitor devd - fmk ( 25 μm ). after size - fractionation by sds - page , proteins were electrophoretically transfered to a nitrocellulose membrane and blots were incubated for 1 h at room temperature with mouse monoclonal antibodies against vmlc1 ( 0 . 2 μg / ml , clone 2c8 , biospacific , emeryville , calif . ; 1 : 10 dilution , clone f109 . 16a12 , biocytex , marseille , france ), vmlc2 ( 1 : 10 dilution , clone f109 . 3e1 , biocytex ), cardiac α / β myosin heavy chain ( 1 : 10 dilution , clone f26 . 4f4 , biocytex ), α - sarcomeric actin ( 1 : 2 , 500 dilution , clone 5c5 , sigma , munchen , germany ) or cardiac troponin t ( 0 . 4 μg / ml , clone 9b1 , biospacific ). bound antibodies were detected with horseradish peroxidase - conjugated antibody against mouse igg ( 1 : 10 , 000 dilution , sigma ) and visualized by chemiluminescence ( ecl detection kit , amersham pharmacia , freiburg , germany ). left ventricle lysates from control and 15 days paced failing male new zealand white rabbits were prepared by homogenization in denaturing lysis buffer ( 50 mm tris - cl , ph 7 . 4 , 5 mm edta , 1 % sds , 10 mm dtt , 1 mm pmsf , 2 μg / ml leupeptin and 15 u / ml dnase i ), heated at 95 ° c . for 5 min , diluted 1 : 10 with nondenaturing lysis buffer ( 50 mm tris - cl , ph 7 . 4 , 300 mm nacl , 5 mm edta , 1 % triton x - 100 , 10 mm iodoacetamide , 1 mm pmsf , 2 μg / ml leupeptin and 0 . 02 % sodium azide ) and centrifuged at 15 , 000 × g for 10 min at 4 ° c . after dilution to 3 . 5 mg protein / ml , supernatants were precleared with excess of protein g - sepharose beads ( sigma ) and incubated for 2 h at 4 ° c . with protein g - sepharose beads ( 30 μl beads / ml lysate ), preconjugated with 100 μg anti - vmlc1 monoclonal antibody ( clone 2c8 , biospacific ). beads containing the immunocomplex were extensively washed with ice - cold nondenaturing lysis buffer , boiled in sds sample buffer and subjected to sds - 15 % page and immunoblotting for vmlc1 , as described above . medtronic pacemakers were implanted into new zealand white rabbits ( weight 3 . 6 ± 0 . 3 kg ; from harlan , munich , germany ). two days afterwards , rapid pacing was initiated at 320 beats / min . under this protocol , a tachycardia - induced heart failure ( hf ) develops reproducibly over one week . pacing was then continued at 360 beats / min , which predictably led to a further deterioriation of heart failure . the average contractility in failing hearts was 2200 ± 320 mmhg / sec ( vs . 4000 ± 390 mmhg / sec in healthy controls ; p & lt ; 0 . 05 ), and lvedp increased from 3 . 6 ± 0 . 4 mmhg to 13 . 5 ± 1 . 2 ( p & lt ; 0 . 05 ). single myocytes were isolated from the left ventricle of control and 15 days paced failing rabbits , and cultured in m199 culture medium ( supplemented with mem vitamins , mem non - essential aminoacids , 25 mm hepes , 10 μg / ml insulin , 100 iu / ml penicillin , 100 μg / ml streptomycin and 100 μg / ml gentamicin ) on laminin - precoated glass slides ( 5 μg / cm 2 ; density of 10 5 cells / cm 2 ) in a humidified atmosphere ( 5 % co 2 ) at 37 ° c . ( laugwitz et al ., 1999 ). two hours after plating , cells were subjected to detection of activated caspase - 3 . activated caspase - 3 was detected in living cells by using caspatag caspase - 3 activity kit ( intergen , oxford , united kingdom ), according to the manufacturer &# 39 ; s instructions . freshly isolated ventricular cardiomyocytes were incubated at 37 ° c . ( 5 % co 2 ) with fam - devd - fmk , a carboxyfluorescein labeled fluoromethyl ketone tetrapeptide inhibitor of caspase - 3 , which is cell permeable and irreversibly binds to activated caspase - 3 . after 1 h incubation , cells were washed , fixed in 4 % paraformaldehyde , permeabilized in 100 % methanol ( at − 20 ° c .) and subjected to hoechst 33258 staining and either to immunofluorescence staining for vmlc1 / vmlc2 , or to phalloidin staining . vmlcs were detected by labeling with specific mouse monoclonal antibodies anti - vmlc1 ( 4 μg / ml , clone 2c8 , biospacific ) and anti - vmlc2 ( 1 : 2 dilution , clone f109 . 3e1 , biocytex ), followed by incubation with texas red goat anti - mouse - igg conjugate ( 10 μg / ml , molecular probes , leiden , the netherlands ). polymerized actin fibers were visualized by texas red - phalloidin ( 3 units / ml , molecular probes ), according to the manufacturer &# 39 ; s instructions . fractional shortening was measured in rabbit adult cardiomyocytes isolated from left ventricle of control and 15 days paced failing myocardium , after detection of activated caspase - 3 . experiments were performed in a temperature - controlled cuvette ( 37 ° c . ), at constant medium flow ( 1 . 8 mm ca 2 + - tyrode &# 39 ; s solution ) and constant electrical field , using an electro - optical monitoring system ( scientific instruments , heidelberg , germany ), as described ( laugwitz et al ., 1999 ). left ventricular contractility was examined before the initiation of rapid pacing and at the end of the protocol ( two weeks after the start of pacing ). the rabbits were anesthetized as described before ; ecg was monitored continuously . the rate of caspase - 3 enzyme activity could be measured by enzymatic cleavage and release of amc from the ac - devd - amc caspase substrate ( biosyntan , berlin , germany ). this parameter was measured as emission at 460 nm upon excitation at 380 nm using u . v . spectrofluorometry . ac - dfve - amc was synthesized by biosyntan , berlin , germany , with a purity of 93 . 5 %. the peptide lyophilised as trifluoracetic acid salt was reconstituted in dmso to 100 mm . 5 μg of purified , active recombinant human caspase - 3 ( cpp32 ) from bd biosciences pharmingen , heidelberg , germany , were diluted in 100 μl 50 mm tris , ph 8 . 0 , with 100 mm nacl , 50 mm imidazole . the reaction buffer contained 20 mm hepes , 100 mm nacl , 10 mm dtt , 1 mm edta , 0 . 1 % ( w / v ) chaps , 10 % sucrose , ph 7 . 2 and the indicated concentrations of ac - dfve - amc . caspase - 3 was added to reaction mixture at a final concentration of 3 nm . after preincubation for 10 min at 37 ° c ., the released fluorogenic amc was monitored every second minute for 20 min in a spectrofluorometer at an excitation wavelength of 380 nm and an emission wavelength of 460 nm . initial velocities and substrate concentrations were fit by non linear regression to the michaelis - menten equation . lineweaver - burk plots were calculated . cesselli , d ., i . jakoniuk , l . barlucchi , a . p . beltrami , t . h . hintze , b . nadal - ginard , j . kajistura , a . leri , and p . anversa . 2001 . oxidative stress - mediated cardiac cell death is a major determinant of ventricular dysfunction and failure in dog dilated cardiomyopathy . cir . res . 89 : 279 - 286 . chien , k . r . 2000 . genomic circuits and the integrative biology of cardiac diseases . nature 407 : 227 - 232 . cohen , g . m . 1997 . caspases : the executioners of apoptosis . biochem . j . 326 : 1 - 16 . haunstetter , a ., and s . izumo . 1998 . apoptosis : basic mechanisms and implications for cardiovascular disease . circ . res . 82 : 1111 - 1129 . hengartner , m . o . 2000 . the biochemestry of apoptosis . nature 407 : 770 - 776 . kamada , s ., h . kusano , h . fujita , m . ohtsu , r . c . koya , n . kuzumaki , and y . tsujimoto . 1998 . a cloning method for caspase substrate that uses the yeast two - hybrid system : cloning of the antiapoptotic gene gelsolin . proc . natl . acad . sci . usa . 95 : 8532 - 8537 . laugwitz , k . l ., a . moretti , h . j . weig , a . gillitzer , k . pinkernell , t . ott , i . pragst , c . stadele , m . seyfarth , a . schömig , and m . ungerer . 2001 . blocking caspase - activated apoptosis improves contractility in failing myocardium . hum . gene ther . 12 : 2051 - 2063 . laugwitz , k . l ., m . ungerer , t . schoneberg , h . j . weig , k . kronsbein , a . moretti , k . hoffmann , m . seyfarth , g . schultz , and a . schömig . 1999 . adenoviral gene transfer of the human v2 vasopressin receptor improves contractile force of rat cardiomyocytes . circulation 99 : 925 - 933 . lowey , s ., g . s . waller , and k . m . trybus . 1993 . function of skeletal muscle myosin heavy and light chain isoforms by an in vitro motility assay . j . biol . chem . 268 : 20414 - 20418 . mallat , z ., a . tedgui , f . fontaliran , r . frank , m . durigon , and g . fontaine . 1996 . evidence of apoptosis in arrhythmogenic right ventricular dysplasia . n . engl . j . med . 335 : 1190 - 1196 . milligan , r . a ., m . whittaker , and d . safer . 1990 . molecular structure of f - actin and location of surface binding sites . nature . 348 : 217 - 221 . morano i , k . hadicke , h . haase , m . böhm , e . erdmann , and m . c . schaub . 1997 . changes in essential myosin light chain isoform expression provide a molecular basis for isometric force regulation in the failing human heart . j . mol . cell cardiol . 29 : 1177 - 1187 . morano , i . 1999 . tuning the human heart molecular motors by myosin light chains . j . mol . med . 77 : 544 - 555 . mittl p r , di marco s , krebs j f , bai x , karanewsky d s , priestle j p , tomaselli k j , grutter m g . structure of recombinant human cpp32 in complex with the tetrapeptide acetyl - asp - val - ala - asp fluoromethyl ketone . j biol chem . 1997 mar 7 ; 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272 ( 15 ): 9677 - 82 . trayer , i . p ., h . r . trayer , and b . a . levine . 1987 . evidence that the n - terminal region of al - light chain of myosin interacts directly with the c - terminal region of actin . a proton magnetic resonance study . eur . j . biochem . 164 : 259 - 266 . vanburen , p ., g . s . waller , d . e . harris , k . m . trybus , d . m . warshaw , and s . lowey . 1994 . the essential light chain is required for full force production by skeletal muscle myosin . proc . natl . acad . sci . usa . 91 : 12403 - 12407 . vemuri , r ., e . b . lankford , k . potter , s . hassanzadaeh , k . takeda , z . x . yu , v . j . ferrans , and n . d . epstein . 1999 . the stretch - activation responce may be critical to the proper funtioning of the mammalian heart . proc . natl . acad . sci . usa . 96 : 1048 - 1053 . wei y , fox t , chambers s p , sintchak j , coll j t , golec j m , swenson l , wilson k p , charifson p s . the structures of caspases - 1 , - 3 , - 7 and - 8 reveal the basis for substrate and inhibitor selectivity . chem biol . 2000 jun ; 7 ( 6 ): 423 - 32 . yin , x ., s . gu , and j . x . jiang . 2001 . the development - associated cleavage of lens connexin 45 . 6 by caspase - 3 - like protease is regulated by casein kinase ii - mediated phosphorylation . j . biol . chem . 276 : 34567 - 34572 . | 6 |
referring to fig1 a tiller generally indicated as 11 is comprised of a main housing 13 and an extention housing 15 . tine shafts carry a plurality of tine teeth 17 and are rotatably supported in the housings 13 and 15 . the tine shafts are driven by hydraulic motor 19 fixably mounted to the tiller housing 13 . an input line 21 is received by the hydraulic motor delivering pressurized hydraulic fluid from a remotely located hydraulic pump ( not shown ). a return line 23 receives spent fluid from the hydraulic motor 19 and delivers it to a filter 25 which thereafter delivers the fluid to a reservoir chamber 27 formed by the housing 13 . a suction line 29 receives cold hydraulic fluid and delivers the hydraulic fluid to the input of the remotely located pump . referring more particularly to fig2 and 3 , the housing 13 is comprised of top wall 30 having fixably mounted atop wall 30 an expansion chamber 31 including filler cap 32 . the reservoir 27 is formed in combination with the top wall 30 , forward wall 35 and rear wall 37 , and end walls 39 and 41 respectively . a bottom wall 33 is fixably mounted to the walls 35 , 37 , 39 and 41 by any conventional means and has a generally arched cross - sectional configuration . a baffle plate 42 extending longitudinally is fixably mounted by any conventional means particularly along the apex of the bottom wall 33 and to the underside of top wall 30 , and also , to end wall 41 separating the reservoir into sections a and b . one end of baffle plate 42 is in spaced apart relationship to end wall 39 . the housing top wall 30 forms the underside of the expansion chamber 31 and has a plurality of apertures 38 extending through wall 30 to each side of baffel 42 to allow communication between reservoir 27 and expansion chamber 31 . a filter line 43 to which filter 25 is fixably mounted to by any conventional means extends through the top wall 30 into section a of the reservoir on one side of baffle plate 42 . the suction line 29 extends through the top wall 30 substantially into section b of the reservoir 27 on the other side of baffle plate 42 . fixably mounted transversely across the top wall 30 of the housing 13 in spaced apart opposite relationship are mounting members 45 , 46 , 47 and 48 . hydraulic motor 19 is fixably mounted in sidewall 41 within a formed mounting sleeve 51 by any conventional means such as by bolts . the motor output shaft 55 extends into the housing 11 and is splined within the tine shaft 59 at 57 . the tine shaft 59 is of conventional design carrying a plurality of tine blade 61 in spaced apart relationship , each tine blade 61 having a plurality of tine teeth 63 fixably mounted thereto in spaced apart relationship . a conventional bearing set 65 is mounted into the lower portion of housing wall 39 and rotatably supports the other end of tine shaft 59 . the housing wall 39 contains a flange 67 extending transversely along the end of top surface 30 . the extention 15 comprised of housing extension 78 . one other end of the extension tine shaft 73 contains a portion 74 which receives a portion of tine shaft 59 extending through end wall 39 and extention end wall 80 and is pinned to shaft 59 at 75 . the two housings are joined along respective walls 39 and 80 by fixably mounting respective wall flanges 67 and 69 by any conventional means such as by bolts . referring now to fig4 it is observed that a tractor can be mounted to either side of the tiller 11 such that the tractor rear wheel 70 can rotate either in the same direction as the tine shaft , or as shown in phantom in the opposite direction of the tine shaft . further , the tiller 11 can be centered relative to the tractor by securing hitch arms 85 to mounting members 46 and 48 , or mounting members 45 and 47 when the tiller extension 15 is also be used . it is further observed that the tiller offers the further advantage of having a segregated hydraulic system which reduces contaminant problems . also , the tiller housing offers good cooling properties which eliminates the necessity to have a separate hydraulic fluid cooling system by providing the reservoir as part of the tiller housing and requiring the fluid to flow longitudinally in section a , over the apex of under surface 33 , between baffel 42 and end wall 39 , and longitudinally in section b before being received in line 29 . | 0 |
as shown in fig1 - 8 , a system 10 and method converting exhaust waste of a combustion engine 12 to carbon nanotubes within an exhaust system 14 in fluid communication with the combustion engine 12 is disclosed . in at least one embodiment , the system 10 may include a filter 16 and a process that converts waste exhaust of combustion engines 12 into carbon nanotubes . the combustion engine 12 may be used in numerous applications , such as , but not limited to , being used as an automotive combustion engine . in at least one embodiment , aspects of the system 10 and method include the filter material 16 , treatment of the filter material , alignment of the filter material and process that yields the maximum amount of carbon nanotubes . the system 10 and method may also include use of a fuel 18 with one or more metal salts that once combusted within a combustion engine 12 produce carbon nanotubes downstream of a combustion chamber , such as , but not limited to , within the exhaust system 14 . in at least one embodiment , the system 10 may include a filter 16 placed downstream of the combustion engine 12 . the filter 16 may be formed from any appropriate material capable of withstanding the environment , such as the heat generated by the combustion engine 12 . in at least one embodiment , the filter 16 may be formed from filter material that is thin , such as less than one mm in thickness , and may be formed from a metal , such as but not limited to iron metal . in at least one embodiment , the filter material forming the filter 16 may be formed from pure iron such as , but not limited to , pure iron sheets . in another embodiment , the filters 16 may be formed from carbonated steal with low percentage of carbon , such as , but not limited to , 0 . 05 or less carbon . in yet another embodiment , a thin layer of iron may be posted on a polymeric or metallic sheet . the thin layer may be produced by one or more physical processes , such as , but not limited to , pulse laser deposition or ablation processes . in the event of using carbonated steel , or iron , a polishing scheme may be used to expose the iron grains on the surface . such processes may not be needed for thin layer depositions as described before . the filter 16 may be positioned in the path of the exhaust waste of a combustion engine , such as an automotive engine . the filter 16 may be placed at an angle below 45 degrees and , in at least one embodiment , may be placed below 15 degrees measured from the streamline of the exhaust waste . in at least one embodiment , the filter 16 may be placed at an angle to the exhaust flow of between 5 degrees and 15 degrees . as such , combustion engine exhaust may be directed past the filter 16 having a surface skewed relative to exhaust flow an angle between 5 degrees and 15 degrees . localized heating of the filter 16 or its surrounding is required to activate the carbon nanotubes formation . though a temperature in the range of 700 degrees celsius is preferred , temperatures as low as 200 degrees celsius have shown carbon nanotubes formation . the efficiency of the tube formation is a function of the filter angle and the temperature at the filter location . in at least one embodiment , carbon nanotubes may form on an exposed surface of the filter 16 such that the carbon nanotubes may be formed from multiwall carbon nanotubes having an average diameter of between 20 and 50 nm and average length of between one micrometer and 10 micrometers . the method of converting exhaust waste of combustion engines 12 to carbon nanotubes , as shown in fig5 - 7 , within an exhaust system 14 in fluid communication with the combustion engine 12 includes generating combustion engine exhaust through combustion of a fuel 18 including a metal salt and heating one or more filters 16 to at least 200 degrees celsius . the method also includes passing combustion engine exhaust past the filter 16 positioned within the exhaust system 14 of the combustion engine 12 , wherein carbon nanotubes form on an exposed surface of the filter 16 . in at least one embodiment , the method may include a process for converting diesel engine exhaust gases into carbon nanotubes . as shown in fig8 , one or more filters 16 may be placed downstream of the combustion engine 12 in at least a portion of the exhaust gases flowing from the combustion engine 12 . the method may include generating combustion engine exhaust through combustion of a fuel 18 including a metal salt whereby the metal salt may be , but is not limited to being , an iron salt . the metal salt may be , but is not limited to being , used in a concentration between about one mg of metal salt / ml of fuel 18 and four mg of metal salt / ml of fuel 18 . concentrations less than this range and without a metallic substrate do not generate carbon nanotubes . in at least one embodiment , the metal salt may have a concentration of two mg of metal salt / ml of fuel 18 . the metal salt may be used together with a fuel 18 , such as , but not limited to , diesel fuel 18 . in at least one embodiment , at least a portion of the fuel 18 may be an algal biodiesel . in another embodiment , at least a portion of the fuel 18 may be a fossil diesel fuel 18 . in yet another embodiment , the fuel 18 may be a mixture of algal biodiesel fuel 18 and fossil diesel fuel 18 . the utilization of algal biodiesel fuel 18 promotes formation of carbon nanotubes by suspending the iron salt within the fossil diesel fuel 18 . in still another embodiment , the fuel 18 may be a mixture of algal biodiesel fuel 18 , ethanol and fossil diesel fuel 18 . the fuel 18 may be formed by introducing one or more metal salts into algal biodiesel to form a mixture . the mixture of one or more metal salts into algal biodiesel may then be mixed into the fossil diesel fuel 18 to form a homogenous suspension . the algal biodiesel creates a homogenous suspension of the iron salt in fossil fuel 18 diesel . the presence of the metal salt increases the formation of carbon nanotubes on the filer 16 . in at least one embodiment , the diesel fuel 18 may be formed from a mixture of between one percent and ten percent algal biodiesel fuel 18 , between one percent and ten percent ethanol and remainder fossil diesel fuel 18 . in another embodiment , the diesel fuel 18 may be formed from a mixture of about five percent algal biodiesel fuel 18 , about five percent ethanol and about 90 percent fossil diesel fuel 18 . combustion of fuel 18 , such as but not limited to diesel fuel 18 , with metal salts , such as , but not limited to one or more iron salts , improves the combustion quality and reduces the formation of soot . the inclusion of biodiesel together with the fossil fuel 18 diesel may help to reduce environmental hazards , such as , but not limited to , co ( x ) and so ( x ). the following examples are not to limit the scope of the invention but to illustrate the invention . a filter made out of a solid structure such as , but not limited to , carbonated steel , was placed in the pathway of a diesel engine exhaust . the engine was allowed to run at normal operation condition for half an hour . the filter was recovered and evaluated using sem . fig1 shows a monograph of the material collected on the solid filter . it showed clumps of carbon particulates . a filter made out of carbonated steel was polished using techniques known in the literature . the surface was examined using optical microscopy . the grains were clearly shown . the filter was placed in the pathway of a diesel engine exhaust . the engine was allowed to run for half an hour under normal operation conditions . the filter was collected and examined using sem . fig2 shows sem monograph of the materials collected on the surface of the filter . it shows clumps of carbonated materials . a similar filter made out of carbonated steel was polished and placed in the pathway of the exhaust horizontally to the exhaust streamlines . the filter zone was heated using a gas burner . the diesel engine was allowed to run in normal condition for half an hour . the filter material was collected and examined using sem . fig3 shows sem monograph showing the formation of carbon nanotubes . a similar filter made out of carbonated steel was polished and placed in the pathway of the exhaust of a diesel engine at an angle of 5 degrees to the streamlines of the exhaust . a diesel engine was allowed to run under normal operating conditions for half an hour . the filter location was heated using a gas burner . the filter was collected an examined using sem . fig4 shows a monograph of the filter surface with carbon nanotubes formed on the surface . it is noticeable that the angle of 5 degrees influenced the formation of more carbon nanotubes . the produced carbon nanotubes are purified by immersing the filter plate in a ionic liquid bath . the purification process using ionic liquids produces 95 % purified carbon nanotubes . without limitation to the composition , ionic liquids have the ability to dissolve carbonated materials other than carbon nanotubes leaving a highly purified carbon nanotube stock . the system and method are not limited to the details of construction or process steps set forth in the following description . instead , the system and method is capable being practiced or carried out in other ways and via other embodiments of the system . as used in this specification and the appended claims , the singular forms “ a ”, “ an ” and “ the ” include plural referents unless the context clearly indicates otherwise . thus , for example , reference to “ a filter ” includes a mixture of two or more filters , and the like . the foregoing is provided for purposes of illustrating , explaining , and describing embodiments of this invention . modifications and adaptations to these embodiments will be apparent to those skilled in the art and may be made without departing from the scope or spirit of this invention . | 5 |
referring now to the drawings and particularly to fig1 and 2 , a lighting fixture is seen generally at 10 to comprise a recessed lighting fixture such as is described in u . s . pat . no . 5 , 690 , 423 , the disclosure of which is incorporated hereinto by reference as aforesaid , the fixture 10 being a particular fixture with which the present invention functions to produce the objects and advantages referred to herein . it is to be understood , however , that lighting fixtures , particularly downlighting fixtures , employing painted steel pans such as are conventional in the art and other pans such as the pan described in u . s . pat . no . 5 , 662 , 414 , assigned to the assignee of the present application and incorporated hereinto by reference , can also be improved through use therewith of the present invention . as shown best in fig2 the lighting fixture 10 is provided with a wire frame pan 12 such as is disclosed in detail in aforesaid u . s . pat . no . 5 , 690 , 423 . the pan 12 mounts a junction box 14 and a can 16 for &# 34 ; rough - in &# 34 ; above a ceiling ( not shown ) to produce downlighting in an environmental space below the ceiling . a standard conduit ( not shown ) extends from the junction box 14 to the can 16 in a conventional manner to allow access of insulated wiring ( not shown ) into the interior of the can 16 to provide power to a lamp ( not shown ) mounted within the interior of the can 16 . the connection of electrical power to lamping within the can 16 through the junction box 14 as well as the provision of finishing trim and the like ( not shown ) is conventional and need not be described in detail herein . the junction box 14 is essentially identical as shown to that junction box described in u . s . pat . no . 5 , 690 , 423 , the main body of the junction box 14 being formable from a flat , stamped piece of metal which is then bent to assemble the junction box 14 with mounting plates 20 and 22 being formed integrally with the junction box 14 . each of the mounting plates 20 and 22 are respectively formed with slots 24 and 26 which align on assembly of the junction box 14 to receive a bar hanger assembly 28 to thus mount said assembly 28 to the fixture 10 . at the opposite end of the lighting fixture 10 , a bar hanger assembly 30 is mounted by the wire frame pan 12 as is described in detail in u . s . pat . no . 5 , 690 , 423 . the bar hanger assembly 30 is thus mounted to the fixture 10 through direct connection to the wire frame pan 12 while the bar hanger assembly 28 is mounted by the junction box 14 by means of the mounting plates 20 and 22 which can be integrally formed with the junction box 14 . the structure and function of the bar hanger assemblies 28 and 30 are essentially identical . while the bar hanger assemblies shown in the aforesaid patents and described in detail in co - pending u . s . patent application ser . no . 08 / 690 , 314 , filed jul . 25 , 1996 , all of these entities being incorporated hereinto by reference , are particularly suited to use with the present invention , it is to be understood that the bar hanger assemblies 28 and 30 can take other forms and can vary from the bar hanger assemblies described in detail in said patent application . a brief discussion of the function of the bar hanger assembly 30 will be provided herein , only one of the bar hanger assemblies 28 , 30 being necessarily described since the structure and function thereof are essentially identical . the bar hanger assembly 30 is formed of a slide element 32 and a track element 34 , the elements 32 and 34 being often referred to as &# 34 ; bar &# 34 ; elements . the track element 34 has a guideway or track 36 formed by the bending over of opposite lateral edges of said track element 34 to form said track 36 . the track 36 receives the slide element 32 thereinto for sliding movement therein . each of the elements 32 , 34 are provided with nailing plates 38 and 40 on respective outermost ends thereof , the nailing plates 38 , 40 being respectively bent at angles of 90 ° relative to the longitudinal axes of the elements 32 , 34 . while these nailing plates can take different forms , it is desirable to stamp barbs 40 , 44 from the respective planar body portions of the nailing plates 38 , 40 , the structure thus described facilitating rapid mounting to wooden joists ( not shown ). the mounting of the lighting fixture 10 to wooden joists in a ceiling is essentially conventional . the bar hanger assemblies 28 , 30 can be adjusted lengthwise by virtue of the ability of the elements 32 , 34 to slide relative to each other . the bar hanger assembly 30 is also capable of sliding relative to the wire frame pan 12 . similarly , the bar hanger assembly 28 can slide within the slots 24 , 26 formed in the mounting plates 20 , 22 of the junction box 14 . when the lighting fixture 10 is to be mounted above a suspended ceiling , j - channel notches ( not shown ) formed at ends of the bar elements 32 , 34 allow mounting in a conventional manner to t - bar structures ( not shown ) of such suspended ceilings . a scale can be formed on the element 34 ( the scale not being shown ) to allow estimation of the degree of elongation necessary for appropriate fitting of the bar hanger assemblies 28 , 30 between joists or between t - bar structures of a suspended ceiling as is conventional in the art . referring now to fig1 through 9 , a bar hanger clip is seen at 50 to comprise a single piece of 0 . 020 inch zinc - plated spring steel formed by stamping or similar operations and the like to comprise a flat , planar base portion 52 joined to a planar body portion 54 by means of a first arcuate section 56 , the plane of the body portion 54 being disposed at slightly less than 90 ° from the plane of the base portion 52 . a second arcuate section 58 joins the other end of the planar body portion 54 to an angled distal portion 60 which is also planar and which rounds at corners 62 and 64 with a radius of approximately 0 . 15 inch . the base portion 52 joins at the end thereof opposite the juncture with the first arcuate section 56 with an angled proximal section 66 which terminates in a third arcuate section 68 , the arcuate section 68 then terminating in recurving fashion to form a terminal planar section 70 which then terminates with a recurved end portion 72 . a portion of the angled proximal section 66 , the entirety of the third arcuate section 68 , the terminal planar body portion 70 and the recurved end portion 72 can be notched at 74 to form spaced hinging legs 76 and 78 . the hinging legs 76 and 78 are clipped over a portion of the wire frame pan 12 as best seen in fig1 and in adjacent relationship to the bar hanger assembly 30 . the clip 50 can then pivot about that portion of the wire frame pan 12 to which it is mounted to be positioned in an unlatched configuration ( seen in fig2 ) such that the bar hanger assembly 30 is not latched in position and can be moved relative to the fixture 10 to an appropriate position as aforesaid . as has also been discussed , the slide element 32 and the track element 34 of the bar hanger assembly 30 can be moved relative to each other to desired positions as long as the clip 50 is maintained in the unlatched position . the bar hanger clip 50 can be pivoted about that portion of the wire frame pan to which it is attached to engage in a snap - fitting manner the bar hanger assembly 30 . in the event that extension of the bar hanger assembly 30 causes the track element 34 to be disposed in opposing relation to the clip 50 , the clip 50 latches to the bar hanger assembly 30 by means of engagement between the second arcuate section 58 of the clip 50 and upper edge portions of the bar hanger assembly 30 , thereby locking the track element 34 in place . this mounting is seen in fig1 in relation to the clip 50 to the left of the drawing . in the event that extension of the bar hanger assembly 30 causes the slide element 32 to oppose the bar hanger clip 50 , the first arcuate section 56 of the clip 50 is caused to engage upper edge portions of the slide element 32 , thereby to lock the slide element 32 in place . this mounting is seen in fig1 in relation to the clip 50 which is shown to be clipped to the slide element 32 . manipulation of the clip 50 can occur through the use of thumb pressure exerted against the angled distal portion 60 of said clip 50 . the clip 50 thus functions in the manner described herein in an unlatched configuration such that the bar hanger assembly 30 and the elements 32 , 34 comprising said assembly 30 can be fitted to the particular dimensions of an installation . the clip 50 is then employed to engage either the slide element 32 or the track element 34 of the bar hanger assembly 30 to produce the locking function described herein . as can best be seen in fig2 an identical bar hanger clip 50 can be employed to perform the same functions relative to the bar hanger assembly 28 mounted by the junction box 14 . a base plate 80 forming the &# 34 ; floor &# 34 ; of the junction box 14 is provided with a slot 82 near an outer edge of the base plate 80 , the elongated piece of material disposed between an outer edge of the slot and an outer edge of the base plate 80 forming a mounting bar 84 which is capable of receiving the hinging legs 76 , 78 thereabout to mount the clip 50 in place adjacent to the bar hanger assembly 28 . the clip 50 can then function in a manner identical to that described previously relative to the operation of the clip 50 and the bar hanger assembly 30 to latch and unlatch the bar hanger assembly 28 . two of the bar hanger clips 50 are therefore normally employed to latch the respective bar hanger assemblies 28 and 30 in place to the lighting fixture 10 once the elements 32 , 34 of each of the assemblies 28 , 30 are appropriately extended to fit the dimensions of a particular installation . the clips 50 are normally latched in position after the fixture 10 has been &# 34 ; roughed in &# 34 ;, that is , after the bar hanger assemblies 28 and 30 have been fixed in place . referring now to fig3 through 6 , a typical bar hanger clip such as the clip 50 is described herein as having certain relative dimensions which allow functioning with bar hanger assemblies of essentially standard dimensions in the art . it is to be understood that the clip 50 can be configured with dimensions other than will be specified hereinafter in order to function with bar hanger assembly structures of given dimensions . a typical width of the clip 50 such as across the flat base portion 52 or the angled distal portion 60 is approximately 0 . 63 inch , the length of the clip 50 as seen from plan or bottom views being approximately 0 . 78 inch . the width of the hinging legs 76 , 78 are each taken to be approximately 0 . 20 inch with the width of the notch 74 , if the clip 50 is so configured , being approximately 0 . 23 inch . inner corners of the hinging legs 76 , 78 are rounded with a radius of approximately 0 . 03 inch . the radius of each of the rounded corners 62 , 64 is approximately 0 . 15 inch . placement of the flat base portion 52 along the x - axis of a cartesian coordinate system would result in the angled distal portion 60 of the clip being approximately 30 ° to the y - axis . the first arcuate section 56 would then have a radius of 0 . 08 inch with the centerline thereof falling on a line which is 0 . 10 inch in the direction of the x - coordinate from a line tangent to the curvature of the first arcuate section and parallel to the y - axis . this same tangent line would be approximately 0 . 04 inch from a line parallel to the y - axis and which intersects the clip 50 at the juncture of the first arcuate section 56 and the planar body portion 54 , the planar body portion 54 being angled slightly toward the y - axis from a position to the left of the y - axis . the plane of the angled distal portion 60 is spaced from a line tangent to the second arcuate section 58 and parallel to said plane at a distance of 0 . 06 inch , the second arcuate section 58 having a radius of 0 . 10 inch . a line perpendicular to the terminal planar body portion 70 and extending to intersect an edge portion of the recurved end portion 72 is spaced a distance of approximately 0 . 28 inch from a tangent line drawn relative to the third arcuate section 68 . the terminal planar body portion 70 extends relative to the plane of the base portion 52 at an angle of approximately 19 °. the third arcuate section 68 has a radius of approximately 0 . 08 inch with the radius of the recurved arcuate end portion 72 being approximately 0 . 04 inch . placement of the center of the circular arc of the first arcuate section 56 at the 0 , 0 juncture of a cartesian coordinate system , causes the center of the circular arc of the second arcuate section 58 to be spaced 0 . 04 inch from the y - axis and 0 . 34 inch from the x - axis . the center of the third arcuate section 68 would be located 0 . 08 inch from the x - axis and 0 . 58 inch from the y - axis . the distance from the plane of the base portion 52 to the distal end of the angled distal portion 60 would be approximately 0 . 1 inch with said distal end of the section 66 being approximately 0 . 19 inch from the y - axis along a normal drawn thereto . the center of the second arcuate section 58 would be approximately 0 . 37 inch from the normal drawn from the distal end of the portion 60 to the y - axis . the distance of the center of the second arcuate section 58 to a line parallel to the x - axis and extending through the center of the first arcuate section 56 would have a length of approximately 0 . 34 inch , the distance from the center of the first arcuate section 56 and the lower face of the base portion 52 being approximately 0 . 10 inch . the distance between a plane parallel to a lower face of the terminal planar body portion 70 and a tangent to the arc of the recurved end portion 72 would be approximately 0 . 12 inch . all other radii are approximately 0 . 06 inch unless particularly specified . given the relative dimensions specified above , the clip 50 is therefore shaped in order to readily allow mounting of the hinging legs 76 , 78 about structural elements which allow pivoting of the clip 50 . the relative dimensions further allow engagement respectively of the first arcuate section 56 or the second arcuate section 58 with the aforesaid portions of the bar hanger assemblies 28 , 30 to produce the functions described herein . while particular clip structures have been described herein as being useful according to the invention , it is to be understood that other structural conformations could readily be devised to provide the function provided by the clip 50 which is explicitly described and shown herein . similarly , other structure herein explicitly described can be configured other than as expressly shown and described herein . accordingly , it can be readily understood in view of the particular embodiments of the invention which are expressly described hereinabove that the invention can be formed in a wide variety of configurations without departing from the intended scope of the invention , the scope of the invention being defined by the recitations of the appended claims . | 5 |
aspects of the disclosed embodiments relate to dispensing of toner material through a telescopic drop tube with a flexible auger that expands and contracts to the sizes and orientation needed . the disclosed embodiments include a supplier and receptacle housing for receiving a material . a variable length component couples the respective housings so as to transport and deliver the material . a motor driven flexible auger positioned in the variable length component is used to transport the material when the variable length component is not vertically oriented . the disclosed embodiments further include a transfer component , telescopic drop tube with rotatable member , and a gear assembly to dispense a material from a supplier to receptacle housing . the telescopic drop tube can expand and contract to a desired length so as to couple supply housing to receptacle housing . the rotatable member is a motor driven flexible auger that transports the material when the telescopic drop tube is not vertically oriented . the rotation of the flexible auger is through the gear assembly . the disclosed embodiment further includes an auger disposed in the transfer component for transporting the material when the component is not in a vertical position . the disclosed embodiments further include a toner transport apparatus for a printing system comprising a toner container , a developer housing , a dispenser , a variable length component , and gear train assembly . the variable length component can be extended away from the toner container to meet design constraints . the dispenser through the gear train assembly provides different orientations resulting in developer housing placement flexibility . the term “ variable length component ”, in the disclosed embodiments , refers to a telescopic component that is extensible or compressible by the sliding of overlapping sections . a “ variable length component ” may also refer to an accordion tube , malleable tube , or the like that is extensible or compressible to a range of lengths . fig1 is a perspective view of a variable length component in a dispenser unit 100 in accordance to possible embodiment . in particular , dispenser unit 100 comprises a variable length component 110 , a gear assembly such as pivot mechanism 145 , an entry port 140 for receiving developer material or toner form a container , and an exit port 130 for delivering the dispensed develop material . the variable length component 110 comprises substantially cylindrical members that move relative to each other . a pivot mechanism 145 such as a gear train and bevel gear set provide the variable length component 110 with rotation 150 defined relative to entry port 140 . the length of the variable length component 110 may be adjusted to compensate for differences in dimensions and positioning of the housings relative to each other . the variable length component defines a predetermined length 125 and a predetermined angle 120 relative to entry port 140 and exit port 130 . the predetermined angle 120 and predetermined length 125 affect the dispensing key elements outlined above . for example , when variable length component 110 is in a non - vertical position , predetermined angle 120 is greater than zero degrees , a rotatable member is needed to transport the toner and to prevent built up on the inside of the variable length component 110 . predetermined length 125 illustrates a scenario where the variable length component is contracted inward or when the variable length component is not extended to its maximum length . in operation , the length of variable length component 110 can be extended 160 to achieve a desired length . likewise , the variable length component 110 could be rotated 150 , oriented or pivoted to a desired angle 120 with the toner container or supplier housing 105 and with the receptacle or developer housing 115 tethered to each end . in a printing apparatus , such as a printer or copier , and a plurality of developer units . the overall function of a developer unit is to apply marking material , such as toner , onto suitably charged areas forming a latent image on an image receptor such as photoreceptor generally found in a printing system ( not shown ), in a manner generally known in the art . in various types of printers , there may be multiple such developer units , such as one for each primary color or other purpose . however , those skilled in the art would appreciate that the marking material may be in any color , such as cyan , red , magenta and yellow . if more than one color is processed in the exemplary printing system , a developer for each color may be provided in a universal developer housing . the main elements of a developer unit are a toner container or supplier housing 105 , which functions generally to hold a supply of developer material , a dispenser unit 100 , which can variously mix and transports the marking material , and receptacle or developer housing 115 , which in this embodiment form to apply developer material to a media to form a latent image . other types of features for development of latent images , such as donor rolls , paddles , scavengeless - evelopment electrodes , commutators , and the like , are known in the art and could be used in conjunction with the to be described tone transport apparatus . refilling each developer housing 115 from the associated supplier housing or toner container 105 can include a distribution mechanism , dispenser unit , flexible tube , or toner transport tube or pipe there between having , for example , an auger or spiral member including a spring rotatable within the tube for transporting the toner from each supplier housing to the respective developer housing . each supplier housing is thus in fluid communication with the respective developer housing . the developer material or toner may then be dispensed into the developer housing 115 during an initial tone up and then during all printing to maintain the proper toner concentration ( tc ). the quantity , level , or toner concentration may be detected by a tc sensor ( not shown ). the concentration amount of the toner supplied to developer housing 115 may be controlled to adjust the concentration . such amount may be determined by the toner concentration detected by the tc sensor to reach a predetermined concentration level based on time interval , specific model type of the printing machine , specific color , and the like , and may be controlled by small increments manually or automatically using a toner dispense motor ( not shown ). the effective length , size , and orientation of dispenser unit 100 are key elements . these elements must be selected with regard to concentration and intended running speed , in pages per minute , of the printing system . typically , but not necessarily , operating a developer unit in accordance with a desired running speed involves rotating one or more of the various rotating members within the developer unit ( augers , magnetic rolls , paddles , etc .) at predetermined feed rates or speeds . however , it should be noted that the use of a rotating member to transport the toner is only needed in non - vertical scenarios . additionally , rotating a rotatable member such as auger at a particular rotational velocity will affect the amount of marking material in the respective housings . therefore , the length , orientation , and other attributes will have an effect on the overall performance of the developer unit 100 when it is run at a given speed . fig2 is a perspective view of a dispenser 200 having a variable length component using an accordion tube in accordance to a possible embodiment . in particular , dispenser unit 200 comprises a variable length component 110 , a gear assembly 145 , an entry port 140 for receiving a material form a container , and an exit port for delivering the dispensed material . the variable length component 110 and the receptacle 115 may be secured by an appropriate engagement method , securing device , or bond . communication between the entry port and the exit port is provided by an accordion tube 210 that extends into receptacle 115 . fig3 is a perspective view of a dispensing apparatus 300 having transfer component , gear assembly illustrated in fig4 , and telescopic drop tube in accordance to a possible embodiment . in particular , the dispensing apparatus comprises an entry port 310 , an exit port 350 , a dispenser or telescopic drop tube 340 , a variable length component 110 , and a gear assembly 360 . gear train assembly 360 connects the telescopic drop tube 340 and variable length component 110 . a material is introduced into variable length component 110 in a direction 330 away from entry port 310 or in a direction 330 towards gear assembly 360 and exit port 350 . a rotating member having a plurality of apertures therein or an auger made from a helical spring can be mounted in either telescopic drop tube 330 or variable length component 110 to transport and deliver the material to its destination . a flexible auger is used when telescopic capabilities and transportation of material is needed for a particular job . a motor rotates 315 the helical spring or member to advance the toner particles through the tube so that toner particles are dispensed from the apertures therein . actuation of the motor can be controlled by a cpu ( not shown ) or a suitably programmed computer ( not shown ). a gear train assembly 360 is a gear train and bevel gear set that enable transmission of power into a rotating member and also rotation 370 of the dispenser about gear train assembly 360 . telescopic drop tube 340 and variable length component 110 could both have telescopic capabilities and both could be equipped with a rotatable member such as auger for transporting the material . the tube would utilize a telescopic tube that can be extended or contracted to variety of fixed ranges to achieve a desired length . the wider of the tubes such as telescopic drop tube 340 would be at the bottom to prevent the build up of material at gear train assembly 360 where the two tubes meet . the tube would contain a flexible auger that expands and contracts corresponding with the length of the tube . the auger is required for non - vertical drop tubes , so that toner material does not build up on the inside of the tubes . rotating coupling mechanism such as gear train assembly 360 would have to be used at the connection between telescopic drop tube 340 and the transfer tube such as variable length component 110 , so that the connection of the drop tube would work regardless of the angles . fig4 is an illustration of gear train assembly 360 in accordance to a possible embodiment . gear train assembly 360 shows an example of a gear construction to which the rotative driving of the rotatable member such as a flexible auger is inputted , reference numeral 410 and 412 designates a first set of gears facing a first axis . reference numeral 414 denotes a second gear facing a second axis . the first set of gears 410 and the second gear 414 work together to generate power and speed to an attached device such as a rotatable member . the gears in the first axis ( 410 , 412 ) are parallel to each other , the gears on the end portions of telescopic drop tube 340 and telescopic component 110 transmit drive from the rotatable member within the tubes . the use of a helical gear or a bevel gear or the like as one of the gears as shown makes it possible to directly bring the gears into meshing engagement . the first gear 410 interposes a gear between the top gear and the bottom gear to thereby construct a gear train , and provide a bevel gear in the gear train to thereby change the inclination of the rotary central shaft . in operation a rotation from a driving member such as a motor at one end of telescopic component 110 causes the top gear of the first gear to rotate in the direction shown by arrow 370 . the rotation of the top gear is translated to the other gears so that second gear 414 rotates and the generated motion is used to rotate the rotatable member . fig5 is a perspective view of a flexible auger 500 in accordance with a possible embodiment . flexible auger 500 has a plurality of blades 510 attached at each end of the telescoping core or variable length component . the flexible auger is disposed within the dispenser unit as shown in fig1 . the rotational core size of the flexible auger is varied to maintain a uniform constant cross sectional filling factor within the dispenser unit . preferably the core is round and the root diameter is varied in a fashion so as to compensate for the volume of developer material that has been picked up at an entry port and used for development at point beyond the exit port . as a general rule the volume discharged by the flexible auger is a function of the diameter ( d ) of the rotational core , flexible auger pitch ( p ), and flexible auger rotational period t ). the pitch of the flexible auger is a variable component that changes with the length . flexible auger 500 expands and contrasts in proportion to length adjustment of the tubing where the flexible auger is disposed within . an expansion and contrasting of the flexible auger causes the pitch to varied . the motor rate or the rotational period needs to be adjusted to maintain a constant flow to compensate for pitch variability . in a first position 505 the flexible auger has a first length 550 and the blades of the flexible auger are a first pitch 520 . in a second position 507 the flexible auger is expanded by an incremental length 540 . the expanded length 560 causes the blades of the flexible auger to a second pitch . although the illustrated embodiments disclose a monochrome xerographic printer where a toner image is transferred from a photoreceptor directly to a print sheet , a “ charge receptor ” can also be an intermediate member or belt that accumulates a set of primary - color toner images from a set of photoreceptors in a color printing apparatus . thus , transfer stations such as generally described and indicated as in the figures can be used to transfer toner images from such an intermediate member to a print sheet . as used herein , the term “ printing apparatus ” may refer to a developer unit installable in a printer ; to a customer - replaceable unit installable in a printer , including or not including a photoreceptor 10 or a developer supply ; to a printer itself ; or to a printing module in a larger , multi - engine printer . it will be appreciated that various of the above - disclosed and other features and functions , or alternatives thereof , may be desirably combined into many other different systems or applications . also that various presently unforeseen or unanticipated alternatives , modifications , variations or improvements therein may be subsequently made by those skilled in the art which are also intended to be encompassed by the following claims . | 6 |
fig1 shows a diagrammatic elevation of the system 10 . a wind diverter 20 sits on top of the vertical , cylindrical wind channel 30 . the wind channel 30 , in turn , rests on top of , and is directly connected to , the fresh water storage tank 40 extending below the surface of the ocean . with continued reference to fig1 , the wind diverter 20 consists of a hollow , curved elbow 21 . an automatic directional vane 26 is attached to the top rear of elbow 21 . horizontal doors 23 and vertical doors 24 attach to the horizontal inlet 65 . air turning vanes 22 are attached to the inside of elbow 21 and extend from the horizontal inlet 65 to the top of a square to round transition 27 . the bottom , round portion of the transition 27 attaches to a short length of cylinder 28 . installed in this cylinder 28 is a bird screen 29 that covers the entirety of the inside of cylinder 28 . this cylinder 28 rests on and is captured by bearings 25 . speaking with reference to fig1 , the curved elbow 21 performs the essential task of diverting wind from the horizontal to the vertical plane . the directional vane 26 operates much like a weather vane by automatically pointing the inlet 65 of the elbow 21 into the wind . the vane 26 attaches at the top rear of the elbow 21 and is large enough and extends far enough to provide the torque necessary from ambient breeze to turn the wind diverter 20 . the horizontal doors 23 and the vertical doors 24 open up to an optimal angle to concentrate air into the elbow 21 without losing efficiency to turbulence and frictional forces . to facilitate this task the doors are as large as practical . the vertical doors 24 are as wide as the inlet 65 . one door will overlap the other when the doors are closed to protect the system from high wind . the horizontal doors are half the vertical dimension of the inlet 65 . this allows them to close without overlapping and be a sufficient length for the outer edges to line up with the outer edges of the vertical doors 24 when both sets of doors are optimally positioned to gather and concentrate wind into the wind diverter 20 . the doors will be hydraulically or pneumatically activated and can be used to throttle wind by partial closing should wind velocity become too high for safe and proper operation of the system 10 . operation of the doors can be automatically controlled by wind sensing and satellite weather data or manually controlled by a human maintenance / operator . turning vanes 22 stabilize the wind as it enters the wind diverter 20 and makes it more laminar as it exits . the turning vanes 22 are curved sheets of material attached to the inside of the curved elbow 21 . they divide the area of the inlet 65 into separate horizontal equal areas . their geometry is such that they smoothly transition these inlet areas to smaller but equal areas at the wind diverter outlet 67 . turning vanes are commonly used in commercial ducting elbows to combat friction and turbulence . between the doors gathering wind and the inlet 65 being larger than the outlet 67 the ambient wind speed is increased before it flows out of the curved elbow 21 and into the rectangular to round transition 27 . the transition 27 has an optimal apex angle to , once again , cut down on frictional forces and turbulence of the air . it transitions down to the same circular size as the upper opening in the vertical wind channel 30 . a short stub column 28 is attached to the circular bottom of the transition 27 . this cylindrical stub column 28 is the same size and shape as the vertical wind channel 30 . bearings 25 are to be placed between the stub column 28 and the channel 30 . these bearings 25 allow the wind diverter 20 to rotate 360 degrees in relation to the wind channel 30 . the bearings 25 are so configured as to capture the wind diverter 20 and keep it from being blown off in a high wind . the bearings 25 will also be designed so as to provide reduced friction bearing surfaces for both downward and uplift loads coming from the wind diverter 20 . a bird screen 29 is installed in the stub cylinder does two things . obviously it keeps birds , bats , and debris from entering the system . it also causes a pressure build - up on top of the screen 29 that evens out the flow from the vertical outlet 67 of the wind diverter 20 into the top of the wind channel 30 . continuing with reference to fig1 , the vertical wind channel 30 is housed by a cylindrical casing plate 31 that extends downward almost to sea level . a gas - to - liquid heat exchanger 50 is installed in the upper portion of the channel 30 . an upper dow inlet header 61 is continuously connected to a lower dow outlet 62 by a number of parallel heat exchanger circuits 63 . the inlet header is fed by the dow inlet piping 51 . the outlet header 62 feeds dow to a downcomer pipe 34 and through a seawater energy reclamation turbine / generator 47 and turbine outlet piping 73 . aligned with the bottom elements of the heat exchanger 50 are channels 36 for collecting condensate from the exchanger . this condensate is introduced into a fresh water collection tank 33 that serves as a temporary storage before it goes into a fresh water collection drain 35 that routes the fresh water through a fresh water energy reclamation turbine / generator 46 . at the bottom of the wind channel 30 is a wind turbine 37 vertically mounted with its axis aligned with the center of the channel 30 . the turbine 37 is attached to a shaft 38 attached to a gearbox / generator 39 . below the turbine 37 are wind outlets 75 spaced symmetrically around the base of the vertical channel 30 . with reference to fig1 , as air leaves the wind diverter 20 it enters the top of the vertical wind channel 30 and the inlet of the gas - to - liquid heat exchanger 50 . the gas - to - liquid heat exchanger 50 allows heat to flow from the ambient air to the cold seawater . the heat exchanger 50 is constructed to offer the least resistance to airflow while transferring as much heat as possible . moisture in the air condenses out on the surfaces of the exchanger 50 . beads of moisture join to form rivulets and run down the fins and pipe to the bottom - most point and drip off . this moisture drips into channels or guttering 36 for collecting water . these channels 36 are designed to offer little air resistance while maximizing capacity for collecting water . their open tops will be in exactly the right place and just wide enough to receive the dripping water . they will be slanted to direct the water into the fresh water collection tank 33 . the gutters will be no wider than the small bore pipe but will get deeper as they approach the wall of the vertical air channel 30 to handle more water . penetrations in the cylindrical casing plate 31 allow the water to enter a fresh water collection tank 33 attached to the outside of casing plate 31 . from the collection tank 33 water goes into the fresh water collection drain 35 . this drain conducts the fresh water through a fresh water energy reclamation turbine / generator 46 producing electricity to be conducted away from the turbine by conductive cables 56 . cold ocean water is introduced into the heat exchanger 50 through the heat exchanger inlet piping 51 that extends between the dow inlet pump 59 and the heat exchanger upper liquid inlet header 61 . it travels multiple parallel passes 63 through the heat exchanger 50 . individual passes will consist of a vertical run of small bore piping so as not to block the air flow . in addition to small - bore piping , fins will be attached to the pipe . these fins will be axial to the pipe , forming vertical paths offering little wind resistance . the fins absorb heat from air passing over them and conduct it to the wall of the pipe where it is transferred to the cold seawater . as the air gets cooler in these channels it becomes denser and falls faster . alternately , passes may consist of plate exchangers where the path for the liquid is formed in a plate and welded to another plate , usually flat . the sectional profile these plates present to the air path are only slightly wider than the channel allowing liquid to pass between the plates . the plate provides a similar heat transfer surface as the fins in the previously described pass involving pipes and fins . likewise , air between these plate exchanger passes becomes cooler , denser , and falls faster as it travels downward through the heat exchanger 50 . the cold seawater flows from the multiple passes 63 into the lower liquid outlet header 62 and into a dow return piping 34 which routes the water through a seawater energy reclamation turbine / generator 47 . this generator creates electricity conducted elsewhere by electrical cables 57 . from the turbine / generator the cold seawater is allowed to mix with ocean surface water where it can enrich the water with nutrients and cool it for oxygen retention . this conditioned ocean surface water can then be used in various forms of aquaculture . alternately , the used seawater can be piped back to the depths of the ocean . once through the heat exchanger 50 , cooled air keeps accelerating until it reaches a horizontally mounted wind turbine 37 in the base of the wind channel 30 . this wind turbine 37 fills most of the area of the channel at this point . the space between the tips of the turbine blade and the inside wall of the cylindrical casing plate 31 will be minimal to keep air from going around the blade tips and bypassing the turbine 37 . the horizontal mounting of the turbine will allow bearings to be used that will be more efficient and last longer than those used in a typical vertically installed wind turbine . the blades of this turbine 37 will not have to endure the same stresses as blades of a vertical wind turbine . the constant loading and unloading of gravitational loads on the blades will be gone as well as intermittent and unbalanced wind loads from support tower interference . as a result , this turbine will be able to operate at the higher normal wind speeds system 10 will generate . the turbine 37 is connected via a shaft 38 to a gearbox / generator 39 . this generates electricity distributed to shore by conducting cables 55 . the generator / gearbox will be housed in an aerodynamic shape to cause as little wind turbulence as possible . as it passes through the turbine , air will exit the vertical channel 30 through symmetrically spaced wind outlets 75 around the base of the channel 30 . description of the water storage tank 40 for system 10 below and securely affixed to the vertical wind channel 30 is the water storage tank 40 . still speaking towards fig1 , a portion of this tank 40 is above sea level but much of it extends below the surface of the ocean to provide stability for the system 10 and storage space for fresh water produced by the system . it is cylindrical in shape and can be the same or a different diameter than the cylindrical casing plate 31 but is structurally integral with the casing plate 31 . at the very top of the water storage tank 40 is the service deck 71 . this deck provides a mounting and access area for the turbine 37 and generator 39 as well as the hydropower reclamation pumps 46 , 47 and the dow inlet pump 59 . it forms the roof of the water storage tank 40 . how far down the water storage tank 40 extends into the ocean is a function of what is needed to stabilize the system 10 and store fresh water . the bottom 41 is sealed from seawater intrusion by ordinary metal fabrication techniques . at the bottom of the tank 40 is the fresh water outlet pump 42 that takes in water through the fresh water tank outlet 44 . the pump 42 is situated inside the fresh water pump access chamber 77 and pumps the fresh water into a pipe 45 that takes the fresh water to shore . ideally , this pipe 45 and the electrical conducting cables 55 would be efficiently combined to save space and installation costs . attached to the bottom of the storage tank are anchoring cables 53 . these attach to seabed anchors 54 . these anchor cables and anchors will be symmetric about the system 10 and sufficient in quantity to keep the system stable and anchored even during high wind and waves . this arrangement is typical for many spar - type offshore platforms . the buoyancy of the water storage tank 40 keeps a positive load on the anchor cables 53 and provides stability to the system 10 . with regards to fig1 , fresh water enters the fresh water storage tank 40 through the inlet pipe 43 . when there is sufficient water in the tank , it is pumped to shore to be used for domestic use or for agriculture . alternatively , it could be lightered to a tanker and shipped anywhere . there will be stairwells or ladder wells 49 to access various levels of the tank for maintenance and to access the fresh water outlet pump 42 at the bottom of the water storage tank . this pump 42 is shown located at the bottom of the water storage tank but may be located at the top of the tank or on the service deck 71 . in addition to stair wells or ladder wells 49 there will be enough air - filled cavities due to structure , servicing , and maintenance requirements to give the water storage tank 40 enough buoyancy to support the service deck 71 , vertical wind channel 30 , and the wind diverter 20 and provide for a safe , stable system 10 . the pipe 45 taking water from the tank to shore will be placed on or under the ocean floor for security of the system . with the most toxic thing it will carry being distilled water ( which could be deadly for some ocean creatures but would quickly dilute to an ambient salinity ) the pipe may be suspended partially submerged at elevations safe from fishing nets . this is a less expensive way to install the piping 45 to shore . fig2 a and 2 b show the rotating wind diverter 20 in more detail with fig2 a showing the doors 23 and 24 open for collecting wind and fig2 b showing the doors closed for protection against high wind . fig2 a and 2 b also show the distribution of several bearings 25 about the bottom periphery of the stub cylinder 28 to take the load of the wind diverter 20 and allow it to rotate . fig3 shows the system 100 as an onshore installation . locating close to the shore line takes advantage of heightened wind activity typical of such a location and gives wider options for material and logistics in construction . this system 100 has a cold ocean water or dow suction pipe 52 that extends from shore to the closest access to such cold water as to provide efficient functioning of the system 100 . this system 100 functions much the same as system 10 in that the fresh water is collected by the same guttering / channels 36 , but the water then feeds through a freshwater collection pipe 112 directly into a reservoir 111 that stores the water for further distribution inland . this reservoir 111 also builds up hydraulic energy to be tapped by a channel or sluice 113 that feeds the water through a turbine / generator 115 . conducting cables 117 carry this electricity to an appropriate device for combining it with electricity from the wind turbine generator 39 and the seawater energy reclamation turbine / generator 47 to produce uniform electrical power that is fed to the grid for distribution . fig4 is a diagrammatic plan view of a system 10 being deployed in multiple locations offshore . the water is pumped from each individual system &# 39 ; s storage to the next until it is received by a system 10 directly connected to a reservoir 111 onshore . electrical energy is gathered in a similar manner to be conveyed to the onshore electrical grid . fig5 shows an independent , ocean - going system 200 where additional infrastructure 220 in the form of several levels or decks has been installed . these levels or decks 220 would rest on and connect multiple spars or flotation jackets 231 that would support said decks . also , penstocks 240 for aquaculture are installed below the embodiment to take advantage of nutrient rich dow . another advantage of dow for aquaculture is the temperature allows for a higher level of oxygen and limits development of unwanted microorganisms . the penstocks 240 would employ netting 245 in vertical 241 and horizontal 243 locations to divide the area into pens . shelving 261 or suspended baskets 265 would be used to support the growth of a variety of mollusks . the first level 223 would house processing facilities for the aquaculture and any other industrial machinery or facilities such as deep ocean mining equipment . this level would also be used to install heat exchangers that would further extract moisture from the ambient air being forced through the system increasing the system &# 39 ; s ability to produce fresh water . the second level 225 would be a communal area ; cafeteria , schools , gym , recreation , shops . the third level 227 would be living area . decks would be added to each level for outdoor activity or gardening . alternatively , the first , second , third , any combination or all of the levels could be a server farm utilizing the cool , relatively dry air to keep the machines cool and working properly . the number of levels should not be limited to three and could be as many as structural design criteria allow . the embodiment shown in fig5 also employs a means for locomotion 235 , being a propeller powered by electricity . these would be located on the bottoms of each support jacket or spar 231 . the dow suction pipe 252 for this embodiment would come from the bottom of the fresh water storage tank 40 to prevent fouling the penstocks 240 . the end of the suction pipe 252 would also employ a propulsion and guidance system 237 to keep the end at depth in the dow or cold ocean water while the system 200 is being moved . a further embodiment of the system 300 is shown in fig6 . in this embodiment the vertical channel 30 and diverter 20 of system 100 is installed in multiple locations in an ocean - going vessel 327 . the cylindrical power column 30 extends through the deck 341 and connects with a common plenum with an inlet 311 near the bow of the vessel 327 and an outlet 313 at the stern . electrical power generated by the multiple systems 100 would power a propeller or propellers that would move the ship 327 forward . the water produced would be transported to a towed barge 350 shown in fig7 via a towing cable / pipe / electrical conductor 331 . this barge 350 consists of three cylindrical tanks ; 353 , 355 , and 357 . they are connected and held stable by struts 355 . water would be stored in the bottom tanks 355 and 357 . excess electrical energy would be used to perform hydrolysis on fresh water or seawater to form hydrogen to be stored in the upper tank 353 . not only can this embodiment 300 haul cargo without the expense of fuel , water and hydrogen can be sold at ports of call . also , the hydrogen could be used to fuel an alternate propulsion system should electrical power not be available for any reason . this type of cargo vessel 300 would be a faster method of shipping cargo without fuel costs than the proposed resurrection of sailing ships . it could also be used as emergency sources of water and electricity for coastal cities in emergency situations such as the aftermath of hurricanes or earthquakes . fig8 shows another embodiment 400 with a simpler wind diverter 80 and a contraction cone 83 installed in the vertical cylinder 30 . the wind diverter 80 is a smaller , simpler device without doors . ambient air is directed into the top of the cylinder 30 . before ambient air reaches the turbine blade 37 it passes through a contraction cone 83 . this is similar a mechanism used in wind tunnels to concentrate air without the air becoming turbulent . this allows the turbine 37 to be smaller but operate at a higher speed . this cuts costs for the turbine blade and simplifies the gearbox portion of the gearbox / generator 39 . this embodiment also shows underwater living levels 90 beneath the water storage portion of the vertical cylinder . these levels 90 are connected with the surface by stairs , ladder , or elevator and can be used for leisure as a resort destination or for scientific endeavors or a combination of the two . | 5 |
as used above and throughout the description of the invention , the following terms , unless otherwise indicated , shall be defined as follows : as used herein the term “( c 1 - c 4 ) alkyl ” refers to a straight or branched , monovalent , saturated aliphatic chain of 1 to 4 carbon atoms and includes , but is not limited to , methyl , ethyl , propyl , isopropyl , butyl , isobutyl , and t - butyl . the term “( c 1 - c 4 ) alkyl ” includes within its definition the term “( c 1 - c 3 ) alkyl ”. as used herein , the term “ halo ” refers to a chlorine , bromine , or fluorine atom , unless otherwise specified herein . as used herein , the term “ ph ” refers to a phenyl group . as used herein the term “— o —( c 1 - c 3 ) alkyl ” refers to a straight or branched , monovalent , saturated aliphatic chain having from 1 to 3 carbon atoms attached to an oxygen atom . typical “— o —( c 1 - c 3 ) alkyl ” groups include methoxy , ethoxy , propoxy , isopropoxy , and the like . as used herein , the term “ fluorosubstituted ( c 1 - c 3 ) alkyl ” refers to a straight or branched , monovalent , saturated aliphatic chain having from 1 to 3 carbon atoms wherein 1 to 7 hydrogen ( s ) have been replaced with a fluorine atom and includes , but is not limited to (— cf 3 ), (— cf 2 cf 3 ), (— chf 2 ), (— cf 2 ch 3 ) and (— ch 2 cf 3 ). “ agonist ( s )” shall refer to those compounds which stimulate the functional response of a receptor . “ neutral antagonist ( s )” shall refer to those compounds which do not alter the basal activity of a receptor but block the functional activity of agonists and inverse agonists by returning the functional response to that of the basal state . “ inverse agonist ( s )” shall refer to those compounds which possess negative intrinsic activity by reversing the constitutive activity of the receptor . inverse agonists act to inhibit or reverse the activity of agonists . “ obesity ” refers to the condition of having a high amount of body fat . a person is considered obese if he or she has a body mass index ( bmi ) of 30 kg / m 2 or greater . a person with bmi = 27 - 30 is generally considered overweight . conventionally , those persons with normal weight have a bmi of 19 . 9 to 25 . 9 . the obesity may be due to any cause , whether genetic or environmental . examples of disorders that may result in obesity or be the cause of obesity include overeating , decreased physical activity and pathological conditions showing reduced metabolic activity . “ pharmaceutically acceptable salts ” and “ salts ” refer to the relatively non - toxic , inorganic and organic acid addition salts , and base addition salts , of compounds of the present invention . see , for example s . m . berge , et al ., “ pharmaceutical salts ,” j . pharm . sci ., 66 , 1 - 19 ( 1977 ). “ pharmaceutical composition ” and “ composition ” are intended to encompass a product comprising the active ingredient , preferably present in pharmaceutically effective amounts , and the inert ingredient ( s ) ( pharmaceutically acceptable excipients ) that make up the carrier , as well as any product which results , directly or indirectly from combination , complexation or aggregation of any two or more of the ingredients , or from dissociation of one or more of the ingredients , or from other types of reactions or interactions of one or more of the ingredients . accordingly , the pharmaceutical compositions of the present invention encompass any composition made by admixing a compound of formula ( i ), ( ia ), ( ib ), ( ic ), ( id ), ( ie ) or ( if ) and any pharmaceutically acceptable excipients . “ prevention ” ( of obesity ) refers to preventing obesity from occurring if the treatment is administered prior to the onset of the obese condition . moreover , if treatment is commenced in already obese subjects , such treatment is expected to prevent , or to prevent the progression of , the medical sequelae of obesity ( e . g ., arteriosclerosis , type ii diabetes , polycystic ovarian disease , cardiovascular diseases , osteoarthritis , dermatological disorders , hypertension , insulin resistance , hypercholesterolemia , hypertriglyceridemia , and cholelithiasis ). “ solvate ” means a physical association of a compound with one or more solvent molecules . this physical association includes hydrogen bonding . in certain instances the solvate will be capable of isolation , for example when one or more solvent molecules are incorporated in the crystal lattice of the crystalline solid . “ solvate ” encompasses both solution - phase and isolable solvates . exemplary solvates include hydrates , ethanolates , methanolates , and the like . “ treating ,” as used herein , unless otherwise indicated , means reversing , alleviating , inhibiting the progress of , or preventing the disorder or condition to which such term applies , or one or more symptoms of such disorder or condition . the term “ treatment ” as used herein , unless otherwise indicated , refers to the act of treating as “ treating ” is defined immediately above . “ mtbe ,” as used herein , unless otherwise indicated , means methyl tert - butyl ether . “ psig ,” as used herein , unless otherwise indicated , means pounds per square inch gauge . “ naotbu ” and “ kotbu ,” as used herein , unless otherwise indicated , means sodium tert - butoxide and potassium tert - butoxide respectively . for the therapeutic utility taught herein , the salt of the claimed compounds must be pharmaceutically acceptable . for further details on pharmaceutically acceptable salts , see journal of pharmaceutical science , 66 , 1 ( 1977 ). it will be understood that the compounds of the present invention described below may exist as distinct crystal forms prepared by crystallization under controlled conditions . in scheme i , a compound of formula ( ii ) may be prepared by the method described by andreichikov and coworkers ( andreichikov , et al . zhurnal organicheskoi khimii 22 ( 10 ), 2208 - 13 ( 1986 )), in which a mixture of an amine of formula ( 1 ) and an aldehyde of formula ( 2 ) is treated with an ester of pyruvic acid ( 3 ), where q 1 is a c 1 - 3 alkyl group , in a suitable solvent . suitable solvents include glacial acetic acid , dioxane , tetrahydrofuran , benzene , and toluene . this reaction may also be performed in the presence of solvent mixtures containing these solvents . suitable esters of pyruvic acid include ethyl pyruvate . the reaction may proceed at temperatures between room temperature and the boiling point of the solvent or solvent mixture . in some cases , the product ( ii ) may precipitate during the course of the reaction or upon addition of a solvent in which the product is not highly soluble . these solvents include diethylether , heptane , mtbe , acetone , water , toluene , and pentane and mixtures thereof . if a precipitate is formed , the compound of formula ( ii ) may be isolated by filtration and vacuum drying . alternatively , the compound may be isolated by concentration of the reaction and chromatography of the residue or by aqueous workup and concentration and chromatography of the organic extracts . in scheme ii , a compound of formula ( iii ) may be prepared by treatment of a compound of formula ( ii ) with water , optionally in the presence of an acid or a mixture of acids . this reaction may also optionally be performed in the presence of additional solvents such as tetrahydrofuran , methanol , acetic acid and toluene . suitable acids include hydrochloric acid , sulfuric acid , acetic acid and trifluoroacetic acid . suitable reaction conditions include treatment of a compound of formula ( ii ) with acetic acid , water and trifluoroacetic acid at about ambient temperature for around 1 hour or treatment of a compound of formula ( ii ) in a mixture of acetic acid and hydrochloric acid at around room temperature for about 22 hours . also , the compound of formula ( iii ) can be prepared by hydrolysis with acetic acid at around 80 ° c . for about 8 hours . also , the compound of formula ( iii ) can be prepared by hydrolysis with mixing with dowex 50 - 2x200 ion exchange resin in aqueous methanol at about ambient temperature for around 5 hours . also , the compound of formula ( iii ) can be prepared by hydrolysis with trifluoroacetic acid in a biphasic mixture with the solvents toluene and water for around 1 hour at about room temperature . it is often advantageous to perform this reaction in the presence of at least one equivalent of 2 , 5 - dimethoxytetrahydrofuran . once the compound of formula ( iii ) has formed , it can be isolated by pouring into water and extraction with organic solvents such as dichloromethane , diethylether , ethyl acetate , isopropyl acetate and toluene . the extract may be dried over a desiccant such as sodium sulfate and concentrated to provide the product as a crude mixture . it is often advantageous to use this compound directly in the next reaction rather than to purify it further . in some cases , pouring the reaction onto ice / water allows precipitation and isolation of the compound of formula ( iii ) through filtration . in scheme iii , a compound of formula ( iv ) may be prepared by treatment of a solution of a compound of formula ( iii ) with a compound of formula ( 4 ). suitable solvents include dichloromethane , tetrahydrofuran , or toluene and may be performed at temperatures ranging from room temperature to around 80 ° c . this reaction may be promoted by removal of water as it is formed by treatment with a dehydrating agent such as na 2 so 4 or mgso 4 or 4a molecular sieves or azeotropic removal of water . this reaction may also be performed in the presence of a catalyst such as p - toluenesulfonic acid , acetic acid or other acidic compound . the compound of formula ( iv ) can be isolated , if desired , by methods known in the art such as by precipitation with a solvent such as isopropyl acetate or by silica gel chromatography . in scheme iv , a compound of formula ( i ), ( ia ), and ( ib ) may be formed by treatment of a compound of formula ( iv ) under suitable reducing conditions . suitable reducing conditions include treatment with nacnbh 3 in the presence of acetic acid with an optional solvent such as dichloromethane at around room temperature for about 30 minutes to about 12 hours , treatment with nabh 4 in an alcoholic solvent , treatment with na ( oac ) 3 bh in the presence of trifluoroacetic acid in a suitable solvent such a toluene at room temperature for about 23 hours , and hydrogenation conditions in which a solution of compound of formula ( iv ) is treated with a suitable metal catalyst under a hydrogen atmosphere . suitable solvents include methanol , ethanol , ethyl acetate and tetrahydrofuran . suitable metal catalysts include palladium on carbon and platinum oxide . compound of formula ( iv ) is dissolved in ethanol and methanol mixture and subjected to a hydrogen atmosphere in the presence of a suitable catalyst such as pd / c at around room temperature for about 24 hours . the reaction is filtered and concentrated in vacuo to obtain the compound of formula ( i ), ( ia ), or ( ib ). the compound of formula ( i ), ( ia ), or ( ib ) can be isolated by means such as aqueous workup or precipitation of the product . further purification may be performed by use of such techniques as scx - 2 ion exchange chromatography , silica gel chromatography , supercritical fluid chromatography , reverse phase chromatography and crystallization . purification may also be performed by treatment of mixtures containing a compound of formula ( i ), ( ia ), or ( ib ) with an acid to provide the salt of compound of formula ( i ), ( ia ), or ( ib ) which may then be purified by crystallization to provide the purified salt of the compound of formula ( i ), ( ia ), or ( ib ). preferred salts include those formed by addition with hydrochloric acid and p - toluenesulfonic acid . in the synthesis of a compound of formula ( i ), ( ia ), or ( ib ), either of the intermediates of formula ( iii ) or formula ( iv ) may be used directly in subsequent reactions without purification of the crude intermediates . single enantiomers of compounds of formula ( i ), ( ia ), or ( ib ) are generally preferred over the corresponding racemates . these enantiomers may be prepared by resolution of a compound of formula ( i ), ( ia ), or ( ib ) using techniques such as preparative chromatography employing a chiral stationary phase . the enantiomers may also be prepared by resolution which comprises formation of a salt of the racemic mixture with an optically active acid and purification of the desired diastereomeric salt . the desired diastereomeric salt may be purified by crystallization . alternatively , any of the intermediates of formula ( ii ), ( iii ), or ( iv ) may be resolved to provide substantially a single enantiomer which may then be converted using the methods described above to provide a compound of formula ( i ), ( ia ), or ( ib ) in its enantiomerically purified form such as compounds of formula ( ic ), ( id ), ( ie ) or ( if ). the intermediates of formula ( ii ), ( iii ), or ( iv ) may be prepared by resolution of compounds of the corresponding racemic compound using techniques such as preparative chromatography employing a chiral stationary phase . an alternative and often preferred method for the preparation of purified enantiomers of compounds of formula ( iii ) is outlined in scheme v . a racemic compound of formula ( iii ) is reacted with a compound of formula ( 5 ), in which q 2 is hydrogen , halogen , or a ( c 1 - c 3 ) alkoxy group , to form a diastereomeric mixture of compounds of formula ( xivc ), ( xivd ), or ( xive ) and ( vb ). preferred compounds of formula ( 5 ) include r - alpha - methylbenzylamine , s - alpha - methylbenzylamine , r - 4 - chloro - alpha - methylbenzylamine , s - 4 - chloro - alpha - methylbenzylamine , r - 4 - methoxy - alpha - methylbenzylamine , and s - 4 - methoxy - alpha - methylbenzylamine . this condensation may be performed by combining a compound of formula ( iii ) and compound ( 5 ) an inert solvent such as methylene chloride , tetrahydrofuran , or toluene and optionally heating from room temperature to around 80 ° c . to until the completion of the reaction . this reaction may be promoted by removal of water as it is formed by treatment with a dehydrating agent such as na 2 so 4 or mgso 4 or 4a molecular sieves or azeotropic removal of water . this reaction may also be performed in the presence of a catalyst such as p - toluenesulfonic acid , acetic acid or other acidic compound . the diastereomers of formula ( xivc ), ( xivd ), or ( xive ) and ( vb ) are then separated using techniques such as silica gel chromatography or crystallization from inert solvents such as isopropanol or mixtures of solvents . the desired diastereomer ( designated ( xivc ), ( xivd ), or ( xive ) in scheme v ) is then hydrolyzed to form the purified enantiomer of formula ( iiia ). suitable hydrolysis conditions include treating a solution of the desired diastereomer in acetic acid with aqueous hydrochloric acid . in some instances , the crude ( iiia ) may contain substantial amounts of the dimer of formula ( vi ). in scheme v , the racemic compound of formula ( iii ) may be crude product resulting from the process outlined in scheme ii . in addition , the purified enantiomer of formula ( iiia ) may be used directly from the hydrolysis reaction , without further purification , in the process outlined in scheme iii . in scheme v , the ( r )- enantiomer of compound ( 5 ) was chosen to exemplify the process . one skilled in the art will recognize that the ( s )- enantiomer of compound ( 5 ) may also be used in this process . the choice of whether to use the ( r )- or ( s )- enantiomer may be made depending on which will yield the desired diastereomer that is more readily isolated . in scheme vi , the compound of formula ( ivb ) may also be formed by treatment of compound of formula ( vi ) with compound ( 4 ) under the same conditions as described for the reaction of compound ( iiia ) with ( 4 ). in some cases , heating the reaction in a microwave reactor may be advantageous . in scheme vii , the compound of formula ( vii ) may be prepared as described . a compound of structure ( 6 ) is coupled to a compound ( 1 ) with agents such as tbtu , edci or hobt and an optional catalysts such as dmap and an appropriate solvent such as dimethylformamide and triethylamine at around room temperature for about 18 hours . aqueous acidic work - up , concentration and silica gel chromatography or trituration with solvents such as hexane gives the compound of structure ( 7 ). the ketone group of compound ( 7 ) is converted to the alcohol group of compound ( 8 ) with a reducing agent such as sodium borohydride in solvent mixtures such as water , methanol , ethanol , and dme at about room temperature to 0 ° c . an alternative and often preferred method , compound ( 7 ) may undergo chiral reduction to form compound ( 8 ) in which one of the enantiomers is enriched . methods for chiral reduction of ketones are known in the art ( see , for instance , singh , synthesis 605 ( 1992 ); wallbaum and martens , tetrahedron : asymmetry 3 , 1475 ( 1992 ); matteoli , beghetto , and scrivanti , j . molecular catalysis a : chemical 140 , 131 ( 1999 ); heiser , broger , and crameri , tetrahedron : asymmetry 2 , 51 ( 1991 )). suitable chiral reducing conditions include treatment under hydrogenation conditions using a chiral catalyst such as ( r - tol - binap ) rucl 2 , and reduction mediated by a chiral oxazaborolidine catalyst ( also known as cbs reduction ; corey , bakshi , and shibata , j . amer . chem . soc . 109 , 5551 ( 1987 )). the reaction is performed in a parr vessel under hydrogenation atmosphere in a suitable solvent such as methanol at around 80 ° c . for about 24 hours . compound ( 8 ) is isolated by acidic aqueous work up and concentration . in the following step , the lactam compound of formula ( vii ) is produced via cyclization of compound ( 8 ) in a solvent such as tetrahydrofuran and with the addition of tosyl chloride by treatment drop - wise with a solution of a base such as kot - bu at about − 40 ° c . the reaction is warmed to room temperature and aqueous ammonium chloride is added and concentrated . the residue is dissolved in an appropriate solvent such as ethyl acetate , washed with brine and dried . work - up and purification by methods known in the art such as silica gel chromatography affords compound of formula ( vii ). alternatively , compound ( 8 ) is subjected to cyclization conditions such as n - butyllithium at around − 78 ° c . in an appropriate solvent such as tetrahydrofuran for about 30 minutes . p - toluenesulfonyl chloride is added . after approximately an additional 18 hours and by methods known in the art such as chiral chromatography , compound ( vii ) is isolated . in scheme viii , a compound of formula ( viii ), in which g is hydrogen , c 1 - 4 alkyl , c 1 - 4 haloalkyl , or phenyl , optionally substituted with c 1 - 3 alkyl or halo , is prepared by treatment of a compound of formula ( vii ) with a compound of formula gcooq 3 , in which q 3 is c 1 - 4 alkyl , under basic conditions such as sodium hydride , in a solvent such as toluene at approximately room temperature followed by silica gel chromatography . compound ( ix ) is then formed by treatment of compound ( viii ) with a compound of formula q 4 so 2 n 3 , in which q 4 is phenyl , optionally substituted with c 1 - 3 alkyl , c 1 - 3 alkoxy , halo , or nhco c 1 - 3 alkyl . the reaction may be performed in a solvent such as acetonitrile and stirred for approximately 30 minutes . work - up and purification by methods known in the art such as silica gel chromatography affords compound of formula ( ix ). in scheme ix , a compound of formula ( i ), ( ia ), and ( ib ) may be prepared by treatment of a solution of a diazolactam of formula ( ix ) with compound ( 4 ) in an inert solvent with a suitable catalyst . suitable catalysts include rh 2 ( oac ) 4 . the compound of formula ( ix ) and compound ( 4 ) are dissolved in toluene under a nitrogen atmosphere and heated to around 45 ° c . the catalyst , rh 2 ( oac ) 4 , is added and the reaction is continued to be stirred at around 45 ° c . for about 30 minutes . concentrating the reaction mixture provides the crude compound of formula ( i ), ( ia ) or ( ib ) which is isolated by methods known in the art such as scx - 2 ion exchange , silica gel chromatography , and supercritical fluid chromatography . in scheme x , the compound ( 4 ) is prepared by treatment of a compound ( 9 ), in which r 10 is hydrogen , c 1 - 4 alkyl , or c 1 - 4 alkyl - c ( o )—, with acetonitrile in the presence of acid to provide a compound of formula ( 10 ). suitable acids include sulfuric acid and trifluoroacetic acid . after combining the above , the reaction is heated to around 45 ° c . for about 28 hours . the reaction is cooled to about 0 ° c . and quenched with aqueous sodium hydroxide . compound ( 10 ) is isolated by precipitation with ethanol and water . compound ( 10 ) is heated in a solution of aqueous hydrochloric acid to around 90 ° c . for about 20 hours . the reaction is quenched with ice and sodium hydroxide . the compound ( 4 ) is isolated after several washes with methyl t - butyl ether and tetrahydrofuran and precipitation with heptane . in scheme xi , compound ( 4 ) is prepared from a compound of formula ( 11 ). anhydrous cerium ( iii ) chloride is prepared by heating cerium ( iii ) chloride heptahydrate to about 140 ° c . under vacuum and then suspended in an appropriate solvent such as tetrahydrofuran at room temperature . the reaction is cooled to − 78 ° c . and methyllithium is added dropwise . compound ( 11 ) in tetrahydrofuran is added dropwise to the solution . the reaction is stirred at around − 78 ° c . for about 30 minutes to 4 hours and warmed around 20 ° c . after about 1 to 20 hours , the reaction is cooled to around − 78 ° c . and aqueous ammonia is added . the reaction is warmed around 20 ° c . for about 1 hour . the compound ( 4 ) is isolated by methods known in the art such as silica gel chromatography . conditions for hplc methods referred to throughout the preparations and examples : gradient : 5 - 100 % acetonitrile / methanol ( 50 / 50 ) w / 0 . 2 % ammonium formate in 7 . 0 minutes then held at 100 % for 1 . 0 minute column temperature : 50 ° c .+/− 10 ° c . gradient : 5 - 100 % acetonitrile / methanol ( 50 / 50 ) w / 0 . 2 % ammonium formate in 3 . 5 minutes then held at 100 % for 0 . 5 minutes column temperature : 50 ° c .+/− 10 ° c . lc column : phenomenex gemini c 18 2 . 0 × 50 mm 3 . 0 μm gradient : 5 - 100 % acn acn w / 0 . 1 % formic acid in 7 . 0 min . then held at 100 % for 1 . 0 min . gradient : 50 - 90 % acetonitrile w / 0 . 03 m phosphate buffer ( phosphate buffer = 5 . 52 g nah 2 po 4 and 1 . 4 ml h 3 po 4 in 2 l milli - q h 2 o ) in 15 minutes . column temperature : 40 ° c . stir 3 -( trifluoromethoxy ) benzaldehyde ( 15 . 0 g , 78 . 6 mmol ), 4 - fluoroaniline ( 22 . 4 ml , 236 mmol ) and ethyl pyruvate ( 8 . 65 ml , 78 . 6 mmol ) in glacial acetic acid ( 60 ml ) at ambient temperature for 72 hours . filter the precipitate and wash with a 3 : 1 heptane / mtbe mixture . dry under vacuum to afford the titled compound ( 20 . 9 g , 60 %) as an off - white powder : ms ( m / z ): 445 ( m − 1 ). yield 81 % ms ( m / z ): 559 ( m − 1 ) dilute reaction with 3 : 1 heptane / mtbe to aid in filtering . isolate additional product from filtrate by trituration with dcm - meoh . isolate additional product from second filtrate by silica gel chromatography . yield 57 % lcms : 5 . 68 min . ( method 3 ); esms m / z 519 . 2 ( m + 1 ), 517 . 2 ( m − 1 ). yield 50 % ms ( m / z ): 479 ( m + 1 ) no dilution prior to filtering . wash filter cake with heptane . yield 87 % ms ( m / z ): 461 ( m + 1 ) dilute with 3 : 1 heptane / mtbe to aid in filtering . yield 38 % ms ( m / z ): 411 ( m + 1 ) isolate additional product from filtrate by silica gel chromatography and crystallization . yield 29 % ms ( m / z ): 577 ( m − 1 ) reaction time : 18 hours yield 33 % ms ( m / z ): 509 ( m − 1 ) reaction time : 5 days yield 56 % ms ( m / z ): 564 . 8 ( m − 1 ) wash precipitate with 2 : 1 heptane / mtbe . yield 64 . 9 % ms ( m / z ): 527 ( m − 1 ) wash precipitate with hexanes . yield 62 . 7 % ms ( m / z ): 529 ( m − 1 ) wash precipitate with hexanes . yield 67 % ms ( m / z ): 543 ( m + 1 ), 541 ( m − 1 ) reaction time : 24 hours use 2 . 5 equivalents of the 4 -( difluoromethoxy ) aniline . concentrate reaction and purify by silica gel chromatography ( 5 - 20 % etoac - hexanes ). yield 37 % ms ( m / z ): 459 ( m + 1 ), 457 ( m − 1 ) reaction time : 24 hours used 2 . 5 equivalents of the 4 -( difluoromethoxy ) aniline . wash precipitate with 4 : 1 heptane / mtbe . stir a mixture of 3 - methylbenzaldehyde ( 1 . 68 ml , 14 . 21 mmol ), ethyl pyruvate ( 1 . 42 ml , 12 . 93 mmol ), acetic acid ( 1 . 85 ml , 32 . 30 mmol ) in anhydrous tetrahydrofuran ( 3 . 15 ml , 38 . 75 mmol ), under an atmosphere of nitrogen . add 4 -( trifluoromethoxy ) aniline ( 3 . 84 ml , 28 . 42 mmol ) dropwise over 2 min . heat the yellow solution to 80 ° c . for 12 h . cool to ambient temperature and filter the yellow precipitate and wash with 10 % acetone / water ( 50 ml ). dry the yellow solid under vacuum at 40 ° c . to afford the title compound ( 4 . 18 g , 64 %). ms ( m / z ): 509 . 1 ( m + 1 ). combine benzaldehyde ( 50 . 0 g , 472 mmol ), ethyl pyruvate ( 55 . 3 g , 476 mmol ) and acetic acid ( 350 ml ) at ambient temperature under a nitrogen atmosphere and stir for ˜ 10 to 15 minutes . add 4 -( trifluoromethoxy ) aniline ( 183 . 8 g , 1038 mmol ) dropwise over a period of ˜ 1 h while maintaining the temperature at ˜ 35 ° c . stir the resulting mixture at ambient temperature overnight (˜ 16 h ). add isopropyl alcohol ( 350 ml ) and water ( 350 ml ). stir the resulting mixture at ambient temperature of 15 min . filter and rinse the solid with 1 : 1 isopropyl alcohol : water ( 2 × 150 ml ). dry in a vacuum oven at 40 ° c . overnight to yield the title compound as a yellow solid ( 191 . 4 g , 82 % yield ). 1 h nmr ( dmso - d 6 , 500 mhz ): δ8 . 43 ( s , 1h ), 7 . 74 ( dt , 2h , j = 9 . 0 hz , 2 . 8 hz ) 7 . 37 ( dt , 2h , j = 9 . 5 hz , 2 . 2 hz ), 7 . 32 ( d , 2h , j = 9 . 0 hz ), 7 . 30 - 7 . 25 ( m , 4h ), 7 . 22 - 7 . 19 ( m , 3h ), 6 . 43 ( d , 1h , j = 3 hz ), 6 . 08 ( d , 1h , j = 2 . 5 hz ); ms ( m / z ): 493 ( m − 1 ). stir 3 -( trifluoromethoxy )- benzaldehyde ( 25 . 0 g , 132 mmol ) and ethyl pyruvate ( 15 . 3 g , 132 mmol ) in glacial acetic acid ( 125 ml ) at ambient temperature for 10 minutes . add 4 -( trifluoromethyl ) aniline ( 46 . 7 g , 290 mmol ) drop - wise over 15 minutes with continued stirring , warm the solution to 30 ° c ., and stir 22 - 24 h . cool the solution to 26 ° c ., add iso - propyl alcohol ( 125 ml ) and water ( 125 ml ). stir the solution at room temperature for 15 minutes , filter the precipitate and wash with a 1 : 1 mixture of iso - propyl alcohol - water ( 100 ml × 2 ). dry under vacuum at 40 ° c . to afford the titled compound ( 60 . 46 g , 84 %) as a white powder : hplc ( method 4 ) retention time : 10 . 9 minutes . ms ( m / z ): 545 . 1 ( m − 1 ). 1 h nmr ( 500 mhz , dmso - d 6 ) δ 8 . 76 ( s , 1 h ), 7 . 86 ( d , 2 h , j = 8 . 5 hz ), 7 . 70 ( d , 2 h , j = 8 . 5 hz ), 7 . 56 ( d , 2 h , j = 9 . 0 hz ), 7 . 47 ( d , 2 h , j = 8 . 5 hz ), 7 . 44 - 7 . 41 ( m , 1 h ), 7 . 37 ( s , 1 h ), 7 . 29 ( d , 1 h , j = 8 . 0 hz ), 7 . 22 ( d , 1 h , j = 8 . 0 hz ), 6 . 66 ( d , 1 h , j = 3 . 0 hz ), 6 . 29 ( d , 1 h , j = 2 . 5 hz ). mix (±)- 1 -( 4 - isopropyl - phenyl )- 3 -( 4 - isopropyl - phenylamino )- 5 -( 3 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 2 . 0 g , 4 . 04 mmol ), glacial acetic acid ( 30 ml ) and hydrochloric acid ( 20 ml ). stir the reaction mixture at ambient temperature for 1 hour . pour onto ice / water , filter the precipitate , wash with water , and dry under vacuum to afford a yellow solid . take the yellow solid and repeat above procedure to afford the titled compound ( 0 . 9 g , 59 %). ms ( m / z ): 378 ( m + 1 ). dissolve (±)- 1 -( 4 - bromo - phenyl )- 5 -( 3 - trifluoromethoxy - phenyl )- pyrrolidine - 2 , 3 - dione ( 14 . 6 g , 35 . 2 mmol ) in dichloromethane ( 35 ml ). add ( r )-(+)- α - methylbenzylamine ( 6 . 8 ml , 52 . 8 mmol ) and stir overnight at ambient temperature . concentrate the reaction mixture under reduced pressure and purify by silica gel chromatography ( ethyl acetate - hexane ) to yield ( s )- 1 -( 4 - bromo - phenyl )- 3 -(( r )- 1 - phenyl - ethylamino )- 5 -( 3 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one - eluting first ( 6 . 6 g , 36 %): ms ( m / z ): 517 . 0 ( m + 1 ). rp hplc : tr = 5 . 53 min ( method 3 ) and eluting second ( r )- 1 -( 4 - bromo - phenyl )- 3 -(( r )- 1 - phenyl - ethylamino )- 5 -( 3 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 5 . 8 g , 32 %): ms ( m / z ): 517 . 0 ( m + 1 ). rp hplc : tr = 5 . 44 min . ( method 3 ) 1 h nmr ( 400 mhz , dmso - d 6 ) δ 7 . 45 ( dd , 4h , j = 18 . 5 , 9 . 2 hz ), 7 . 33 ( d , 2h , j = 7 . 5 hz ), 7 . 28 - 7 . 19 ( m , 3h ), 7 . 15 - 7 . 05 ( m , 2h ), 7 . 15 - 7 . 05 ( m , 2h ), 6 . 99 ( d , 1h , j = 7 . 9 hz ), 6 . 90 ( s , 1h ), 5 . 89 ( d , 1h , j = 7 . 0 hz ), 5 . 85 ( d , 1h , j = 2 . 2 hz ), 5 . 14 ( d , 1h , j = 2 . 6 hz ), 4 . 35 - 4 . 26 ( m , 1h ), 1 . 43 ( d , 3h , j = 7 . 0 hz ). prepare the following compound essentially by the method of preparation 28 , 31 and 32 . cool the reaction mixture to room temperature and add isopropyl acetate ( 40 ml ) and toluene ( 160 ml ) in a single portion . wash the mixture with water ( 3 ×) and then ph 7 buffer ( 2 ×). separate layers and observe that the aqueous layer is ph = 7 . wash the organic layer with water ( 1 ×) and brine ( 1 ×). observe that the organic layer contains the titled compound . lc - ms esi m / z : 416 ( m - h ). mix ethanol ( 120 ml ), glacial acetic acid ( 15 ml ), water ( 3 . 0 ml , 164 . 7 mmol ), trifluoroacetic acid ( 6 . 2 ml , 82 . 4 mmol ), (±)- 5 -( 3 - trifluoromethoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- 3 -( 4 - trifluoromethyl - phenylamino )- 1 , 5 - dihydro - pyrrol - 2 - one ( 30 . 0 g , 54 . 9 mmol ), and 2 , 5 - dimethoxy - tetrahydrofuran ( 10 . 7 ml , 82 . 4 mmol ). warm the solution to 50 ° c . and stir the reaction mixture for 15 - 18 hours . discontinue heating the solution , add water ( 35 ml ), and cool the reaction mixture to − 19 ° c . filter the slurry and wash the solid with a 1 : 4 mixture of water - methanol ( 20 ml ). transfer the filtrate to a separatory funnel and wash with 6 % brine ( 280 ml ), then add 6 % brine ( 100 ml ), methanol ( 40 ml ), diethyl ether ( 100 ml ), and saturated sodium bicarbonate solution ( 43 ml ) to the organic phase . separate the layers , add methanol ( 60 ml ) to the organic phase , and concentrate the solution to approximately 1 volume containing (±)- 3 - hydroxy - 5 -( 3 - trifluoromethoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one . add ( r )-(+)- α - methyl benzylamine ( 45 . 0 ml , 349 . 8 mmol ) to the organic layer described in preparation 34 or 35 , containing (±)- 3 - hydroxy - 5 -( 3 - trifluoromethoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one . stir the solution at ambient temperature for 72 hours . concentrate the reaction mixture and purify by silica gel chromatography ( 5 - 15 % etoac - hexane ) to yield ( s )- 1 -( 4 - trifluoromethyl - phenyl )- 3 -(( r )- 1 - phenyl - ethylamino )- 5 -( 3 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 32 . 4 g , 37 %) as a tan foam and ( r )- 1 -( 4 - trifluoromethyl - phenyl )- 3 -(( r )- 1 - phenyl - ethylamino )- 5 -( 3 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 26 . 0 g , 29 %) as a pale orange oil . 1 h nmr ( 400 mhz , dmso - d 6 ) δ 7 . 74 ( d , 2h , j = 8 . 8hz ), 7 . 62 ( d , 2h , j = 8 . 8 hz ), 7 . 39 - 7 . 34 ( m , 3h ), 7 . 28 ( dd , 2h , j = 7 . 7 , 7 . 1 hz ), 7 . 21 - 7 . 14 ( m , 4h ), 6 . 04 ( d , 1h , j = 7 . 5 hz ), 5 . 91 ( d , 1h , j = 2 . 6 hz ), 5 . 21 ( d , 1h , j = 2 . 6 hz ), 4 . 31 - 4 . 23 ( m , 1h ), 1 . 42 ( d , 3h , j = 7 . 0 hz ). ms ( m / z ): 507 ( m + 1 ). 1 h nmr ( 400 mhz , dmso - d 6 ) δ 7 . 76 ( d , 2h , j = 8 . 8hz ), 7 . 62 ( d , 2h , j = 8 . 8 hz ), 7 . 34 ( d , 2h , j = 7 . 0 hz ), 7 . 28 - 7 . 20 ( m , 3h ), 7 . 14 - 7 . 06 ( m , 2h ), 7 . 02 ( d , 1h , j = 7 . 9 hz ), 6 . 96 ( s , 1h ), 5 . 96 - 5 . 92 ( m , 2h ), 5 . 19 ( d , 1h , j = 2 . 6 hz ), 4 . 36 - 4 . 27 ( m , 1h ), 1 . 44 ( d , 3h , j = 7 . 0 hz ). ms ( m / z ): 507 ( m + 1 ). prepare the following compounds essentially by the method of preparation ( 34 or 35 ) and 36 and 37 . combine (±) - 5 - phenyl - 1 -( 4 - trifluoromethoxyphenyl )- 3 -( 4 - trifluoromethoxyphenylamino )- 1 , 5 - dihydro - pyrrol - 2 - one ( 100 g , 202 mmol ), 2 , 5 - dimethoxytetrahydrofuran 932 . 4 g , 244 mmol ), toluene ( 400 ml ), water ( 150 ml ), acetic acid ( 50 ml ) and trifluoroacetic acid ( 23 . 5 g , 203 mmol ) under a nitrogen atmosphere . stir for 3 h while maintaining the temperature between 35 ° c . and 45 ° c . cool to ambient temperature and transfer to a separatory funnel with toluene ( 100 ml ). separate the phases and wash the organic phase with water ( 2 × 500 ml ). transfer the organic phase to a separate flask with toluene ( 100 ml ). add ( r )-(+)- α - methyl benzylamine ( 29 . 4 g , 243 mmol ). stir at ambient temperature until the reaction is complete (˜ 18 h ). concentrate the solution under reduced pressure ( 40 ° c . to 46 ° c . at ˜ 26 mm hg ) to a total volume of 250 ml . add isopropyl alcohol ( 500 ml ). concentrate the resulting solution under reduced pressure ( 30 ° c . to 39 ° c . at ˜ 26 mm hg ) to a total volume of 250 ml . add isopropyl alcohol ( 250 ml ). cool the solution to 0 ° c . to − 5 ° c . and seed with the title compound . cool to − 12 ° c . stir for 1 . 5 h , filter , and rinse the solid with cold isopropyl alcohol ( 100 ml ). dry on the filter to afford 46 . 5 g of a tan solid . slurry a portion of this solid ( 42 . 0 g ) in heptane ( 300 ml ) at ambient temperature for 2 h . filter and rinse the solid with heptane ( 2 × 30 ml ). dry the solid to yield the title compound as a light tan solid ( 26 . 0 g , 32 % yield ). 1 h nmr ( cdcl 3 , 500 mhz ): δ7 . 50 ( dt , 2h , j = 8 . 5 hz , 2 . 0 hz ), 7 . 34 - 7 . 28 ( m , 4h ), 7 . 22 - 7 . 17 ( m , 4h ), 7 . 09 ( d , 2h , j = 8 . 5 hz ), 7 . 00 ( dd , 2h , j = 7 . 3 hz , 1 . 8 hz ), 5 . 41 ( d , 1h , j = 3 . 0 hz ), 5 . 05 ( d , 1h , j = 3 . 0 hz ), 4 . 65 ( br s , 1h ), 4 . 34 ( q , 1h , j = 6 . 7 hz ), 1 . 55 ( d , 3h , j = 6 . 7 hz ); ms ( m / z ): 439 ( m + 1 ). charge thf ( 20 ml , 5 vols ) to a flask containing (±)- 5 -( 3 - methyl - phenyl )- 1 -( 4 - trifluoromethoxy - phenyl )- 3 -( 4 - trifluoromethoxy - phenylamino )- 1 , 5 - dihydro - pyrrol - 2 - one ( 4 . 18 g , 8 . 22 mmol ). add acetic acid ( 1 . 88 ml , 32 . 89 mmol ,) to the above clear solution to afford a yellow solution . add 2 , 5 - dimethoxytetrahydrofuran ( 1 . 28 ml , 9 . 87 mmol ,), then add water ( 0 . 2 ml , 9 . 87 mmol ). add tfa ( 1 . 25 ml , 16 . 44 mmol ,) to the reaction mixture and observe a slight exotherm ( 23 to 30 ° c .). heat the reaction mixture to 40 ° c . for 22 hours . pour the brown solution into water ( 50 ml ) and extract with ethyl acetate ( 50 ml × 2 ). wash the organic phase with saturated sodium bicarbonate solution ( 20 ml × 2 ), brine ( 50 ml ), dry over magnesium sulfate and evaporate to afford the titled compound . ms ( m / z ): 350 . 1 ( m + 1 ). charge toluene ( 20 ml ) to a flask containing (±)- 5 - m - tolyl - 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidine - 2 , 3 - dione ( 4 . 13 g ; 11 . 82 mmol ). add 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamine ( 4 . 83 g , 23 . 65 mmol ) to the above solution in an atmosphere of n 2 . heat the reaction mixture to 80 ° c . for 24 hours . cool to ambient temperature and evaporate in vacuo . dissolve in meoh ( 90 ml ) and pass through an scx - 2 ion exchange resin cartridge . evaporate the meoh wash to give the crude product . purify on an scx - 2 ion exchange resin cartridge ( eluent with methanol ) and then by chromatography on a silica gel column eluting with iso - hexane / ethyl acetate ( 80 : 20 ) to afford the titled compound ( 2 . 54 g , 58 %). ms ( m / z ): 536 . 1 ( m + 1 ). add water ( 550 ml ) and trifluoroacetic acid ( 142 ml , 1 . 8 mol ) to a stirred slurry of ( r )- 1 -( 4 - trifluoromethoxy - phenyl )- 3 -(( r )-( 1 - phenyl - ethylamino )- 5 - phenyl - 1 , 5 - dihydro - pyrrol - 2 - one ( 275 g , 621 mmol ) in 1 . 37 l of toluene . stir the resulting biphasic mixture for 3 . 5 h at ambient temperature under a nitrogen atmosphere . transfer the mixture into reactor equipped with a bottom valve by cannula and dilute with water ( 2 . 0 l ) and toluene ( 2 . 0 l ). discard the aqueous layer , and wash the organic phase with 1n hcl ( 1 l ). transfer the organic layer into a new flask and charge with acetic acid ( 200 ml ), and 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamine ( 191 g , 939 mmol ). stir the mixture for 2 hours at ambient temperature and then heat to 40 ° c . for 96 h . add mtbe ( 2 . 0 l ) and wash with water ( 2 . 0 l ). discard the aqueous layer and wash the organic phase with saturated sodium hydrogen carbonate ( 2 . 0 l ). dry the mtbe phase with magnesium sulfate , filter and concentrate to an oil under reduced pressure ( 10 torr , 30 ° c .). dilute the oil with 1 . 0 l of 15 % mtbe / hexanes and stir the resulting slurry for 1 hour at ambient temperature . isolate the solid by vacuum filtration , rinsing the solid with 200 ml of 15 % mtbe / hexanes ( 200 ml ). dry the solid under reduced pressure to obtain ( 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 - phenyl - 1 -( 4 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pryrrol - 2 - one as a white solid ( 326 g , 88 %). 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 78 ( 1 h , d , j = 4 hz ), 8 . 05 ( 1 h , dd , j = 4 , 8 hz ,), 7 . 80 ( 1 h , d , j = 8 hz ), 7 . 63 ( 2 h , m ), 7 . 26 ( 2 h , m ), 7 . 08 - 7 . 18 ( 5 h , m ,), 7 . 02 ( 2 h , m ), 5 . 72 ( 2 h , m ), 4 . 77 ( 1 h , m ), 1 . 65 ( 3 h , s ), 1 . 62 ( 3h , s ); ms ( m / z ): 522 . 0 ( m + 1 ). dry cerium ( iii ) chloride heptahydrate ( 22 . 4 g , 30 . 1 mmol ) at 140 ° c . under vacuum overnight . cool to ambient temperature and add thf ( 120 ml ). stir the mixture for 30 min . to 2 hours . cool the mixture to − 78 ° c . and add methyllithium ( 1 . 6 m in et 2 o ; 38 ml , 30 mmol ) dropwise . stir the reaction mixture at − 78 ° c . for 30 min . to 1 hour and then add a solution of 2 - chloropyridine - 5 - carbonitrile 2 . 77 g , 20 . 0 mmol ) in thf ( 20 ml ). stir 30 min . to 4 hours at − 78 ° c ., allow the reaction mixture to warm to 20 ° c . for 1 hour . cool the reaction mixture to − 78 ° c . and add aqueous ammonia ( 38 ml ). allow the reaction mixture to warm to 20 ° c . for 1 hour . decant the supernatant and wash the solid residue with dichloromethane . concentrate in vacuo the combined organic layers . transfer the resultant residue to a column of silica gel ( 330 g ) and elute ( 0 - 10 % [ 1 m ammonia in methanol ]/ dichloromethane ) to yield 2 . 21 g ( 64 . 8 %) of the titled compound as a yellow oil . ms ( m / z ): 171 . 0 ( m + 1 ). 1 h nmr indicated pure desired product . 1 h nmr ( cdcl 3 ): δ = 8 . 53 ( d , j = 2 . 4 hz , 1 h ), 7 . 82 ( dd , j = 8 . 4 , 2 . 4 hz , 1 h ), 7 . 26 ( dd , j = 8 . 4 , 0 . 8 hz , 1 h ), 1 . 87 ( s , 2 h ), 1 . 50 ( s , 6 h ) ppm . add a solution of dimethyl sulfoxide ( 0 . 82 ml , 11 . 5 mmol ) in dichloromethane ( 2 ml ) over a period of 5 minutes to a solution of oxalyl chloride ( 0 . 46 ml , 5 . 28 mmol ) in dichloromethane ( 10 ml ) cooled to − 78 ° c . stir 10 minutes then add a solution of ( 3 - trifluoromethylsulfanyl - phenyl )- methanol ( 1 . 00 g , 4 . 80 mmol ) in dichloromethane ( 4 ml ). stir 15 minutes then add triethylamine ( 3 . 35 ml , 24 . 0 mmol ). slowly warm to ambient temperature , add water and separate the organic layer . extract the aqueous layer with dichloromethane . dry ( sodium sulfate ) the combined organic layers , filter , and concentrate in vacuo . purify by silica gel chromatography ( 10 % ethyl acetate / hexane ) to afford the titled compound as a yellow liquid ( 896 mg , 91 %). 1 h nmr ( 400 mhz , dmso ) δ 7 . 74 ( dd , j = 7 . 6 , 7 . 6 , 1h ), 8 . 01 ( d , j = 7 . 9 , 1h ), 8 . 09 ( d , j = 7 . 5 , 1h ), 8 . 12 ( s , 1h ), 10 . 03 ( s , 1h ). deoxygenate a mixture of 2 - bromo - 5 - cyanopyridine ( 1 . 83 g , 10 . 0 mmol ), cyclopropylboronic acid ( 1 . 1 g , 13 mmol ), palladium ( ii ) acetate ( 0 . 11 g , 0 . 49 mmol ), and potassium phosphate ( 7 . 4 g , 35 mmol ) in toluene ( 40 . 00 ml ) and water ( 2 ml ) by bubbling nitrogen through the mixture . add tricyclohexylphosphine ( 1 . 0 ml , 1 . 0 mmol , 1 m in toluene ). heat the reaction mixture at 100 ° c . for 14 hours and allow the reaction mixture to cool . decant the supernatant and wash the leftover sludge with dichloromethane . concentrate the combined organics in vacuo . purify by silica gel chromatography ( 0 - 5 % ethyl acetate / hexane ) to afford the titled compound as a white crystalline solid ( 774 mg , 47 %). 1 h nmr ( 400 mhz , cdcl 3 ) δ 1 . 08 ( m , 4h ), 2 . 05 ( m , 1h ), 7 . 23 ( dd , j = 8 . 2 , 1 . 0 hz , 1h ), 7 . 73 ( dd , j = 8 . 0 , 2 . 4 hz , 1h ), 8 . 66 ( d , j = 1 . 2 hz , 1h ). prepare the titled compound , via the procedure described in the german patent entitled “ preparation of 6 -( haloalkyl )- 3 - pyridinecarboxylic acids ”. mueller , peter . ( bayer a .- g ., germany ). eur . pat . appl . ( 2003 ), 13 pp . ep 1340747 a1 20030903 . 1 h nmr ( dmso - d 6 , 500 mhz ): δ 9 . 19 ( s , 1h ), 8 . 53 ( dd , 1h , j = 1 . 5 , 8 . 5 ), 8 . 04 ( d , 1h , j = 8 ), 4 . 38 ( q , 2h , j = 7 ), 1 . 34 ( t , 3h , j = 7 ). cool the contents of an inerted reaction vessel containing technical grade 6 - trifluoromethyl - nicotinic acid ethyl ester ( 45 . 6 moles ; 10 . 00 kg ) and tert - butyl methyl ether ( 71 . 6 l ; 53 . 0 kg ) to 10 - 15 ° c ., and add the solution into a separate inerted reaction vessel cooled to 5 - 12 ° c . containing 3 m methylmagnesium chloride ( 136 . 8 moles ; 45 . 6 l ; 46 . 2 kg ) and tetrahydrofuran ( 76 . 5 l ; 68 . 0 kg ). observe a moderate exotherm during the addition , and maintain the internal reaction temperature between 15 - 25 ° c . confirm that the starting ester is completely consumed by hplc , and cool the reactor contents to 0 - 3 ° c . add the contents from the reaction vessel slowly to a separate reactor cooled to 0 - 5 ° c . containing hydrochloric acid ( 203 moles ; 16 . 67 l ; 20 . 0 kg ) and water ( 81 . 0 l , 81 . 0 kg ), and observe gas evolution . separate the layers and extract the aqueous phase once with tert - butyl methyl ether ( 59 . 5 l ; 44 . 0 kg ). combine the organic layers and wash with a 20 % sodium chloride solution ( 189 . 3 moles ; 46 . 5 l ; 55 . 3 kg ). filter the organic solution , concentrate to approximately 1 volume , and dilute with acetonitrile ( 31 . 8 l ; 25 . 0 kg ). concentrate the solution to approximately 1 volume to provide the titled compound as a technical grade oil ( 7 . 9 kg ; 84 . 4 %, based on hplc ) in acetonitrile . use the crude material as a solution in acetonitrile without further purification . a pure sample of the product can be obtained by following the procedure given below . purification ( optional ): charge the titled compound ( 1 . 81 kg , 8 . 82 moles ) to a 22 - l separatory funnel with methyl t - butyl ether ( 3 l , 2 . 2 kg ), water ( 500 ml ) and saturated aqueous sodium bicarbonate ( 500 ml ) and stir for 10 min . separate the bright yellow aqueous layer and transfer the organic phase to a 22 - l flask . add magnesium sulfate ( 200 g , 1 . 66 moles ) to the flask , stir 10 min . then filter . concentrate the filtrate to an oil and co - evaporate twice with acetonitrile ( 2 × 3 l ) to afford the titled compound as an oil weighing 1 . 64 kg ( 90 . 6 %). 1 h nmr ( dmso - d 6 , 500 mhz ): δ 8 . 85 ( d , 1 h , j = 2 . 5 hz ), 8 . 10 ( dd , 1 h , j = 2 , 8 hz ), 7 . 81 ( d , 1 h , j = 8 hz ), 5 . 42 ( s , 1 h ), 1 . 47 ( s , 6 h ). add acetonitrile ( 67 . 4 l ; 53 . 0 kg ) to a reaction vessel containing 2 -( 6 - trifluoromethyl - pyridin - 3 - yl )- propan - 2 - ol ( 52 moles ; 12 . 8 kg ) and cool to 0 - 5 ° c . add concentrated sulfuric acid ( 372 moles ; 19 . 8 l ; 36 . 5 kg ) slowly , maintaining the internal reaction temperature between 0 - 15 ° c . heat the solution to 25 - 30 ° c . for 24 hours , and observe the completion of the reaction by hplc . cool the mixture to 0 ° c . while stirring and add water ( 95 . 0 l ; 95 . 0 kg ). add a solution of aqueous ammonia ( 57 . 5 kg ) to adjust the solution ph to 8 . 0 - 9 . 0 , and then add tert - butyl methyl ether ( 81 . 1 l ; 60 . 0 kg ). separate the lower aqueous layer , concentrate the organic layer to approximately 3 volumes , and cool the contents of the reaction to − 5 - 0 ° c . filter the resultant solids and dry under vacuum until constant weight and collect ( 13 . 4 kg ; 87 . 3 %, based on hplc ) of the titled compound as a pale yellow solid in 81 . 8 % purity . 1 h nmr ( dmso - d 6 , 500 mhz ): δ 8 . 68 ( d , 1 h , j = 2 hz ), 8 . 30 ( s , 1 h ), 7 . 92 ( dd , 1 h , j = 2 . 5 , 8 . 5 hz ), 7 . 79 ( d , 1 h , j = 5 . 8 hz ), 1 . 82 ( s , 3 h ), 1 . 56 ( s , 6 h ). heat a mixture of n -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethyl ]- acetamide ( 93 . 5 moles , 19 . 1 kg ), concentrated hydrochloric acid ( 805 . 9 moles ; 66 . 2 l ; 79 . 4 kg ), and water ( 79 . 4 l ; 79 . 4 kg ) to 95 - 100 ° c . with stirring under nitrogen for 24 hours . cool the reaction mixture to 20 - 35 ° c . and observe completion of the reaction by hplc . cool the reaction vessel to 10 - 20 ° c . and add tert - butyl methyl ether ( 105 . 4 l ; 78 . 0 kg ). separate the phases , and discard the organic layer . add 15 % sodium hydroxide ( 910 . 9 moles ; 205 l ; 242 . 9 kg ) to the aqueous phase and observe a ph of 9 . 5 - 10 . 5 . extract the aqueous layer with ethyl acetate ( 3 × 89 ml ; 3 × 80 . 0 kg ), combine the organic layers , and discard the aqueous phase . concentrate the solution to approximately 2 volumes , add tert - butyl methyl ether ( 174 l ; 129 . 1 kg ), and concentrate the solution to approximately 2 volumes . dilute the reaction vessel with n - heptane ( 168 l ; 115 . 0 kg ), concentrate the solution to approximately 2 volumes , and dilute with additional n - heptane ( 30 l , 20 . 7 kg ). cool the contents of the reaction mixture to 0 - 5 ° c . and stir the mixture for 2 hours at 0 - 5 ° c . filter and dry the resultant solids under vacuum at 35 - 45 ° c . to afford the titled compound ( 14 . 19 kg ; 74 . 3 %, based on hplc ) as a 97 . 9 % pure tan powder . add a solution of 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamine ( 280 g , 1 . 37 moles ) in methyl t - butyl ether ( 1 . 4 l ) to a solution of p - toluenesulfonic acid monohydrate ( 212 . 5 g , 1 . 23 moles ) in tetrahydrofuran ( 980 ml ). observe a ph of 2 . 0 and an exotherm to 28 ° c . cool to 18 ° c . and filter solids . rinse filter cake with methyl t - butyl ether ( 1 . 4 l ). vacuum dry the filter cake at ambient temperature and collect 408 g ( 79 %) of the titled compound as a white solid . 1 h nmr ( dmso - d 6 , 500 mhz ): δ 8 . 94 ( d , 1h , j = 2 . 5 ), 8 . 53 ( br s , 3h ), 8 . 2 ( dd , 1h , j = 5 . 5 , 8 ), 8 . 02 ( d , 1h , j = 8 ), 7 . 46 ( d , 2h , j = 8 ), 7 . 10 ( d , 2h , j = 7 . 5 ), 2 . 27 ( s , 3h ), 1 . 68 ( s , 6h ). weigh into 5 - l 3 - neck flask 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamine ; compound with toluene - 4 - sulfonic acid ( 990 g , 2 . 63 moles ). add methyl t - butyl ether ( 2 . 48 l ) to form a suspension that is cooled by an ice - bath . add a 5 m solution of sodium hydroxide ( 578 . 64 ml , 2 . 89 moles ) to afford a biphasic mixture at ph 12 . 2 . separate the phases and extract the organic phase with water ( 125 ml ). remove the organic phase and concentrate under reduced pressure to afford a residue ( 200 g ). extract the aqueous phase with a mixture of methyl t - butyl ether ( 990 ml ) and tetrahydrofuran ( 1 . 32 l ). separate the organic phase and concentrate under reduced pressure to afford another residue ( 200 g ). observe that the aqueous phase is ph 10 . 1 and add 5n naoh ( 157 . 8 ml , 0 . 789 mol ) to give ph 13 . extract the aqueous phase with dichloromethane ( 1 . 32 l ). separate the phases and concentrate the organic phase to a third residue . combine the three residues of amine , suspend in heptane ( 1 l ) with mixing , and concentrate the suspension to afford 427 g ( 79 . 5 %) of the purified titled compound as a white crystalline solid . 1 h nmr ( cdcl 3 , 500 mhz ): δ 8 . 91 ( d , 1h , j = 2 . 5 ), 8 . 05 ( dd , 1h , j = 2 , 8 ), 7 . 64 ( d , 1h , j = 8 . 5 ), 1 . 68 ( br s , 2h ), 1 . 55 ( s , 6h ). add a 1 m solution of diisobutylaluminum hydride in toluene ( 76 mmol ) dropwise to a solution of m - ethylbenzonitrile ( 38 mmol ) in toluene ( 50 ml ) under nitrogen in a dry ice - acetone bath . stir for 30 minutes then add acetic acid ( 20 ml ) dropwise followed by water ( 100 ml ). stir the reaction for 2 hours . separate the layers and extract the aqueous with toluene . dry the combined organic layers over sodium sulfate , and evaporate to give the title compound ( 4 . 5 g , 88 % yield ). 1 hnmr ( 400 . 43 mhz , cdcl 3 ): δ 9 . 97 ( s , 1h ), 7 . 69 - 7 . 66 ( m , 2h ), 7 . 46 - 7 . 40 ( m , 2h ), 2 . 71 ( q , j = 7 . 6 hz , 2h ), 1 . 25 ( t , j = 7 . 5 hz , 3h ). dissolve ethyl 3 - acetylbenzoate ( 5 . 2 mmol ) in dichloromethane ( 13 ml ) in a polypropylene tube . add ( bis ( 2 - methoxyethyl ) amino sulfur trifluoride ( deoxofluor ) ( 10 . 4 mmol ) and ethanol ( 15 ul ). purge with nitrogen , seal the tube , and heat at 60 ° c . for 18 hours . add additional deoxofluor ( 10 . 4 mmol ) and heat for an additional 24 hours . pour the cooled reaction into 5 % aqueous sodium bicarbonate , extract with dichloromethane , dry the combined organic extracts over sodium sulfate , filter and evaporate . purify over silica ( 40 g ) eluting with 1 : 1 dichloromethane : hexane collecting the first eluting material . evaporate to give the title compound as a clear colorless liquid in 68 % yield . 1 hnmr ( 400 . 43 mhz , cdcl 3 ): δ 8 . 15 ( s , 1h ), 8 . 08 ( d , j = 7 . 9 hz , 1h ), 7 . 67 ( d , j = 7 . 9 hz , 1h ), 7 . 48 ( t , j = 8 . 1 hz , 1h ), 4 . 37 ( q , j = 7 . 2 hz , 2h ), 1 . 96 - 1 . 87 ( m , 3h ), 1 . 38 ( t , j = 7 . 0 hz , 3h ). add a solution of 3 -( 1 , 1 - difluoro - ethyl )- benzoic acid ethyl ester ( 3 . 57 mmol ) in thf ( 5 ml ) dropwise to a 1m solution of lithium aluminum hydride in thf ( 4 . 3 ml ) at room temperature . stir for 20 minutes then add ice followed by a mixture of concentrated sulfuric acid and ice ( approximately 1 : 1 v : v ). extract with ethyl ether , dry the organic extracts over sodium sulfate , filter , and evaporate to give the title compound in 97 % yield . gcms mw 172 ( m ). 1 h nmr ( 400 . 43 mhz , cdcl 3 ): δ 7 . 49 ( s , 1h ), 7 . 41 - 7 . 39 ( m , 3h ), 4 . 70 ( s , 2h ), 1 . 94 - 1 . 85 ( m , 3h ). add a solution of [ 3 -( 1 , 1 - difluoro - ethyl )- phenyl ]- methanol ( 3 . 47 mmol ) in dichloromethane ( 10 . 5 ml ) dropwise to a suspension of 3 , 3 , 3 - triacetoxy - 3 - iodophthalide ( 3 . 64 mmol ) in dichloromethane ( 10 . 5 ml ) at room temperature . stir for 30 minutes . add diethyl ether ( 10 ml ) and 5 % aqueous sodium bicarbonate ( 10 ml ) containing sodium thiosulfate ( 3 g ). mix well for 20 minutes . separate the layers , and extract the aqueous with ethyl ether . combine the organic layers , wash with brine , dry over sodium sulfate , filter , and evaporate to give a yellow solid . purify over silica ( 40 g ) eluting with 0 to 50 % dichloromethane in hexanes . evaporate until most solvent is removed being careful not to drive off the volatile product . dry additionally by blowing a nitrogen stream over the product to give the title compound in 70 % yield . 1 hnmr ( 400 . 43 mhz , cdcl 3 ): δ 10 . 03 ( s , 1h ), 8 . 00 ( s , 1h ), 7 . 92 ( d , j = 7 . 5 hz , 1h ), 7 . 75 ( d , j = 7 . 0 hz , 1h ), 7 . 59 ( t , j = 7 . 7 hz , 1h ), 1 . 98 - 1 . 89 ( m , 3h ). irradiate ( 200 c , ˜ 6 w [ 150 w max . ], ˜ 25 psi ) a solution of 3 - cyanophenol ( 9 . 5 g , 80 mmol ), cyclopropyl bromide ( 8 . 0 ml ; 100 mmol ), and 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene ( 18 ml , 120 mmol ) divided equally into five 10 - ml tubes for 15 min . with stirring and cooling . after cooling , take the dark reaction mixtures together in water ( 200 ml ) and extracted with ether ( 200 ml ). wash the organic layer with 0 . 2 m aq naoh ( 40 ml , salted ), 0 . 2 m aq hcl ( 100 ml , salted ), and water ( 100 ml , salted ). dry the organic layer ( na 2 so 4 ) and rotary evaporate ( 30 ° c .) yielding 3 - cyclopropoxybenzonitrile ( 4 . 56 g , 28 . 65 mmol , 36 % yield ) as a dark brown liquid . gcms : 4 . 20 min . ; eims m / z 159 . add diisobutylaluminum hydride ( 1 . 0 m in dichloromethane ; 47 ml , 47 mmol ) over a period of 5 min . to a solution of 3 - cyclopropoxybenzonitrile ( 6 . 45 g , 39 . 3 mmol ) in anhydrous dichloromethane ( 200 ml ) cooled in an isopropanol / dry ice bath (− 78 ° c .). remove the bath and allow the reaction solution to warm . after 1 hour ( 18 ° c . ), dilute the reaction solution with ether ( 20 ml ) and cool to 5 ° c . in an ice bath . add water ( 2 ml ), followed by 5 m naoh ( 2 ml ), and then more water ( 5 ml ). remove the ice bath and stir the reaction mixture at 20 ° c . for 15 min . add anhydrous mgso 4 and stir the reaction mixture for 15 min . filter the mixture through diatomaceous earth and rotary evaporate ( 30 ° c .) the filtrate giving crude 3 - cyclopropoxybenzaldehyde ( 6 . 33 g , 39 mmol , 99 % yield ) as an orange - yellow oil . gcms : eims m / z 162 . stir 4 -( 3 - fluoro - phenyl )- 4 - oxo - butyric acid [ c . a . 69797 - 46 - 2 ] ( j . med . chem . ( 1983 ) 26 381 ) ( 1 . 96 g , 10 mmol ), 4 - trifluoromethoxyaniline ( 1 . 77 g , 10 mmol ) and o -( 1h - benzotriazol - 1 - yl )- n , n , n ′, n ′- tetramethyluronium tetrafluoroborate ( tbtu ) ( 3 . 5 g , 11 mmol ) in dimethylformamide ( 30 ml ). add triethylamine ( 2 . 02 g , 20 mmol ). stir at room temperature for 48 hours . pour into dilute aqueous hcl ( 250 ml ) and extract into ethyl acetate . wash the organic phase three times with water , dry over anhydrous magnesium sulfate , evaporate and purify on a silica gel column ( dichloromethane - ethyl acetate ) to give the titled compound ( 3 . 13 g , 88 % yield ) ms ( m / z ): 356 ( m + 1 ). stir 4 -( 3 - fluoro - phenyl )- n -( 4 - trifluoromethoxy - phenyl )- 4 - oxo - butyramide ( 3 . 0 g , 8 . 5 mmol ) in ethanol ( 70 ml ) at room temperature . add sodium borohydride ( 650 mg , 17 . 2 mmol ) portionwise and stir at room temperature until tlc indicates that no starting material remains . add acetone to quench excess borohydride , concentrate the reaction mixture under reduced pressure , redissolve in ethyl acetate and wash with brine . dry over anhydrous magnesium sulfate , evaporate under reduced pressure to give the titled compound ( 2 . 0 g , 67 % yield ) ms ( m / z ): 358 ( m + 1 ). stir 4 -( 3 - fluoro - phenyl )- n -( 4 - trifluoromethoxy - phenyl )- 4 - hydroxy - butyramide ( 2 . 45 g , 6 . 86 mmol ) and p - toluenesulfonyl chloride ( 1 . 63 g , 8 . 60 mmol ) in dry tetrahydrofuran ( 30 ml ) under nitrogen . cool to − 40 ° c . and slowly add potassium t - butoxide ( 1m in tetrahydrofuran ) ( 17 . 2 ml , 17 . 2 mmol ). allow to warm slowly to room temperature and stir for 2 hours . add aqueous nh 4 cl solution and extract with ethyl acetate , wash with brine and dry over anhydrous magnesium sulfate . evaporate and purify on a silica gel column ( dichloromethane - ethyl acetate ) to give (±)- 5 -( 3 - fluoro - phenyl )- 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 1 . 9 g , 82 % yield ) ms ( m / z ): 340 ( m + 1 ). perform supercritical fluid chromatography ( sfc ) analysis on a berger minigram system configured with 6 - way column and solvent switching . perform sfc purification on a berger multigram ii system . equip both systems with a knauer variable wavelength uv detector supplied by mettler - toledo autochem ( leicester , uk ). deliver liquid co 2 to the laboratory by a berger gds - 3000 system supplied also by mettler - toledo autochem . separate the racemic mixture by supercritical fluid chromatography on an adh column eluting with 30 % methanol / propan - 2 - amine in supercritical carbon dioxide to give the two enantiomers . add ( r )- 5 -( 3 - fluoro - phenyl )- 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 0 . 89 g , 2 . 63 mmol ) to a suspension of sodium hydride ( 0 . 61 g , 15 . 36 mmol ) in dry toluene ( 40 ml ) and stir at room temperature under nitrogen . add methanol ( 0 . 29 ml , approx . 16 mmol ) followed by methyl p - chlorobenzoate ( 1 . 2 g , 7 . 0 mmol ). heat under reflux overnight . cool , add aqueous nh 4 cl solution , extract with ethyl acetate . collect the organic phase , dry over anhydrous magnesium sulfate , evaporate and purify on a silica gel column ( isohexane - ethyl acetate ) to give the titled compound ( 1 . 1 g , 88 % yield ) ms ( m / z ): 478 ( m + 1 ). dissolve sodium azide ( 2 . 6 g , 40 mmol ) and tetrabutylammonium bromide ( 260 mg , 0 . 8 mmol ) in 2n sodium hydroxide solution ( 50 ml ), add isohexane ( 50 ml ) and stir while cooling in an ice - water bath . add trifluoromethanesulfonic anhydride ( 2 . 0 ml , approx 12 mmol ) dropwise , stir for 10 minutes with cooling . dissolve ( 5r )-( 3 -( 4 - chlorobenzoyl - 5 -( 3 - fluoro - phenyl )- 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 1 . 1 g , 2 . 3 mmol ) in acetonitrile ( 30 ml ), add to the reaction mixture and stir vigorously for 30 minutes . dilute the reaction mixture with ethyl acetate ( 150 ml ) and wash with brine . collect the organic phase , dry over anhydrous magnesium sulfate , evaporate and purify on a silica gel column ( isohexane - ethyl acetate ) to give the titled compound ( 590 mg , 70 % yield ) ms ( m / z ): 366 ( m + 1 ). dissolve (±)- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( m - tolyl )- 1 -( 4 - trifluoro methoxy - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 2 . 19 g ; 4 . 09 mmol ) in acetic acid ( 15 ml ) and add sodium cyanoborohydride ( 0 . 77 g , 12 . 27 mmol ). stir for 12 hours at ambient temperature . pour into ice / water ( 50 ml ) and extract with ethyl acetate ( 50 ml × 2 ). wash the organic phase with saturated sodium bicarbonate ( 20 ml × 3 ), brine ( 20 ml ), dry over magnesium sulfate and evaporate in vacuo to an oil . purify on an scx - 2 ion exchange resin cartridge ( eluent methanol followed 2m nh 3 in methanol ) and then by chromatography on a silica gel column ( eluent ethyl acetate / iso - hexane ) to give the titled compound as a racemic mixture ( 1 . 60 g , 73 %). ms ( m / z ): 538 . 2 ( m + 1 ). perform supercritical fluid chromatography ( sfc ) analysis on a berger minigram system configured with 6 - way column and solvent switching . perform sfc purification on a berger multigram ii system . equip both systems with a knauer variable wavelength uv detector ( mettler - toledo autochem ( leicester , uk )). liquid co 2 is delivered to the laboratory by a berger gds - 3000 system supplied also by mettler - toledo autochem . separate the racemic mixture by supercritical fluid chromatography on an adh column eluted with 30 % methanol / propan - 2 - amine in supercritical carbon dioxide to give ( 3r , 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( m - tolyl )- 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 0 . 62 g , 47 . 6 %), eluted with 10 % isopropyl alcohol / propan - 2 - amine in supercritical carbon dioxide , retention time 0 . 65 min ., ms ( m / z ): 538 . 2 ( m + 1 ). prepare p - toluene sulfonic salt with p - toluene sulfonic acid ( 219 mg , 1 eq ) in isopropyl alcohol and filter the crystals . 1 h nmr ( 400 . 13 mhz , meod ): δ 9 . 08 ( d , j = 2 . 0 hz , 1h ), 8 . 41 ( dd , j = 2 . 2 , 8 . 6 hz , 1h ), 7 . 94 ( d , j = 8 . 3 hz , 1h ), 7 . 72 ( d , j = 8 . 3 hz , 2h ), 7 . 41 - 7 . 37 ( m , 2h ), 7 . 23 - 7 . 05 ( m , 8h ), 5 . 21 ( dd , j = 6 . 1 , 9 . 3 hz , 1h ), 4 . 36 ( dd , j = 8 . 6 , 11 . 5 hz , 1h ), 2 . 83 - 2 . 76 ( m , 1h ), 2 . 38 ( s , 3h ), 2 . 26 ( s , 3h ), 2 . 22 - 2 . 11 ( m , 1h ), 2 . 01 ( d , j = 1 . 5 hz , 6h ), and elute ( 3s , 5s )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( m - tolyl )- 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 0 . 58 g , 45 . 1 %), with 10 % isopropyl alcohol / propan - 2 - amine in supercritical carbon dioxide , retention time 1 . 03 min ., ms ( m / z ): 538 . 2 ( m + 1 ), prepare p - toluene sulfonic salt with p - toluene sulfonic acid ( 205 mg , eq ) in isopropyl alcohol and filter the crystals . 1 h nmr ( 400 . 13 mhz , meod ): δ 9 . 08 ( d , j = 2 . 2 hz , 1h ), 8 . 40 ( dd , j = 2 . 2 , 8 . 3 hz , 1h ), 7 . 95 ( d , j = 8 . 3 hz , 1h ), 7 . 72 ( d , j = 8 . 1 hz , 2h ), 7 . 40 - 7 . 37 ( m , 2h ), 7 . 23 ( d , j = 8 . 1 hz , 2h ), 7 . 18 - 7 . 14 ( m , 3h ), 7 . 09 - 7 . 02 ( m , 3h ), 5 . 21 ( dd , j = 6 . 1 , 9 . 3 hz , 1h ), 4 . 35 ( dd , j = 8 . 6 , 11 . 2 hz , 1h ), 2 . 84 - 2 . 77 ( m , 1h ), 2 . 38 ( s , 3h ), 2 . 26 ( s , 3h ), 2 . 22 - 2 . 10 ( m , 1h ), 2 . 01 ( d , j = 1 . 7 hz , 6h ). prepare the following compounds essentially by the method of example 1 and example 2 . add trifluoroacetic acid ( 3 . 5 ml , 46 . 1 mmol ) dropwise to a biphasic mixture of ( r )- 3 -(( r )- 1 - phenyl - ethylamino )- 5 -[ 3 -( 2 , 2 , 2 - trifluoro - ethoxy )- phenyl ]- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 4 . 8 g , 9 . 22 mmol ) in toluene ( 24 ml ) and water ( 9 . 6 ml ). stir at ambient temperature for 60 min . observe significant formation of ( r )- 5 -[ 3 -( 2 , 2 , 2 - trifluoro - ethoxy )- phenyl ]- 1 -( 4 - trifluoromethyl - phenyl )- pyrrolidine - 2 , 3 - dione ( lc ms 77 %, ret . time = 4 . 08 min ., method 3 , ms ( m / z ): 416 ( m − 1 ). separate the aqueous layer and wash the toluene layer with water , ph 7 buffer and saturated sodium chloride solution . add acetic acid ( 4 . 23 ml , 73 . 8 mmol ) and 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamine ( 3 . 77 g , 18 . 4 mmol ) to the toluene solution containing ( r )- 5 -[ 3 -( 2 , 2 , 2 - trifluoro - ethoxy )- phenyl ]- 1 -( 4 - trifluoromethyl - phenyl )- pyrrolidine - 2 , 3 - dione . heat to 55 ° c . for 18 hours . observe significant formation of ( r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -[ 3 -( 2 , 2 , 2 - trifluoro - ethoxy )- phenyl ]- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( lc ms 100 %, ret . time = 5 . 26 min ., method 3 , ms ( m / z ): 604 ( m + 1 ). dilute reaction mixture with ethyl acetate and wash with water and saturated sodium chloride solution , dry over sodium sulfate , filter and concentrate to dryness . dissolve the crude ( r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -[ 3 -( 2 , 2 , 2 - trifluoro - ethoxy )- phenyl ]- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one in acetic acid ( 46 ml ) and add sodium cyanoborohydride ( 1 . 16 g . 18 . 4 mmol ). stir 15 min . at ambient temperature . concentrate under reduced pressure . dissolve the residue in ethyl acetate and wash with saturated sodium bicarbonate solution and saturated sodium chloride solution , dry over sodium sulfate , filter and concentrate under reduced pressure . purify the residue by silica gel chromatography ( 5 - 50 % ethyl acetate - hexane ) and purify again by silica gel chromatography ( 0 - 1 % methanol - dichloromethane ) to obtain ( 3r , 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -[ 3 -( 2 , 2 , 2 - trifluoro - ethoxy )- phenyl ]- 1 -( 4 - trifluoromethyl - phenyl )- pyrrolidin - 2 - one ( 2 . 36 g , 42 %) as a clear colorless oil . ms ( m / z ): 606 ( m + 1 ). 1 h nmr ( dmso - d 6 , 400 mhz ): δ8 . 98 ( d , 1h , j = 2 . 2 hz ), 8 . 26 ( dd , 1h , j = 8 . 4 , 2 . 2 hz ), 7 . 82 ( d , 1h , j = 8 . 4 hz ), 7 . 58 ( d , 2h , j = 8 . 8 hz ), 7 . 52 ( d , 2h , j = 8 . 4 hz ), 7 . 20 ( dd , 1h , j = 7 . 4 , 7 . 4 hz ), 6 . 97 ( dd , 1h , j = 2 . 0 , 2 . 0 hz ), 6 . 89 ( d , 1h , j = 7 . 9 hz ), 6 . 84 ( dd , 1h , j = 7 . 9 , 2 . 2 hz ), 5 . 17 ( dd , 1h , j = 9 . 7 , 6 . 2 hz ), 4 . 72 - 4 . 61 ( m , 2h ), 3 . 48 - 3 . 41 ( m , 1h ), 2 . 88 ( d , 1h , j = 4 . 8 hz ), 2 . 71 - 2 . 63 ( m , 1h ), 1 . 68 ( dd , 1h , j = 22 . 0 , 10 . 5 hz ), 1 . 51 ( s , 3h ), 1 . 47 ( s , 3h ). salt formation : tosylate — add one equivalent p - toluenesulfonic acid monohydrate and crystallize from methanol - isopropanol . yield 82 %, ms ( m / z ): 606 . use thf in place of toluene during the hydrolysis step . remove thf under reduced pressure and replace with toluene and continue extractive work up . yield 41 %. 1 h nmr ( dmso - d 6 , 400 mhz ): δ 8 . 98 ( d , 1h , j = 2 . 2 hz ), 8 . 26 ( dd , 1h , j = 8 . 4 , 2 . 2hz ), 7 . 82 ( d , 1h , j = 7 . 9hz ), 1 h nmr ( dmso - d 6 , 400 mhz ): δ 8 . 98 ( d , 1h , j = 2 . 2 hz ), 8 . 26 ( dd , 1h , j = 8 . 4 , 2 . 2hz ), 7 . 82 ( d , 1h , j = 7 . 9hz ), 7 . 14 ( m , 1h ), 5 . 26 ( dd , 1h , j = 9 . 7 , 6 . 6hz ), 3 . 48 - 3 . 42 ( m , 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 97 ( s , 1h ), 8 . 26 ( d , j = 7 . 6 , 7 . 6hz ), 7 . 27 - 7 . 17 ( m , 6h ), 7 . 12 ( d , 1h , j = 7 . 9 6 . 4hz ), 3 . 40 ( dd , 1h , j = 9 . 2 , 9 . 2hz ), 2 . 89 ( s , 1h ), 2 . 73 - 2 . 65 ( m , 1h ), 1 . 64 ( dd , 1h , j = 22 . 0 , 10 . 5hz ), 1 . 50 ( s , 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 98 ( s , 1h ), 8 . 26 ( d , j = 8 . 8hz ), 7 . 49 ( d , 2h , j = 8 . 3hz ), 7 . 34 ( dd , 1h , j = 7 . 8 , 7 . 8hz ), 7 . 24 ( d , 1h , j = 7 . 9hz ), 7 . 14 ( s , 1h ), 7 . 06 ( d , j = 9 . 7 , 6 . 6hz ), 3 . 48 - 3 . 40 ( m , 1h ), 2 . 91 ( d , 1h , j = 4 . 8 hz ), 2 . 76 - 2 . 68 ( m , 1h ), 1 . 67 ( ddd , 1h , j = 11 . 0 , 11 . 0 , 11 . 0 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 97 ( s , 1h ), 8 . 25 ( d , j = 7 . 9 , 7 . 9hz ), 7 . 27 ( s , 4h ), 7 . 22 ( d , 1h , j = 7 . 9hz ), 7 . 12 ( s , 1h ), 7 . 06 ( d , 1h , j = 8 . 3hz ), 6 . 72 ( dd , 1h , j = 51 . 4 , ( ddd , 1h , j = 11 . 0 , 11 . 0 , 11 . 0 hz ), 1 . 49 ( s , 3h ), 1 . 45 ( s , 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 97 ( s , 1h ), 8 . 25 ( d , j = 16 . 3 , 9 . 2hz ), 7 . 18 ( dd , 1h , j = 7 . 9 , 7 . 8hz ), 6 . 93 ( s , 1h ), 6 . 88 - 6 . 81 ( m , 2h ), 5 . 08 ( dd , 1h , j = 9 . 4 , 6 . 4hz ), 4 . 71 - 4 . 60 ( m , 2h ), 3 . 43 - 3 . 36 ( m , 1h ), 2 . 84 ( d , 1h , j = 4 . 0 hz ), 2 . 67 - 2 . 58 ( m , 1h ), 1 . 65 ( ddd , 1h , j = 10 . 8 , 10 . 8 , 10 . 8 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 97 ( d , 1h , j = 2 . 2 hz ), 8 . 25 ( dd , 1h , j = 8 . 4 , 1 . 8hz ), 7 . 81 ( d , 1h , j = 8 . 4 hz ), 7 . 37 ( d , 2h , j = 9 . 2hz ), 7 . 25 - 7 . 12 ( m , 7h ), 5 . 12 ( dd , 1h , j = 9 . 7 , 6 . 6hz ), 3 . 44 - 3 . 37 ( m , 1h ), 2 . 88 ( d , 1h , j = 4 . 0 hz ), 2 . 65 ( ddd , 1h , j = 13 . 3 , 6 . 9 , 5 . 2hz ), 1 . 63 ( ddd , 1h , 1 h nmr ( 400 mhz , dmso - d 6 ) δ 8 . 93 ( d , 1h , j = 2 . 2 hz ), 8 . 20 ( dd , 1h , j = 8 . 1 , 2 . 0 hz ), 7 . 78 ( d , 1h , j = 8 . 4 hz ), 7 . 62 ( d , 2h , j = 9 . 2hz ), 7 . 29 - 7 . 21 ( m , 4h ), 7 . 18 - 7 . 10 ( m , 3h ), 5 . 45 ( dd , 1h , j = 8 . 6 , 2 . 0 hz ), 3 . 53 - 3 . 46 ( m , ( ddd , 1h , j = 12 . 7 , 8 . 1 , 2 . 1hz ), 1 . 46 ( s , 3h ), 1 . 42 ( s , 3h ). 1 h nmr ( 400 . 43 mhz , meod ): δ 9 . 03 ( d , j = 2 . 6hz , 7 . 12 ( m , 7h ), 5 . 21 ( dd , j = 6 . 2 , 9 . 2hz , 1h ), 4 . 29 ( dd , j = 1 h nmr ( 400 . 43 mhz , meod ): δ 9 . 03 ( d , j = 2 . 6hz , 7 . 12 ( m , 7h ), 5 . 21 ( dd , j = 6 . 2 , 9 . 2hz , 1h ), 4 . 29 ( dd , j = yield 31 % use 0 . 3 equivalents of hoac and 3 equivalents of amine in enamine formation ( second step ). lc - ms esi m / z : 590 ( m + h ) + , retention time 4 . 73 min , yield 39 % use 0 . 3 equivalents of hoac in enamine formation ( second step ). lc - ms esi m / z : 506 ( m + h ) + , retention time 4 . 16 min , add trifluoroacetic acid ( 83 . 5 ml , 1 . 10 mol ) and sodium triacetoxyborohydride ( 175 g , 828 mmol ) to a slurry of 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]-( r )- 5 - phenyl - 1 -( 4 - trifluoromethoxy - phenyl )- 1 , 5 - dihydro - pryrrol - 2 - one ( 288 g , 552 mmol ) in toluene ( 2 . 80 l ) under a nitrogen atmosphere . stir for 45 min , and add acetic acid ( 200 ml ). after stirring 3 h , add trifluoroacetic acid ( 100 ml ) and sodium triacetoxyborohydride ( 56 g , 265 mmol ). after stirring for 24 hours at ambient temperature , heat the slurry to 35 ° c . after 2 hours , cool the mixture to ambient temperature and transfer by cannula into water ( 3 . 0 l ). dilute with mtbe ( 2 . 0 l ), agitate the biphasic mixture , and discard the aqueous phase . wash the organic layer with water ( 2 . 0 l ) and saturated sodium hydrogen carbonate solution ( 2 . 0 l ). concentrate the organic layer to an oil under reduced pressure ( 10 torr , 30 ° c . ), and dissolve in isopropyl alcohol ( 2 . 0 l ). to the resulting solution , charge para - toluene sulfonic acid monohydrate ( 100 . 7 g , 518 mmol ) and water ( 200 ml ). heat the slurry to 65 ° c . then slowly cool to ambient temperature and stir for 12 hours . filter the slurry and wash the precipitate with isopropyl acetate ( 250 ml ). dry the white solid on a nitrogen press for 5 hours to give ( 3r , 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 - phenyl - 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one tosylate ( 298 g , 82 %): 1 h nmr ( 400 mhz , dmso - d 6 ) δ 10 . 10 ( 1h , br ), 9 . 08 ( 1h , d , j = 4 hz ), 8 . 39 ( 1h , dd , j = 4 , 8 hz ), 8 . 04 ( 1h , d , j = 8 hz ), 7 . 49 ( 2h , m ), 7 . 38 ( 2h , m ), 7 . 21 - 7 . 28 ( 7h , m ), 7 . 10 ( 2h , m ), 5 . 21 ( 1h , dd , j = 4 , 8 hz ), 4 . 27 ( 1h , br s ), 2 . 69 ( 1h , m ), 2 . 26 ( 3h , s ), 2 . 02 ( 1h , m ), 1 . 85 ( 6h , m ); ms ( m / z ): 524 . 2 ( m + 1 ). add trifluoroacetic acid ( 1 . 5 ml , 20 mmol ) to a mixture of ( r )- 3 -(( r )- 1 - phenyl - ethylamino )- 5 -( 3 - cyclopropoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 1 . 92 g , 4 . 01 mmol ) in toluene ( 10 ml ) and water ( 4 ml ). stir at ambient temperature for 60 min . observe significant formation of ( r )- 5 -( 3 - cyclopropoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- pyrrolidine - 2 , 3 - dione . lcms , ret . time = 4 . 14 min ., method 3 , ms ( m / z ): 376 . 0 ( m +), 374 . 0 ( m − 1 ). add a solution of 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamine ( 1 . 2 g , 5 . 9 mmol ) in toluene ( 10 ml ) to the reaction solution . then add acetic acid ( 1 . 9 ml , 33 mmol ). heat at 50 ° c . for 14 hours . concentrate under reduced pressure . purify the residue by silica gel chromatography ( 0 - 10 % ethyl acetate - hexane ) to obtain ( r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( 3 - cyclopropoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one as a tan foam . lcms , ret . time = 5 . 40 min ., method 3 , ms ( m / z ): 562 . 0 ( m +), 560 . 0 ( m − 1 ). dissolve ( r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( 3 - cyclopropoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- 1 , 5 - dihydro - pyrrol - 2 - one ( 1 . 09 g , 1 . 94 mmol ) in acetic acid ( 20 ml ) and add sodium cyanoborohydride ( 240 mg . 3 . 8 mmol ). stir 1 hour at ambient temperature . concentrate under reduced pressure . dissolve the residue in dichloromethane and wash with saturated sodium bicarbonate solution , dry over sodium sulfate , filter and concentrate under reduced pressure . purify the residue by silica gel chromatography ( 0 - 15 % ethyl acetate - hexane ) to obtain ( 3r , 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( 3 - cyclopropoxy - phenyl )- 1 -( 4 - trifluoromethyl - phenyl )- pyrrolidin - 2 - one ( 645 mg , 59 %) as a white foam . lcms , ret . time = 5 . 04 min , method 3 ms ( m / z ): 564 . 0 ( m + 1 ). dissolve ( 5r )- 3 - diazo - 5 -( 3 - fluoro - phenyl )- 1 -( 4 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 295 mg , 0 . 81 mmol ) and 1 - methyl - 1 -( 6 - chloro - pyridin - 3 - yl )- ethylamine ( 0 . 6 g 3 . 5 mmol ) in dry toluene ( 8 ml ). stir under nitrogen and heat to 45 ° c . add rhodium acetate dimer dihydrate ( 40 mg , 0 . 09 mmol ). stir at 45 ° c . for 30 minutes then concentrate the reaction mixture under reduced pressure . purify on an scx - 2 ion exchange resin cartridge ( eluent methanol followed 2m nh 3 in methanol ) and then by chromatography on a silica gel column ( eluent dichloromethane / methanol ) to give the titled compound as a diastereomer mixture ( 330 mg , 80 %). perform supercritical fluid chromatography ( sfc ) analysis on a berger minigram system configured with 6 - way column and solvent switching . perform sfc purification on a berger multigram ii system . equip both systems with a knauer variable wavelength uv detector supplied by mettler - toledo autochem ( leicester , uk ). deliver liquid co 2 to the laboratory by a berger gds - 3000 system supplied also by mettler - toledo autochem . separate the diastereomer mixture by supercritical fluid chromatography on an adh column eluting with 25 % methanol / propan - 2 - amine in supercritical carbon dioxide . prepare the tartrate salt with tartaric acid ( 1 eq ) in methanol and isolate the salt by evaporation of the solvent to give example 56 and example 57 . 1 h nmr ( 400 . 13 mhz , meod ): δ8 . 58 ( s , 1h ), 8 . 10 ( d , j = 8 . 3 hz , 1h ), 7 . 45 - 7 . 39 ( m , 3h ), 7 . 31 - 7 . 26 ( m , 1h ), 7 . 16 ( d , j = 8 . 3 hz , 2h ), 7 . 08 ( d , j = 7 . 8 hz , 1h ), 7 . 01 ( d , j = 9 . 8 hz , 1h ), 6 . 94 ( t , j = 8 . 3 hz , 1h ), 5 . 16 ( t , j = 7 . 6 hz , 1h ), 4 . 54 ( s , 2h ), 3 . 59 ( t , j = 9 . 3 hz , 1h ), 2 . 85 - 2 . 65 ( m , 1h ), 1 . 81 ( q , j = 10 . 9 hz , 1h ), 1 . 60 ( s , 6h ). yield 63 %, retention time 0 . 71 min . tartrate salt . 1 h nmr ( 400 . 13 mhz , meod ): δ8 . 55 ( s , 1h ), 8 . 55 ( s , 1h ), 8 . 06 ( d , j = 8 . 1 hz , 1h ), 7 . 65 ( d , j = 7 . 8 hz , 2h ), 7 . 42 ( d , j = 8 . 3 hz , 1h ), 7 . 34 - 7 . 30 ( m , 1h ), 7 . 22 ( d , j = 8 . 3 hz , 2h ), 6 . 99 - 6 . 92 ( m , 3h ), 5 . 42 ( d , j = 9 . 0 hz , 1h ), 4 . 54 ( s , 2h ), 3 . 62 ( t , j = 8 . 9 hz , 1h ), 2 . 49 - 2 . 41 ( m , 1h ), 2 . 19 - 2 . 14 ( m , 1h ), 1 . 55 ( s , 6h ). prepare the following compounds essentially by the method of example 55 , 56 and 57 . dissolve ( 3r , 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 1 -( 4 - bromo - phenyl )- 5 -( 3 - trifluoromethoxy - phenyl )- pyrrolidin - 2 - one ( 1 . 25 mmoles ; 750 mg ), cyclopropylboronic acid ( 1 . 62 mmoles ; 139 mg ), tribasic potassium phosphate n - hydrate ( 4 . 36 mmoles ; 925 mg ), and tricyclohexylphosphine ( 124 . 51 μmoles ; 34 mg ) in toluene ( 5 ml ) and water ( 275 μl ) and degas the solution for 5 minutes then place under a nitrogen atmosphere . add pd ( oac ) 2 ( 62 μmoles ; 14 mg ) and heat the mixture at 90 ° c . overnight . dilute with ethyl acetate ( 50 ml ) and filter through celite . wash the filtrate with water , 1n hcl , saturated aqueous sodium bicarbonate , brine , dry over anhydrous sodium sulfate , filter , and concentrate in vacuo to a brown residue . purify the residue by flash chromatography on silica with gradient 0 -& gt ; 50 % ethyl acetate in hexane to afford the title compound ( 3r , 5r )- 3 -[ 1 - methyl - 1 -( 6 - trifluoromethyl - pyridin - 3 - yl )- ethylamino ]- 5 -( 3 - trifluoromethoxy - phenyl )- 1 -( 4 - cyclopropyl - phenyl )- pyrrolidin - 2 - one ( 1 . 13 mmoles ; 639 . 00 mg ; 91 . 07 % yield ). lc / ms m / z 564 . 2 ( m + 1 ), tr = 4 . 87 min ( method 3 ). test exemplified compounds . measure gtp - γ 35 s binding in a 96 well format using a modified antibody capture technique previously described ( delapp et al . 1999 ). briefly incubate , cho or sf9 cell membranes expressing cb 1 or cb 2 , respectively ( applied cell sciences , gaithersburg , md . ; perkinelmer life sciences , boston , mass . ); prepare as previously described ( delapp et al ., 1999 ), exemplified compounds and 500 μm gtp - γ - 35 s ( perkinelmer life sciences , boston , mass .) for 30 minutes ( incubate all at room temperature ) in gtp - binding assay buffer ( 20 mm hepes , 100 mm nacl , 5 mm mgcl 2 , ph 7 . 4 ). perform antagonist dose responses in the presence of a saturating dose of full agonist ( methanandamide ). add a mixture containing 0 . 27 % nonidet p40 detergent ( roche , indianapolis , ind . ), anti - gi antibody ( final dilution of 1 : 300 ; covance , princeton , n . j . ), and 1 . 25 mg anti - rabbit antibody scintillation proximity assay beads ( ge healthcare , piscataway , n . j .) and seal the plates and incubate for an additional 3 hours . centrifuge the plates at 700 × g for 10 minutes using a beckman gs - 6r centrifuge and count for 1 minute per well using a wallac microbeta trilux scintillation counter ( perkinelmer , boston , mass .). to analyze data , first subtract background from all wells . determine percent agonist efficacy by normalizing agonist / inverse agonist dose response data to a full agonist ( methanandamide ) response . calculating antagonist percent inhibition data by normalizing to results generated with a saturating concentration of methanandamide . analyze the data using a 4 - parameter logistic reduced fit with activity base and xlfit3 ( idbs , emeryville , calif .). determine k b values using a modification of the cheng - prusoff relationship : k b = ic50 /( 1 +[ agonist ]/ ec50 ) where ic50 is determined from a four parameter fit of displacement curves , [ agonist ]= ec50 of full agonist , and ec50 is determined from a four parameter fit of a full agonist concentration response curve ( cheng and prusoff 1973 ). calculate mean k b values as a mean of at least three independent determinations ± standard error of the mean ( sem ). table 15 summarizes the antagonist / inverse agonist properties of example 49 in cho cells expressing human or rat cb 1 receptors or sf9 cells expressing human cb 2 receptors . the data indicate that example 49 is a potent cb 1 antagonist / inverse agonist at both rat and human receptors with low antagonism of human cb 2 receptors . example 49 ( table 16 ) is an inverse agonist at the human cb 1 receptor as evidenced by agonist efficacy less than zero which indicates that the compound decreased basal constitutive activity of the cb 1 receptor in vitro . the exemplified compounds ( table 17 ) exhibit potent human and rat cb 1 antagonism / inverse agonism with only low affinity antagonism / inverse agonism of the human cb 2 receptor . exemplified compounds of this invention are potent cb 1 antagonist / inverse agonist at both rat and human receptors with low antagonism of human cb 2 receptors . exemplified compounds of this invention are inverse agonist at the human cb 1 receptor as evidenced by agonist efficacy less than zero which indicates that the compound decreased basal constitutive activity of the cb 1 receptor in vitro . delapp n w , mckinzie j h , sawyer b d , vandergriff a , falcone j , mcclure d and felder c c ( 1999 ). determination of [ 35 s ] guanosine - 5 ′- o -( 3 - thio ) triphosphate binding mediated by cholinergic muscarinic receptors in membranes from chinese hamster ovary cells and rat striatum using an anti - g protein scintillation proximity assay . j pharmacol exp ther 289 : 946 - 955 . cheng y c and prusoff w h . 1973 . relationship between the inhibition constant ( ki ) and the concentration of inhibitor which causes 50 percent inhibition ( i50 ) of an enzymatic reaction . biochem pharmacol 22 : 3099 - 3108 . receive nih male swiss mice ( harlan sprague - dawley , weigh 20 - 25 g ) 7 - 10 days prior to testing . house 12 mice / cage . test animals that weigh 25 - 30 g . on the day of test , bring animals to the testing room at least 1 hr prior to dosing , when doing starts , 6 - 8 min . intervals between each dosing with mouse receiving either vehicle or exemplified compounds by p . o ., and then put it into a clean cage afterwards ( 4 mice / cage ). depending on pretreatment time , start the test accordingly . mice fst : place nih - swiss mice in clear plastic cylinders ( diameter : 10 cm ; height : 25 cm ) filled to 6 cm with 22 - 25 ° c . water for six min . record the duration of immobility during the last 4 min . of the six - minute trial . a mouse is regarded as immobile when floating motionless or making only those movements necessary to keep its head above the water . copy the data - immobility ( second ) into jmp data sheet , and analyze by anova - dunnett &# 39 ; s test . record the minimum effective dose ( med ) as the lowest dose of compound at which statistically significant decrease in immobility time is observed versus a vehicle control . methods for accessing bioavailabilty are well appreciated in the art . one such reference is medicinal research reviews vol 21 no . 5 382 - 396 ( 2001 ). the exemplified compounds in table 17 have the following biological data . | 2 |
as shown in fig1 , a conventional wheelbarrow 2 includes handles 4 , a container 8 disposed above the handles , legs 12 mounted below the handles and wheel 16 connected to the handles via an axle assembly 18 . when in a resting position , wheel 16 and legs 12 form a tripedal support for container 8 . to transport wheelbarrow 2 , operator 20 grasps grips 22 of handles 4 and lifts them to a convenient height , causing the wheelbarrow to pivot around the rotational axis of axle assembly 18 so that legs 12 rise off the ground . wheel 16 is free to rotate , allowing operator 20 to push wheelbarrow 2 to the desired destination . operator 20 discharges the contents of container 8 by rotating handles 4 , for example by lowering the left handle and raising the right handle , causing wheelbarrow 2 to rotate with respect to the point where wheel 16 contacts the ground ( not shown ). referring to fig2 , the illustrated lifting apparatus comprises a strap 32 of fabric webbing threaded through rectangular passage 43 in a length of flexible tubular padding 44 . padding 44 may be composed of a resilient foam material . each end of strap 32 is threaded through an adjustable locking buckle 40 , an eye 39 of a hook 36 , and back through the buckle . buckle 40 is a conventional buckle that includes a releasable locking mechanism . referring to fig4 , the locking mechanism of illustrated buckle 40 comprises toothed barrel 45 and a toothed cam 46 . toothed cam 46 is pivotable , relative to the barrel , between an engaged position , for allowing strap 32 to move relative to the buckle in only a tightening , or shortening , direction , and a released position , for allowing the strap to move both in the tightening direction and in a loosening , or lengthening , direction . pulling strap 32 in the loosening direction when cam 46 is in the engaged position jams the strap between barrel 45 and the cam , preventing movement of the strap . a lever 47 assists in moving cam 46 to the released position . a spring ( not shown ) holds cam 46 in the engaged position unless operator 20 depresses the lever 47 . referring again to fig1 the lifting apparatus assists operator 20 by transferring the load to be supported by the operator from operator &# 39 ; s hands 24 to operator &# 39 ; s shoulders and back 28 . to use the lifting apparatus , operator 20 would pre - adjust the effective length of strap 32 , i . e . the distance between hooks 36 , using adjustable locking buckles 40 . in use the appropriate effective length will vary by situation , but it can be estimated by placing strap 32 around the back of the operator &# 39 ; s neck , with padding 44 centered approximately on the spine . the free ends of strap 32 should then be hanging in front of operator &# 39 ; s arms 24 . each end should be adjusted so hooks 36 hang slightly below the operator &# 39 ; s fingertips when the arms are at the sides . to engage wheelbarrow 2 with the apparatus , the operator stands between handles 4 and places strap 32 on the operator &# 39 ; s neck with padding 44 centered on the spine . if hooks 36 can reach handles 4 while the operator is standing upright , the effective length of strap 32 is too great and must be reduced . after ensuring the effective length of strap 32 is properly adjusted , the operator bends or squats down in order to lower hooks 36 and temporarily engage them with handles 4 while maintaining slack in the strap . it will be appreciated that once the effective length of strap 32 has been adjusted for the particular operator and the particular wheelbarrow , it will not generally be necessary to change the adjustment . when hooks 36 are engaged with handles 4 , operator 20 begins to stand , taking hold of grips 22 to aid in balancing wheelbarrow 2 . when strap 32 becomes taut legs 12 of wheelbarrow 2 lift off the ground and a significant portion of the weight of the wheelbarrow will be transferred through the strap to operator &# 39 ; s shoulders and back 28 . padding 44 on strap 32 distributes the load across a greater surface area of operator &# 39 ; s shoulders and back 28 for the operator &# 39 ; s comfort . when lifting the wheelbarrow , the operator preferably will lift by straightening at the knees and hips , keeping the back as upright as possible so as to reduce the possibility of injury . by transferring the weight of wheelbarrow 2 to the operator &# 39 ; s shoulders and back through strap 32 , the operator uses the strongest muscles to lift the wheelbarrow and is better able to use hands and arms to aid in balancing and maneuvering the wheelbarrow . thus the lifting apparatus can enable the operator to lift heavier loads . discharging the contents of wheelbarrow 2 is performed in the conventional manner described above . when operator 20 raises one handle above the other strap 32 will move through passage 43 of padding 44 while the padding remains in place on the neck of the operator . hooks 36 may be sized to fit snugly on wheelbarrow handles 22 so that they remain on handles 22 when operator 20 releases tension on strap 32 . alternatively , the ends of hooks 36 may be designed so that their ends extend partially over the tops of handles 22 so that they remain on the handles when operator 20 releases tension on strap 32 . in a second embodiment of the invention , strap 32 is attached to handles 4 by means of rings 38 , as shown in fig3 . instead of applying the hooks from below , the operator will thread handles 4 through rings 38 . the hooks 36 or rings 38 allow the operator to easily slip the lifting mechanism off handles 4 . in a third embodiment of the invention , the hook or ring is omitted and the handle is threaded through loop 52 formed in strap 32 by locking cam buckle 40 , as shown in fig4 . fig4 also illustrates additional padding 49 in central region 50 of padding 44 to provide additional protection to the operator &# 39 ; s neck . the illustrated embodiments of the invention are compatible with a wheelbarrow of similar design to the conventional wheelbarrow described above . the illustrated embodiments of the invention do not interfere with the operation of other conventional wheelbarrow accessories and safety devices , such as the “ wheelbarrow braking system ” described in u . s . pat . no . 5 , 690 , 191 and the “ wheelbarrow disk brake assembly ” described in u . s . pat . no . 6 , 443 , 267 or the various versions of the motorized wheelbarrows such as the “ motorized wheelbarrow ” described in u . s . pat . no . 5 , 878 , 827 and the “ motorized wheelbarrow ” described in u . s . pat . no . 5 , 465 , 801 . although inexpensive to manufacture , a lifting apparatus in accordance with the invention thus allows an operator to easily lift , control and maneuver even very heavily loaded wheelbarrows and helps reduce operator fatigue . it will be appreciated that the invention is not restricted to the particular embodiments that have been described and illustrated , and that variations may be made therein without departing from the scope of the invention as defined in the appended claims and equivalents thereof . unless the context indicates otherwise , a reference in a claim to the number of instances of an element , be it a reference to one instance or more than one instance , requires at least the stated number of instances of the element but is not intended to exclude from the scope of the claim a structure or method having more instances of that element than stated . | 0 |
exemplary embodiments of the invention relate to a two - stage positioning technique . in accordance with an exemplary positioning system , a coarse position estimate may be computed within a coarse area of interest , and a fine position estimate may be is computed within a fine area of interest . within the coarse area of interest , a mobile positioning unit may use a narrow band communication technique to estimate the coarse position of the mobile positioning unit . within the fine area of interest , the positioning unit may use a wide band communication technique to estimate the fine position of the positioning unit . in embodiments , the fine positioning within the fine area of interest may be computed using both narrow band and wide band communications to obtain a more accurate estimate of the positioning unit compared to using narrow band communications alone . in embodiments , the positioning unit may be disposed within a vehicle such as a railway vehicle . the positioning unit may be used to control a braking system of the vehicle to stop the movement of the vehicle at a point of interest with sub - meter accuracy . fig1 is a block diagram of a positioning system , according to an exemplary embodiment of the invention . as shown in fig1 , the positioning system 100 may include a vehicle 102 equipped with a positioning unit 104 . the vehicle 102 may include a rail - way vehicle such as a locomotive , an automobile , a marine vessel , or any other suitable type of vehicle . further , it will be appreciated that embodiments are not limited to determining the position of a vehicle . for example , the positioning unit 104 may be disposed within other types of mobile devices , such as mobile phones , for example . the positioning unit 104 may be configured to estimate the position of the vehicle 102 in relation to a point of interest 106 . the point of interest 106 may be a geographical location that is relevant in some way to the vehicle 102 . for example , the point of interest 106 may coincide with the location of a loading dock or a passenger platform . the area within the vicinity of the point of interest 106 may be divided into a coarse area of interest 108 and a fine area of interest 110 . the coarse area of interest 108 defines an area within which the positioning unit 104 will compute an estimated coarse position of the vehicle 102 . the fine area of interest 110 defines an area within which the positioning unit 104 will compute an estimated fine position vehicle 102 . to determine the position of the vehicle 102 , the positioning unit 104 may communicate with radio responsive devices disposed in the vicinity of the point of interest 106 . as used herein , the term radio responsive device may be used to refer to active reflectors , passive reflectors , and wireless communication devices . an active reflector refers to a radio communication device that can receive , generate , and transmit radio signals using , for example , analog circuits . examples of active reflectors include transponders , repeaters , and the like . a passive reflector refers to a radio reflective device such as a piece of metal . a wireless communication device refers to communication devices that can receive digital signals , process the data contained in the signals , and generate and transmit new digital signals that contain additional data . examples of wireless communication devices include wireless routers , and the like . as used herein , the term “ communicate ” and variations thereof are used in relation to active reflectors , passive reflectors , and wireless communication devices . in other words , “ communicating ” with a radio responsive device includes sending an outbound signal to the radio responsive device and receiving a corresponding inbound signal from the radio responsive device , regardless of whether the inbound signal is generated by an active reflector or wireless communication device , or reflected from a passive reflector . fig1 shows two radio responsive devices referred herein as a coarse positioning device 112 and a fine positioning device 114 . both the coarse positioning device 112 and the fine positioning device 114 may be disposed at fixed positions about the point of interest 106 . the positions of the devices 112 and 114 are known values . for example , coordinates describing the positions of the devices 112 and 114 in relation to the point of interest 106 may be stored to the positioning unit 104 , programmed into the logic of the positioning unit 104 , or otherwise accessible by positioning unit 104 . to compute an estimated position of the vehicle 102 , the positioning unit 104 determines a position of the vehicle 102 in relation to either the coarse positioning device 112 or the fine positioning device 114 or both . the position of the vehicle 102 in relation to the point of interest 106 can then be determined based on the known position of the coarse positioning device 112 or the fine positioning device 114 in relation to the point of interest 106 . in embodiments , the positioning unit 104 determines the position of the vehicle 102 by determining a distance between the vehicle 102 and the radio responsive devices . for example , the positioning unit 104 may transmit an outgoing signal from the vehicle 102 to one of the radio responsive devices , receive a return signal from one of the radio responsive devices , and compute a time - of - flight of the signals . the time - of - flight refers to an amount of time elapsed between the transmission of the outbound signal and the receipt of the inbound signal . the time - of - flight can be used to compute a distance measurement . in embodiments wherein the vehicle 102 is a railway vehicle , the path of the railway may provide another set of data that can be used to determine the position of the vehicle 102 based on the distance measurement . in this way , a single distance measurement may be used to determine the position of the vehicle 102 . data describing the path of the railway may be stored to the positioning unit 104 , programmed into the logic of the positioning unit 104 , or otherwise accessible by positioning unit 104 . as described below in relation to fig2 , the position of the vehicle 102 may also be computed using two or more distance measurements based on signals received from two or more radio responsive devices . as noted above , the positioning unit 104 computes a coarse position within the coarse are of interest 108 and a fine position within a fine area of interest 110 . the coarse position is computed based on communications with the coarse positioning device 112 , which may be an active or passive reflector or a wireless communication device . to compute the coarse position , the positioning unit 104 communicates with the coarse positioning device 112 using a narrow - band signal . for example , the bandwidth of the narrow - band signal may be approximately 5 to 40 megahertz . the extent of the coarse area of interest 108 corresponds to the distance at which signals can be communicated between the positioning unit 104 and the coarse positioning device 112 . the fine position is computed based on communications with the fine positioning device 114 , which may be an active or passive reflectors or a wireless communication device . to compute the fine position , the positioning unit 104 communicates with the fine positioning device 114 using a wide - band signal that has a bandwidth greater than the narrow - band signal that is used to communicate with coarse positioning device 112 . for example , the bandwidth of the wide - band signal may be approximately 500 megahertz to 2 gigahertz . the extent of the fine area of interest 108 corresponds to the distance at which signals can be communicated between the positioning unit 104 and the fine positioning device 112 . as indicated by the extent of the coarse area of interest 108 , the narrow - band signal used during coarse positioning enables a greater communication range compared to the wide - band signal . for example , the coarse area of interest 108 may extend approximately 1 kilometer around the coarse positioning device 112 , whereas the fine area of interest 110 may extend approximately 50 meters around the fine positioning device 114 . however , the wide - band signal used during fine positioning enables the computation of a more precise vehicle position compared to the narrow - band signal . for example , the use of the wide - band signal may enable the computation of position estimates with a precision of less than a meter , whereas the narrow - band signal may enable the computation of position estimates with a precision of a few meters . in embodiments , the coarse positioning device 112 is a wireless communication device that communicates with the positioning unit 104 using an ieee 802 . 11 standard protocol , such as wifi . the positioning unit 104 may periodically transmit outbound signals to be received by the coarse positioning device 112 in an attempt to establish a communication link with the coarse positioning device 112 . when the vehicle 102 is within the coarse area of interest 108 , the outbound signals can be received by the coarse positioning device 112 . in response to the outbound signal , the coarse positioning device 112 may generate and transmit a corresponding inbound signal back to the positioning unit 104 at the same frequency as the outbound signal . the inbound signal may transmit one or more data packets to the positioning device 112 . each inbound data packet may include an identifier that identifies the particular coarse positioning device 112 sending the data packet . the positioning unit 104 may then compute a coarse estimate of the vehicle position based on the round - trip time - of - flight of the outbound and inbound signals . the positioning unit 104 may continue to periodically send outbound signals to the coarse positioning device 112 in order to periodically re - compute the vehicle position as the vehicle 102 moves through the coarse area of interest 108 . additionally , when the vehicle 102 enters the coarse area of interest 108 , the positioning unit 104 may begin periodically transmitting outbound signals to be received by the fine positioning device 114 in an attempt to establish communications with the fine positioning device 114 . the positioning unit 104 may communicate with the fine positioning device 114 by transmitting ultra - wideband ( uwb ) pulses to the fine positioning device 114 . in embodiments , the fine positioning device 114 is a passive reflector , which reflects the outbound pulses back to the positioning unit 104 . in embodiments , the fine positioning device 114 is an active reflector , which , in response to receiving the outbound pulses , generates and transmits a corresponding inbound signal back to the positioning unit 104 at the same frequency as the outbound signal . in embodiments , the signal generated by the active reflector may be amplitude modulated or phase modulated the create a unique signature that identifies the fine positioning device 114 generating the signal . in embodiments , the fine positioning device 114 is a wireless communication device that communicates with the positioning unit 104 using an standard uwb protocol , such as iso / iec 26907 and ieee 802 . 15 . 4a , among others . the inbound uwb signals generated by the fine positioning device 114 may include one or more data packets , each of which includes an identifier that identifies the particular fine positioning device 114 sending the data packet . the vehicle 102 is within the fine area of interest 110 when the inbound signals generated or reflected by the fine positioning device 114 can be detected by the positioning unit 102 . upon the receipt of the inbound signals , e . g ., uwb pulses , the positioning unit 104 can compute a fine estimate of the vehicle position based on the round - trip time - of - flight of the outbound and inbound signals . the positioning unit 104 may continue to periodically send outbound signals to the fine positioning device 114 in order to periodically re - compute the vehicle position as the vehicle 102 moves through the fine area of interest 110 . as described further below in reference to fig2 , an exemplary positioning system may include any suitable number of coarse positioning devices 112 and any suitable number of fine positioning devices 114 . fig2 is a block diagram of a positioning system , according to an exemplary embodiment of the invention . as in the positioning system 100 described in reference to fig1 , the positioning system 200 may include a vehicle 102 equipped with a positioning unit 104 that computes an estimate of the vehicle position based on communications with a number of radio responsive devices disposed at fixed positions about a point of interest 106 . the exemplary positioning system 200 shown in of fig2 includes a set of four coarse positioning devices 112 and a set of four fine positioning devices 114 . other exemplary embodiments of a positioning system may include one , two , three , five , or more coarse positioning devices 112 and one , two , three , five , or more fine positioning devices 114 . as used herein , the term “ set ” as in the phrase “ set of radio responsive devices ” is used to refer to one or more . furthermore , embodiments are not limited to positioning systems that include an equal number of coarse positioning devices 112 and fine positioning devices 114 . as described above in relation to fig1 , the positioning unit 104 may determine the position of the vehicle 102 by transmitting radio signals to the radio responsive devices , receiving return signals from the radio responsive devices , measuring the time - of - flight , and computing a corresponding distance based on the time - of - flight measurements . in the embodiment shown in fig2 , the positioning unit 104 may compute a plurality of distance measurements for each level of positioning . for example , a distance measurement may be computed for each of the coarse positioning devices 112 and each of the fine positioning devices 114 . the plurality of distance measurements can be used to compute a more precise position of the vehicle , for example , using trilateration . to trilateration , each distance measurement corresponds with the radius of a circle centered at the corresponding radio responsive device from which the signal was received . the intersection of the circles provides the vehicle location . three signals may be used to determine a specific point in two - dimensional space . four signals may be used to determine a specific point in three dimensional space . as an example , when the vehicle 102 is within the coarse area of interest 108 , the outbound signals sent by the positioning unit 104 can be received by each of the coarse positioning devices 112 . in an embodiment wherein the coarse positioning devices 112 are wireless communication devices , the coarse positioning devices 112 may generate and transmit a corresponding inbound signal back to the positioning unit 104 upon receiving the outbound signal from the positioning unit 104 . to enable the positioning unit 104 to associate each inbound signal with the proper coarse positioning device 112 , each coarse positioning device 112 may add a unique identifier to the return signal that it generates , as described above . the positioning unit 104 may then compute the distance between the vehicle 102 and each of the coarse positioning devices 112 , based on the round - trip time - of - flight of the outbound signal and the plurality of inbound , signals . the coarse estimate of the vehicle position may then be computed based , for example , on trilateration of the computed distances . in a similar fashion , the fine estimate of the vehicle position may be computed using the signals received from the plurality of fine positioning devices 114 . in embodiments wherein each of the fine positioning devices is an active reflector , each fine positioning device 114 may use a different level of amplitude modulate or phase modulate for the signal that it generates , which enables the positioning unit 104 to associate each inbound signal with the proper fine positioning device 114 . fig3 is block diagram of a vehicle that includes a positioning unit , in accordance with exemplary embodiments of the invention . as shown in fig3 , the positioning unit 104 may include a processor 300 and a memory 302 comprising a non - transitory , computer - readable medium . the memory 302 may include volatile memory such as random access memory ( ram ) used during the execution of various operating programs , including operating programs used in embodiments of the present invention . the memory 302 can also include a storage system for the long - term storage of operating programs and data , including the operating programs and data used in embodiments of the present invention . for example , the memory 302 can include a hard disk drive , an optical drive , a universal serial bus ( usb ) drive , solid state memory , and the like . in embodiments , the processor 300 and the memory 302 may be implemented as an application specific , integrated circuit ( asic ). in embodiments , the positioning unit 104 may be implemented on a general - purpose computing device , for example , laptop computer , a smart phone , and the like . the positioning unit 104 may include two physical layers or phys , referred to herein as phy a 304 and phy b 306 . each phy 304 and 306 is communicatively coupled to the processor 300 and enables the positioning unit 104 to communicate with the radio responsive positioning devices 112 and 114 ( fig1 and 2 ). as an example , phy a 304 may be used to communicate with the coarse positioning devices 112 and phy b 306 may be used to communicate with the fine positioning devices 114 . each of phy a 304 and phy b 306 may include one or more transceivers , amplifiers , signal processors , and any other circuitry which may be used to enable the positioning unit 104 to transmit and receive radio signals . phy a 304 and phy b 306 may each be operatively coupled to a corresponding antenna 308 , which may be disposed in or on the vehicle 102 . in an embodiment , phy a 304 and phy b 306 may be coupled to the same antenna 308 . phy a 304 may be used to acquire information used for computing a coarse estimate of the vehicle position while the vehicle 102 is in the coarse area of interest 108 . phy b 306 may be used to acquire information used for computing a fine estimate of the vehicle position while the vehicle 102 is in the fine area of interest 110 . in an embodiment , phy a 304 communicates with the coarse positioning devices 112 using a first bandwidth , and phy b 306 communicates with the fine positioning devices 114 using a second bandwidth larger than the first bandwidth . for example , the first bandwidth may be approximately 5 to 40 megahertz and the second bandwidth may approximately 500 megahertz to 2 gigahertz . further , phy a 304 may communicate with the coarse positioning devices 112 using an ieee 802 . 11 protocol such as wifi . pry b 306 may communicate with the fine positioning devices 114 by transmitting ultra - wideband ( uwb ) pulses and receiving corresponding echoes from the fine positioning devices 114 . in embodiments , the positioning unit 104 may be communicatively coupled to a central control unit 310 of the vehicle 102 . the position estimates computed by the positioning unit 104 may be output to the central control unit 310 . the central control unit 310 may use the position estimate for a variety of purposes . in an embodiment , the position estimate may be communicated to a person such as a vehicle operator through a user interface . in an embodiment , the central control unit 310 may be operatively coupled to a braking system of the vehicle 102 . in such embodiments , the central control unit 310 may compute a braking signal based , at least in part , on the position estimate received from the positioning unit 104 . the braking signal may determine a degree of braking to be applied to the vehicle 102 may be computed based , for example , on the speed of the vehicle 102 and the distance of the vehicle 102 from the point of interest 106 . the braking signal may be sent from the central control unit 310 to the braking system 312 to engage the brakes of the vehicle 102 until the vehicle 102 is stopped at the point of interest 106 . within the coarse area of interest 108 , the braking signal may be based on the coarse position estimate provided by the positioning unit 104 . within the fine area of interest 110 , the braking signal may be based on the fine position estimate provided by the positioning unit 104 . further , the positioning unit 104 may be configured to automatically switch between outputting a coarse position estimate and outputting a fine position estimate based , at least in part , on whether the vehicle 102 is within the coarse area of interest 108 or the fine area of interest 110 . for example , when the positioning unit 104 is able to establish communications through phy b 306 , the positioning unit 104 may automatically switch from outputting a coarse position estimate to outputting a fine position estimate . in some embodiments , when the vehicle 102 is within the fine area of interest 110 , the positioning unit 104 may compute both a fine position estimate and a coarse position estimate , in which case both phy a 304 and phy b 306 may be operating simultaneously to obtain information for computing the vehicle position . in other embodiments , when the vehicle 102 is within the fine area of interest 110 , the positioning unit 104 may compute only a fine position estimate , in which case only phy a 304 may be operating . fig4 is a block diagram of a method of determining a position , in accordance with exemplary embodiments of the invention . the method 400 may be performed by the positioning unit 104 and is described herein with reference also to fig1 - 3 . the method 400 may begin at block 402 , wherein the vehicle 102 is approaching the coarse area of interest 108 . during this time , the vehicle 102 continues to attempt to establish communications with the set of coarse positioning devices 112 even though the vehicle 102 may be outside the radio range of the coarse positioning devices 112 . upon entering the coarse area of interest 108 , the process flow may advance to block 404 . at block 404 , the positioning unit establishes communications with one or more of the coarse positioning devices 112 . this indicates that the vehicle 102 is within the coarse area of interest 108 . based on the information received from the coarse positioning devices 112 , the coarse estimate of the vehicle position may be computed as described above . for example , the vehicle position may be determined by measuring the time - of - flight of the signals sent to and received from the coarse positioning devices 112 . the position of the vehicle 102 may be tracked as the vehicle 102 moves through the coarse area of interest 108 by periodically transmitting signals to and receiving signals from the coarse positioning devices 112 . as described in relation to fig3 , communications with the coarse positioning devices 112 may be accomplished using a dedicated physical layer , for example , phy a 304 , which uses a narrow - band signal . while tracking the position of the vehicle 102 through the coarse area of interest , the positioning unit 104 may output the coarse estimate of the vehicle position to the central control unit 310 . the central control unit 310 may begin engaging the braking system 312 of the vehicle 102 based on the coarse position of the vehicle as described above . at block 406 , after entering the coarse area of interest , the positioning unit 104 may also begin attempting to communicate with the fine positioning devices 114 . upon entering the fine area of interest 110 , the process flow may advance to block 408 . at block 408 , the positioning unit 104 establishes communications with one or more of the fine positioning devices 114 , which indicates that the vehicle 102 is within the fine area of interest 110 . for example , the positioning unit 104 may detect echoes reflected from the fine positioning devices 114 or receive data packets generated by the fine positioning devices 114 . when the positioning unit 104 is able to detect the signals transmitted by or reflected from the fine positioning devices 114 , the fine estimate of the vehicle position may be computed as described above . for example , the vehicle position may be determined by measuring the time - of - flight of the signals sent to and received from the fine positioning devices 114 . the position of the vehicle 102 may be tracked as the vehicle 102 moves through the fine area of interest 110 by periodically transmitting signals to and receiving signals from the fine positioning devices 114 . as described in relation to fig3 , communications with the fine positioning devices 112 may be accomplished using a dedicated physical layer , for example , phy b 306 , which uses ultra - wideband pulses . while tracking the position of the vehicle 102 through the fine area of interest 110 , the positioning unit 104 may output the fine estimate of the vehicle position to the central control unit 310 . in embodiments , the positioning unit 104 may automatically stop outputting a coarse position estimate and begin outputting a fine position estimate upon entering the fine area of interest 106 . in embodiments , the positioning unit may output both a coarse position estimate and a fine position estimate . within the fine area of interest 110 , the engagement of the braking system 312 of the vehicle 102 may be based on the fine position estimate as described above . eventually , the central control unit 310 may cause the vehicle 102 to stop within the vicinity of the point of interest 106 , for example , within 1 meter of the point of interest 106 . when the vehicle 102 starts moving away from the point of interest 106 , the process flow described above may be performed in the reverse order . in other words , a fine position estimate may be computed while the vehicle 102 is in the fine area of interest 110 until the signals from the fine positioning devices 114 can no longer be detected . once the vehicle 102 leaves the fine area of interest , the positioning unit may automatically switch to computing a coarse position estimate . the positioning unit 104 may track the vehicle position through the coarse area of interest 108 until the positioning unit 104 is out of radio range of the coarse positioning devices 112 . it is to be understood that the above description is intended to be illustrative , and not restrictive . for example , the above - described embodiments ( and / or aspects thereof ) may be used in combination with each other . in addition , many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope . the dimensions , values , and types of materials described herein are intended to illustrate embodiments of the invention , but are by no means and are exemplary in nature . other embodiments may be apparent upon reviewing the above description . the scope of the invention , therefore , should be determined with reference to the appended claims , alone : with the fall scope of equivalents to which such claims are entitled . in the appended claims , any usage of the terms “ including ” and “ in which ” are indicated the plain - english equivalents of the respective terms “ comprising ” and “ wherein .” moreover , in the following claims , the terms “ first ,” “ second ,” “ third ,” “ upper ,” “ lower ,” “ bottom ,” “ top ,” “ up ,” “ down ,” etc , are used merely as labels , and are not intended to impose numerical or positional requirements on their objects . further , the limitations of the following claims are not written in means - plus - function format and are not intended to be interpreted based on 35 u . s . c . § 112 , sixth paragraph , unless and until such claim limitations expressly use the phrase “ means for ” followed by a statement of function void of further structure . as used herein , an element or step recited in the singular and proceeded with the word “ a ” or “ an ” should be understood as not excluding plural of said elements or steps , unless such exclusion is explicitly stated . furthermore , references to “ one embodiment ” of the invention are not to be interpreted as excluding the existence of additional embodiments that also incorporate the recited features . moreover , unless explicitly stated to the contrary , embodiments “ comprising ,” “ including ,” or “ having ” an element or a plurality of elements having a particular property may include additional such elements not having that property . certain changes may be made in the above - described apparatus , without departing from the spirit and scope of the invention herein involved . accordingly , it is intended that all of the subject matter of the above description or shown in the accompanying drawings shall be interpreted merely as examples illustrating the inventive concept herein and shall not be construed as limiting the invention . | 6 |
the amide derivatives ( i ) of the present invention have an excellent juvenile hormone - like activity against insect pests . they exhibit various actions such as metamorphosis inhibition , embryogenesis inhibition and sterilization and are thus efficacious as growth regulators , chemosterilants , ovicides or reproduction inhibitory agents on various insect pests such as agricultural , forestal , hygienic and stored grain insect pests . they are also efficacious against insect pests having an increased resistance to commercial insecticides . in the formula ( i ) which represents the amide derivatives of the present invention , examples of the halogen atom represented by r 2 , r 3 , r 4 are fluorine , chlorine and bromine . examples of the c 1 - c 3 alkyl group represented by r 3 and r 4 are methyl , ethyl , n - propyl and isopropyl . examples of the c 1 - c 3 haloalkyl group represented by r 4 is trifluoromethyl , difluoromethyl , 2 - fluoroethyl , 2 , 2 , 2 - trifluoroethyl , 2 - chloroethyl , 3 - fluoropropyl , 2 - fluoropropyl , 3 - chloropropyl and 3 - bromopropyl , etc . examples of the c 1 - c 3 alkoxy group represented by r 4 is methoxy , ethoxy , n - propoxy and isopropoxy . examples of the c 1 - c 3 haloalkoxy group represented by r 4 is trifluoromethoxy , difluoromethyl , bromodifluoromethoxy , 2 - fluoroethoxy , 2 , 2 , 2 - trifluoroethoxy , 3 - fluoropropoxy , 2 - fluoropropoxy , 2 - chloroethoxy , 3 - chloropropoxy , 3 - bromopropoxy and 1 , 1 , 2 , 2 - tetrafluoroethoxy , etc . examples of the c 3 - c 8 alkyl group represented by r 5 is n - propyl , n - butyl , n - pentyl , n - hexyl , n - heptyl , n - octyl , isopropyl , sec - butyl , isobutyl , 2 - pentyl , 2 - methylbutyl , 3 - methylbutyl , 2 - ethylpropyl , 3 - methyl - 2 - butyl , neo - pentyl , 2 - methyl - 2 - butyl , 2 - hexyl , 2 - methylpentyl , 3 - methylpentyl , 4 - methylpentyl , 2 - ethylbutyl , 3 - hexyl , 3 - methyl - 2 - pentyl , 4 - methyl - 2 - pentyl , 2 , 3 - dimethylbutyl , 3 , 3 - dimethylbutyl , 2 , 2 - dimethylbutyl , 2 - methyl - 2 - pentyl , 3 - methyl - 3 - pentyl , 2 - methyl - 3 - pentyl and 3 , 3 - dimethyl - 2 - butyl , butyl , etc . examples of the c 3 - c 8 haloalkyl group represented by r 5 is 3 - fluoropropyl , 2 , 2 , 3 , 3 , 3 - pentafluoropropyl , 3 - chloro - 2 - butyl , 3 - chloropropyl , 2 - chloropropyl , 2 , 3 - dichloropropyl , 1 , 3 - dichloro - 2 - propyl , 3 - bromopropyl , 2 - bromopropyl , 1 - bromo - 2 - propyl , 2 , 3 - dibromopropyl , 4 - fluorobutyl , 4 , 4 , 4 - trifluorobutyl , 3 , 3 , 4 , 4 , 4 - pentafluoro - 2 - butyl , 2 , 2 , 3 , 3 , 4 , 4 , 4 - heptafluorobutyl , 4 - chlorobutyl , 3 - chlorobutyl , 2 , 3 , 4 - trichlorobutyl , 4 - bromobutyl , 3 - bromobutyl , 5 - fluoropentyl , 5 - chloropentyl , 5 - bromopentyl , 6 - fluorohexyl , 6 - chlorohexyl , 6 - bromohexyl , 7 - chloroheptyl and 8 - chlorooctyl , etc . examples of the c 3 - c 8 alkenyl group represented by r 5 is allyl , 2 - methylallyl , 1 - methyl - 2 - propenyl , 1 , 1 - dimethyl - 2 - propenyl , 2 - butenyl , 3 - butenyl , 2 - ethyl - 2 - butenyl , 2 - methyl - 2 - butenyl , 2 - methyl - 3 - butenyl , 2 - pentenyl , 2 - hexenyl , 5 - hexenyl , 2 - ethyl - 2 - pentenyl , 2 - heptenyl and 2 - octenyl , etc . examples of the c 3 - c 8 haloalkenyl group represented by r 5 is 2 , 3 - dichloroallyl , 2 , 3 - dibromoallyl , 2 - chloro - 2 - propenyl , 3 - chloro - 2 - propenyl , 2 - bromo - 2 - propenyl , 2 - chloromethyl - 2 - propenyl , 2 - chloro - 3 - butenyl , 3 - chloro - 2 - butenyl , 4 - chloro - 2 - butenyl , 4 - bromo - 2 - butenyl and 2 - chloro - 2 - octenyl , etc . examples of the c 3 - c 8 alkynyl group represented by r 5 is 2 - propynyl , 1 - methyl - 2 - propynyl , 1 - ethyl - 2 - propynyl , 1 - propyl - 2 - propynyl , 2 - butynyl , 1 - ethyl - 2 - butynyl , 1 - propyl - 2 - butynyl , 2 - pentynyl , 4 - methyl - 2 - pentynyl , 2 - methyl - 2 - pentynyl , 2 - hexynyl , 3 - hexynyl , 2 - heptynyl and 2 - octynyl , etc . examples of the c 3 - c 8 haloalkynyl group represented by r 5 is 1 - chloro - 2 - propynyl , 1 - bromo - 2 - propynyl , 1 - chloro - 2 - butynyl , 1 - chloro - 2 - pentynyl , 1 - chloro - 2 - hexynyl and 1 - chloro - 2 - octyl , etc . examples of the alkoxyalkyl group having 3 to 8 carbon atoms represented by r 5 is 2 - methoxyethyl , 2 - ethoxyethyl , ethoxymethyl , isopropoxymethyl , n - propoxymethyl , isobutoxymethyl , 2 - isopropoxyethyl , 2 - methoxypropyl , 2 - methoxybutyl , 2 - ethoxypropyl , 2 - ethoxybutyl , 2 - methoxy - 2 - methylpropyl , 2 - ethoxy - 2 - methylpropyl , 2 - butoxyethyl and 2 - hexyloxyethyl , etc . examples of the halogenated alkoxyalkyl group having 3 to 8 carbon atoms represented by r 5 is 2 -( 1 , 1 , 2 , 2 - tetrafluoroethoxy ) ethyl , 2 -( 2 , 2 , 2 - trifluoroethoxy ) ethyl and 2 - difluoromethoxymethyl , etc . examples of the c 3 - c 8 cycloalkyl group represented by r 5 is cyclopropyl , cyclobutyl , 1 - methylcyclopropyl , cyclopentyl , cyclohexyl , 4 - methylcyclohexyl , 4 - ethylcyclohexyl , 2 - methylcyclohexyl and 1 - methylcyclohexyl , etc . examples of the c 3 - c 8 halocycloalkyl group represented by r 5 is 1 - chlorocyclopropyl , 2 , 2 - difluorocyclopropyl , 2 , 2 - dichlorocyclopropyl , 3 - chlorocyclohexyl , 4 - 4 - chlorocyclohexyl and 1 - chlorocyclohexyl , etc . examples of the cycloalkylalkyl group having 4 to 9 carbon atoms represented by r 5 is cyclopropylmethyl , cyclobutylmethyl , cyclopentylmethyl , cyclohexylmethyl , 2 - cyclopropylethyl , 2 - cyclohexylethyl , 3 - cyclohexylpropyl and 2 , 2 , 3 , 3 - tetramethylcyclopropylmethyl , etc . examples of the halogenated cycloalkylalkyl group having 4 to 9 carbon atoms represented by r 5 is dichlorocyclopropylmethyl and 2 , 2 - dichloro - 3 , 3 - dimethylcyclopropylmethyl etc . among the amide derivatives ( i ), preferred are those wherein r 1 is a group of the formula : -- y -- c 6 h . sub . ( 5 - m ) ( r 4 ) m or a group of the formula : -- z -- r 5 ; r 2 is , the same or different , a hydrogen atom , a fluorine atom or a chlorine atom ; r 3 is a halogen atom ; r 4 is , the same or different , a hydrogen atom , a halogen atom or a methyl group ; r 5 is a c 3 - c 6 alkyl group or an alkoxyalkyl group having 3 to 6 carbon atoms ; w is an oxygen atom ; x is an oxygen atom or a sulfur atom ; y is an oxygen atom or a methylene atom ; z is an oxygen atom or a single bond when r 5 is c 3 - c 6 alkyl group , or a single bond when r 5 is an alkoxyalkyl having 3 to 6 carbon atoms , n is an integer of 1 ; m is an integer of 1 or 2 . more preferred are those wherein r 1 is a group of the formula : -- y -- c 6 h . sub . ( 5 - m ) ( r 4 ) m or a group of the formula : -- z -- r 5 ; r 2 is a hydrogen atom ; r 3 is a chlorine atom ; r 4 is , the same or different , a hydrogen atom , a fluorine atom , a chlorine atom or a methyl group ; r 5 is a c 3 - c 6 alkyl group or an alkoxyalkyl group having 3 to 6 carbon atoms ; w is an oxygen atom ; x is an oxygen atom or a sulfur atom ; y is an oxygen atom or a methylene group ; z is an oxygen atom or a single bond when r 5 is a c 3 - c 6 alkyl group , or a single bond when r 5 is an alkoxyalkyl group having 3 to 6 carbon atoms ; n is an integer of 1 ; m is an integer of 1 or 2 . most preferred are those wherein r 1 is a group of the formula : -- y -- c 6 h . sub . ( 5 - m ) ( r 4 ) m or a group of the formula : -- z -- r 5 ; r 2 is a hydrogen atom ; r 3 is a chlorine atom ; r 4 is , the same or different , a hydrogen atom , a fluorine atom , a chlorine atom or a methyl group ; r 5 is a c 3 - c 6 alkyl group or an alkoxyalkyl group having 3 to 6 carbon atoms ; w is an oxygen atom ; x is an oxygen atom or a sulfur atom ; y is an oxygen atom or a methylene group ; z is an oxygen or a single bond when r 5 is a c 3 - c 6 alkyl group , or single bond when r 5 is an alkoxyalkyl group having 3 to 6 carbon atoms ; n is an integer of 1 ; m is an integer of 1 or 2 . the amide derivetives ( i ) of the present invention can be produced by various processes , among which typical examples are shown below . the amide derivative ( i ) is produced by reacting an amine compound of the formula : ## str3 ## wherein r 1 , r 2 , r 3 , w , x and n are each as defined above with an acid halide of the formula : ## str4 ## wherein l is a halogen atom and x is as defined above . the reaction may be carried out usually in an inert solvent in the presence of a base at a temperature of from about - 20 ° c . to the boiling point of the solvent , preferably from about - 5 ° c . to the boiling point of the solvent . the molar proportion of the amine compound ( ii ) and the acid halide ( iii ) to be used for the reaction is not limitative but is preferred to be nearly equal . examples of the inert solvent are aliphatic hydrocarbons ( e . g . hexane , heptane , ligroin , petroleum ether ), aromatic hydrocarbons ( e . g . benzene , toluene , xylene ), halogenated hydrocarbons ( e . g . chloroform , carbon tetrachloride , 1 , 2 - dichloroethane , chlorobenzene , 1 , 2 - dichlorobenzene ), ethers , ( e . g . diethyl ether , diisopropyl ether , dioxane , tetrahydrofuran , ethylene glycol dimethyl ether ), ketons ( e . g . acetone , methyl ethyl ketone , methyl isobutyl ketone , isophorone , cyclohexanone ), esters ( e . g . ethyl acetate , butyl acetate ), nitro compounds ( e . g . nitrobenzene ), nitriles ( e . g . acetonitrile , isobutylonitrile ), tertiary amines ( e . g . pyridine , triethylamine , n , n - diethylaniline , tributylamine , n - methylmorpholine ), acid amines ( e . g . formamide , n , n - dimethylformamide , n , n - dimethylacetoamide ), sulfur compounds ( e . g . dimethyl sulfoxide , sulfolane ), water and mixtures thereof . examples of the base are organic bases ( e . g . pyridine , triethylamine , n , n - diethylaniline ), alkali metal hydroxides ( e . g . sodium hydroxide , potassium hydroxide ), alkali metal carbonates ( e . g . sodium carbonate , potassium carbonate , sodium hydrogencarbonate , calcium carbonate ), alkali metal hydrides ( e . g . sodium hydride ), alkali metal alkoxide ( e . g . sodium methoxide , sodium ethoxide ). when necessary or desired , an ammonium salt such as triethylbenzylammonium chloride and tetrabutylammonium bromide may be added to the reaction system as a catalyst . after completion of the reaction , post - treatment may follow in a per se conventional manner such as extraction with an organic solvent and concentration . when necessary or desired , the product may further be purified by chromatography , distillation , recrystallization , etc . the amide derivative ( i ) wherein x is a sulfur atom is produced by reacting an amide compound of the formula : ## str5 ## wherein r 1 , r 2 , r 3 , w and n are each as defined above with phosphorus pentoxide or a lawesson &# 39 ; s reagent . the reaction may be carried out usually in an inert solvent in the presence of a catalyst at a temperature of from about 0 ° c . to the boiling point of the inert solvent , preferably from about a room temperature to the boiling point of the inert solvent . the molar proportion of the amide compound ( iv ) and phosphorus pentoxide or a lawesson &# 39 ; s reagent is not limitative but is preferred to be nearly equal . the lawesson &# 39 ; s reagent described above means a compound having the formula : ( ch 3 oc 6 h 4 pss ) 2 . examples of the inert solvent are aromatic hydrocarbons ( e . g . benzene , toluene , xylene ), aliphatic hydrocarbons ( e . g . hexane , heptane ), pyridines ( e . g . pyridine , picoline ) and mixtures thereof . after completion of the reaction , post - treatment may follow in a per se conventional manner such as extraction with an organic solvent and concentration . when necessary or desired , the product may further be purified by chromatography , distillation , recrystallization , etc . among the starting compounds in the above processes , the acid halide ( iii ) is a known compound and available on the commercial market . the amine compound ( ii ) is obtainable from appropriate commercial products by a conventional procedure as shown below . ## str6 ## wherein r 1 , r 2 , r 3 , w and n are each as defined above and e is a halogen atom . the two kinds of methods ( i ) and ( ii ) in the above processes can be used properly according to r 1 of the ( thio ) phenol compound ( v ). examples of the halogen atom represented by e are , the same or different , chlorine , bromine and iodine . the amine compound ( ii ) is produced by reducing the ethyl halide compound of the formula : ## str7 ## wherein r 1 , r 2 , r 3 , w , n and e are each defined above . futhermore , the ethyl halide compound ( vii ) is produced by reacting the ( thio ) phenol compound of the formula : ## str8 ## wherein r 1 , r 2 , r 3 , w and n are each as defined above with the halide compound of the formula : the reaction of the ( thio ) phenol compound ( v ) and the halide compound ( vi ) to give the ethyl halide compound ( vii ) may be carried out usually in an inert solvent in the presence of a base at a temperature of from about 0 ° c . to the boiling point of the solvent , preferably from about a room temperature to the boiling point of the solvent . the molar proportion of the ( thio ) phenol compound ( v ) and the halide compound ( vi ) to be used for the reaction is not limitative but is ordinary to be from about 1 : 1 to 1 : 10 . the amount of the base to the ( thio ) phenol compound ( v ) is also limitative but it is preferably to be from about one to two equivalents . moreover , the amine compound ( ii ) is produced by amination of the ethyl halide compound ( vii ) such as a method of reacting hydrazine with a phthalimide derivative obtained by reacting the ethyl halide compound ( vii ) with phthalimide . the reaction of the ethyl halide compound ( vii ) and phthalimide to give the phthalimide derivative may be carried out usually in an inert solvent in the presence of a base at a temperature of from about 0 ° c . to the boiling temperature . the molar proportion of the ethyl halide compound ( vii ) and phthalimide to be used for the reaction is not limitative but is ordinary to be from about 1 : 1 to 1 : 5 . examples of the inert solvent are alcohols ( e . g . methanol , ethanol ), aliphatic hydrocarbons ( e . g . hexane , heptane ), aromatic hydrocarbons ( e . g . benzene , toluene , xylene ), ethers ( e . g . diethyl ether , diisopropyl ether , dioxane , tetrahydrofuran ), ketons ( e . g . acetone , methyl ethyl ketone , methyl isobutyl ketone ), nitriles ( e . g . acetonitrile , isobutylonitrile ), acid amines ( e . g . formamide , n , n - dimethylformamide , n , n - dimethylacetoamide ), sulfur compounds ( e . g . dimethyl sulfoxide , sulfolane ), nitromethane , water and mixtures thereof . the reaction of the phthalimide derivative and hydrazine to give the amine compound ( ii ) may be carried out usually in an inert solvent at a temperature of from about 0 ° c . to the boiling temperature . the molar proportion of the phthalimide derivative and hydrazine ( or its hydrate ) to be used for the reaction is not limitative but is ordinary to be from about 1 : 1 to 1 : 10 . examples of the inert solvent are alcohols ( e . g . methanol , ethanol ), aliphatic hydrocarbons ( e . g . hexane , heptane ), aromatic hydrocarbons ( e . g . benzene , toluene , xylene ), ethers ( e . g . diethyl ether , diisopropyl ether , dioxane , tetrahydrofuran ), acid amines ( e . g . formamide , n , n - dimethylformamide , n , n - dimethylacetoamide ), nitromethane , water and mixtures thereof . the phthalimide derivative can be used with or without its purification in the above reaction . the amine compound ( ii ) is produced by reducing the nitrile compound of the formula : ## str9 ## wherein r 1 , r 2 , r 3 , w and n are each defined above . futhermore , the nitrile compound ( viii ) is produced by reacting the ( thio ) phenol compound ( v ) with chloroacetonitrile . the reaction from the ( thio ) phenol compound ( v ) and chloroacetonitrile to the nitrile compound ( viii ) may be carried out usually in an inert solvent in the presence of base at a temperature of from about 0 ° c . to the boiling point of the solvent , preferably from about a room temperature to the boiling point of the solvent . the molar proportion of the ( thio ) phenol compound ( v ) and chloroacetonitrile to be used for the reaction is not limitative but is ordinary to be from about 1 : 1 to 1 : 5 . the amount of the base to the ( thio ) phenol compound ( v ) is also not limitative but it is preferably to be from about one to five equivalents . moreover , the amine compound ( ii ) is produced by reducing the nitrile compound ( viii ) in the presence of a reducing reagent . examples of the reducing reagent are boron hydride , aluminum hydride , lithium aluminum hydride , raney nickel - hydrogen , palladium - hydrogen , platinum oxide - hydrogen , rhodium - alumina - hydrogen , etc . the reaction conditions such as the solvent , the temperature and molar propertion of starting materials , etc . may vary within broad ranges depending upon the kind of the reducing reagent , but can be readily determined by a conventional manner . examples of the amide derivatives ( i ) of the present invention are shown in table 1 and table 2 . the amide derivatives ( i ) of the present invention have some asymmetric carbon atoms and can form optical isomers . those optical isomers and their mixtures fall within the scope of the present invention . table 1______________________________________ ## str10 ## substituted position ( r . sup . 2 ). sub . n r . sup . 3 ( r . sup . 4 ). sub . m y of y w x______________________________________h cl h o 4 o oh cl 2 - f o 4 o oh cl 3 - f o 4 o oh cl 4 - f o 4 o oh cl 2 , 4 - f . sub . 2 o 4 o oh cl 3 , 5 - f . sub . 2 o 4 o oh cl 3 - cl o 4 o oh cl 4 - cl o 4 o oh cl 3 - br o 4 o oh cl 3 , 5 - cl . sub . 2 o 4 o oh cl 3 - ch . sub . 3 o 4 o oh cl 3 - c . sub . 2 h . sub . 5 o 4 o oh cl 3 - n - c . sub . 3 h . sub . 7 o 4 o oh cl 3 - n - c . sub . 4 h . sub . 9 o 4 o oh cl 3 - iso - c . sub . 3 h . sub . 7 o 4 o oh cl 3 - cf . sub . 3 o 4 o oh cl 3 - cf . sub . 2 h o 4 o oh cl 3 - c . sub . 2 f . sub . 5 o 4 o oh cl h o 4 o oh cl 3 - f o 4 o oh cl 4 - f o 4 o oh cl 2 , 4 - f . sub . 2 o 4 o oh cl 3 , 5 - f o 4 o oh cl 3 - ch . sub . 3 o 4 o oh cl 3 - cl o 4 o oh cl h o 4 o oh cl 3 - f o 4 o oh cl 3 , 5 - f . sub . 2 o 4 o oh cl 3 - cl o 4 o oh cl 3 - cl o 4 o oh cl 3 , 5 - f . sub . 2 o 4 o oh cl 3 - cl o 4 o oh cl h o 4 o o5 - f cl h o 4 o o5 - cl cl 3 , 5 - f . sub . 2 o 4 o o5 - ch . sub . 3 cl 3 , 5 - f . sub . 2 o 4 o o6 - f cl 3 , 5 - f . sub . 2 o 4 o o6 - cl cl h o 4 o oh cl h o 5 o oh cl 3 - f o 5 o oh cl 3 , 5 - f . sub . 2 o 5 o oh cl 2 , 4 - f . sub . 2 o 5 o oh cl 3 - cl o 5 o oh cl 3 - ch . sub . 3 o 5 o o4 - cl cl h o 5 o oh cl h s 5 o oh cl h o 5 o sh cl 3 , 5 - f . sub . 2 o 5 o sh f h o 4 o oh f 3 - f o 4 o oh f 3 , 5 - f . sub . 2 o 4 o oh f 3 - ch . sub . 3 o 4 o oh f 3 , 5 - f . sub . 2 o 5 o oh f 3 , 5 - f . sub . 2 o 4 o sh ch . sub . 3 h o 4 o oh ch . sub . 3 3 - f o 4 o oh ch . sub . 3 3 , 5 - f . sub . 2 o 4 o oh ch . sub . 3 3 - cl o 4 o oh ch . sub . 3 3 - ch . sub . 3 o 4 o oh ch . sub . 3 3 , 5 - f . sub . 2 o 4 o sh ch . sub . 3 h s 4 o oh ch . sub . 3 3 , 5 - f . sub . 2 o 5 o oh c . sub . 2 h . sub . 5 h o 4 o oh iso - c . sub . 3 h . sub . 7 h o 4 o oh cl h ch . sub . 2 4 o o5 - cl cl h ch . sub . 2 4 o o5 - ch . sub . 3 cl h ch . sub . 2 4 o o5 - f cl h ch . sub . 2 4 o oh cl h ch . sub . 2 4 o sh cl h ch . sub . 2 5 o oh cl h ch . sub . 2 5 o sh cl h nh 4 o oh f h ch . sub . 2 4 o oh ch . sub . 3 h ch . sub . 2 4 o oh br h ch . sub . 2 4 o o______________________________________ table 2__________________________________________________________________________ ## str11 ## substituted position ( r . sup . 2 ). sub . nr . sup . 3 r . sup . 5 z of z w x__________________________________________________________________________h cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh br ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh f ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh ch . sub . 3 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh c . sub . 2 h . sub . 5 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh isoc . sub . 3 h . sub . 7 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o o5 - cl cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o o5 - f cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o o5 - ch . sub . 3cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o sh cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 s oh cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 s sh cl ch ( c . sub . 2 h . sub . 5 ) c . sub . 2 h . sub . 5 o 4 o oh cl ch ( c . sub . 2 h . sub . 5 ) c . sub . 2 h . sub . 5 o 4 o sh cl ch ( ch . sub . 3 ). sub . 2 o 4 o oh cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 5 o oh cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 5 o sh cl ch . sub . 2 ch ( ch . sub . 3 ). sub . 2 o 4 o oh ch . sub . 3 ch . sub . 2 ch ( ch . sub . 3 ). sub . 2 o 4 o oh cl ch . sub . 2 c ( ch . sub . 3 ). sub . 3 o 4 o oh cl ch . sub . 2 ccl ( ch . sub . 3 ). sub . 2 o 4 o oh cl ch . sub . 2 ccl ( ch . sub . 3 ). sub . 2 o 4 o sh cl ch . sub . 2 ccl ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o oh cl ch . sub . 2 chc ( ch . sub . 3 ). sub . 2 o 4 o oh cl ch . sub . 2 c ( ch . sub . 3 ) ch . sub . 2 o 4 o oh cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 o oh cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 o sh cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 s oh cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 s s5 - cl cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 o o5 - f cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 o oh cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 5 o oh cl ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 5 o sh cl ch ( ch . sub . 3 )( n - c . sub . 3 h . sub . 7 ) o 4 o oh cl ch ( ch . sub . 3 )( n - c . sub . 4 h . sub . 9 ) o 4 o oh cl ch ( ch . sub . 3 )( n - c . sub . 3 h . sub . 7 ) o 4 o sh ch . sub . 3 ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 o oh f ch . sub . 2 och . sub . 2 ch ( ch . sub . 3 ). sub . 2 -- 4 o oh cl ch . sub . 2 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 -- 4 o oh cl ch . sub . 2 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 -- 4 o s5 - cl cl ch . sub . 2 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 -- 4 o oh cl ch . sub . 2 ch ( c . sub . 2 h . sub . 5 ) c . sub . 2 h . sub . 5 -- 4 o oh cl ch . sub . 2 ch ( c . sub . 2 h . sub . 5 ) c . sub . 2 h . sub . 5 -- 4 o sh cl ch . sub . 2 ch ( c . sub . 2 h . sub . 5 ) c . sub . 2 h . sub . 5 -- 5 o oh cl ch . sub . 2 ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 4 o o4 - cl cl ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 5 o o4 - f f ch ( ch . sub . 3 ) c . sub . 2 h . sub . 5 o 5 o oh cl cyclo - c . sub . 6 h . sub . 11 o 4 o oh cl cyclo - c . sub . 6 h . sub . 10 ( 4 - ch . sub . 3 ) o 4 o oh cl cyclo - c . sub . 6 h . sub . 10 ( 2 - cl ) o 4 o oh cl cyclo - c . sub . 6 h . sub . 11 -- 4 o oh cl cyclo - c . sub . 3 h . sub . 5 ch . sub . 2 o 4 o oh cl cyclo - c . sub . 3 h . sub . 5 ch . sub . 2 -- 4 o oh cl cyclo - c . sub . 6 h . sub . 11 ch . sub . 2 -- 4 o oh cl cyclo - c . sub . 3 h . sub . 4 ( 1 - ch . sub . 3 ) ch . sub . 2 o 4 o o__________________________________________________________________________ examples of the insect pests against which the amide derivatives ( i ) of the present invention exhibit controlling effects are as shown below . planthoppers such as brown planthopper ( nilaparvata lugens ), white - backed rice planthopper ( sogatella furcifera ) and small brown planthopper ( laodelphax striatellus ); leafhoppers such as green rice leafhopper ( nephotettix cincticeps ), nephotettix virescense , nephotettix nigropictus , zig - zag rice leafhopper ( recilia dorsalis ), tea green leafhopper ( empoasca onukii ) and grape leafhopper ( arboridia apicalis ); aphids such as cotton aphid ( aphis gossypii ) and green peach aphid ( myzus persicae ); bugs ; whiteflies ( aleyrodidae ) such as sweet potato whitefly ( bemisia tabaci ) and greenhouse whitefly ( trialeurodes vaporariorum ); scales ; mealy bugs ; lace bugs ( tingidae ); psyllids ( psyllidae ), etc . pyralid moths ( pyralidae ) such as rice stem borer ( chilo suppressalis ), rice leafroller ( cnaphalocrocis medinalis ) and indian meal moth ( plodia interpunctella ); noctuidae such as tobacco curworm ( spodoptera litura ), rice armyworm ( pseudaletia separate ), cabbage armyworm ( mamestra brassicae ) and beet semi - looper ( autographa nigrisigna ); agrothis spp . such as turnip cutworm ( agrothis segetum ) and black cutworm ( agrothis ipsilon ); heliothis spp . ; pieridae such as common cabbageworm ( pieris rapae crucivora ); tortricid moths ( tortricidae ) such as adoxophyes spp . and grapholita spp . ; carposinidae such as lyonetiid moths ( lyonetiidae ), leafblotch miners ( gracillariidae ), gelechiid moths ( gelechiidae ) and tussock moths ( lymantriidae ); diamondback moth ( plutella xylostella ), clothes moths ( tineidae ), casemaking clothes moth ( tinea translucens ) and webbing clothes moth ( tineola bisselliella ), etc . mosquitos ( calicidae ) such as common mosquito ( culex pipiens pallens ) and culex tritaeniorhynchus ; aedes spp . such as aedes aegypti and aedes albopictus ; anopheles spp . such as anopheles sinensis ; midges ( chironomidae ); muscidae such as housefly ( musca domestica ) and false stablefly ( muscina stabulans ); calliphoridae ; sarcophagidae ; lesser housefly ( fannia canicularis ); anthomyiid flies ( anthomyiidae ) such as seedcorn maggot ( delia platura ) and onion maggot ( delia antique ); fruit flies ( tephritidae ); shore flies ( ephydridae ); small fruit flies ( drosophilidae ); moth flies ( psychodidae ); black flies ( simuliidae ); tabanidae ; stable flies ( stomoxyidae ); etc . leaf beetles ( chrysomelidae ) such as cucurbit beetle ( aulacophora femoralis ), striped flea beetles ( phyllotrata striolata ), western corn rootworm ( diabrotica virgifora ) and southern corn root worm ( diabrotica undecimpunctata ); scarabs ( scarabaeidae ) such as cupreous chafer ( anomala cuprea ) and soybeen beetle ( anomala rufocuprea ); weevils ( cureulionidae ) such as maize weevil ( sitophilus zeamais ), rice water weevil ( lissorhoptrus oryzophilus ) and adzuki bean weevil ( callosobruchys chineneis ), etc . ; darkling beetles ( tenebrionidae ) such as yellow mealworm ( tenebrio moliter ) and red flour beetles ( tribolium castaneum ); anobiidae ; coccinellidae such as twenty - eight - spotted ladybirds ( epilachna vigintioctopunctata ); powderpost beetles ( lyctidae ); false powderpost beetles ( bostrychidae ); cerambysidae , etc . blattellidae such as german cockroach ( blattella germanica ); blattidae such as smokybrown cockroach ( periplaneta fuliginosa ), american cockroach ( periplaneta americana ), brown cockroach ( periplaneta brunnea ) and oriental cockroach ( blatta orientalis ), etc . thrips such as thrips palmi , yellow tea thrips ( scirtothrips dorsalis ) and flower thrips ( thrips hawaiiensis ), etc . ants ( formicidae ); sawflies ( tenthredinidae ) such as cabbage sawfly ( athalia rosae ruficornis ), etc . among the insect pests as above exemplified , the amide derivatives ( i ) are particularly effective in controlling those belonging to hemiptera and also exhibit a remarkable controlling effect on planthoppers and leafhoppers in a field of rice plant or aphids . the amide derivatives ( i ) may be used alone as insecticides or in mixtures with other insecticides and / or acaricides to enhance or expand their insecticidal or pesticidal use . examples of the other insecticides and / or acaricide include organophosphorus compounds ( e . g . fenitrothion ( o , o - dimethyl o -( 3 - methyl - 4 - nitrophenyl ) phosphorothioate ), fenthion ( o , o - dimethyl o -[ 3 - methyl - 4 -( methylthio ) phenyl ] phosphorothioate ), diazinon ( o , o - diethyl - o -( 2 - isopropyl - 6 - methyl - pyrimidin - 4 - yl ) phosphorothioate ), chlorpyrifos ( o , o - diethyl - o -( 3 , 5 , 6 - trichloro - 2 - pyridyl ) phosphorothioate ), acephate ( o , s - dimethyl acetylphosphoramidothioate ), methidathion ( s - 2 , 3 - dihydro - 5 - methoxy - 2 - oxo - 1 , 3 , 4 - thiadiazol - 3 - ylmethyl o , o - dimethylphosphorodithioate ), disulfoton ( o , o - diethyl s - 2 - ethylthioethyl phosphorothioate ), ddvp ( 2 , 2 - dichlorovinyldimethylphosphate ), sulprofos ( o - ethyl o - 4 -( methylthio ) phenyl s - propyl phosphorodithioate ), cyanophos ( o - 4 - cyanophenyl o , o - dimethyl phosphorothioate ), dioxabenzofos ( 2 - methoxy - 4h - 1 , 3 , 2 - benzodioxaphosphinine - 2 - sulphide ), dimethoate ( o , o - diethyl - s -( n - methylcarbamoylmethyl ) dithiophosphate ), phenthoate ( ethyl 2 - dimethoxyphosphinothioylthio ( phenyl ) acetate ), malathion ( diethyl ( dimethoxyphosphinothioylthio ) succinate ), trichlorfon ( dimethyl 2 , 2 , 2 - trichloro - 1 - hydroxyethylphosphonate ), azinphos - methyl ( s - 3 , 4 - dihydro - 4 - oxo - 1 , 2 , 3 - benzotriazin - 3 - ylmethyl o , o - dimethylphosphoro - dithioate ) and monocrotophos ( dimethyl ( e )- 1 - methyl - 2 -( methylcarbamoyl ) vinyl phosphate ), etc . ); carbamate derivatives ( e . g . bpmc ( 2 - sec - butylphenyl methylcarbamate ), benfuracarb ( ethyl n -[ 2 , 3 - dihydro - 2 , 2 - dimethylbenzofuran - 7 - yloxycarbonyl ( methyl ) aminothio ]- n - isopropyl - beta - alaninate ), propoxur ( 2 - isopropoxyphenyl n - methylcarbamate ), carbosulfan ( 2 , 3 - dihydro - 2 , 2 - dimethyl - 7 - benzo [ b ] furanyl n - methylcarbamate ), carbaryl ( 1 - naphthyl - n - methylcarbamate ), methomyl ( s - methyl - n -[( methylcarbamoyl ) oxy ] thioacetimidate ), ethiofencarb ( 2 -( ethylthiomethyl ) phenyl methylcarbamate ), aldicarb ( 2 - methyl - 2 -( methylthio ) propionaldehyde o - methylcarbamoyloxime ) and oxamyl ( n , n - dimethyl - 2 - methylcarbamoyloxyimino - 2 -( methylthio ) acetamide ), etc . ); pyrethroides ( e . g . ethofenprop ( 2 -( 4 - ethoxyphenyl - 2 - methylpropyl - 3 - phenoxybenzylether ), fenvalerate (( rs )- alpha - cyano - 3 - phenoxybenzyl ( rs )- 2 -( 4 - chlorophenyl )- 3 - methylbutyrate ), esfenvalerate (( s )- alpha - cyano - 3 - phenoxybenzyl ( s )- 2 -( 4 - chlorophenyl )- 3 - methylbutyrate ), fenpropathrin (( rs )- alpha - cyano - 3 - phenoxybenzyl 2 , 2 , 3 , 3 - tetramethylcyclopropanecarboxylate ), cypermethrin (( rs )- alpha - cyano - 3 - phenoxybenzyl ( 1rs , 3rs )( 1rs , 3rs )- 3 -( 2 , 2 - dichlorovinyl )- 2 , 2 - dimethylcyclopropanecarboxylate ), permethrin ( 3 - phenoxybenzyl ( 1rs , 3rs )( 1rs , 3rs )- 3 -( 2 , 2 - dichlorovinyl )- 2 , 2 - dimethylcyclopropanecarboxylate ), cyhalothrin (( r , s )- alpha - cyano - 3 - phenoxybenzyl ( z )-( 1rs , 3rs )- 3 -( 2 - chloro - 3 , 3 , 3 - trifluoropropenyl )- 2 , 2 - dimethylcyclopropanecarboxylate ), deltamethrin (( s )- alpha - cyano - m - phenoxybenzyl ( 1r , 3r )- 3 -( 2 , 2 - dibromovinyl )- 2 - dimethylcyclopropanecarboxylate ) and cycloprothrin (( rs )- alpha - cyano - 3 - phenoxybenzyl ( rs )- 2 , 2 - dichloro - 1 -( 4 - ethoxyphenyl ) cyclopropanecarboxylate ), etc . ); thiadiazine derivatives ( e . g . buprofezin ( 2 - tert - butylimino - 3 - isopropyl - 5 - phenyl - 1 , 3 , 5 - triadiazin - 4 - one ), etc . ); nitroimidazolidine derivatives ( e . g . imidacloprid ( 1 -( 6 - chloro - 3 - pyridylmethyl )- n - nitro - imidazolidin - 2 - ylideneamine ), etc . ); nereistoxin derivatives ( e . g . cartap ( s , s &# 39 ;-( 2 - dimethylaminotrimethylene ) bis ( thiocarbamate ), thiocyclam ( n , n - dimethyl - 1 , 2 , 3 - trithian - 5 - ylamine ) and bensultap ( s , s &# 39 ;- 2 - dimethylaminotrimethylene di -( benzenethiosulphonate ), etc . ); halogenated hydrocarbons ( e . g . endosulfan ( 6 , 7 , 8 , 9 , 10 , 10 - hexachloro - 1 , 5 , 5a , 6 , 9 , 9a - hexahydro - 6 , 9 - methano - 2 , 4 , 3 - benzodioxathiepin - 3 - oxide ) and gamma - bhc ( 1 , 2 , 3 , 4 , 5 , 6 - hexachlorocyclohexane ), etc . ); benzoylphenylurea derivatives ( e . g . chlorfluazuron ( 1 -[ 3 , 5 - dichloro - 4 -( 3 - chloro - 5 - trifluoromethylpyridin - 2 - yloxy ) phehyl ]- 3 -( 2 , 6 - difluorobenzoyl ) urea ), teflubenzuron ( 1 -( 3 , 5 - dichloro - 2 , 4 - difluorophenyl )- 3 -( 2 , 6 - difluorobenzoyl ) urea ) and flufenoxuron ( 1 -[ 4 -( 2 - chloro - 4 - trifluoromethylphenoxy )- 2 - fluorophenyl ]- 3 -( 2 , 6 - difluorobenzoyl ) urea , etc . ); formamidine derivatives ( e . g . amitraz ( n , n &# 39 ;-[( methylimino ) dimethylidyne ]- di - 2 , 4 - xylidine ) and chlordimeform ( n &# 39 ;-( 4 - chloro - 2 - methylphenyl )- n , n - dimethylmethanimidamide ), etc .). on the practical use of the amide derivatives ( i ) as insecticides , they may be employed as such but are normally mixed with appropriate additives such as solid carriers , liquid carriers , gaseous carriers , feed , etc . to formulate their compositions . when desired or necessary , surfactants and other adjuvants may be further incorporated therein . the compositions may be prepared into any conventional forms such as oil sprays , emulsifiable concentrates , wettable powders , flowable concentrates ( e . g . water - based suspension formulations , water - based emulsion formulations ), granules , dusts , aerosals , heating smoking formulations ( e . g . self - burning - type smoking formulations , chemical reaction - type smoking formulations , porous ceramic plate - type smoking formulations ), ulv formulations , poison baits , etc . the composition of the present invention contains generally the amide derivative ( s ) ( i ) as the active ingredient in an amount of from about 0 . 001 % to 95 % by weight based on the composition . examples of the solid carrier usable for making the composition are fine powders or granules of clays ( e . g . kaolin clay , diatomaceous earth , synthetic hydrated silica , bentonite , fubasami clay , terra alba ), talc , ceramics , other inorganic minerals ( e . g . sericite , quartz , sulfur , activated carbon , calcium carbonate , hydrated silica ), chemical fertilizers ( e . g . ammonium sulfate , ammonium phosphate , ammonium nitrate , urea , ammonium chloride ), etc . examples of the liquid carrier include water , alcohols ( e . g . methanol , ethanol ), ketones ( e . g . acetone , methyl ethyl ketone ), aromatic hydrocarbons ( e . g . benzene , toluene , xylene , ethylbenzene , methylnaphthalene ), aliphatic hydrocarbons ( e . g . hexane , cyclohexane , kerosene , gas oil ), esters ( e . g . ethyl acetate , butyl acetate ), nitriles ( e . g . acetonitriles , isobutyronitrile ), ethers ( e . g . diisopropyl ether , dioxane ), acid amides ( e . g . n , n - dimethylformamide , n , n - dimethylacetamide ), halogenated hydrocarbons ( e . g . dichloromethane , trichloroethane , carbon tetrachloride ), dimethylsulfoxide , vegetable oils ( e . g . soybean oil , cotton seed oil ), etc . examples of the gaseous carrier , i . e . a propellant , include freon gas , butane gas , lpg ( liquefied petroleum gas ), dimethyl ether , carbon dioxide , etc . examples of the surfactant are alkylsulfates , alkylsulfonates , alkylarylsulfonates , alkyl aryl ethers and polyoxyethylene derivatives thereof , polyethylene glycol ethers , polyvalent alcohol esters , sugar alcohol derivatives , etc . examples of the adjuvants such as binders and dispersing agents are casein , gelatin , polysaccharides ( e . g . starch powders , gum arabic , cellulose derivatives , alginic acid ), lignin derivatives , bentonite , sugars , synthetic water - soluble high molecular weight substances ( e . g . polyacrylic alcohol , polyvinylpyrrolidone , polyacrylic acid ), etc . examples of the stabilizer include pap ( acidic isopropyl phosphate ), bht ( 2 , 6 - di - tert - butyl - 4 - methylphenol ), bha ( mixture of 2 - tert - butyl - 4 - methoxyphenol and 3 - tert - butyl - 4 - methoxyphenol ), vegetable oils , mineral oils , surfactants , fatty acids or esters thereof , etc . the base material for self - burning - type smoking formulations may include , for example , burning heat - generating agents such as nitrates , nitrites , guanidine salts , potassium chlorate , nitrocellulose , ethyl cellulose and wood powders , pyrolysis - promoting agents such as alkali metal salts , alkaline earth metal salts , dichromates and chromates , oxygen - supplying agents such as potassium nitrate , burning - supporting agents such as melamine and wheat starch , extenders such as diatomaceous earth , binders such as synthetic pastes , etc . the base material for chemical reation - type smoking formulations can include , for example , heat - generating agents such as alkali metal sulfides , alkali metal polysulfides , alkali metal hydrosulfides , hydrated salts of alkali metals and calcium oxide , catalyzing agents such as carbonaceous substances , iron carbide and activated clay , organic foaming agents such as azodicarbonamide , benzenesulfonyl hydrazides , dinitrosopentamethylenetetramine , polystyrene and polyurethane , fillers such as natural fiber pieces and synthetic fiber pieces , etc . the base material for poison baits may contain feed components such as crop powders , essential vegetable oil , sugars and crystalline cellulose , antioxidants such as dibutylhydroxyrtolune and nordihydroguaiaretic acid , preservatives such as dehydroacetic acid , feeding error preventing agnets such as red paper powders , incentive flavors such as cheese flavor and onion flavor , etc . flowable concentrates ( water - based suspension or emulsion formulations ) are generally obtained by dispersing about 1 to 75 parts by weight of the amide derivative ( i ) as the active ingredient finely and uniformly into water containing about 0 . 5 to 15 parts by weight of a dipersing agent , about 0 . 1 to 10 parts by weight of a suspending agent ( e . g . protective colloids , compounds giving a thixotropic property ) and optionally about 0 to 10 parts by weight of an auxiliary agent ( s ) such as a defoaming agent , an anti - corrosive agent , a stabilizing agent , a spreading agents , penetration auxiliaries , antifreezing agent , an anti - bacterial agent , an antimolding agent and the like . the use of an oil , into which the active ingredient is hardly soluble , in place of water affords oil - based suspension formulations . examples of the protective colloids as above mentioned are gelatin , casein , gums , cellulose ethers , polyvinyl alcohol , etc . examples of the compounds giving a thixotropic property are bentonite , aluminum magnesium silicate , xanthane gum , polyacrylic acid , etc . the composition of the present invention thus obtained may be used as such or after diluting with water . it may be also used in a mixture with any other active component or composition chosen from insecticides , nematocides , acaricides , fungicides , bacteriocides , herbicides , plant growth regulators , synergistic agents , fertilizers , soil conditioners , animal feed , etc . alternatively , the composition of the invention may be applied separately but simultaneously with said other active component or composition . for the purpose of controlling insect pests in the agricultural field , the amide derivative ( i ) according to the present invention may be applied to the insect pests or the locus where the insect pests propagate generally in an amount of about 0 . 001 g to 500 g , and preferably about 0 . 1 g to 500 g per 10 ares . when the amide derivative ( i ) is applied in a form of emulsifiable concentrate , wettable powder , flowable concentrate or the like after dilution with water , its concentration may be from about 0 . 0001 to 1000 ppm . granules , dusts , etc . may be used as such , i . e . without water dilution . when the amide derivative ( i ) is used for household or public hygiene , it may be used in the form of emulsifiable concentrate , wettable powder , flowable concentrate or the like with water dilution , etc . in this case , the concentration of the active ingredient may be from about 0 . 0001 to 10 , 000 ppm . in case of oils , aerosol , fumigants , ulv formulations , poison baits , etc ., they may be applied as such . however , the doses and concentrations may vary within broad ranges depending upon the composition , the application time , the place applied , the application method , the kind of insect pests , the condition of damage , etc . and may be increased or decreased , irrespective of the general ranges set forth above . practical and presently preferred embodiments of the invention will be hereinafter explained in more detail referring to production examples , formulation examples and test examples . these examples , however , should not be construed to be limitative . in the following production examples , % is by weight unless otherwise indicated . to a mixture of 200 g ( 0 . 667 mol ) of 2 -[ 2 - chloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethylamine , 81 g ( 0 . 80 mol ) of triethylamine and 8 liter of toluene , there was added dropwise a solution of 70 g ( 0 . 67 mol ) of cyclopropane carbonylchloride in 2 liter of toluene with stirring at a temperature of from 5 ° c . to 10 ° c . after 2 hours , the reaction mixture was stirred at a room temperature for 15 hours . after the reaction was completed , the resultant mixture was washed twice with water , dried over anhydrous magnesium sulfate and concentrated under reduced pressure . the residue was subjected to silica gel chromatography to give 163 g of n -{ 2 -[ 2 - chloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide as a white crystal ( m . p . 89 °- 90 ° c .). to a mixture of 230 g ( 0 , 667 mol ) of 2 -[ 2 - bromo - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethylamine , 81 g ( 0 . 80 mol ) of triethylamine and 8 liter of toluene , there is added dropwise a solution of 70 g ( 0 . 67 mol ) of cyclopropane carbonyl chloride in 2 liter of toluene with stirring at a temperature of from 5 ° c . to 10 ° c . after 2 hours , the reaction mixture is stirred at a room temperature for 15 hours . after the reaction is completed , the resultant mixture is washed twice with water , dried over anhydrous magnesium sulfate and concentrated under reduced pressure . the residue is subjected to silica gel chromatography to give n -{ 2 -[ 2 - bromo - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide . to a mixture of 185 g ( 0 . 667 mol ) of 2 -[ 2 - chloro - 4 -( 3 - tolyloxy ) phenoxy ] ethylamine , 81 g ( 0 . 80 mol ) of triethylamine and 8 liter of toluene , there is added dropwise a solution of 70 g ( 0 . 67 mol ) of cyclopropane carbonyl chloride in 2 liter of toluene with stirring at a temperature of from 5 ° c . to 10 ° c . after 2 hours , the reaction mixture is stirred at a room temperature for 15 hours . after the reaction is completed , the resultant mixture is washed twice with water , dried over anhydrous magnesium sulfate and concentrated under reduced pressure . the residue is subjected to silica gel chromatography to give n -{ 2 -[ 2 - chloro - 4 -( 3 - tolyloxy ) phenoxy ] ethyl }- cyclopropane carboxyamide . to a mixture of 162 g ( 0 . 667 mol ) of 2 -( 2 - chloro - 4 - propoxymethylphenoxy ) ethylamine , 81 g ( 0 . 80 mol ) of triethylamine and 8 liter of toluene , there is added dropwise a solution of 70 g ( 0 . 67 mol ) of cyclopropane carbonyl chloride in 2 liter of toluene with stirring at a temperature of from 5 ° c . to 10 ° c . after 2 hours , the reaction mixture is stirred at a room temperature for 15 hours . after the reaction is completed , the resultant mixture is washed twice with water , dried over anhydrous magnesium sulfate and concentrated under reduced pressure . the residue is subjected to silica gel chromatography to give n -[ 2 -( 2 - chloro - 4 - propoxymethylphenoxy ) ethyl ]- cyclopropane carboxyamide . to a mixture of 181 g ( 0 . 667 mol ) of 2 -[ 2 - chloro - 4 -( 2 - methylbutoxymethyl ) phenoxy ] ethylamine , 81 g ( 0 . 80 mol ) of triethylamine and 8 liter of toluene , there is added dropwise a solution of 70 g ( 0 . 67 mol ) of cyclopropane carbonyl chloride in 2 liter of toluene with stirring at a temperature of from 5 ° c . to 10 ° c . after 2 hours , the reaction mixture is stirred at a room temperature for 15 hours . after the reaction is completed , the resultant mixture is washed twice with water , dried over anhydrous magnesium sulfate and concentrated under reduced pressure . the residue is subjected to silica gel chromatography to give n -{ 2 -[ 2 - chloro - 4 -( 2 - methylbutoxymethyl ) phenoxy ] ethyl }- cyclopropane carboxyamide . in the same procedure with the same molar proportion of materials as production example 1 , n - 2 -[ 2 - chloro - 4 -( 1 - methylpropoxy ) phenoxy ] ethyl - cyclopropane carboxyamide is obtained by using 2 -[ 2 - chloro - 4 -( 1 - methylpropoxy ) phenoxy ] ethylamine instead of 2 -[ 2 - chloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethylamine . in the same way , n -{ 2 -[ 2 - chloro - 4 -( 4 - trifluoromethylphenoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide , n -{ 2 -[ 2 - chloro - 4 -( 1 - methyethoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide , n -[ 2 -( 2 - chloro - 4 - heptylphenoxy ) ethyl ]- cyclopropane carboxyamide , n -[ 2 -( 2 - chloro - 4 - cyclohexyloxyphenyl ) ethyl ]- cyclopropane carboxyamide or n -{ 2 -[ 2 , 5 - dichloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide is obtained by using 2 -[ 2 - chloro - 4 -( 4 - trifluoromethylphenoxy ) phenoxy ] ethylamine , 2 -[ 2 - chloro - 4 -( 1 - methylethoxy ) phenoxy ] ethylamine , 2 -( 2 - chloro - 4 - heptylphenoxy ) ethylamine , 2 -( 2 - chloro - 4 - cyclohexyloxyphenoxy ) ethylamine or 2 -[ 2 , 5 - dichloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethylamine . a mixture of 500 mg ( 1 . 52 mmol ) of n -[ 2 -( 4 - benzyl - 2 - chlorophenoxy ) ethyl ]- cyclopropane carboxyamide , 614 mg ( 1 . 52 mmol ) of a lawesson &# 39 ; s reagent and 20 ml of anhydrous toluene was refluxed by heating with stirring . after 20 minutes , the reaction mixture was cooled and concentrated under reduced pressure . the residue was subjected to silica gel chromatography to give 487 mg of n -[ 2 -( 4 - benzyl - 2 - chlorophenoxy ) ethyl ]- cyclopropane thiocarboxyamide as a colorless oily substance n d 23 . 6 1 . 6041 ). after one week , the oily substance caked as a white solid ( m . p . 90 °- 92 ° c .). in the same procedure with the same molar proportion of materials as production example 7 , n -{ 2 -[ 2 - chloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethyl }- cyclopropane thiocarboxyamide is obtained by using n -{ 2 -[ 2 - chloro - 4 -( 3 , 5 - difluorophenoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide instead of n -[ 2 -( 4 - benzyl - 2 - chlorophenoxy ) ethyl ]- cyclopropane carboxyamide . in the same way , n -{ 2 -[ 2 - chloro - 4 -( 3 - chlorophenoxy ) phenoxy ] ethyl }- cyclopropane thiocarboxyamide is obtained by using n -{ 2 -[ 2 - chloro - 4 -( 3 - chlorophenoxy ) phenoxy ] ethyl }- cyclopropane carboxyamide . the compound numbers of the amide derivatives ( i ) are shown below . some examples of the amide derivatives ( i ) as produced in the same manner as above are also included . a mixture of 14 . 99 g of 2 - chloro - 4 -( 3 - chlorophenoxy ) phenol , 4 . 44 g of chloro acetonitrile and 8 . 94 g of potassium carbonate in 150 ml dimethylformamide was stirred at a temperature of 70 ° to 80 ° c . in an oil bath for 5 hours . the reaction mixture was cooled to room temperature , poured into water and extracted twice with 100 ml of ethyl acetate . the extracts were conbined together , washed twice with 200 ml of water , dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 14 . 0 g of [ 2 - chloro - 4 -( 3 - chlorophenoxy ) phenoxy ] acetonitrile as a crude product . a solution of 14 . 0 g of the crude product as above obtained in 200 ml of tetrahydrofuran was kept at 0 ° c ., and 200 ml of borane - tetrahydrofuran complex ( 1 . 0m tetrahydrofuran solution ) were dropwise added thereto with stirring at a temperature of 0 ° to 5 ° c . the resultant mixture was stirred at room temperature overnight and then poured into 300 ml of water , followed by removal of tetrahydrofuran by distillation under reduced pressure . the reaction product was salted out and extracted three times with 100 ml of ethyl acetate . the extracts were combined together , washed with 200 ml each of a 5 % aqueous solution of hydrochloric acid , water and a 10 % aqueous solution of sodium hydroxide , dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 11 . 4 g of 2 -[ 2 - chloro - 4 -( 3 - chlorophenoxy ) phenoxy ] ethylamine . yield : 65 %. n d 24 . 3 : 1 . 5842 . in formulation examples as set forth below , parts and % are all by weight . the compound numbers correspond to those in production examples . to a solution of 10 parts of each of compounds nos . 1 to 23 in 35 parts of xylene and 35 parts of dimethylformamide , 14 parts of polyoxyethylene styrylphenyl ether and 6 parts of calcium dodecylbenzenesulfonate are added , and the resultant mixture is thoroughly mixed while stirring to give an emulsifiable concentrate containing the active ingredient in 10 %. twenty parts of each of compounds nos . 1 to 23 are added to a mixture of 4 parts of sodium laurylsulfate , 2 parts of calcium ligninsulfonate , 20 parts of fine powders of synthetic hydrated silica and 54 parts of diatomaceous earth , and the resultant mixture is stirred in a mixer to give a wettable powder containing the active ingredient in 20 %. five parts of sodium dodecylbenzenesulfonate , 30 parts of bentonite and 60 parts of clay are added to 5 parts of each of compound no . 14 and the resultant mixture is pulverized and kneaded with a suitable amount of water . the mixture is granulated in a granulator and air - dried to give granules containing the active ingredient in 5 %. five parts of fine powder of synthetic hydrated silica , 5 parts of sodium dodecylbenzenesulfonate , 30 parts of bentonite and 55 parts of clay are added to 5 parts of each of compound nos . 1 , 3 , 5 , 6 , 7 , 8 , 10 , 12 , 13 and 15 and the resultant mixture is pulverized and kneaded with a suitable amount of water . the mixture is granulated in a granulator and air - dried to give granules containing the active ingredient in 5 %. to a mixture of 1 part of fine powders of synthetic hydrated silica , 1 part of an aggregating agent (&# 34 ; driless b &# 34 ; manufactured by sankyo co ., ltd .) and 7 . 7 parts of clay , 0 . 3 part of each of compound no . 14 is added , and the resultant mixture is well pestled in a mortar and further stirred in a mixer . to the thus obtained mixture , there are added 90 parts of cut clay , followed by mixing to give dusts containing the active ingredient in 0 . 3 %. a mixture of 0 . 3 part of each of compound nos . 1 , 3 , 5 , 6 , 7 , 8 , 10 , 12 , 13 and 15 and 0 . 03 part of fine powders of synthetic hydrated silica is stirred well in a mixer and pulverized by the aid of a centrifugal pulverizer to the resultant mixture , 0 . 97 part of fine powers of synthetic hydrated silica , 1 part of &# 34 ; driless b &# 34 ; and 7 . 7 parts of clay are added , and the resulting mixture is pestled in a mortar and stirred in a mixer . ninety parts of cut clay are added thereto , and further mixing is effected in a sack to give dusts containing the active ingredient in 0 . 3 %. a mixture of 0 . 3 part of each of compound no . 14 , 2 parts of fenitrothion ( o , o - dimethyl o -( 3 - methyl - 4 - nitrophenyl ) phosphorothioate as an organo - phosphorus insecticide , 3 parts of fine powders of synthetic hydrated silica , 1 part of &# 34 ; driless b &# 34 ; and 3 . 7 parts of clay are pestled in a mortar and stirred in a mixer . then , 90 parts of cut clay are added thereto , and the resultant mixture is further mixed in a sack to give dusts . a mixture of 0 . 3 part of each of compound nos . 1 , 3 , 5 , 6 , 7 , 8 , 10 , 12 , 13 and 15 and 0 . 03 part of fine powders of synthetic hydrated silica is stirred in a mixer and pulverized by a centrifugal pulverizer . after addition of 2 parts of fenitrothion , 2 . 97 parts of fine powders of synthetic hydrated silica , 1 part of &# 34 ; driless b &# 34 ; and 3 . 7 parts of clay thereto , the resultant mixture is pestled in a mortar and stirred in a mixer . then , 90 parts of cut clay are added thereto , and the resultant mixture is further mixed in a sack to give dusts . a mixture of 0 . 3 part of each of compound no . 14 , 2 parts of bpmc ( o - sec - butylphenyl n - methylcarbamate ) as a carbamate insecticide , 3 parts of fine powders of synthetic hydrated silica , 1 part of &# 34 ; driless b &# 34 ; and 3 . 7 parts of clay are pestled in a mortar and stirred in a mixer . then , 90 parts of cut clay are added thereto , and the resultant mixture is further mixed in a sack to give dusts . a mixture of 0 . 3 part of each of compound nos . 1 , 3 , 5 , 6 , 7 , 8 , 10 , 12 , 13 and 15 and 0 . 03 part of fine powders of synthetic hydrated silica is stirred in a mixer and pulverized by a centrifugal pulverizer . after addition of 2 parts of bpmc , 2 . 97 parts of fine powders of synthetic hydrated silica , 1 part of &# 34 ; driless b &# 34 ; and 3 . 7 parts of clay thereto , the resultant mixture is pestled in a mortar and stirred in a mixer . then , 90 parts of cut clay are added thereto , and the resultant mixture is further mixed in a sack to give dusts . to a solution of 1 part of each of compound nos . 1 to 23 in an appropriate amount of acetone , 5 parts of fine powders of synthetic hydrated silica , 0 . 3 part of pap ( acidic isopropyl phosphate ) and 93 . 7 parts of clay are added , and the resultant mixture is stirred in a mixer , followed by evaporation of acetone to give dusts containing the active ingredient in 1 %. to 40 parts of an aqueous solution containing 2 parts of polyvinyl alcohol , 10 parts of each of compound no . 14 are added , and the resultant mixture is stirred in a mixer . to the thus obtained dispersion , 40 parts of an aqueous solution containing 0 . 05 part of xanthane gum and 0 . 1 part of aluminum magnesium silicate are added , followed by addition of 10 parts of propylene glycol . the mixture is gently stirred to give a flowable concentrate containing the active ingredient in 10 %. to 28 . 5 parts of an aqueous solution containing 2 parts of polyvinyl alcohol , 20 parts of each of compound nos . 1 , 3 , 5 , 6 , 7 , 8 , 10 , 12 , 13 and 15 and 1 . 5 parts of sorbitan trioleate are added , and the resultant mixture is finely pulverrized by the aid a sand grinder to give particles of less than 3 microns in average particle size . to the resultant mixture , 40 parts of an aqueous solution containing 0 . 05 part of xanthane gum and 0 . 1 part of aluminum magnesium silicate are added , followed by addition of 10 parts of propylene glycol . the mixture is gently stirred to give a flowable concentrate containing the active ingredient in 20 %. into a mixture of 5 parts of xylene and 5 parts of trichloroethane , 0 . 1 part of each of compound nos . 1 to 23 is dissolved , and the resultant solution is mixed with 89 . 9 parts of deodorized kerosene to give an oil spray containing the active ingredient in 0 . 1 %. a solution of 0 . 1 part of each of compound nos . 1 to 23 , 0 . 2 part of tetramethrin ( 2 , 2 - dimethyl - 3 -( 2 - methyl - 1 - propenyl ) cyclopropanecarboxylic acid ( 1 , 2 , 3 , 4 , 5 , 7 - hexahydro - 1 , 3 - dioxo - 2h - isoindol - 2 - yl ) methyl ester ) and 0 . 1 part of d - phenothrin ( 2 , 2 - dimethyl - 3 -( 2 - methyl - 1 - propenyl ) cyclopropanecarboxylic acid ( 3 - phenoxyphenyl ) methyl ester ) in a mixture of 10 parts of trichloroethane and 59 . 6 parts of deodorized kerosene is filled in an aerosol container . after provision of a valve , 30 parts of a propellant ( liquefied petroleum gas ) is filled through the valve under compression to give an oil - based aerosol . a solution of 0 . 2 part of each of compound nos . 1 to 23 , 0 . 2 part of d - allethrin (( 2 , 2 - dimethyl - 3 -( 2 - methyl - 1 - propenyl ) cyclopropanecarboxylic acid 2 - methyl - 4 - oxo - 3 -( 2 - propenyl )- 2 - cyclopenten - 2 - yl ester ), 0 . 2 part of d - phenothrin , 5 parts of xylene , 3 . 4 parts of deodorized kerosene and 1 part of an emulsifier (&# 34 ; atmos 300 &# 34 ;®, atlas chemical co ., ltd .) in 50 parts of distilled water is filled in an aerosol container . after provision of a valve , 40 parts of a propellant ( liquefied petroleum gas ) is filled through the valve under compression to give a water - based aerosol . each of compound nos . 1 to 23 ( 100 mg ) is dissolved in an appropriate amount of acetone , and the resultant solution is impregnated with a porous ceramic plate ( 4 . 0 × 4 . 0 × 1 . 2 cm ) to give a fumigant . the following test examples show some of test results which support the controlling effect of the amide derivatives ( i ) on insect pests . the compound numbers correspond to those as shown in production examples . the compounds used for comparison are as follows : ______________________________________com - poundsymbol chemical structure remarks______________________________________ ## str12 ## compound disclosed in u . s . pat . no . 4 , 859 , 706______________________________________ an emulsifiable concentrate prepared according to formulation example 1 was diluted with water to make a predetermined concentration . the dilution was sprayed onto rice plants cultivated in polyethylene cups at a rate of 20 ml / 2 pots on a turning table . after air - drying , the plants were infested with about ten 3rd instar nymphs of brown rice planthopper ( nilaparvata lugens ). after 10 days , the number of normal adults was counted to obtain an emergence inhibitory rate . the results are shown in table 3 . table 3______________________________________compound no . concentration ( ppm ) inhibitory rate (%) ______________________________________ 1 5 100 0 . 05 100 3 5 100 0 . 05 100 4 5 100 0 . 05 100 5 5 100 0 . 05 100 6 5 100 0 . 05 100 7 5 100 8 5 100 0 . 05 10010 5 100 0 . 05 10011 5 100 0 . 05 10012 5 100 0 . 05 10013 5 100 0 . 05 10014 5 100 0 . 05 10015 5 100 5 10016 0 . 5 100a 5 0______________________________________ an emulsifiable concentrate prepared according to formulation example 1 was diluted with water to make a predetermined concentration . the dilution was sprayed onto potted cotton plants ( in a stage of 8 - 9 days after sowing ) infested with 1st instar nymphs of cotton aphids ( aphis gossypil ) at a rate of 30 ml / 2 pots on a turning table . before spraying and one week after spraying , the humber of nymphs and aduts was counted , and a reproduction inhibitory index was expressed by the following equation : ## equ1 ## wherein the judgement of activity is based on the following standard : a : less than 1 ( excellent effect ) as a result , compound no . 1 showed a as the reproduction inhibitory index at a concentration of 10 ppm . | 2 |
a fastener in accordance with a preferred embodiment of the invention is shown in fig1 and designated generally by reference numeral 10 . in this embodiment , the fastener 10 comprises a clinch fastener having a tapered frusto - conical head 11 with a bottom surface 15 , an undercut 13 , and a barrel - shaped shank 17 . the bottom surface 15 functions as a displacer of material in the receiving ( lower ) panel 34 . the undercut 13 extends from the bottom surface 15 and receives the displaced material of the lower panel 34 . the barrel - shaped shank 17 has a tapered , distal end for guiding the fastener into the receiving hole in a metal panel . the bottom displacer surface 15 is oriented substantially perpendicular to a central vertical axis “ a ”. fig2 shows a punch 20 and die 22 for making a receiving hole in a metal panel 24 in which the fastener 10 is inserted . the punch 20 is typically ground to size and the die must have a clearance aperture 25 for the punch 20 and slug to pass through . the profile of the hole in the panel 24 after punching has an upper straight wall portion 23 , and a lower , tapered tear - out portion 26 having a larger diameter 26 than the upper portion . the “ upper ” and “ lower ” portions are described with reference to the orientation of the panel shown in fig2 ; however , fig3 and 5 , the panel is shown inverted ( compared to fig2 ) and the straight wall portion is located in the lower portion of the hole and the tapered portion is located in the upper portion of the hole . fig3 shows an enlarged section of two panels 32 , 34 that are connected using the fastener 10 described above and installed in accordance with an assembly method of the invention . in this embodiment , the head 11 of the fastener 10 has a shape that generally complements the shape of the hole in the upper panel 32 . the head 11 of the fastener 10 is dimensioned to be installed flush with the top surface 30 of the top panel 32 . the tapered head 11 maintains the mechanical ability to captivate the upper panel 32 to the fastener 10 in the upward direction . in the assembly shown in fig3 , the bottom panel 34 is composed of softer material than the fastener 10 , which permits the use of a clinch undercut 13 . the displacer surface 15 pushes metal from the bottom panel 34 into the undercut 13 located just above the shank , which holds the fastener 10 to the bottom panel 34 . in a preferred embodiment , the top panel 32 has nearly the same hardness as the fastener 10 . the locking taper feature of the fastener 10 is illustrated in fig4 a and 4b , which show both the installation and static condition of the fastener 10 as described in fig1 and 3 . fig4 a and 4b illustrate and describe the forces and scheme necessary to determine the minimal tapering required for self - locking . the orthogonal force of the uniformly distributed taper “ fn ” is modeled at the midline of the conical section at “ dm ”. quite simply , the locking taper will retain the tapered portion of the fastener in the top panel when the vertical component of the friction force exceeds the vertical component of the normal force and the installation force is removed or is zero . the friction force acts in the direction opposite the direction the fastener is being pushed . when the installation force is removed , the vertical component of the normal force acts to push the fastener out of the top panel . the friction force holds the fastener in place in the opposite direction . referring to the static diagrams of fig4 a and 4b , the theoretical force needed to extract the tapered connector “ fe ” may be calculated as follows : understanding that the coefficient of friction “ μ ”= tan ( ψ ) where ψ is an implicit sliding angle the angle for locking can be defined in terms of the coefficient of friction as this locking taper force ( fe ) was calculated using a conservative coefficient of friction for lubricated metal on metal of 0 . 06 . in another preferred embodiment , the locking taper force ( fe ), dimensions of the tapered hole , and dimensions of the tapered head are calculated by taking into account “ galling ”, which is another contributing locking mechanism between the mating sheets . galling is a form of wear between sliding surfaces . for the fastener and assembly shown in fig1 - 5 , the sliding surface is the interface between the tapered head 11 of the fastener 10 and the punched hole in the harder panel 24 . in the presence of a high force compressing the surfaces together , galling occurs as material from both surfaces is pulled with the contacting surface . galling is caused by a combination of friction and adhesion between the surfaces , followed by a tearing of the crystalline structure of the materials involved . the galling surfaces deposit material on the mating surface , effectively creating a friction or cold weld . common materials that are prone to galling are titanium , stainless steel , and aluminum . an assembly of two mating panels and a method of assembling the panels in accordance with a preferred embodiment of the invention are illustrated in fig5 a - d . referring to fig5 a , the fastener 10 is initially positioned in the hole in the top panel 32 in the orientation shown therein with the tapered surfaces properly aligned . next , as seen in fig2 , a press tool 53 forces the fastener 10 downwardly into the top panel 32 from the tapered side of the hole while the bottom panel 34 is supported by an anvil 54 . then , as seen in fig5 c and 5d , when the fastener 10 is pressed by the tool 53 against the anvil 54 with sufficient force , material from both panels flow slightly to form a uniform boundary between the two panels , which creates a very tight fit at high pressure between the fastener 10 and panels 32 , 34 . in this configuration , the fastener 10 can only be removed in the reverse direction of its installation . furthermore , the tapered fastener head 11 is locked in the top panel 32 by the above - described locking taper force or galling or both . fig5 a shows a profile of a punched hole , which has a first portion with straight walls , and a second portion which is conical and faces upward . as installation of the fastener progresses , fig5 b and 5c show how the interface between the fastener and the hard top panel become unified in a common geometry . pressure has made the top panel flow slightly to the fully conical shape , perfectly mated to the fastener 10 . the tapered head locking fastener exhibits high forces between the mating tapered surface , as well as high friction during installation . in one exemplary embodiment of the invention , when a stainless steel fastener is pressed into a hard stainless steel top panel , galling occurs and aids in the retention of the fastener . the same can be said of any other combination of metals prone to galling . fig5 d shows the fully - installed fastener clinched into the softer bottom panel 54 resulting in the attachment of the two panels . the foregoing is to be considered illustrative only of the principles and possible embodiments of the invention . further , since numerous modifications and changes will readily occur to those skilled in the art , it is not desired to limit the invention to the exact construction and operation shown and described . accordingly , suitable modifications and equivalents may be resorted to , all falling within the scope of the invention which shall be determined only by the following claims and their legal equivalents . | 5 |
in order to combat the magnetic noise in dynamoelectric machines for use in more modern applications where the noise is problematic for consumer satisfaction , component interaction , etc . the present inventor has departed from the conventional wisdom of the full pitch and fractional pitch stator cores . the reasoning behind the departure is a recognition that the tangential force , caused by cogging torque of rotor poles as they pass each stator core tooth is additive with the radial force , caused by torque ripple . the reason these two forces are additive , and therefore combine to form a large force creating magnetic noise , is that for a full pitch winding , they both exhibit the same order of frequency , that is the number of poles times the number of phases and for a typical fractional pitch winding , they both exhibit an order of frequency which is a multiple of the number of phases . to minimize magnetic noise the number of slots in a stator core should be as taught herein , whereby the order of frequency of the tangential force and the order of frequency of the radial force will be as far removed from one another as practicable and preferably both not a multiple of the number of phases . in other words , noise can be reduced if it is ensured through careful selection of the number of poles , phases and slots to interact such that an order of frequency of a tangential force of the resulting alternator is different than any multiple of the number of phases of the alternator and different than an order of frequency of a radial force of the alternator . the above is achievable in a dynamoelectric machine by selecting a stator core slot configuration defined by : where p = number of poles ph = number of phases n = any one of a set of whole numbers inclusive from 1 through the number of phases − 1 and m = a whole integer greater than or equal to 0 . as can be seen by the formula , the number of slots can never be equal to the number of phases times the number of poles or even a multiple of the number of phases times the number of poles . a stator is defined has having an unusual number of slots when the number of slots is not equal to , or a multiple of , the number of phases times the number of poles . for example , a stator having 3 phases and 12 poles is defined as having an unusual number of slots when the number of slots is not equal to 36 , 72 , 108 , etc . the typical automotive alternator has three phases or six phases . one example of a stator core configured as taught herein is one in which m = 0 and 85 , 86 , 87 , 88 or 89 slots are utilized with a rotor having 14 poles and the machine including six phases . it will be recognized that such a number of slots does not agree with either a full pitch system or a fractional pitch system . furthermore , it is desirable to have m = 0 so that the number of slots is minimized to reduce winding complexity and to maintain stator slot fill factors ( fewer partially filled slots )— this is especially true when the number of slots is already large . the number of slots can be large if the number of phases is large , such as when ph = 6 for a dual winding ( wye or delta ) commonly known to those skilled in the art . the number of slots can also be large when a design common to those skilled in the art is utilized wherein the number of slots equals two times the number of phases times the number of poles — in this case the invention art results in a stator having a number of slots greater than two times the number of phases times the number of poles . altering the number of slots in a stator core from the conventional number brings with it certain difficulties regarding installation of windings in the stator . this is because the winding pattern will not begin and end in adjacent slots . for this reason , it is taught herein that particular slots are to be skipped in the winding process . skipping slots roughly diametrically opposed from one another provides improved spatial balancing of applicable electromagnetic forces . because of the skipped slots , industry standard type conductors are not used . rather conductors having a unique pattern of endloops and slot segments are utilized . due to the unique pattern of endloops , a hairpin type winding would require numerous shapes of hairpins and therefore , it is desirable , but not necessary , to form the conductor from one continuous conductor as can be seen in fig1 . referring to fig1 , one embodiment of a conductor 10 is illustrated . this particular embodiment is configured for an 86 slot stator core . it will be appreciated that there are “ normal ” endloops 12 interconnected by slot segments 14 and two skip - endloops 16 . although not shown in fig1 , the continuous conductor will be inserted into a stator core such that the slot segments 14 are disposed in the core slots . skip - endloops 16 are intended to enable a slot segment 14 adjacent the skip - endloop 16 to be received in a slot different than the one in which it would have landed had the skip - endloop been a standard endloop . stated another way , skip - endloops 16 position adjacent slot segments into slots that are farther away from one another than “ normal ” endloops 12 . the term adjacent slot segments , utilized herein , refers to two slot segments , which are attached to the same endloop . such conductors allow for irregular slot counts to be wound without winding overlap issues . as noted , the fig1 embodiment of conductor 10 is intended for an 86 - slot stator core to be operable with a 14 pole rotor and 6 phases . it will be appreciated that such a machine should bear 84 slots if full pitch or a multiple of six slots if fractional pitch . typically , the number of “ normal ” endloops 12 greatly outnumbers the amount of skip - endloops 16 . this is true because the number of skip - endloops 16 is proportional to the number of additional slots (( m × ph )+ n ) over the standard number of slots ( number of poles × number of phases ) and as previously mentioned ; it is desirable to minimize the number of slots . therefore a conductor exhibits ( from left to right ) a series of at least two consecutive “ normal ” endloops 12 before having a skip - endloop 16 . while the specific conductor of fig1 is designated for use with an 86 slot stator core , it should be appreciated that machines with 14 poles and 6 phases are not limited to 86 slots to obtain the benefit of the invention . rather , a 14 pole , 6 phase machine is to possess 85 , 86 , 87 , 88 , or 89 slots with m = 0 or 91 , 92 , 93 , 94 , or 95 slots with m = 1 and so forth . any of these number of slots for a 14 pole , 6 phase machine will achieve the desired reduction in magnetic noise . referring to fig2 a and 2b and still using the 86 slot example , two winding passes are illustrated , one in each figure . note that in each figure , there is included a broken line section . this section is intended to represent a duplication of the bending pattern of the conductor illustrated on the left side of the figure . in each case , the bend pattern illustrated is repeated three more times in the broken line section to complete one full length conductor ( the same is true for the conductors shown in fig7 a and 7b , treated hereunder ). for simplicity , the winding is also shown in fig2 a , 2b , 7 a , 7 b and 11 to be in a linear state as if they were separated from the core and rolled out flat . six phases are evidenced by the six conductors illustrated in each figure . the first pass p 1 ( fig2 a ), bears conductors having a form identical to that shown in fig1 hereof . the second pass p 2 ( fig2 b ) bears a slightly different configuration but which includes identical numerals . it is to be appreciated that the term “ skip ” is provided on the drawings with lead arrows to indicate where a stator slot exists but is not to be populated by a slot segment 14 during that particular pass . in the embodiment depicted in fig2 a and 2b , slot 43 and 86 are skipped in the first pass p 1 and slot 37 and 80 are skipped in the second pass p 2 . additional winding passes will repeat the fig2 a and fig2 b patterns in alternating manner . the schematic view of this winding pattern of fig2 a and 2b can be seen in fig3 after the completion of eight passes . illustrated in fig3 , as a partial cross sectional representation of a stator core , is a configuration wound as in fig2 a / 2 b and where slot 37 and 43 of the stator core are populated by only 4 slot segments each and therefore slots 37 and 43 ( as well as slots 80 and 86 not shown in fig3 ) are populated by fewer slot segments than the rest of the slots , after eight passes . the resulting winding of fig2 a and 2b conductors is further illustrated schematically in fig4 so that the step of each phase of conductors radially inwardly at the end of each pass can be visualized . it is to be understood that p 1 - p 8 are passes . further , in order to make fig1 a and 10b ( discussed hereinafter ) clear , each lead on each conductor ( each conductor will have two leads ) is labeled separately . for example , leads a 1 and a 7 extend from each end of a single conductor . similarly , a 6 and a 12 extend from each end of a single conductor . the same is true for the leads marked with a b prefix . referring to fig5 , and in conjunction with the above disclosure , it will be apparent how the leads and therefore the conductors are received into slots in the stator core . relatedly , fig6 is a partial cross sectional view of an alternate wind pattern wherein the wind pattern of fig2 a is repeated twice followed by the wind pattern of fig2 b repeated twice , with this pattern repeated until the completion of eight passes . in this embodiment slot 37 and 43 have only 4 slot segments each and the slot segments are grouped in pairs within these slots . the desirability of this pattern is that the slot segments are disposed in the slots 37 and 43 in pairs such that the typical stator varnishing operation would bond the pairs together , creating a more rigid assembly of slot segments in less - populated slots 37 and 43 . as shown in the relative position on the drawing sheet of fig2 a and 2b , the second pass may be shifted from the first pass by ph slots , such that the conductors of a particular phase of the second pass are shifted from the conductors of the same phase of the first pass . in another alternate embodiment , referring to fig7 a ( again having 86 slots ), the first pass is similar to that illustrated in fig2 a except that the skip endloops 16 are positioned to cause the conductor to skip slot 37 and slot 80 . in the first pass p 1 , all conductors skip slots 37 and 80 . the illustration of fig7 b differs from that of fig7 a . fig7 b presents a distinct second phase p 2 conductor from that of fig7 a in that the skip endloops 16 are positioned to cause it to populate slot 37 as opposed to slot 38 and slot 80 as opposed to slot 81 . in the second pass p 2 , all conductors skip slots 38 and 81 . in this embodiment , as in the fig2 a / 2 b embodiment , first and second passes may alternate or two first passes and two second passes may alternate or any other similar alternating pattern . the desirability of this pattern is ease of manufacturing because only the first phase is disposed in different slots depending on the pass . referring to fig8 , another embodiment is schematically illustrated wherein the winding pattern of fig7 a / 7 b are employed where four spaced slot segments are illustrated in slots 37 and 38 , after eight passes . referring to fig9 yet another alternate winding pattern is illustrated that uses a pattern that is the same for each pass . the pattern for example could be like that of fig7 a . such arrangements will leave two slots , as for example 37 and 80 , empty . the desirability of this pattern is ease of manufacturing because all of the conductors of each phase have the same shape ( the conductors are the same except shifted one slot from another ). to ensure clarity in the understanding of the disclosure herein by one less familiar with alternators , reference is made to fig1 wherein a schematic cross - section view of a prior art alternator is illustrated . the alternator 100 includes a pulley 102 connected to a rotor shaft 104 upon which a pair of pole pieces 106 and 108 are rotationally supported . pole pieces 106 , 108 are configured to present a plurality of pole fingers 110 , 112 ( two visible ) circumferentially around the shaft 104 . rotor core windings 114 are positioned between fingers 110 / 112 . the alternator 100 further includes a stator core 116 having a number of slots , the number being of full or fractional pitch , as explained above ( not shown ) and stator core windings 118 therein . the noted alternator components are supported in position by a front end frame 120 and a rear end frame 122 . portions of the rotor and associated rotating poles create an induced current in the stator core windings , which current is usable as generated electrical energy . referring to fig1 , a cascade style winding pattern is illustrated . while the illustrated style is itself known in the art , it is not know in combination with the stator core slot configuration taught herein . in view of the unconventionality of the foregoing teaching regarding the configuration and windings of a stator core , it is prudent to include schematic wiring diagrams to ensure complete understanding by a reader . with reference to fig1 a and 12b , a dual wye and a 3 - phase distributed wye diagram are illustrated . in fig1 a , each leg of the wye is connected in parallel , for example , a 2 and b 2 are connected to each other and also to a diode pair 130 as shown . connections are likewise for each other pair of diode end leads of each conductor . in addition , each leg of the wye is connected at the neutral point 132 or 134 respectively . as can be seen in fig1 a , one wye winding is shifted by approximately 30 degrees with respect to the other wye winding . returning to fig1 b , the 3 - phase wye uses a single neutral point 136 and only three diode pairs 138 . additional conductor lead connections are connected in parallel at each node 140 , 142 and 144 as illustrated . as can be seen in fig1 b , each phase is comprised of two portions wherein one portion is shifted approximately 30 degrees from the other portion . | 8 |
the preferred and alternative exemplary embodiments of the present invention include a channel - context compression algorithm that operates through a hardware engine in a processor having 16 - bit data words . however , the algorithm will operate effectively for processors using 32 - bit or other sizes of data words . the exemplary encoder is an adaptive packing operation . referring to fig1 , input to the encoder is divided into blocks 10 of four 16 - bit words 12 illustrated as samples s 1 through s 4 . the blocks 10 may contain any reasonable number of words as samples , such as six , eight , or ten words . these words 12 are treated as twos - complement integers . each block 14 is examined to find the word with the maximum number of significant bits . this number of significant bits is called the packing width and each word in the block can be represented with this number of bits . for example , if the word s 1 ( 18 ) has the largest magnitude in block ( 16 ) of − 100 , then block b n 16 is assigned a packing width p n = 8 bits for each of the words s 1 through s 4 . the p n least significant bits of the four words s 1 through s 4 ( 12 ) in block b n ( 16 ) are then packed into a block of 4 * p n bits . there is no loss of information in this packing operation . fig1 also shows a prefix header h 20 that is added to the beginning of the packed block 16 to represent the change in packing width from the previous block b n − 1 ( 22 ). in the example this change is defined as p n - p n − 1 . this difference is encoded as a variable - length sequence using between one and seven bits . the packing size for each block b 1 to b n + 1 must be known in order to determine how to unpack each block . representing the difference in packing size between blocks 10 occupies fewer bits in a processor memory as compared to using a set number of bits each time , for example four bits for the change in size between each block b 1 through b n + 1 . to form the prefix header 20 , the packing width difference is computed modulo sixteen and then encoded as follows : 0 is encoded as the single bit 0 ; 1 or 15 are encoded as the 3 bits 11 ×, where x = 1 for 1 and x = 0 for 15 ; 2 and 14 are encoded as the 4 bits 101 ×, where x = 1 for 2 and x = 0 for 14 ; 3 through 13 are encoded as the 7 bits 100xxxx where xxxx directly gives the numbers 3 through 13 . the codes 100xxxx where xxxx represents 0 - 2 or 14 - 15 are not valid codes ; however , the 6 - bit code 100000 is used as a last block marker . the compressed output consists of the prefix header 20 followed by the packed block 12 . these bits are packed into 16 bit words , from most significant bit to least significant bit . when a word is full , packing continues with the most significant bit of the next word . the last block 22 has a longer prefix to identify the end of the packed data . the prefix for block 22 consists of the 6 - bit last block marker 100000 , followed by 2 bits giving the number of words in the last block , 00 for one word , 01 for two words , 10 for 3 words and 11 for 4 words , followed by the normal block prefix . after this last block 22 is packed , any remaining bits in the last output word can be ignored . this last block prefix is not necessary if the number of input words is known to the decoder ahead of time . in a worst case expansion of data over a large number of input words , all 16 - bits are required to represent each block . in this case , the four 16 - bit words 12 in each block 10 are placed , unchanged , into the output stream with an additional 0 bit representing no change from the previous block &# 39 ; s packing width . thus the worst - case expansion is one bit for every sixty - four bits . other scenarios are possible giving the same expansion . for instance , blocks can alternate between 15 - bit packing widths and 16 - bit packing widths . in this case , every block has a 3 - bit prefix representing a packing width delta of plus or minus one . therefore , for every two input blocks there will be 3 + 4 * 15 + 3 + 4 * 16 bits = 130 bits , which is again is one bit for every 64 bits expansion averaged over 2 blocks . the maximum expansion over the long run is always one bit for every 64 bits even though one of the blocks has a 3 - bits for 64 - bits expansion . alternating between 13 - bit and 16 - bit packing widths , with 7 - bit prefixes again results in 7 + 4 * 13 + 7 + 4 * 16 bits = 130 bits over 2 blocks . fig2 is a graphical illustration of channel context memory contents for a typical voice over ip application . in this case the input signal is a noise signal encoded with pulse code modulation ( pcm ) that has been sampled at 8000 samples per second . there are 4428 16 - bit words channel context memory contents , including taps from an echo canceller , that are graphed over time on axis 26 . the words are graphed as two &# 39 ; s complement numbers in 16 - bit format from − 32768 to 32767 on axis 28 . the preferred compression algorithm may be applied to a processor containing numerous such channels to pack thousands of context memory data words into a smaller memory area , thereby significantly decreasing total die area and decreasing chip costs . if the exemplary compression algorithm is used in a voice over internet protocol ( voip ) application , where available mips ( million instructions per second ) is not the limiting factor , this compression technique can increase the number of channels per processor chip . available mips can be increased by increasing the clock rate , or adding more cores in a multi - core chip design . even in situations where available mips is the limiting factor , this compression technique can be used to reduce the amount of on - chip memory required resulting in a smaller die size and accompanying lower cost per channel . a small power reduction will also result from a lower static power from the smaller memory . fig3 is a functional illustration of data movement within processor 30 by the hardware engine between shared ram ( random access memory ) 32 and local memory 34 . the compressed context for a channel would be expanded by hardware compression / expansion engine 35 and moved 36 from shared ram 32 to local memory 34 prior to processing data in a channel . when processing for that channel is complete , the channel context would be compressed by hardware compression / expansion engine 35 and moved 38 from local memory 34 back into shared ram 32 . the compression algorithm allows for the design of a simple compression / expansion hardware engine , which compresses / expands data and moves it simultaneously . the hardware compression / expansion engine performs an expansion function with a source and destination address . when the expansion function is completed the channel is processed and then the engine also performs a compression function with a source and destination address . if compression is performed with a hardware engine , then most of the context will be processed . however , if compression is performed in software , the best tradeoff between mips and memory might be to process only those portions of the context that consistently compress well . if an application contains constants or other data for each channel that does not change or rarely changes , then after that data is uncompressed in a write operation to local memory , it is not necessary for the hardware engine to re - compress and write the constant data back into shared memory . as stated previously , the compressed contexts for all of the channels will be stored in some pool of shared memory . the size of each compressed context will vary , and the final size is not known until the compression actually occurs . a fixed - size buffer could be allocated ahead of time for each channel , but memory will be wasted if that buffer is too large . an additional data movement step is required , implemented either in hardware or software , for handling the spillover case , where a compressed context is larger than that fixed size . alternatively , memory could be allocated from a global pool of smaller fixed size blocks that are chained together . in this solution , there must be a pointer word for every memory block . larger block sizes will use fewer pointers , however this will result in more wasted memory in the last block of a compressed context . another disadvantage of this method that the hardware compressor will have to be more complex to handle the chained block method . as a minimum , the hardware will have to handle the chaining of blocks as contexts are expanded or compressed . in addition , the hardware engine may require allocation techniques to allocate and free blocks of memory in realtime . in the preferred exemplary embodiment , a combination of hardware and software is used to handle compressed contexts efficiently , but without too much hardware complexity . a global pool of fixed - size memory blocks is used . the context handler engine is able to read from , and write to , pre - allocated chained blocks of memory but would not handle allocation and freeing of memory itself . initially , each compressed context is stored in the minimum number of memory blocks necessary . when a channel number n − 1 begins processing , software sets up the context handler engine to expand the channel context for channel n from the pool storage into local memory 34 . when channel n − 1 finishes processing , the software increases the compressed context storage area for channel n − 1 to a size large enough to handle the worst case by allocating new blocks . software will then set up the context handler engine to write out the compressed context for channel n − 1 . after the compression operation is complete , the context handler engine will store the number of blocks actually used to write out this context . meanwhile channel n will run and upon processing completion , the software will use the information in that register to free up any blocks of storage not used by the compressed context from channel n − 1 . software then increases the compressed context storage area for channel n , and the cycle continues . with this method , there is always room to store any channels &# 39 ; context with no spillover problem and extra memory is only needed for one channel at a time . if the memory required by all of the compressed contexts exceeds the amount that was anticipated , the processor implements an emergency graceful degradation algorithm to ensure all channels keep running . reducing the length of an echo canceller &# 39 ; s delay line rom 128 ms to 64 ms or reducing the length of a jitter buffer are examples from a voice over ip application where memory could be recovered in an emergency . fig4 illustrates a functional bock diagram of an exemplary hardware compression engine 40 . the exemplary compression engine is assumed to be a 2 - port device with a read port to access uncompressed words and a write port to write out compressed words . words are read from source memory 42 into a 64 - bit input register 44 , four words at a time . packed words are written out from a 64 - bit output register ( or ) 45 . four words are processed in parallel to speed up processing . however , where processing speed is not an issue , a lower complexity serial approach may be implemented . the exemplary compression algorithm is executed in eight steps , which could be pipelined so that four input words are processed each clock . there is a 64 - bit input register ( ir ) 44 , a 71 - bit packed block register ( pbr ) 46 and a 64 - bit output register ( or ) 45 . n r , the number of valid bits in the or 45 , is initialized to 0 . b , the packing width of the previous block , is set to some default value . in the encoder 40 , four words are read from the source memory 42 into the 64 - bit input register ( ir ) 44 . the number of significant bits , b new , in the largest - magnitude word is found . delta b = b new − b is computed , b is set to b new , and the block prefix 20 , with length l p , is generated from delta b . the four words in the ir 44 are packed with the packing logic array 52 and gen b logic 54 and interleaved by multiplexers ( mux ) 58 and 56 into the 4 * b bits , bits 0 :( 4 * b − 1 ) of the pbr 46 . the pbr 46 is then left shifted by 71 − 4 * b − l p bits . the block prefix 20 is placed into the l p msbs ( most significant bits ) of the pbr 46 . the new packed l p + 4 * b bits in the pbr 46 can be as any as 71 bits . the or 44 and the pbr 46 , concatenated together in barrel shifter 50 as one 135 - bit register , is shifted left by n 1 = min ( 64 − n r , l p + 4 * b ) bits . n r is then updated as n r = n r + n 1 . if n r = 64 , then the or 44 is written out to four words in the destination memory 48 and the or 45 and the pbr 46 , concatenated together in barrel shifter 50 as one 135 - bit register , is shifted left by n 2 = min ( 64 , l p + 4 * b − n 1 ) bits . n r is updated as n r = n 2 . if , once again n r = 64 , the or 45 is written out to four words in the destination memory 48 and the or 45 and the pbr 46 , concatenated together in barrel shifter 50 as one 135 - bit register , is shifted left by n 3 = l p + 4 * b − n 1 − n 2 bits . n r is then updated as n r = n 3 . fig5 illustrates an exemplary hardware expansion engine 60 used in the preferred embodiment . the exemplary expansion engine is a 2 - port device with a read port to access compressed words and a write port to write out uncompressed words . packed words are read from source memory 42 and interleaved through mux 62 into a 64 - bit input register 62 , four words at a time . unpacked words are written out from a 64 - bit output register 68 . four words are processed in parallel to speed up processing . however , where processing speed is not an issue , a lower complexity serial approach may be implemented . the exemplary algorithm executes decoder 60 in eight steps , which could be pipelined so that four output words are processed each clock . to start the processing , sixty - four bits are read from the source memory 42 into the 64 - bit input residue register ( irr ) 70 and the next sixty - four bits are read from the source memory 42 and interleaved through 2 : 1 mux 62 into the 64 - bit input register ( ir ) 64 . the number of valid bits in the ir 64 , n 1 , is set to sixty - four and b , the packing width of the previous block , is set to some default value . the next block prefix 20 is determined from the seven msbs of the irr 70 using the gen b logic 74 . b is modified by delta b of the block prefix 20 to obtain the number of significant bits in the successive block and l p is set to the length of the prefix . the irr 70 and the ir 64 , concatenated together as one 128 - bit register in barrel shifter 72 , are shifted left by n new = max ( n 1 , l p ) bits . n 1 is then updated as n 1 = n 1 − nnew . if n 1 = 0 , then sixty - four bits are read from the source memory 42 into the ir 64 , the irr 70 and ir 64 , concatenated together as one 128 - bit register in barrel shifter 72 , is shifted left by lp − n new bits and n 1 is updated as n 1 = 64 + n new − l p . the 4 * b msbs of the irr 70 are unpacked by the unpacking logic array using gen b logic 74 and unpack logic 76 into the 64 - bit output register ( or ) 68 . the 64 - bit or 68 is written out to four words in the destination memory 48 . the irr 70 and ir 64 , concatenated together as one 128 - bit register in barrel shifter 72 , is next shifted left by n new = max ( n 1 , 4 * b ) bits . n 1 is then updated n 1 = n 1 − n new . if n 1 = 0 , sixty four bits are read from the source memory 42 into the ir 64 , the irr 70 and ir 64 , concatenated together as one 128 - bit register in barrel shifter 72 , is shifted left by 4 * b − n new bits and n 1 is then updated as n 1 = 64 + n new − 4 * b . fig6 illustrates the graph of fig2 combined with a graph 72 of the compression ratio ( e . g ., packing lengths ) for each of the blocks of four words . in graph 72 , a zero compression line 74 is placed along the 35 , 000 mark of axis 28 and a one compression line 76 is placed along the 45 , 000 mark of axis 28 . graph 72 illustrates compressed bits divided by uncompressed bits and shows a comparison of compression to the uncompressed words of fig2 along axis 26 . expansion of compressed data occurs where the graphed line in 72 rises above the one line 76 . in graph 72 , the 4428 words on axis 26 are compressed to 2796 words , a savings of 63 %. as observed in fig6 , the regions from approximately 400 to 1000 and 1500 to 2500 compress very well . the regions from approximately 1000 to 1300 and 3700 to 4000 are examples of regions that do not compress well . however , most regions do provide compression and any expansion is minimal . therefore , the more memory that is compressed by the exemplary algorithm , the more memory that is saved in the process . because many varying and different embodiments may be made within the scope of the inventive concept herein taught , and because many modifications may be made in the embodiments herein detailed in accordance with the descriptive requirements of the law , it is to be understood that the details herein are to be interpreted as illustrative and not in a limiting sense . | 7 |
the advantage of using double capacitors will be set forth herein in relation to an advantageous embodiment of the invention . here the advantages of the teaching according to the invention can be particularly clearly verified . if the efficiency is identified as the ratio of the delivered to the stored energy , it will be seen that the residual energy in the case of the parallel - serial connection only ever constitutes a quarter of that which is still stored on the individual capacitor . in the example with a tilt of 50 % the efficiency is 75 % in the case of the individual capacitor , whereas it is 93 . 75 % in the case of the two partial capacitors . the lower initial energy ( 80 %) is afforded by the lower residual energy ( 6 . 25 %) of the two partial capacitors . the individual capacitor needs 1 . 25 times the energy in order to achieve the same effect . heretofore the approach by way of the degree of utilization ( tilt ) in the calculation in equation ( 11 ) gave a relative ratio between c 1 and c 2 . if we ask which specific time constant rc 1 is concealed behind a 50 % tilt , attention is directed to table 1 at the end of this detailed description . specified therein for a tilt of 50 % is an rc 1 of between 6 . 4 and 6 . 6 ms , on average 6 . 5 ms , which with a defibrillation impedance of 50ω gives a preferred capacitance for the capacitor c 1 of 130 μf . the individual capacitor of the dual combination in accordance with equation ( 12 ) then has a capacitance of : in accordance with the invention therefore when settling for a time constant on the basis of a look - up table ( table 1 ) it is possible to determine the corresponding value for the pulse duration , tilt and efficiency for the individual capacitor . the partial capacitor corresponding thereto can then be ascertained with equation ( 11 ), for the parallel - serial use . this and the parameters resulting therefrom are summarized in table 1 from which it is possible to select the respective combination insofar as either the partial capacitor with an assumed load is predetermined , or a degree of efficiency which permits a large capacitor with at the same time a low voltage . in the foregoing example of the energy calculation for a 50 % tilt , it is possible to see that the levels of energy delivered are the same for both circuitry versions . that is due to the fact that the initial voltage and the mean voltage are equal for both versions . for a tilt of less than 50 %, the series connection of the partial capacitors during the residual discharge means that a higher voltage is produced than during the first phase so that the overall mean value of the voltage is higher with two capacitors . as it is not the delivered energy but the time integral in relation to voltage that is the crucial parameter in terms of defibrillation , the initial voltage can be reduced when using the double capacitors to the amount by which the voltage mean values increase . for tilts of greater than 50 %, the initial voltage in the case of the two - capacitor system will have to be set at a correspondingly higher level . the reduction in the capacitance of the two - capacitor system together with the increase in the mean voltage mean that the normalized stored energy ( nse2 ) of a two - capacitor system above an rc - value which governs the 50 % tilt extends markedly more shallowly than the curve for the one - capacitor system ( see fig1 ). the curve for the normalized stored energy ( nse1 ) of the one - capacitor system corresponds to the curve which is shown as fig8 in reference 4 from the background of the art , but which was there given with a normalized time constant . the normalized stored energy of the two - capacitor system ( nse2 ) is afforded by multiplication from the reduced capacitance ( 2c 2 / c 1 ), the mean voltage altered by voltage doubling ( mv1 / mv2 ) and the nse1 value of the one - capacitor system curve . the former simply arises out of equation ( 11 b ) by forming the ratio of 2c 2 to c 1 , and multiplying it by the square of the ratio of the mean values of the voltages ( mv1 : mv2 ) 2 and the corresponding value of nse1 ( see table 1 ). an example will illustrate this operating procedure . with a time constant rc 1 of 20 ms the tilt − 0 . 340 ( see table 1 ), and the normalized mean value of the voltage nmv1 = 0 . 818 , which also applies in regard to parallel discharge of the two c 2 - capacitors . the mean value of serial discharge is 0 . 72 ( this follows from discharge to half the value ) multiplied by double the exponential final value of ( 1 − tilt ) corresponding to 0 . 66 , that is to say 0 . 72 · 1 . 32 = 0 . 95 . that gives an overall weighted mean value nmv2 of ( 5 . 87 ms · 0 . 818 + 2 . 45 ms · 0 . 95 ): 8 . 32 ms = 0 . 857 ( duration of the parallel discharge = 5 . 87 ms , and that of the serial discharge = 2 . 45 ms , the overall duration = 8 . 32 ms ) which is 1 . 048 times higher than the mean value in the case of one - capacitor discharge . the initial voltage can be correspondingly lowered , which corresponds to a reduction in the stored energy to 0 . 911 . with equation ( 11 b ) and by analogy with ( 12 / 13 ), it is possible to calculate f or rc 1 = 20 ms an energy ratio e2 : e1 of 0 . 706 , which results in an overall reduction of 0 . 911 0 . 706 = 0 . 643 , or , to put that another way : the normalized stored energy of the one - capacitor system nse1 of 2 . 591 is reduced in the case of the two - capacitor system to an nse2 of 0 . 911 · 0 . 705 · 2 . 591 = 1 . 666 . for comparison : with a tilt of 50 % nse1 = 1 . 46 and nse2 = 1 . 17 ( see table 1 ). on the assumption that with a 50 % tilt with an rc 2 of 2 . 6 ms 10 j is required for defibrillation , the one - capacitor system with rc 1 of 6 . 5 ms would correspondingly require 12 . 5 j for the same effect . a two - capacitor system with a tilt of 34 % and an rc 2 of 7 . 06 ms would rise to 14 . 2 j and finally the one - capacitor system with rc 1 of 20 ms would rise to 22 . 1 j . the calculation once more demonstrates the finding that the pure energy information says nothing about the effectiveness thereof . in comparison with the example with a time constant of 20 ms , with an rc 1 of 10 ms the energy is reduced to only 0 . 966 (= 0 . 984 2 ) by virtue of the excessive increase in voltage , while as stated , with a 50 % tilt , there is no longer any difference as the mean voltage value is equal for both discharges . it follows therefrom that the new method fits in well in particular with the implementation of defibrillators with large capacitors and a correspondingly low voltage . investigations of three works ( references 5 - 7 ) in which the tilt was experimentally researched with a very low level of energy input showed that the energy with optimized tilt can actually be reduced to about 70 % in comparison with a tilt of 80 % ( in an experiment of 88 %). if consideration is further given to the reduction due to the two - capacitor system of for example 80 % for a 50 % tilt , then the highest mark of 30 j which was earlier established is reduced by the described two - capacitor systems to 0 . 8 · 0 . 7 · 30 j = 17 j with the same effectiveness . the maximum energy required would therefore fall still further if the capacitors were selected to be still smaller than the above - calculated 52 μf with a tilt of 50 %, which however involves increased voltages . thus for example a capacitor of 104 μf ( 2 · 52 μf ) requires just on 570 v in order to be charged up to the 17 j corresponding to the 30 j at an 80 % tilt value . therefore table 1 with the parameters nse1 and nse2 represents the required input in order to be able to effect defibrillation with the predetermined parameter ( this is generally the capacitor ) in comparison with the theoretically lowest delivered energy nde with an rc 1 of 2 . 36 ms ( in an 8 - digit calculation that value is to be unambiguously defined ). the input for nse1 or nse2 which can be read off as a function of the time constant rc 1 could also be interpreted as a reciprocal value which then can be interpreted as efficiency η in relation to the theoretical optimum . a horizontal line in graph 1 , that is to say a predetermined level of efficiency , demonstrates the possibility in relation to larger capacitors for the two - capacitor system or conversely it also shows that under some circumstances a one - capacitor system can be more worthwhile than a two - capacitor system beyond an rc 1 of 20 ms . a vertical line clearly shows the lower degree of input ( or higher efficiency ) if the two - capacitor system were embodied instead of the one - capacitor system . the time constant rc 2 associated with the vertical line rc 1 can be read off in table 1 . the depicted two - capacitor system always reduces its residual voltage u2 ( residue ) to half the value of the corresponding one - capacitor system u1 ( residue ). that means however that the new system can only supply half the voltage for a bi - phase pulse . in accordance with the current school of thought this is deemed to be detrimental as the second phase is attributed with a crucial action which in our view it does not enjoy . nonetheless discharge of the residual voltage of the two - capacitor system is advantageous , preferably if that again happens in parallel . that would counteract in particular “ over - stimulation in the proximity of the cardiac electrode ” ( reference 4 ). how the delivered energy nde1 of the one - capacitor system increases as a reference value with an increasing time constant ( lower curve ), how the stored energy nse1 of the one - capacitor system increases over - proportionally with the time constant ( upper curve ), how the stored energy of the two - capacitor system nse2 ( curve in the middle ) remains markedly below that of the one - capacitor system nse1 , particularly when large time constants are involved , and how far away we are from the theoretical minimum nde1 at rc 1 = 2 . 36 ms . while nse1 or nse2 represent the input which must be provided in relation to the theoretical minimum with a one - capacitor system or a two - capacitor system , the reciprocal η = 1 / nse1 and η 2 = 1 / nse2 corresponds to the efficiency in which both electrical and also physiological optimization is expressed and which relates to the theoretical minimum of the delivered energy nde1 with an rc 1 of 2 . 36 ms . [ 0085 ] fig2 is a representation of the discharge calculated with equation ( 12 ) at 50 % tilt for rc 1 and rc 2 . the rc 1 curve ends at t / rc = 0 . 9 ( in reality at 4 . 5 ms ) at a normalized voltage of 0 . 5 , while the exponential curvature can scarcely be perceived . that is also expressed in the mean normalized voltage nmv1 which at 0 . 721 is only slightly lower than the linear mean value at 0 . 75 . “ mean value ” means that the wedge part of the discharge curve above the mean value line is equal in terms of surface area to that beneath the discharge curve . more specifically , in the total of three discharge curves with rc 1 , 2 · rc 2 and ½ · rc 2 it will be apparent , which has been theoretically worked out with formula ( 7 ), that the mean value of the voltage depends only on the tilt and not on the time constant . in all three discharges the wedge compensation effect is very beautifully demonstrated by the one line at 0 . 721 . that affords the same normalized voltage for both discharge curves and thus the same physiological effectiveness . [ 0086 ] fig3 predetermines an rc 1 discharge at 70 % ( tilt then 30 %, rc 1 = 27 . 5 ms ). the curve ends at an t / rc of 0 . 94 ( in actual fact at 9 . 8 ms ). at 0 . 625 ( 6 . 6 ms in reality ) the discharge is terminated with 2 · rc 2 and voltage doubling to the normalized value of 1 . 4 begins . after 2 . 8 ms the discharge procedure with ½ · rc 1 has then occurred again at 0 . 7 , and the line nmv3 indicates the mean value which is 0 . 165 higher than that of the rc 1 curve . as a result the discharge with rc 2 and subsequent voltage doubling is physiologically more effective with the same initial voltage ( here 1 ). the effectiveness becomes the same if the initial voltage of the rc 2 curve is reduced to 94 % in relation to the rc 1 curve . in energy terms that denotes a reduction to 88 %. in this example however the efficiency 12 at 0 . 53 ( see table 1 ) is already very low , which again is already reached by an rc 1 discharge at approximately an rc 1 of 11 . 5 ms ( corresponding to a tilt of 41 %). it is not only possible to deduce that for each time constant rc 1 there is an individual optimum tilt , but also how great the chronaxie time is , which in the calculation forms the important value for normalization of the system of equations . with knowledge of the optimum tilt and the corresponding time constant it is possible to ascertain from table a of [ 4 ], at which tilt which normalized time constant v = rc / chronaxie occurs . the chronaxie in relation to defibrillation of implanted units is to be fixed approximately at : estimates show that this value may individually alter by ± 30 %, which however has a less than 20 % effect on the results or upon optimization . if there should be a chronaxie which is markedly different from 2 ms , for example due to other electrodes or other defibrillation modes , it is nonetheless possible to use the results in table 1 , it is only necessary to multiply all time values by the factor c : the time constant rc 1 in the first column arises out of multiplication of the value v in table a from reference 4 with the chronaxie in accordance with equation ( 16 ) of 2 ms . the pulse duration t1 in the second column is obtained like rc 1 from the value x in table a and chronaxie . the tilt was created in such a way that the first two columns in table a of ref . 4 were over - written with the new values for rc 1 and t1 . nmv1 is the mean value of the voltage as a function of rc 1 and during the pulse duration t1 . a calculation formula was already afforded with equation ( 3 ). in deriving that formula the expression t1 / rc 1 which occurs upon integration was replaced by the expression in [ u ( o ): u ( residue )]. the normalized mean voltage nmv1 in accordance with equation ( 7 ) is thereby dependent only on the tilt . the normalized delivered energy nde1 ( related to the minimum at rc 1 − 2 . 36 ms ) was obtained like tilt from table a of reference 4 . the efficiency eta from that table a was electrically defined as the ratio of delivered energy ( nde ) to stored energy ( nse ). the mode of operation of the method according to the invention is to be set forth in summarizing form once again hereinafter as follows : the normalized stored energy nse1 is defined by the quotient nde1 divided by eta . rc 2 is determined in accordance with equation ( 11 a ). t ( 2 ) ( time during the discharge of rc 2 ) is calculated from the combination of equations ( 5 ) and ( 8 ): t ( 3 ) ( time during the discharge of the series circuit to half the voltage value ) is determined in analogous fashion : nmv ( 2 ) is the mean voltage during the time t ( 2 ) corresponding to equation ( 7 ). nmv ( 3 ) is the mean voltage during t ( 3 ) which with the equations ( 5 ) and ( 7 ) having regard to discharge to half the value is calculated as follows : mv1 : mv2 is the quotient which characterizes the increase ( or reduction ) in voltage on the basis of the parallel - series circuit configuration . 2c 2 : c 1 indicates the reduction in the stored energy in the case of the two - capacitor system in comparison with the one - capacitor system . the reciprocal value of nse2 represents the efficiency η 2 which is related to the energy minimum nde1 at rc 1 = 2 . 36 ms . nse2 : nse1 is identical to the ratio of the efficiencies η 1 : η 2 and demonstrates the superiority of the two - capacitor system in particular in relation to a high rc 1 . ( in the same manner , as indicated previously , it is also possible to calculate systems with more than two capacitors ). accordingly the combination of theoretically well - founded pulse duration or tilt with the principle of voltage doubling by means of two capacitors affords a technical advance which can be used in various ways . measurement of the time constant during parallel or sequential discharge can thus be advantageously used to ascertain the corresponding tilt and to cause the pulse to cease when it is reached . that applies both in regard to the individual capacitors and also in regard to the serial connection thereof . it is thus best possible to do justice to any situation with an unknown defibrillation impedance . all calculations were based on the assumption that the chronaxie in the defibrillation procedure is 2 ms . if that value should be found to be incorrect , for example fluctuating by up to 30 %, the method of the invention would not be rendered ineffective as a result as as a consequence the tilt changes by less than 16 %. that affords the advantageous development of making the tilt which is so important in terms of the effectiveness of the method variable by up to 20 % by programming . the curve nse2 in fig1 demonstrates the input which is to be achieved with the two - capacitor system and which cannot be surpassed by any system known at the present day . the reciprocal of that value ( nse2 − 1 ) defines the efficiency η 2 which gives the defibrillator its name . this therefore means not one defibrillator but a family which is dimensioned in accordance with the equations ( 11 ) for the two - capacitor system and which is optimized in the inverse relationship to the equation ( 22 ): c 1 / 2c 2 = ratio of the capacitances of the one — and two - capacitor systems respectively , all values are set out in table 1 as a function of the time constant rc 1 for the range between 1 . 0 ms and 100 ms . for the comer points of a realistic range of between 2 . 5 ms and 20 ms the eta values read as follows : η 2 ( 2 . 5 ms )= 0 . 969 ( 3 % more energy necessary in comparison with the reference value nde1 ( 2 . 36 ms )), and η 2 ( 20 ms )= 0 . 60 , thus η 2 is higher by the factor of 1 . 56 than the reduction in input as shown in fig1 by virtue of two capacitors or the increase in efficiency ( as a reciprocal value of input ) η 2 is to be attributed exclusively to optimization of the pulse which in the case of a “ bi - phase ” pulse would correspond to the first phase . there is nothing against also discharging the residual voltage of the two - capacitor system as a second inverted phase , in which case that should preferably take place in the form of a parallel discharge . referring to fig4 an advantageous structural embodiment of the invention in the form of an implantable cardioverter defibrillator ( icd ) is shown in the form of a block circuit diagram . for operation thereof this embodiment thus also makes use of the method according to the invention . the block circuit diagram shows the co - operation in principle of the groups shown in the following figures . a defibrillator portion 1 produces the pulses which are to be delivered to the heart in a defibrillation phase and includes the energy source required for that purpose . the defibrillator portion 1 is connected to a control portion 2 containing the groups which establish the stimulation defibrillation times and determine the configuration in respect of time of the defibrillation pulses . a cardiac pacemaker portion 3 contains the usual functions of an implantable pacemaker and implements control in respect of time of the stimulation pulses which are necessary to maintain the normal cardiac activity in the bradycardia and tachycardia range . that also includes recognition of irregularities in cardiac activity from the intracardial electrocardiogram recorded by way of the implanted electrodes . the control portion 2 also has control over the pacemaker portion 3 so that in that way the functions thereof can also be remotely programmed and controlled in time - synchronized relationship with the behavior of the heart . the groups 1 through 3 are combined in a casing 4 which is represented symbolically by a broken line . the implanted portions which are disposed in the casing 4 are remotely controllable and remotely settable by a programming portion 5 from outside the body . in addition the configuration in respect of time of the cardiac events and the stimulation and defibrillation measures which are thereupon initiated is recorded in the control portion and if necessary can be transmitted by means of the programming portion to the exterior of the body and can there be evaluated by the doctor . [ 0121 ] fig5 shows in detail the functional components of the defibrillator portion 1 . in this case an energy source 11 which is in the form of a conventional battery serves as a power supply for this group . connected on the output side of the energy source 11 is a voltage transformer 12 which boosts the output voltage of the battery to a settable supply voltage u for charging up the subsequent capacitors c 1 and c 2 . the internal resistance of the voltage transformer 12 is such that charging - up of the capacitors c 1 and c 2 takes place in a suitably short period of time , after which in the situation requiring defibrillation it was activated by way of a suitable control line from the control portion 2 . the capacitors c 1 and c 2 can be connected by way of various switching elements s 11 through s 34 in various ways to the voltage transformer 12 on the one hand and the cardiac electrode 13 on the other hand , as is described in greater detail hereinafter . in this respect , activation of one or more of the switching elements s 11 through s 34 means that the switching element in question in switched into the conducting condition for a predetermined period of time . for the charging operation , the capacitors c 1 and c 2 are connected directly to the output of the voltage transformer 12 by activation of the switching elements s 11 and s 22 , so that the capacitors are charged up to their set initial voltage . in that case the charging operation is effected in a suitably short period of time according to the internal resistance of the voltage transformer . discharge of the energy stored in the capacitors c 1 and c 2 to the electrode 13 which is connected to the heart is effected either sequentially in respect of time by successive activation of the switching elements s 12 for c 1 and s 12 and s 24 for c 2 for two successive periods of time or by simultaneous activation of the corresponding switching elements in a single period of time . in this case , connection to the heart by way of the electrodes 13 is effected by activation of the switching elements s 31 and s 32 each in a first polarity . a further discharge configuration is afforded by a series connection of the capacitors c 1 and c 2 by activation of the switching elements s 22 and s 23 . in this case once again the switching elements s 31 and s 33 are activated for discharge in the first polarity . to reverse the discharge configurations for a possible residual discharge in the bi - phase mode of operation , the switching elements s 32 and s 34 are activated instead of the switching elements s 31 and s 33 . reference is now made to fig6 to describe the production of the controls signals , with the control portion 2 , which cause activation of the switching elements s 11 through s 34 for predetermined periods of time . the timer blocks shown in fig6 are respectively activated by a starting pulse by an input signal which is fed to the illustrated block from the left - hand side in the drawing . they respectively remain active for a predetermined period of time which is characteristic for the block and which can possibly be altered by way of external programming means ( programming portion 1 in fig1 ) and in that respect deliver a suitable control signal to the above - mentioned switching elements s 11 through s 34 of the defibrillator portion shown in fig5 . the signal connections in question leave the respective timer block upwardly in the drawing . after the expiry of the period of time which is characteristic of the respective timer block the timer blocks in question each output a control pulse which possibly serves for activation of a subsequent timer block . the corresponding signal paths leave the respective timer block towards the right in the drawing . when defibrillation is necessary , the timer block t 1 which determines the charging times of the capacitors c 1 and c 2 by means of control signals and the switching elements s 11 and s 22 is supplied with a suitable starting signal from a time control unit 21 which holds the supremacy in terms of time control . after charging is concluded that procedure is terminated by a suitable end signal to the timer block t 1 . the time duration of the charging procedure can possibly be set from the exterior , like also the charging voltage of the voltage transformer 12 in fig5 . the output signal of the timer block t 1 is fed to three and - gates 22 through 24 , to the further input of each of which passes a respective one of three control signals of the time control unit 21 , which select which of three subsequently connected timer blocks t 21 , t 22 or t 231 is activated by the output signal of the timer block t 1 . in this respect , the choice of the respective timer block determines which of three first discharge configurations is selected for the capacitors c 1 and c 2 . these are parallel discharge ( t 21 ), individual discharge ( t 22 ) and sequential discharge ( t 231 and t 232 ). in that way it is possible by means of the time control unit by virtue of external programming to establish which of the three first discharge configurations is adopted . in the case of the parallel discharge configuration being selected , the switching elements s 12 , s 22 , s 24 , s 31 and s 33 are activated by the time control unit t 21 . in contrast , in the case of the individual capacitor discharge configuration being selected , the switching elements s 12 , s 31 and s 33 are activated by the time control unit t 22 and , in the case of selection of the sequential discharge configuration , the switching elements s 12 , s 31 and s 33 are activated firstly — as in the above - mentioned case — by the time control unit t 231 . the control signals for termination of the signal output for the various timer blocks are produced by a control unit for discharge termination as indicated at 25 . that control unit determines the end of discharge of the capacitors c 1 and c 2 to provide for optimization in accordance with the invention of the discharge energy from the time constant arising in regard to discharge and the remaining residual discharge voltage which is ascertained in dependence thereon . ascertaining the discharge voltage in that way can be effected either by using a look - up table in the manner of table 1 in such a way that , after the time constant rc 1 has been ascertained the corresponding tilt value ( or that of the corresponding residual voltage ) is outputted , or that value is calculated on the basis of the specified relationships . to ascertain the appropriate operating parameters which are also used as an input parameter for the group 26 , the arrangement has a volt meter 26 which ascertains the current voltage at the electrodes 13 . the configuration of the voltage at the beginning of the discharge is taken — derived from the corresponding starting signal as the output signal of the time control block t 1 — with the beginning of the first phase of discharge of the capacitors c 1 and c 2 respectively , by means of a suitable group , to determine the time constant of the discharge procedure , which forms the product of the respective discharge capacitance and the resistance of the electrode 13 . the discharge voltage at which discharge is terminated depends on that time constant . that is effected with what is known as a look - up table in which the residual voltages at which the discharge is to be terminated in the respective phase are recorded in dependence on the ascertained time constant . that table is shown in greater detail as table 1 . when the voltage which is ascertained for the respective discharge configuration on the basis of the ascertained time constant is reached , a signal is delivered to the time control block which controls the discharge , that signal terminating the corresponding discharge time and possibly starting the next discharge phase by the appropriate control signal which indicates termination of the period of time in question . that is effected by activation of the subsequent time control block . in the case of sequential discharge , after discharge of the first capacitor c 1 to the ascertained discharge voltage , the second capacitor is discharged ( to the same discharge voltage ). for that purpose , the block t 232 is activated by the output signal of the block t 231 and activates the switching elements s 22 , s 24 , s 31 and s 33 . termination of that discharge phase again occurs when the predetermined discharge voltage is reached . in a corresponding fashion , a timer pulse starting a subsequent time control block is also supplied by the block t 232 . that is effected by the discharge voltage associated with the respectively ascertained time constant being ascertained from the control unit for the end of discharge as indicated at 25 , and being fed to the voltage comparator 28 through 30 associated with the respective discharge phase ( active time control block ). as soon as the current discharge voltage which is ascertained by the volt meter 26 reaches or falls below the value held in the respective voltage comparator , it delivers the control signal for terminating discharge in the respective phase . the output pulses of the time control blocks t 21 , t 22 and t 232 are combined together by way of an or - gate 31 . the output signal of that or - gate 31 serves for actuation of the subsequent time control blocks . in the normal case this is the time control block t 3 which triggers serial discharge of the two capacitors c 1 and c 2 by activation of the switching blocks s 22 , s 23 , s 31 and s 33 . that serial discharge can possibly also be omitted under certain circumstances . this is also established by the time constants determined with the group 27 . a selection block 32 determines the further discharge sequence by means of two and - gates 32 and 33 . in dependence on the output signal of the selection block which in turn is actuated by the control unit 25 for terminating discharge , the output signal of the or - gate 31 is passed either by way of the and - gate 33 to the time control block t 3 or by way of the and - gate 34 and a further or - gate 35 to the time control block t 4 . in the case of activation of the time control block t 3 the above - described serial discharge takes place while in the other situation parallel bi - phase residual discharge similarly takes by way of the time control block t 4 . in this respect the residual charge of the capacitors c 1 and c 2 is discharged after attainment of the respective end of the discharge procedure , at the threshold voltages in question , with a bi - phase voltage reversal . in this respect , the arrangement ascertains by way of the voltage comparator 30 when the output voltage at the electrodes has reached a residual voltage . that residual voltage is fixedly stored in the voltage comparator . in the other situation , more specifically when series discharge is skipped , activation of the time control block t 4 for activating bi - phase discharge is effected by way of the and - gate 34 on the basis of the corresponding output signal of the selection circuit 32 immediately after activation of one of the time control blocks t 21 , t 22 or t 232 . instead of the normalized residual voltage or the tilt , “ shut - down ” of the respective capacitor combination at the intended residual voltage can also be effected by means of a suitable time presetting which is respectively established starting from the initial voltage , on the basis of the ascertained time constant . the time control blocks shown in fig3 are then not each reset by an external control signal which marks the end of the respective period of time , but receive the remaining residual time ascertained as set forth hereinbefore , transmitted from the unit 25 . then , after expiry of the residual time , this being controlled by suitable timer means , delivery of the signal identifying the end of the respective period of time takes place for evaluation of the further control procedures towards the right in the drawing , as was described hereinbefore . the invention is not limited to the illustrated embodiments and in particular it is not bound to a configuration in just hardware or just software terms as the primary consideration is the described functionality , more specifically the described behavior of the system as a reaction to the input conditions set forth . in this respect the structure of timing members used can also serve as a starting point for the design of a suitable flowchart as a basis for control software , in which respect the procedures which are reproduced in parallelized mode only have to be edited in the manner of a flowchart with the corresponding logical links for serial processing . it therefore also immaterial whether the system is used as an implantable or external system or also as part of a larger overall system . thus the described functionality can also serve for example as an operating procedure for a system of higher order , and in particular in regard to ascertaining the respective operating parameters it is possible to make use with the same degree of success both of the respectively specified calculation methods and also look - up tables in which the stored values are each looked up and read off . | 0 |
a process for producing aromatic hydrocarbons from a reaction gas containing methane according to selected embodiments of the present invention is illustrated in fig1 . as shown , the reaction gas is fed to a reactor 10 , in which the reaction gas may be heated under non - oxidative conditions to produce aromatic hydrocarbons and other products such as hydrogen . the reaction gas may be a natural gas . typical natural gases may include , e . g . 75 to 99 mol % of methane ( ch 4 ), 0 . 01 to 15 mol % of ethane ( c 2 h 6 ), 0 . 01 to 10 mol % of propane ( c 3 h 8 ), up to 0 . 30 mol % of carbon dioxide ( co 2 ), and other minor components . the reaction gas may also be any other synthesized or naturally existing gases or mixtures of gases that contain low carbon alkanes , or other low carbon aliphatic hydrocarbons , such as c 1 - c 4 hydrocarbons . the actual reactions occurring in reactor 10 may be complicated and may vary in different embodiments depending on various factors as can be understood by those skilled in the art . in many instances , the complete reaction mechanisms may not be completely understood . however , the overall reactions may include a reaction result that can be described as : in selected embodiments , ethane is also expected to be present in reactor 10 . ethane may be included in the input gases such as the reaction gas , or may be formed in reactor 10 . as such , the overall performance of the aromatization process can be enhanced by including in reactor 10 a combination of catalysts where a first catalyst is more active for catalyzing aromatization of methane and a second catalyst is more active for catalyzing aromatization of ethane . a catalyst is more active if it provides a higher yield of the desired product , or if it has a longer lifetime as an active catalyst for the desired reaction without re - activation , or both . the catalysts may be placed in a catalyst bed 12 as illustrated in fig2 ( not separately shown in fig1 ). as depicted in fig2 , catalyst bed 12 is in a conduit 14 in reactor 10 , in which the reaction gas passes through and the aromatization reactions take place . the space in conduit 14 where the reaction gas contacts the catalysts and reacts is referred to as the reaction zone . in selected embodiments , conduit 14 may be arranged vertically and the reaction gas may be flown downward as depicted in fig2 . other arrangements are also possible . at least two different types of catalysts are placed in catalyst bed 12 . as depicted in fig2 , a first catalyst 16 is placed upstream ( on top as depicted in fig2 ) in catalyst bed 12 , and a second catalyst 18 is placed downstream ( at the bottom as depicted in fig2 ) in catalyst bed 12 . in selected embodiments , catalyst 16 is a mo / mcm - 22 catalyst , and catalyst 18 is a mo / zsm - 5 catalyst . mcm - 22 and zsm - 5 are each well - known aluminosilicate zeolites , and those of ordinary skill in the art will be aware of such compounds , their physical structures , and techniques for producing such structures . other possible catalysts that can be used , their selection and preparation will be described further below . in different embodiments , the catalysts may also be arranged differently as discussed elsewhere herein . reactor 10 , catalyst bed 12 and conduit 14 may be designed and constructed according to any suitable conventional techniques with the exception of the catalysts in catalyst bed 12 and with any possible or necessary modification in view of , or to accommodate , the combination of catalysts described herein . for example , reactor 10 may be a continuous flow reactor , and catalyst bed 12 may a fixed catalyst bed . the sizes and shapes of reactor 10 , catalyst bed 12 and conduit 14 may be selected by those skilled in the art according to known techniques for designing gas phase reactors . the different components in the reactor may also be constructed using suitable materials known to those skilled in the art with the additional requirement that they be compatible with the combination of catalysts described herein some optional and necessary components of reactor 10 , and optional or necessary equipments and devices for operating reactor 10 , are not depicted in the figures , but these can be readily understood and provided by those skilled in the art in view of the present disclosure . during operation , the reaction gas is passed through catalyst bed 12 in conduit 14 at selected temperature , pressure and flow rate . the temperature , pressure , flow rate , and other operating conditions in conduit 14 , are selected and controlled to provide non - oxidative dehydroaromatization conditions . as will be understood by those skilled in the art , to avoid oxidative reactions , the reactants used for the production process should be non - oxidative , and the reaction gas should not contain or contact oxidative substances such as oxidative gases . in selected embodiments , the reaction temperature in the reaction zone may be about 650 ° c . and the pressure in conduit 14 may be about 0 . 1 mpa or about 1 atm . in some embodiments , the reaction temperature may be selected from the range of about 500 to about 900 ° c ., such as from about 600 to about 700 ° c . ; and the reaction pressure may be selected from the range of 0 . 1 to about 1 mpa , such as from about 0 . 1 to about 0 . 5 mpa . in selected embodiments , the space velocity of the reaction gas in conduit 14 may be about 10 h − 1 . in some embodiments , the space velocity of the reaction gas may be in the range of about 5 to about 15 h − 1 , such as from about 7 to about 12 h − 1 . the space velocity , reaction temperature , and reaction pressure can affect the reaction results and process performance , and thus may be selected to optimize certain aspects of the reaction process for a given application . as a result of the reactions that occur in reactor 10 , aromatic hydrocarbons and other products such as hydrogen gas are produced . possible aromatic hydrocarbons produced in reactor 10 include benzene , toluene , xylene , naphthalene , ethylbenzene , styrene , or mixtures thereof . in particular , the reaction conditions may be optimized to produce one or more of benzene , toluene , and xylene in selected embodiments . conveniently , when a combination of different catalysts as described herein is provided and present in reactor 10 , improved processing performance may be obtained , as compared to a process using only one of the catalysts . for example , it has been found that mo / zsm - 5 is very efficient for catalyzing ethane aromatization reaction . tests show that when only mo / zsm - 5 was used , 100 % ethane conversion could be obtained for a long time with stable benzene yield . however , the benzene yield decreased quickly when the catalyst was becoming deactivated . by comparison , mo / mcm - 22 has been found to be more efficient for methane aromatization reaction . when only mo / mcm - 22 was used , the benzene yield could be maintained at a relatively high level for a certain period of time , but this catalyst exhibited low activity for ethane aromatization reaction . tests have shown that when the combination of a mo / zsm - 5 catalyst and a mo / mcm - 22 catalyst was used for natural gas aromatization reaction , the conversion performance from both ethane and methane to benzene , toluene and xylene products could be improved or maximized , as compared to using any one of these catalysts . without being limited to any specific theory , it is believed that mo / mcm - 22 can efficiently convert methane to aromatics . during this conversion , some ethane may be produced . the produced or unreacted ( if present in the input reaction gas ) ethane can be efficiently converted to aromatics when it is in contact with mo / zsm - 5 . as a result , the overall performance of the process can be enhanced . test results indicated that both benzene yield and catalytic stability could be increased when both mo / zsm - 5 and mo / mcm - 22 were used . with an embodiment of the present invention , the benzene yield can be expected to increase by 30 % over a 150 h processing period , as compared to a conventional process for non - oxidative dehydroaromatization of methane using one type of catalyst . as can be understood , similar results or improvement could be expected if mo / mcm - 22 is replaced with another catalyst that is more efficient or active for catalyzing methane aromatization , and mo / zsm - 5 is replaced with another catalyst that is more efficient or active for catalyzing ethane aromatization . for example , other catalysts that have a zeolite structure with pore channel sizes similar to those of mcm - 22 or zsm - 5 may be suitable catalysts in selected embodiments . suitable catalysts may have different pore structures that are similar to those of mcm - 22 or zsm - 5 respectively . different pore structures may be selected based on their effects on catalytic activity . in some embodiments , the catalysts may have mo - loading of about 1 % to about 15 %, and si / 2a1 ratio of 25 to 45 . in view of the discussion above , the catalysts in catalyst bed 12 may be arranged to optimize the performance , such as by arranging the catalysts in a way that the reaction gas first comes into contact with catalyst 16 and then comes into contact with catalyst 18 . however , in some embodiments , improved performance could still be obtained if the reaction gas , such as natural gas , first comes into contact with catalyst 18 and then comes into contact with catalyst 16 . in selected embodiments , catalysts 16 and 18 may be pre - mixed and the mixture may be placed in catalyst bed 12 , without a separation section for each catalyst . in any of the aforementioned arrangements , the weight ratio of catalyst 16 and catalyst 18 may be about 1 : 1 , or may be of another value such as from 1 : 10 to 10 : 1 . the ratio may be selected to optimize certain aspects of the reaction performance or for other considerations for a given application . to activate the catalysts and improve performance , the catalysts may be subjected to pre - treatment before passing the reaction gas through conduit 14 . for example , in some embodiments , the catalysts may be heated in the presence of propane at a temperature of at least 300 ° c ., such as from 450 ° c . to 650 ° c ., or from 475 ° c . to 525 ° c . the pre - treatment may last from about 10 to 100 minutes , such as about 20 to 40 minutes . the catalysts may be prepared and pre - treated as described in wo 2009 / 091336 to liu et al ., published jul . 23 , 2009 , the entire contents of which are incorporated herein by reference . a mo / mcm - 22 catalyst may also be prepared as described in the examples below . the catalysts may be regenerated after deactivation , such as by an oxidation process to remove coke deposits . regeneration of deactivated catalysts may be useful and can reduce costs in some commercial applications . as now can be understood , in different embodiments each of catalysts 16 and 18 may be an aluminosilicate zeolite modified by a transition metal . the zeolite for the first catalyst ( catalyst 16 ) may be based on mcm - 22 zeolite . the zeolite for the second catalyst ( catalyst 18 ) may be based on zsm - 5 zeolite . it is noted that in the literature mcm - 22 is sometimes referred to as hmcm - 22 or h - mcm - 22 , and zsm - 5 is sometimes referred to as h - zsm - 5 or hzsm - 5 . the zeolite for the first catalyst may also be another zeolite that has an mww type framework , and the zeolite for the second catalyst may be another zeolite that has an mfi type framework . for example , the catalysts , aluminosilicates , zeolites and metal modifiers described in wo 2009 / 091336 may be suitable candidates for selection . particular combinations of the different components described therein may be selected and used depending on the particular application in particular , a suitable transition metal may be molybdenum . in some embodiments , molybdenum may provide better performance than other metals . in some embodiments , tungsten or rhenium may be used . other non - limiting examples of transition metals include , but are not limited to sc , ti , v , cr , mn , fe , co , ni cu , zn , y , zr , nb , tc , ru rh , pd , ag , cd , hf , ta , w , re , os , ir , pt , au , hg , a lanthanide , or an actinide . the loading of the metal in the zeolite may be selected to optimize production performance . for example , when mo is used , its loading may be from about 1 wt % to 15 %, such as about 3 wt % to about 12 wt %. one or both of the catalysts may have a si / 2al ratio of from 10 to 100 , such as 25 to 45 . in some embodiments , this ratio may be about 30 or about 35 . the ratio may be selected to provide the desired acidity . conventional techniques for preparation of different zeolites and catalysts , and for dehydroaromatization of methane and other alkanes , may be modified or adapted by those skilled in the art in view of the present disclosure for use in some embodiments of the present disclosure . some of such techniques are disclosed in the references listed in the background section , and in the following references : u . s . pat . no . 4 , 139 , 600 to rollman et al ., published feb . 13 , 1979 ; u . s . pat . no . 4 , 954 , 325 to rubin et al . ; u . s . pat . no . 6 , 239 , 057 to ichikawa et al ., issued may 29 , 2001 ; u . s . pat . no . 6 , 552 , 243 to allison et al ., issued apr . 22 , 2003 ; and us 2011 / 0038789 to lai et al ., published feb . 17 , 2011 , the entire contents of each of which are incorporated herein by reference . it should be understood that the specific embodiments described herein are for illustration purposes . various modifications to these embodiments are possible and may be apparent to those skilled in the art . some embodiments of the invention are further illustrated with the following non - limiting examples . for the following examples , mo / zsm - 5 and mo / mcm - 22 were prepared by impregnating zsm - 5 and mcm - 22 zeolites respectively , according to conventional impregnation techniques . zsm - 5 was obtained commercially from zeolyst , with si / 2al ratio of about 30 . mcm - 22 with si / 2al ratio of about 35 was prepared as follows . sodium hydroxide ( 0 . 18 g ), sodium aluminate anhydrous ( 0 . 20 g ), and distilled water ( 27 . 60 g ) were mixed in a mixture until dissolution . hexamethyleneimine ( hmi , 1 . 73 g ) was added to the mixture and the resulting mixture was stirred for about 10 min . ludox hs - 40 colloidal silica ( 5 . 25 g ) and mcm - 22 seed ( 0 . 04 g ) were added and the final mixture ( 35 ml ) was stirred for 4 h at room temperature . gel was formed from the mixture and was moved to an autoclave , and was heated in a parr - reactor ( oven ) at 150 ° c . ( 30 rpm ) for 14 days . the product was filtered and dispersed in water until the ph of the filtrate was no greater than 9 . the catalysts were pre - treated ( activated ) according to the processes described in wo 2009 / 091336 to liu et al ., the entire contents of which are incorporated herein by reference . in the natural gas used , the main component was methane . the natural gas also contained small amounts of c 2 , c 3 , and c 4 hydrocarbons and co 2 , and trace amount of c 5 and c 6 hydrocarbons . natural gas was used as the reaction gas and was passed through a catalyst bed as illustrated in fig2 . mo / zsm - 5 was placed at the bottom of the catalyst bed ( i . e . downstream in the gas flow path ) and an equal amount of mo / mcm - 22 was placed on top of mo / zsm - 5 in the catalyst bed ( i . e . upstream in the gas flow path ). the reaction conditions were maintained at a temperature of about 650 ° c ., a pressure of about 0 . 1 mpa , and a flow rate of the natural gas of about 7 . 5 ml / min . no oxidative gases were included in the reaction gases to provide non - oxidative conditions . representative production results are shown in fig3 ( marked as “ example i ”). in this example , the reaction gas , catalysts used and reaction conditions were the same as in example i , except that in the catalyst bed , mo / zsm - 5 was placed on top ( upstream ) and mo / mcm - 22 was placed at the bottom ( downstream ). representative production results are shown in fig3 ( marked as “ example ii ”). in this example , the reaction gas , catalysts used and reaction conditions were the same as in example i , except that in the catalyst bed , mo / zsm - 5 and mo / mcm - 22 were mixed with one another . thus , the reaction gas came into contact with the two catalysts at about the same location in the flow path . representative production results are shown in fig3 ( marked as “ example iii ”). in this example , the reaction gas and reaction conditions were the same as in example i . however , only mo / zsm - 5 was placed in the catalyst bed and used as the catalyst . representative production results are shown in fig3 ( marked as “ example iv ”). in this example , the reaction gas and reaction conditions were the same as in example i . however , only mo / mcm - 22 was placed in the catalyst bed and used as the catalyst . representative production results are shown in fig3 ( marked as “ example v ”). as can be seen from fig3 , the benzene yield and catalyst life were both higher when a combination of mo / mcm - 22 and mo / zsm - 5 was used as the catalysts . example i ( mo / mcm - 22 upstream and mo / zsm - 5 downstream ) provided the highest benzene yield and catalytic life ( see data points represented by triangles in fig3 ). it was expected that at 650 ° c ., mo / mcm - 22 initially efficiently converted methane in the natural gas to benzene and ethane ; and the produced ethane and the unconverted ethane in the natural gas are then efficiently converted to benzene by the mo / zsm - 5 catalyst downstream . while performance was also improved in examples ii and iii as compared to examples iv and v , the improvement was not as pronounced as in example i . it will be understood that any range of values herein is intended to specifically include any intermediate value or sub - range within the given range , and all such intermediate values and sub - ranges are individually and specifically disclosed . it will also be understood that the word “ a ” or “ an ” is intended to mean “ one or more ” or “ at least one ”, and any singular form is intended to include plurals herein . it will be further understood that the term “ comprise ”, including any variation thereof , is intended to be open - ended and means “ include , but not limited to ,” unless otherwise specifically indicated to the contrary . when a list of items is given herein with an “ or ” before the last item , any one of the listed items or any suitable combination of two or more of the listed items may be selected and used . of course , the above described embodiments are intended to be illustrative only and in no way limiting . the described embodiments are susceptible to many modifications of form , arrangement of parts , details and order of operation . the invention , rather , is intended to encompass all such modification within its scope , as defined by the claims . | 8 |
any omega - aminonitrile may be used as a monomer for this invention . preferred are the omega - aminonitriles shown in u . s . pat . no . 4 , 568 , 736 i . e . those having the formula : where r is a divalent organic racial and r &# 39 ; is hydrogen or a univalent organic radical . preferred compounds are those where both r and r &# 39 ; are linear aliphatic radicals , and the compound has 6 to 12 carbon atoms . representative examples include , 6 - aminocapronitrile , 4 - aminomethylbenzonitrile , 12 - aminododecanenitrile , etc . suitable diamines include aliphatic diamines having 3 to 12 carbon atoms . hexamethylene diamine is preferred . suitable diacids include aliphatic and aromatic diacids . the aliphatic and the aromatic acids may contain 6 to 12 carbon atoms . adipic acid and terephthalic acids are preferred . the omega - aminonitrile is hydrolyzed during the process , but if the amount of omega - aminonitrile exceeds the amount necessary to make a copolyamide having more than 40 % by weight derived from the omega - aminonitrile , then there will be so many unhydrolyzed groups in the product that the molecular weight of the product is unsatisfactory , that is , the polymer will have a number average molecular weight of less than 9000 . in the reaction mixture , the diamine and the diacid should be present in approximately equal molar amounts in order to make a product with a satisfactory molecular weight . water should be present in the aqueous solution in the amount of at least 25 weight percent , but not more than about 50 weight percent . a . temperature . the final polymerization temperature is normally chosen based on the melting point of the polyamide . the final temperature is usually at least 10 ° c . higher than the melting point . temperatures above about 310 ° c . will lead to polymer degradation . to achieve a reasonable rate of increase in molecular weight , the final temperature is usually at least 260 to 270 ° c . at lower temperatures the rate of reaction is reduced so longer reaction times are required to make high molecular weight polymer . b . pressure . copolymers have been made with pressures between about 13 and 25 atmospheres , preferably in the range 15 - 21 atmospheres . at higher pressure poorer polymer color and molecular weight are observed . at lower pressures more unreacted aminonitrile is lost by vaporization from the reaction . 1 . a 300 cc stainless steel autoclave was charged with 100 grams of 51 . 5 % aqueous nylon 66 salt solution ( an equal molar mixture of adipic acid and hexamethylene diamine ) and 11 grams of 6 - aminocapronitrile . 2 . a regulator controlling the pressure in the system was set for 250 psig ; i . e . pressure will build up in the system to 250 psig and then vapor will be released through this regulator to control the pressure at this setting . 3 . the autoclave was closed and purged several times with 20 psig of nitrogen to purge air from the system . 4 . the contents of the autoclave were agitated and heated in 60 minutes to 250 ° c . heat was supplied by an electric band heater surrounding the autoclave . the temperature was controlled . 5 . after reaching 250 ° c ., the pressure in the system was reduced from 250 psig to atmospheric pressure over one hour by adjusting the pressure regulator . during the pressure reduction the temperature was increased to 275 ° c . 6 . the reaction continued while heating at 275 ° c . and one atmosphere pressure for 45 minutes . 7 . the heat and the agitation on the autoclave were turned off . the contents of the autoclave were cooled under an atmosphere of steam . 8 . after cooling , the polymer was removed in a block from the autoclave and crushed . the polymer was dried at 90 ° c . under vacuum . the relative viscosity ( rv ) of an 8 . 4 wt % polymer solution in 90 . 0 % formic acid was found to be 34 . inherent viscosities ( ivs ) were measured in sulfuric acid for the polymers that were insoluble in formic acid . ______________________________________copolymerization of 6 - aminocapronitrile % nylon 6 in molecularexample # salt final polymer rv weight * ______________________________________1 nylon 6t ** 40 % 1 . 0 *** 17 , 0002 nylon 66 10 % 44 15 , 6003 nylon 66 20 % 34 -- 4 nylon 66 25 % 29 -- 5 nylon 66 30 % 23 -- 6 nylon 66 40 % 17 9 , 200______________________________________ *( number average molecular weight determined by gel permeation chromatography ) ** hexamethylene diamine and terephthalic acid *** inherent viscosity ______________________________________copolymerization of 12 - aminododecanenitrile % nylon 12 in molecularexample # salt final polymer rv weight______________________________________7 nylon 66 20 % 16 -- ______________________________________ | 2 |
fig1 schematically shows an exploded view of a mountable flush - mounted switch in the form of a door - opener switch as per one exemplary embodiment of the invention in front of a panel 50 on which it is intended to be mounted , and having a plug 40 for the electrical connection . the door - opener switch thus has three subassemblies , which have been given the reference signs 10 , 20 and 30 and which are described in the following text . fig2 shows an exploded view of the door - opener switch according to fig1 , with the individual elements that make up the subassemblies . fig3 , to which reference is also already made in this connection , shows finally a cross - sectional view of the door - opener switch in the assembled state , with fastening screws 21 , but without the panel 50 or the plug 40 . apart from opening doors , such a flush - mounted switch can also be used for a multiplicity of other switching functions , such as requesting light signals , elevators and other tasks , in which a large actuation surface is sensible and a visual response and high security against vandalism are desired . one of the three subassemblies mentioned comprises a central button 10 , which comprises an activation push cap 11 , which makes up and fills the entire round extent of the button 10 . in the center of the push cap 11 there is a depressed region 114 , in which a symbol insert 12 can be inserted . the push cap 11 is connected to a welding ring 13 , in particular by sonic welding via the seal 112 . a housing 14 projects downwardly out of the subassembly , and so the button 10 has a protruding flange region 15 . the flange region 15 protrudes over the cover 14 , as seen from the direction of use of the door - opener switch . its structure can be seen from fig3 and fig5 . the flange 15 is provided to be positioned on the fastening ring 20 , and has for this purpose a complementary configuration on its underside , said fastening ring 20 previously being fastened to , for example , a panel 50 during mounting of the door - opener switch . the panel 50 , which may be part of a door and is then usually aligned vertically , has a housing receptacle 51 , which may be a simple through - hole or blind hole , for receiving the cover 14 with a substantially precise fit , and a number of screw holes 52 . three screw holes 52 are provided here , corresponding to three screw openings 23 in the fastening ring 20 . the three countersunk screw openings 23 are provided at an angular spacing of 120 degrees to one another in orientation flanges 22 on the fastening ring . in principle , it would also be possible to make the material of the fastening ring 20 thicker in the radial direction , if there is only at least one orientation element which keeps the button 10 in a rotationally fixed manner with respect to the fastening ring 20 . as can be seen in connection with fig2 , there are corresponding trapezoidal fastening recesses at the locations of the fastening orientation flanges 22 , so that the button 10 can be inserted in a rotationally fixed manner on the fastening ring 20 . to this extent , it is essential that the fastening ring 20 does not , seen radially , have a uniform internal configuration . this is achieved here by the receptacles 22 of the screw openings 23 . the orientation element can also be given by a non - round cover 14 , which is insertable into a then complementary receptacle 51 in the panel in precisely one or ( for example in the case of polygons ) in various positions . instead of a screw connection , the fastening ring 20 can also be designed for a rivet connection or it can in principle be attached by welding , soldering or adhesive bonding . what is essential is the alignment of the fastening ring 20 for aligning the symbol field 12 via the fastening recesses 64 of the button 10 . the fastening ring 20 has here three bayonet shoulders 24 , which protrude outwardly on the flanges 22 and do not make up the entire height of the fastening ring 20 . in other words , under the protruding bayonet shoulders 24 there is a lower rim 26 as far as the lower edge of the fastening ring 20 . as in the case of the fastening holes 23 themselves , there can also be different shapes and numbers of these bayonet shoulders 24 ; there do not have to be three bayonet shoulders 24 and they do not have to be at the same angular spacing ; what is essential is that it is possible to lock the button 10 by way of the support ring 30 which engages over said bayonet shoulders 24 and will be described further below . instead of the bayonet shoulders , it is possible also to provide a snap connection , so that the fastening ring 20 is snapped on and latches in place with a click . in the case of another solution , the fastening ring 20 can also be fastened by way of laterally and radially extending screws . the fastening ring 20 further has an outwardly directed locking tab 25 , which can be brought into engagement with a complementary tab which cannot be seen in the support ring 30 in fig1 . by rotation of the support ring 30 in a manner corresponding to the arrows indicated on the fastening ring 20 , the inner tab provided in the support ring 30 runs onto the inclined flank or ramp 27 of the locking tab 25 until it slides into the space , located behind the latter , in the receptacle and thus locks the support ring 30 with respect to the fastening ring 20 . advantageously , a lateral service opening 35 is provided in the support ring 30 , it being possible by way of said service opening 35 to push back the fastening ring 20 , the material of which is thin in the region of the locking tab 25 and partially the ramp 27 , so that the support ring 30 can then be rotated in the opposite direction to the arrows indicated on the fastening ring 20 and can thus be released . the support ring 30 itself has a cylindrical side wall 34 , on the outer side of which said service opening 35 is provided , specifically precisely next to the tab , which projects inwardly , counterclockwise as seen from above , and which , when the switch is assembled , comes to lie next to the run - on ramp 27 and the end , the tab 25 , thereof . on its top side , the support ring 30 is provided with an inwardly directed collar 31 , which is supported on a complementary shoulder 16 of the button 10 . the inner edge of the collar 31 projects to the outer rim of the push cap 11 , in particular in the unpressed state of the push cap 11 . provided on the lower edge of the side wall 34 of the support ring 30 are in this case three inwardly projecting bayonet shoulders 32 , which can be interlocked with the complementary shoulders 24 of the fastening ring 20 ; in other words , in the mounted state of the support ring 30 in which it is locked by the tab 25 , the inwardly projecting bayonet shoulders 32 are located precisely opposite the lower rim 26 underneath the bayonet shoulders 24 . the number and shape of these elements are therefore configured in a complementary manner . the elevations 33 serve to center the support ring 30 during mounting . provided on the underside of the cover 14 itself is the plug receptacle 142 , which can be seen in fig2 and into which the plug 40 can be plugged . the snap - action lug 43 secures the plug against undesired detachment and thus serves as a protection against falling off . in order to detach the plug connection , the lug 43 is raised and the plug withdrawn . the electrical contacts are in this case cast in the plug 40 . an o - ring 41 seals the contact point with respect to penetrating moisture . the plug 40 is then connected in a conventional manner to a cable 42 . in this way , it is possible to supply the door - opener switch as the abovementioned subassemblies without a pigtail , thereby increasing service - friendliness . fig2 shows in somewhat more detail an exploded view of the button 10 , before the latter is assembled . the central element of the button 10 is the housing 60 , which has towards the inside an opening , into which the cover 14 can be placed from below . advantageously , there is provided in this interior space a loudspeaker plate 61 which forms a bracket and onto which there can be placed a foam mat 62 , to which the loudspeaker 63 is applied . the loudspeaker 63 then projects through a loudspeaker opening 73 in the circuit board 70 . the housing 60 has , in the form illustrated in fig2 , the non - planar underside , which has three trapezoidal fastening recesses 64 , which are then provided for the orientable locking of the cover on the fastening ring 20 . the circuit board 70 having a large diameter , which approaches the size of the push cap 11 , has in this case three cutouts 75 , which are provided at an irregular angular spacing , at a radial spacing which corresponds to the housing diameter , the three complementary fastening latches 65 of the cover 60 , which fix the circuit board 70 in the housing 60 , projecting through said cutouts 75 . the angular spacings could also be provided at different spacings , in particular also equally at a spacing of 120 degrees . the circuit board 70 is otherwise preferably round having three trapezoidal recesses 74 on the circumference , said recesses 74 being complementary to the recesses 64 in the housing 60 . the electric circuit is applied in a conventional manner , preferably using smd technology , to the circuit board 70 , but is not illustrated here . in order to illuminate the door - opener switch , there is provided at least one light guide 72 , which can be plugged in particular onto the circuit board 70 . in the case of the exemplary embodiment illustrated , it comprises , in two concentric portions 76 and 77 , in each case three guide portions , which cover an angular portion of 120 degrees and are separated by led receptacles , which cannot be seen in fig2 , such that three leds are provided for the outer portion 77 and three leds are provided for the inner portion 76 , said leds activating the individual visual displays . the push cap 11 is preferably a translucent injection molded part , resembling for example smoked glass , in a soft spring element 112 , which is attached by one - component or two - component injection molding and after mounting is connected in a fixed manner via the welding ring 13 to the housing 60 . the one - component or two - component execution of the connected element of push cap 11 plus axial spring element 112 ensures a sealed connection . the push cap 11 has an outer raised circular ring 113 , which makes up a part of the outer actuating surface . this circular ring 113 is beveled on the inside and is adjoined by a depression 114 which has in this case three locking shoulders 115 , under which there is a free space . in this case , the elevations 131 on the circular ring 113 play a role in the orientation of the elements to be connected . provided in the center of the push cap 11 in the illustrated exemplary embodiment are four trapezoidal openings 11 , which are provided in particular for better transmission of the acoustic signal that can be generated by the loudspeaker 63 . these openings 111 are dispensed with for the variant without a loudspeaker ; however , they can also be dispensed with in a configuration with a loudspeaker or only three of them could be provided . in order to provide sealing with respect to the exterior space of the door - opener switch , a diaphragm film 121 is placed on the depression 114 and is attached to the latter for example by sonic welding or adhesive bonding . a planar symbol insert 12 having a symbol 122 , which is printed on or is present in an incorporated raised or sunken manner , is locked in the depression 114 via the locking shoulders 115 such that corresponding bayonet elements 123 are provided on the underside of the symbol insert 12 . in other words , the symbol insert 12 is placed on the depression 114 so that the bayonet shoulders 123 are arranged between the bayonet element 115 and subsequently the symbol insert 12 is rotated about the longitudinal axis of the button 10 and thus locked . provided as a receptacle 116 in the center of the depression 114 is an elevation , into which the switching mat 171 having a corresponding centered rubber element can be inserted from below . the switching mat 71 is illustrated in more detail in fig4 , which shows a view from below of the switching mat 71 of the door - opener switch . the material of the switching mat 71 is substantially flexible rubber . the switching mat 71 has a central switching mat elevation 171 , which fits precisely into the complementary opening in the push cap 11 , said opening being provided on the underside of the receptacle 116 . this switching mat elevation 171 merges at its edges into a flange which forms the basic surface area 172 of the switching mat 71 . provided to the side of this surface area 172 are two opposing lateral projections 174 , with in each case one fastening foot 175 being preferably integrally molded on each projection 174 on the side opposite the switching mat elevation 171 . these fastening feet 175 are provided to be inserted into corresponding openings on the circuit board 70 . provided on the circuit board is a central first contact and a second contact , which is arranged in a preferably circular manner around this first contact at a spacing having an isolating gap , wherein the switch is activated when the two contacts are connected . for this purpose , a central recess 176 has been provided in the switching mat 71 , said central recess 176 having a central electrically conductive metal plate 173 which forms the conductive switching surface . by way of a pressure at any point on the push cap 11 , the central switching mat elevation 171 is pressed down ; this causes the conductive switching surface 173 in the recess 176 to snap over and leads to the closing of the contact . as a result of the use according to the invention of the fastening ring 20 , it is possible to fasten the door - opener switch by means of the necessary screws 21 within the diameter of the push cap 11 and thus underneath the activation disk of the button 10 and thus under the button 10 . this makes it possible to construct a smaller switch in the case of an activation diameter of the same size or to achieve a larger activation surface in the case of a switch of the same size . on account of the arrangement of the smoked - glass push cap 11 , the activation surface thereof can be used directly also as a translucent surface . on account of the depression 114 in the push cap 11 having the insert 12 , it is possible to achieve better guidance for the user . although it is possible to activate the switch at any point on the push cap 11 , since activation takes place centrally via the switching mat 71 , the depression provides the user more simply with a haptic confirmation of his actuation . a problem with the switch according to this design is the pressure equalization , since , on account of the wide activation surface , even with a short switching path a considerable displacement of air takes place , and this air cannot escape in the now sealed switch . a housing which is known from the prior art and is closed off in a permeable manner by a foam material is possible for pressure equalization over a relatively long time , and thus in a door - opener switch for a mountain railroad train which travels through regions at various heights and is used there , but this element is not suitable for ensuring pressure equalization in the case of button activation , since in this case the equalization has to take place quickly , i . e . within a few milliseconds . therefore , according to fig5 , the pressure equalization means is integrated according to the invention in the cover 14 , since the air displaced by the movement of the push cap 11 during switching can expand and be distributed directly within the cover 14 and thus pressure equalization with respect to the outside is ensured . fig5 shows a view from below of the door - opener switch having the fastening ring 20 and the housing 14 . the support ring 30 is likewise already placed on the button 10 , and so the locking thereof is directly discernible . the tab 25 is present on a protruding bayonet shoulder 32 and can be released by pressure on the service opening 35 . the bayonet shoulders 32 on the circumference of the support ring 30 engage over the bayonet shoulders 24 of the fastening ring 20 , which are arranged in a complementary manner . during mounting on a panel 50 , the fastening screws would then project through the openings 23 into the panel . the light guide 72 consists of two rings 76 and 77 separated by a partially executed incision , the light guide 72 being interrupted in a known manner by radially provided incisions ; these provide what are known as hotspots at which the light supplied by the leds that emit to the sides can escape from the light guide 72 in the axial direction of the door - opener switch , in particular through the push cap 11 , and is clearly discernible to the user in a manner scattered by the smoked glass , regardless of the external light conditions . moreover , on account of the smoked - glass coloration of the push cap , the lighting contrast is increased , thereby improving the discernibility of the lighting in sunshine . in fig3 , the two inner 76 and outer 77 light guides can be seen , the location of an led being provided with the reference sign 78 . the pin strip 141 produces the electrical connection between the cover 14 and the circuit board 70 . fig6 shows a perspective view from above of the cover 14 of a door - opener switch according to a further exemplary embodiment of the invention . identical features are provided in the drawings with identical reference signs . the upwardly open cover 14 has at its upper rim a circumferential connecting bead 143 , which is inserted into a complementary opening in the housing 60 and is attached for example by sonic welding . a latching connection is also possible . in fig7 , which shows a cross - sectional view through the assembled door - opener switch according to fig6 , this connection can be seen . six contact pins 144 , which are connected electrically to the circuit board 70 in a socket strip 79 fastened to the circuit board 70 , emerge from the pin strip 141 . a difference from the exemplary embodiment in fig1 resides in the pressure equalization diaphragm 145 , which is a silicone diaphragm . provided in the base 148 of the cover 14 is an inwardly directed hollow - cylindrical wall 147 , on the free end of which the circumferential clamping bead 146 of the pressure equalization diaphragm 145 is placed in a sealing manner . it is maintained that hollow - cylindrical does not imply a circular wall 147 . a hollow prism or an ellipse is also a hollow cylinder . the pressure equalization diaphragm 145 has a thin , elastic diaphragm wall , which can expand in particular between the hollow - cylindrical walls 147 of the cover 14 in the direction of a pressure equalization opening 150 which is located centrally between the walls 147 in the base 148 of the cover 14 . the function is in this case as follows . fig7 shows the rest position of the push cap 11 , in which the latter is spaced apart above the circuit board 70 so that there is a cavity 151 between the circuit board and the push cap and , of course , further air - containing spaces throughout housing 60 , which is sealed off by the cover 14 . pressure differences between the environment and this internal cavity 151 , which result when the switch is used at doors of mountain vehicles on account of the latter traveling over a period of several minutes up to an hour from a valley station to a mountain station , can be compensated by diffusion of air through the pressure equalization diaphragm 145 . it is somewhat different when the switch is actuated , said actuation taking place rapidly in fractions of a second and likewise displacing the air column . on account of the flat construction of the push cap with a large actuation surface , a certain quantity of air has to be displaced despite the short switching path . this quantity of air can now flow through openings in the circuit board 70 into the region of the pressure equalization diaphragm 145 and push out the latter downwardly in the direction of the pressure equalization opening 150 , since there is a direct connection to the environment via this opening 150 . in this case , the sealing of the switch remains ensured . the quantity of air displaced out of the no longer existing cavity 151 forms an air column in the then expanded diaphragm cavity 152 between the walls 147 of the cover 14 , held by the diaphragm wall 149 and secured by the small opening 150 , so that air can escape or flow in , but no physical damage to the diaphragm need be feared . the pressure equalization diaphragm 145 can also be called a diaphragm bellows . it may have a bellows - like wall ( not illustrated in the drawings ). particularly when no such bellows walls that slightly extend the cavity are present , an additional restoring force , which corresponds to the stretching of the diaphragm material , is also generated when a user releases the pressure on the push cap 11 again . fig7 shows yet further changes to the region of the push cap 11 in the exemplary embodiment with respect to fig1 . these changes can also be used on their own in an exemplary embodiment according to fig1 and the embodiment of fig1 can also be used only with a diaphragm 145 according to fig6 . instead of the circular axial spring element 112 , which is fastened to the push cap 11 preferably during the production process , and is then welded to the housing 60 by way of the welding ring 13 , it is also possible to provide a spring surface which is formed by the spring element 212 , is in the form of a circular ring in plan view , and has an inner bead 213 and an outer bead 214 . the outer bead 214 is clamped , in a similar manner to in fig1 , in a receptacle between the housing 60 and the welding ring 13 and the housing 60 and welding ring 13 are then preferably welded . the inner bead 213 is received in a receptacle in an additional ring 215 , with in this case , too , the additional welding ring 215 and the push cap 11 then preferably being welded . | 7 |
fig1 a and 1b show an example double - sided loop strap 100 having a front side 104 and a back side 102 , each of which features a field of upstanding , hook compatible loops 106 . note that the convention of “ front ” and “ back ” is used herein for discussion purposes only , and is not intended to carry any significant meaning that would affect the scope of the present disclosure . in this example , loop strap 100 is a multi - layer construction fashioned from a preform elongated strip of loop material 108 defining a pair of free longitudinal edges 110 ( see fig1 c ). edges 110 are folded over to form two inwardly facing arms 112 meeting edge - to - edge near a center area of the strip . as shown , strip 108 features a flexible base 114 bearing a field of upstanding loops 106 on one side . in particular , the loops extend from an outward surface of the base which is bounded by the free longitudinal edges . the structure and physical properties of strip 108 may vary in different implementations . for example , the strip can have a woven loop structure ( e . g ., having napped or un - napped loops ), a knitted loop structure and / or a non - woven loop structure . the materials used to manufacture strip 108 may also vary . for example , nylon , polyester , polypropylene , and / or aramid fibers can be used to manufacture the preform loop strip . though not exhaustive , the foregoing examples illustrate the numerous different types of hook compatible fabrics that can be used in conjunction with the present technique . in general , the structure and material of the strip are selected based on an intended application of the product . referring back to fig1 a and 1b , arms 112 are held in place against an inboard portion of flexible base 114 by an array of discrete bonded regions 118 . as shown , each of the bonded regions is surrounded by an unbonded area of loop material . bonded regions 118 can be formed , for example , using a heat staking process ( e . g ., ultrasonic heat staking ) to fuse the folded , overlapping layers of loop material together at various discrete points . in this particular example , a single patterned band or row of bonded regions 118 a extends along and overlaps the two longitudinal edges 110 to form a seam that holds strip 108 in a folded , two - layer configuration . an additional pattern of bonded regions 118 b extends broadly over the other portions of the folded strip 108 to secure arms 112 firmly in place against flexible base 114 . using patterned arrays of discrete bonded regions to secure the preform strip in a folded configuration can be advantageous in many different applications . in particular , this type of construction may provide more flexibility than a similar strap , for example , where adhesives or a sewn seam are used to secure the folded outboard portions of the strip in place . moreover , the present technique offers a substantial amount of air permeability so that the strap is “ breathable ” when in contact with a user &# 39 ; s skin . the outlining footprint of the bonded regions can vary between different implementations of the double - sided loop strap , so as to provide structurally different products . for example , the size of the bonded regions may differ from one application to the next . with other factors being equal , larger bonded regions will provide the strap more structural stability and bond strength than will smaller bonded regions . however , the stability and strength provided by the larger bonded regions comes at the cost of reduced flexibility , air permeability , and closure performance ( e . g ., shear , tensile , and peel strength ). in particular , the reduction in closure performance is a result of the reduced loop material available for hook engagement , as the loops are pressed down and fused in the bonded regions . similarly , the pattern density of the bonded regions can be a significant variable between different implementations . in particular , a denser pattern of bonded regions will tend to provide more dimensional stability and bond strength , while offering less flexibility , air permeability and closure performance . generally , the above - described physical properties will vary according to a ratio comparing the total area of bonded regions to the total unbonded area of the strap . that is , structural stability and bond strength will increase when the total area of the bonded regions increases relative to the total unbonded area . on the other hand , flexibility , air permeability , and closure performance will increase when the total unbonded area increases relative to the total area of the bonded regions . of course , various other properties of the loop strap may also be affected by the configuration of the bonded regions . referring again to fig1 a and 1b , bonded regions 118 b are provided in a precise geometrically regular pattern of uniform density , which provides substantially consistent and isotropic physical properties across strap 100 . in some examples , however , the pattern of bonded regions is purposefully irregular to provide different physical properties around specific areas of strap 100 , and / or to provide some directionality to these physical properties . fig2 a shows an example where bonded regions 118 b ′ are established in an irregular pattern . in particular , the pattern density of the bonded regions gradually increases from the center area of the strap in the direction of the outboard folds . in this embodiment , strap 100 ′ would be stronger and stiffer at the outboard areas and more flexible and breathable near the center . additionally , peel strength would be greater near the center of the strap than around the outboard areas , because there is more loop material available for hook engagement . fig2 b shows an example where bonded regions 118 b ″ are established in another irregular pattern , where the distance between the bonded regions is smaller in the widthwise direction of the strap than in the lengthwise direction . in this case , strap 100 ″ would be more flexible in the lengthwise direction and more rigid in the widthwise direction . as noted above , the row of bonded regions 118 a overlaps edges 110 to form a seam along the back side 102 of strap 100 . in the previous examples , bonded regions 118 a are generally circular and distributed at a constant interval along longitudinal edges 110 . fig3 shows an example where bonded regions 118 a ′″ are provided in different types of shapes , so as to form a visually distinguishable graphic . in this embodiment of strap 100 ′″, bonded regions 118 a ′″ are shaped as individual letters “ v ”, “ e ”, “ l ”, “ c ”, “ r ”, and “ 0 ”. numerous types of shapes can be used to form graphic images such as for logos , brand names , and the like . fig3 also provides an example where the bonded regions near the center area of the strap cover a greater area than the bonded regions near the outboard folds . this type of configuration would provide more bond strength and rigidity near the seam , the part of the strap offering the least structural integrity . fig4 a and 4b show another embodiment of a double - sided loop strap 200 . strap 200 is similar to strap 100 described above . for example , strap 200 is a two - layered construction presenting hook compatible loops 206 on both a front side 204 and a back side 202 of the strap . in this example , strap 200 is a composite structure fashioned from two separate preform strips of loop material 208 a and 208 b , each of which includes a flexible base 214 a , b bearing a field of upstanding loops 206 a , b extending from an outward surface bounded by free longitudinal edges 210 a , b . the strips are similar , but provide different types of loops , with loops 206 a being presenting less loft than loops 206 b . as shown , longitudinal edges 210 a of strip 208 a are folded over flexible base 214 a to meet the respective edges 210 b of strip 208 b . two similar sets of discrete bonded regions 218 a are provided to secure the respective edges 210 a and 210 b in place against an inboard portion of flexible base 214 a . as shown , each set of bonded regions 218 a provides a row of regions extending along and overlapping the respective edges 210 a and 210 b . similar to the previous examples , a pattern of bonded regions 218 b extends broadly over other portions of strips 208 a and 208 b to secure the strips in a tightly bound construction . fig5 a and 5b show yet another double - sided loop strap 300 having a front side 304 and a back side 302 , each of which presents a field of upstanding , hook compatible loops 306 facing outward therefrom . similar to the previous examples , loop strap 300 is a two - layer construction fashioned from a preform elongated strip of loop material 308 with free longitudinal edges 310 folded over to form two inwardly facing arms 312 . in particular , strip 308 includes a flexible base 314 bearing a field of upstanding loops 306 extending from an outward surface bounded by longitudinal edges 310 . in this example , a thin layer of resinous grip material 322 is deposited on an inboard portion of flexible base 314 , on the back side of the base opposite loops 306 ( see fig5 c ). longitudinal edges 310 are folded over the outer portions of the layer of grip material 322 , such that outer portions of the layer of grip material are sandwiched between the two layers of loop material , while the center portion remains exposed between edges 310 . as shown , the exposed surface of the grip material is recessed relative to the neighboring loop - bearing surface and bounded by the longitudinal edges . in various implementations , the exposed grip surface can have a lateral extent of between 10 and 90 percent of the overall width of the strap . in general , the loop strap will exhibit more gripping ability when a greater amount of the grip surface is exposed . the additional grip would come at a cost of closure performance , as less loop material is provided for engagement . various implementations and applications may necessitate different configurations of the strap with regards to the grip surface . for example , a strap designed for use on luggage may require nearly the entire surface to be grip material , and does not require breathability for comfort to the user . a strap utilized to secure a knee brace may need very little grip material in order to provide adequate security to the user , and will allow for more air movement through the strap , to enhance the user &# 39 ; s comfort . in this embodiment , the folded longitudinal edges can be secured in place using an appropriate adhesive , sewing or by heat staking , as discussed above . in some examples , the grip material itself serves as an adhesive , such that the folded edges are held in place against the base solely by adhesion from the grip material . grip material 322 can have any appropriate composition so as to provide a substantially non - slip surface . by “ non - slip ” surface , we refer to any surface designed to inhibit or prevent a smooth slipping or sliding motion by providing adequate surface friction . the grip material can provide a relatively high coefficient of friction ( e . g ., a dynamic coefficient of friction greater than about 0 . 3 ), and may be generally “ soft ” or “ skin friendly ” to the touch . for example , soft elastomers ( e . g ., styrenic block copolymers , such as styrene - isoprene - styrene , styrene isoprene / butadiene styrene , and styrene - butadiene - styrene ), rubbers ( e . g . flouroelastomers ) or silicones can be used . other suitable compositions can also be used . for example , various plastics with modified lower molecular weight constituents and thermoplastic elastomers ( e . g ., modified polypropylene or modified polyethylene ) can serve as a grip material . in some examples , the grip material is particularly well designed for skin contact , featuring a tack free , non - allergenic , and non - irritant composition . fig6 a and 6b show an additional example of loop strap 300 ′ where the layer of grip material 322 ′ provides a pattern of molded , upstanding treads 324 that provide additional surface friction for mitigating slip . in this example , the grip material includes three undulating treads extending lengthwise down the strip . of course , other appropriate configurations are also contemplated . for example , more or less treads can be provided ; the treads can extend widthwise across the strip ( as opposed to lengthwise , see fig8 ); the treads can be substantially straight ( as opposed to undulating ); and / or the height and thickness of the treads can vary . fig7 a and 7b show yet another example of loop strap 300 ″ where the deposited grip material 322 ″ includes a foaming agent ( e . g ., a heat activated foaming agent ). in these examples , the loop strap is generally constructed as described above with reference to fig5 a - 5c . after construction , the foaming agent is activated to expand the layer of grip material 322 ″, raising the exposed non - slip surface to be level with the neighboring loop material . in some examples , the non - slip surface is raised above the loop material . fig8 shows an example implementation of a double - sided loop strap 400 featuring an exposed non - slip surface having upstanding slip inhibiting treads 424 formed of an appropriate grip material 422 . in this case , the loop strap 400 is used in conjunction with a buckle 480 to form an adjustable cinch strap , such as may be used to support a medical or sports device on a user . the cinch strap is formed by threading a free - end 482 of loop strap 400 through buckle 480 , wrapping the loop strap around an object , re - threading the free - end back through the buckle , and folding the strap back on itself . in this example , free - end 482 provides a patch of loop compatible fasteners ( e . g ., hooks ) to engage the loop material on either side of the grip material 422 , thus securing the strap in place . as discussed above , the non - slip surface can be level or above the surrounding loop material . in this case , the upstanding treads 424 can be designed to engage one another when the strap is folded back on itself , impeding the ability of the strap to easily release back through the buckle , essentially creating a one - way cinch strap . if the grip connection between both elements is designed with appropriate strength for the application , the uni - directionality , coupled with the presence of the buckle , could even hold the strap in place , without the above mentioned loop compatible fasteners on the free - end of the strap . in some examples , the non - slip surface is recessed relative to the surrounding loop material . this configuration would render the loop strap more comfortable when pressed against a user &# 39 ; s skin and provide less interference with the buckle of the cinch strap . either of these above described configurations may prove useful in various applications . fig9 a and 9b show another example loop strap 500 having a front side 504 and a back side 502 , each of which presents a field of upstanding , hook compatible loops 506 . in particular , loop strap 500 is a two - layer construction fashioned from a preform elongated strip of loop material 508 including a flexible base bearing a field of loops 506 and defining free longitudinal edges 510 , which are folded over to form two inwardly facing arms 512 . each of arms 512 defines a patterned set of discrete apertures 526 that extend entirely through the flexible base . similar to the previous examples , a thin layer of grip material 522 is deposited on an inboard portion of the flexible base . however , in this case , longitudinal edges 510 are completely folded over the layer of grip material 522 to meet near a center portion of strip 508 , such that the layer of grip material is entirely sandwiched between the two layers of loop material . as shown , apertures 526 are aligned with the grip material 522 so as to leave various portions of the grip material surface exposed . the exposed surface of the grip material is recessed relative to the neighboring loop - bearing surface and bounded by the edges of the apertures . several of the foregoing examples ( shown in fig5 a - 9b ) provide double - sided loop straps that offer a substantially non - slip surface of grip material bounded by folded portions of a preform strip of loop material . the folded portions of the loop material effectively hide the edges of the deposited resinous grip material , which may be unsightly and rough because it can be difficult to produce a uniform resin edge . fig1 a shows an example apparatus 628 which is suitable for manufacturing a double - sided loop strap 600 , such as described above . apparatus 628 receives a preform strip of loop material 608 provided in the form of an elongated flexible substrate carrying a field of upstanding loops on one side . preform strip 608 is fed to a folding device 630 that folds the longitudinal edges of strip 608 inward to overlap an inboard portion of the flexible base . the folded , two - layer strip is introduced to a heat staking machine 632 that creates the prescribed patterns of bonded regions by fusing the two layers of material together at various discrete points . the resulting double - sided loop strap 600 is then spooled onto a final product roll 638 . the folding device and heat staking machine can be selected from a wide variety of conventional equipment . in the present example , heat staking machine 632 includes a patterned roller 634 having individual projections extending from its outer surface , and a horn 636 for facilitating the ultrasonic vibration with the folded strip 608 against the patterned roller . fig1 b - 10e show how apparatus 628 can be adapted for forming a non - slip surface on the double sided loop strap by depositing grip material on a back side of the preform strip of loop material prior to folding . in fig1 b , a resin applicator 640 is positioned upstream of folding device 630 . resin applicator 640 extrudes a solid layer of grip material onto the back of the loop surface prior to folding . the rollers 634 , 636 after the folding station can either be used to simply seal the folded product utilizing the grip material as the bonding agent or could be ultrasonic welders to bond the fold in place ( as described above ). in fig1 c , resin applicator 640 ′ extrudes multiple strands of grip material onto the back of the loop surface prior to folding . in fig1 d , a resin applicator 640 ″ is designed to extrude dots of grip material onto the back of the loop surface prior to folding . in fig1 e , a roll of film based grip material 642 is placed on the back of the loop surface prior to folding . in this example , the film of grip material includes an array of openings to improve breathability of the double - sided loop strap . the grip material , however , can also be a solid film or a film that includes micro perforations . while a number of examples have been described for illustration purposes , the foregoing description is not intended to limit the scope of the invention , which is defined by the scope of the appended claims . there are and will be other examples and modifications within the scope of the following claims . for example , modifications could include punching holes in the loop strip to further improve flexibility and breathability of the double - sided loop strap . | 0 |
in one aspect of the present invention , there is provided a thermal curable dielectric material to produce a prepreg in a successive process in the following examples 4 - 1 to 4 - 7 . the process uses the dielectric material as a coating on a substrate which may be a fiberglass cloth . the apparatus for producing the prepreg includes a pasting tank wherein there are provided a plurality of rolls . the pasting tank is filled with the dielectric material . a roll of fiberglass cloth may enter the pasting tank and pass the plurality of rolls . the fiberglass cloth is sufficiently impregnated with the dielectric material , and then surplus dielectric material is removed by a metering roller . a heat treatment for curing the dielectric material and removing the solvent is required at 100 ° c . to 350 ° c . for 1 minute to 5 hours , preferably at 150 ° c . to 300 ° c . for 1 minute to 3 hours . the prepreg is obtained after the cured dielectric material is cooled down and the fiberglass cloth is wrapped . a double - sided copper - clad laminate is produced by providing several prepregs in a neat stack between two electrodeposited copper foils , conducting a hot pressing process under 40 to 900 psi , raising temperature from 80 ° c . to 200 ° c . in 30 minutes , and then hot pressing at 200 ° c . for 120 minutes , and then cooling down to room temperature in 30 minutes in a vacuum pressing machine . the prepreg includes a fiberglass cloth of electrical grade 2116 and the dielectric material . generally , a double - sided copper - clad laminate with a thickness of 1 . 0 mm is produced by providing 4 sheets of prepregs in a neat stack between two electrodeposited copper foils , with a thickness of 1 . 5 mm is produced by providing 7 sheets of prepregs , and with a thickness of 2 . 0 mm is produced by providing 10 sheets of prepregs . the dielectric material of the present invention may form a stable homogeneous solution in a solvent with a low boiling point . the properties of a copper - clad laminate with the dielectric material of the invention were determined including tg , heat decomposition temperature , heat decomposition time , solder heat resistance ( 288 ° c . ), thermal expansion coefficient , water absorption , thermal conductivity , dielectric constant , dielectric loss tangent and flammability according to ipc - tm - 650 test method manual . the determining results show the copper - clad laminate with the dielectric material of the invention has high tg , excellent dielectric properties such as dk and df , low water absorption , high thermal resistance and high thermal conductivity . the copper - clad laminate is suitable used as a substrate for electronic elements and ic package . tg , dk and df were compared with different ratio and amount of ppe . the tg level may be affected by the amount of ppe used . also , the amount of ppe may also have an effect on the dk and df value . when the amount of ppe is high , dk and df may be high . when the amount of ppe is low , dk and df may be low . typically , a low value for the dk and df is preferred . in addition , the thermal expansion coefficient may be raised when ppe is added , and bmi is added to balance the effect . in table 1 , part number sa9000 of ppe with chemical name of polyphenylene oxide ( ppo ) or polyphenylene ether ( ppe ) is produced by sabic co ., ltd . the coefficient of thermal expansion was measured with different species and amount of bmi resin . the more the amount of bmi resin is , the lower the coefficient of thermal expansion is . in the example , there are three kinds of comparison comprising three groups that a1 - a5 shows different amount of bmi with the same species , a6 - a8 shows the same amount of bmi with different species and a9 - a15 shows about the same total amount of bmi with more than two species . in table 2 , part numbers 2300 , 4000 , 5100 and tmh of bmi are produced by daiwakasei industry co ., ltd , in which part number 2300 has chemical name of phenyl methane maleimide , part number 4000 has chemical name of 2 , 2 ′- bis [ 4 -( 4 - maleimidophenoxy ) phenyl ] propane , part number 5100 has chemical name of 3 , 3 ′- dimethyl - 5 , 5 ′- diethyl - 4 , 4 ′- diphenylmethane bismaleimide and part number tmh has chemical name of 1 , 6 ′- bismaleimide -( 2 , 2 , 4 - trimethyl ) hexane . it can be found from group a1 - a5 that by increasing the amount of bmi resin , the thermal expansion coefficient would decrease . however , by increasing the amount of bmi resin , the water absorption would also increase . as to group a6 - a8 , different bmi resins may reduce the thermal expansion coefficient , but would also affect the water absorption . regarding group a9 - a15 , different combination of bmi resins may reduce the thermal expansion coefficient , and affect the water absorption also . in the invention , the object of addition of bmi to the dielectric material is to reduce the thermal expansion coefficient . however , the more the amount of bmi resin is , the higher the water absorption is . therefore , the polymer additives are added to reduce the water absorption . the water absorption was measured with different species and amount of polymer additives . polybutadiene ( pb ) and styrene - maleic anhydride ( sma ) were used as the polymer additives in the invention . it can be found from using the different amount of pb with the same species that by increasing the amount of pb , the water absorption would decrease . however , with the increasing amount of pb , the coefficient of thermal expansion would also increase . as to using different species of pb in combination with sma , it shows sma can reduce the water absorption and the coefficient of thermal expansion , but df may remain high . however , pb can be used to reduce df . in table 3 , part numbers ricon100 , ricon130ma8 , ricon150 and ricon257 of pb are produced by sartomer co ., ltd , in which part number ricon 100 has chemical name of butadiene styrene copolymer , part number ricon130ma8 has chemical name of butadiene adducted with maleic anhydride , part number ricon 150 has chemical name of polybutadiene resin and ricon 257 has chemical name of polybutadiene grafted with styrene and benzene in toluene solution . in table 3 , sma with s : m = 3 : 1 indicates that the ratio of styrene to maleic anhydride is 3 to 1 . generally , the ratios are about 1 : 1 ˜ 12 : 1 . the dielectric material of the invention may comprise at least one crosslinking agent with 40 - 80 parts by weight selected from the following groups consisting of triallyl cyanurate ( tac ), triallyl isocyanurate ( taic ) and 4 - tert - butylstyrene . the properties of a copper - clad laminate with the dielectric material of the invention were measured with different species of crosslinking agents . it can be found by using tac that tg and the coefficient of thermal expansion were poor , and water absorption , dk and df were of ordinary level . as to taic , all the properties of a copper - clad laminate with the dielectric material of the invention were of ordinary level . regarding 4 - tert - butylstyrene , the coefficient of thermal expansion , water absorption and df were excellent , but dk is low , if desired , the dielectric material of the invention may optionally comprise flame retardants . a halogen - containing flame retardant of decabromodiphenyl ethane with 7 - 15 phr based on the total weight of ppe , bmi , polymer additives and crosslinking agents may be added to the dielectric material of the invention . the dielectric material of the invention may comprise at least one flame retardant without halogen with 12 - 14 phr based on the total weight of ppe , bmi , polymer additives and crosslinking agents selected from the following groups consisting of phosphor - containing flame retardants and phosphates . the phosphor - containing flame retardants and phosphates are produced by albemarle co ., ltd . the phosphates are like tetrakis ( 2 , 6 - dimethylphenyl ) 1 , 3 - phenylene bisphosphate . the dielectric material of the invention may optionally comprise fillers . the suitable fillers such as fused silica and sphere - shaped silica may be used . the suitable amount of filler is 8 - 50 phr based on the total weight of ppe , bmi , polymer additives and crosslinking agents . it can be found from the fused silica and the sphere - shaped silica with the same amount that the sphere - shaped silica has lower dk and df than the fused silica . the dielectric material of the invention may optionally comprise catalysts including peroxides having 116 ° c .- 128 ° c . for a half life of 10 hours . the suitable amount of peroxide is 2 - 8 phr based on the total weight of ppe , bmi , polymer additives and crosslinking agents . the preferable catalyst is a peroxide having 119 ° c . for a half life of 10 hours . the dielectric material of the invention may comprise ppe , but not comprise epoxy resin . the desired values of dk and / or df cannot be obtained , if epoxy resin is added to the dielectric material of the invention . when reacting epoxy resin with the dielectric material of the invention , the open rings of the epoxy resin may produce excess oh groups , therefore causing the dk and df value to remain high and unable to decrease . | 7 |
a chemical copper plating solution having the following composition as given below under ( a ) was placed in a plating tank 1 as shown in fig1 and subjected to chemical copper plating under the following plating conditions as given below under ( b ). the plating solution was circulated and stirred by a circulation pump 2 and a mixer 3 . the plating solution was sampled for analysis by a sampling pump 4 through a cooler 5 and a three - way electromagnetic valve 6 , and led to a ph detection cell 7 for the plating solution , the cell comprising a main electrode chamber 7 &# 39 ; and a reference electrode chamber 7 &# 34 ;, and a difference in potential was detected between a copper oxide electrode 8 , prepared by etching naked copper wire ( purity 99 . 9 %) with a diameter of 1 mm in 0 . 1 n nitric acid at a liquid temperature of 50 ° c . for 10 seconds and then oxidizing the etched copper wire in an aqueous 0 . 1 n caustic soda solution at a liquid temperature of 50 ° c . for 30 minutes and a silver - silver chloride electrode 9 as a reference electrode by means of a controller 10 . numeral 11 is a membrane . ______________________________________cuso . sub . 4 . 5h . sub . 2 o 13 gedta - 2na 40 gnaoh 12 g ( ph 12 . 3 ) 37 % formalin 3 mlk . sub . 2 s 0 . 0001 gpolyethyleneglycolstearylamine 0 . 1 gwater to make total volume 1 l______________________________________ ______________________________________plating temperature : 70 ° c . plating load : 500 cm . sup . 2 copper plateplating solution volume : 5 lplating rate : 3 . 0 μm / hr______________________________________ when the detected potential was smaller than the potential preset in the controller 10 as an absolute value , a signal was transmitted from the controller 10 to a makeup pump 12 to supply a makeup solution as given above under ( e ) to the plating tank 1 from a makeup solution tank 13 for adjusting ph of the plating solution , through a valve 14 , and the mixer 3 until the detected potential exceeded the preset potential . the sampled solution leaving the ph detection cell was thrown away . on the other hand , an aqueous saturated kcl solution was continuously supplied to the reference electrode chamber 7 &# 34 ; from a standard tank 15 as a standard solution for the reference electrode by the sampling pump 4 , as given above under ( c ) to obtain a stable potential from the silver - silver chloride electrode in the reference electrode chamber 7 &# 34 ;. the aqueous saturated kcl solution leaving the reference electrode chamber 7 &# 34 ; was also thrown away . furthermore , an aqueous 7 n nitric acid solution was supplied to the main electrode chamber 7 &# 39 ; from a washing solution tank 16 as a washing solution for the copper oxide electrode for about 10 seconds through the sampling pump 4 before conducting the automatic control of the plating solution , as given above under ( d ), by switching the three - way electromagnetic valve 6 . the plating solution could be thus automatically controlled for a continuation of 168 hours , where the sampling rate of the sampling pump 4 was 50 ml / l , the detection temperature of the sampled plating solution was about 25 ° c . owing to the cooler 5 , and the preset potential for the ph of the plating solution was - 0 . 260 v . a chemical treating solution as given below under ( a ) was used in metal pickling . the ph of chemical treating solution was continuously controlled to - 0 . 08 ( 1 . 2 n in hydrogen ion concentration ) in the same system as in fig1 in the same manner as in example 1 , except that a copper oxide electrode as given below under ( b ), a makeup solution for adjusting ph of the chemical treating solution as given below under ( d ), and a standard solution for reference electrode as given below under ( e ) were used , a titrating solution as given below ( c ) was added to the main electrode chamber 7 &# 39 ; of fig1 and the chemical treating solution adjusted to ph 11 or higher was led thereto . ( b ) copper oxide electrode prepared by etching naked copper wire ( purity 99 . 99 %) with a diameter of 1 mm in a 0 . 5 n hcl solution at a liquid temperature of 30 ° c . for 5 seconds and then oxidizing the etched copper wire in 0 . 5 n koh at liquid temperature of 30 ° c . for 15 minutes . ( d ) makeup solution for adjusting ph of the treating solution : 12 n hydrochloric acid a chemical treating solution as given below under ( a ) was used in alkali washing of metal . the ph of the chemical treating solution was kept continuously at 13 . 7 with a copper oxide electrode , a titrating solution , a makeup solution for adjusting ph of treating solution , and a standard solution for reference electrode as given below under ( b )-( e ) in the same manner as in example 1 in the same system as shown in fig1 . the similar results as in example 1 were obtained . ( b ) copper oxide electrode prepared by etching naked copper wire ( purity 99 . 9 %) with a diameter of 1 mm in a 0 . 5 n h 2 so 4 solution at a liquid temperature of 30 ° for 5 seconds and then oxidizing the etched copper wire in 0 . 5 n naoh at a liquid temperature of 30 ° c . for 15 minutes . ______________________________________12 n hydrochloric acid 37 . 5 mlkh . sub . 2 po . sub . 4 6 . 8 gwater to make total volume 1 l______________________________________ in chemical copper plating with the same chemical copper plating solution as in example 1 in the same manner as in example 1 , the ph and the concentration of formaldehyde were controlled . the ph control was carried out in the same manner as in example 1 , and control of formaldehyde was carried out with an automatic analyzing solution , a copper oxide electrode , a washing solution for the copper oxide electrode , and a makeup solution for adjusting the concentration of formaldehyde as given below under ( a )-( e ). ______________________________________na . sub . 2 so . sub . 3 100 gwater to make total volume 1 l______________________________________ ( b ) copper oxide electrode prepared by etching naked copper wire ( purity : 99 . 99 %) with a diameter of 1 mm in 14 n nitric acid at a liquid temperature of 18 ° c . for one second , and then oxidizing the etched copper wire in 1 n caustic soda at 18 ° c . for 5 minutes . ( c ) electrode ( the same as used in the ph measurement ) copper oxide - electrode - calomel electrode ( using an aqueous saturated kcl solution ) ______________________________________37 % formalin 200 mlwater to make total volume 1 l______________________________________ the control system is given in fig2 . at first , the ph control of the chemical copper plating solution was carried out by means of members 1 - 18 in fig2 in the same manner as in example 1 , and the similar results as in example 1 were obtained . the sample solution leaving the ph detection cell 7 of fig2 was led to a mixter 19 together with an automatic analyzing solution for formaldehyde as given above under ( a ), sampled from a titrating solution tank 17 through a three - way electromagnetic valve 18 by the sampling pump 4 , and thoroughly mixed together , and then led to a main electrode chamber 20 &# 39 ; of a formaldehyde concentration detection cell 20 , where a difference in potential was detected between an copper oxide electrode 8 &# 39 ; and a silver - silver chloride electrode 8 by means of the controller 10 . numeral 11 &# 39 ; is a membrane . when the detected potential was smaller than the preset potential in the controller , a signal was transmitted to a makeup pump 21 to supply a makeup solution as given above under ( e ) from a makeup solution tank 22 for adjusting the concentration of formaldehyde to the plating tank 1 through a valve 23 and the mixer 3 until the detected potential exceeded the preset potential . on the other hand , an aqueous saturated kcl solution was continuously supplied to the reference electrode chamber 7 &# 34 ; from the standard solution tank 15 by the sampling pump 4 as the standard solution for the reference electrode to obtain a stable potential from the silver - silver chloride electrode 9 in the reference electrode chamber 7 &# 34 ;. the sampled solution of the plating solution leaving the formaldehyde concentration detection cell 20 and the aqueous saturated kcl solution leaving the reference electrode chamber 7 &# 34 ; were thrown away . furthermore , an aqueous 7 n nitric acid solution was supplied to the detection cells 7 and 20 from the washing solution tank 16 as a washing solution for the copper oxide electrode as given above under ( d ) through the sampling pump 4 for about 10 seconds before conducting the automatic control of the plating solution by switching the three - way valves 6 and 18 . according to the aforementioned automatic control system for the ph and the formaldehyde concentration of the plating solution , the plating solution could be automatically controlled for a continuation of 168 hours , where the sampling rate of the sampling pump 4 was 50 ml / l , the temperature of detected plating solution was about 25 ° c . owing to the cooler 5 , the preset potential for the ph of the plating solution was - 0 . 260 v , and the preset potential for the formalin concentration was - 0 . 300 v . under these conditions , the ph of the plating solution could be automatically controlled to 12 . 3 ± 0 . 07 and the formalin concentration to 3 ± 1 ml / l . in chemical copper plating with the same chemical copper plating solution as used in example 1 , in the same manner as in example 1 , the ph , the concentration of cupric ions , and the concentration of the complexing agent were controlled . the ph control was carried out in the same manner as in example 1 , and control of the concentration of cupric ions and the concentration of the complexing agent was carried out with automatic analyzing solutions , an electrode , a makeup solution for adjusting the copper concentration and a makeup solution for adjusting the complexing agent concentration as given below under ( a )-( e ). ______________________________________cuso . sub . 4 . 5h . sub . 2 o 14 . 107 ghcoona 64 g12 n hydrochloric acid 30 mlwater to make total volume 1 l______________________________________ ______________________________________ triethylenetetramine 100 ml12 n hydrochloric acid 164 mlwater to make total volume 1 l______________________________________ ______________________________________fe . sub . 2 ( so . sub . 4 ). sub . 3 ( nh . sub . 4 ). sub . 2 so . sub . 4 . 24h . sub . 2 o 50 . 260 gwater to make total volume 1 l______________________________________ ( c ) electrode ( for measuring the concentrations of cupric ions and complexing agent ) ______________________________________cuso . sub . 4 . 5h . sub . 2 o 250 gwater to make total volume 1 l______________________________________ ______________________________________edta . 2na 100 gwater to make total volume 1 l______________________________________ control system is shown in fig3 . at first , the ph control was carried out by members 1 to 14 in fig3 and the similar results as in example 1 were obtained . the sampling solution leaving the ph detection cell 7 of fig3 was led to a mixer 25 together with an automatic analyzing solution for cupric ions as given above under ( a ), sampled from a titrating solution tank 24 by the sampling pump 4 , thoroughly mixed , and led to a main electrode chamber 26 &# 39 ; of a cupric ion concentration detection cell 26 , where a difference in potential was measured between a platinum electrode 27 and a silver - silver chloride electrode 9 &# 34 ; by means of the controller 10 . numeral 11 &# 39 ; is a membrane . when the detected potential was smaller than the preset potential in the controller , a signal was transmitted to a makeup pump 28 from the controller 10 to supply a makeup solution as given above under ( d ) to the plating tank 1 from a makeup solution tank 29 for adjusting the cupric ion concentration through a valve 30 and the mixer 3 until the detected potential exceeded the preset potential . on the other hand , an aqueous saturated kcl solution was continuously supplied to a reference electrode chamber 26 &# 34 ; from the reference electrode chamber 7 &# 34 ; of the ph detection cell 7 to obtain a stable potential from the silver - silver chloride electrode 9 &# 34 ; in the reference electrode chamber 26 &# 34 ;. the aqueous saturated kcl solution leaving the reference electrode chamber 26 &# 34 ; of the cupric ion concentration detection cell 26 was led to a reference electrode chamber 9 &# 34 ;&# 39 ; of a complexing agent concentration detection cell 35 , and then thrown away . the sampled solution leaving the cupric ion concentration detection cell 26 was led to a mixer 32 together with a triethylenetetramine solution as given above under ( b - 1 ), sampled from a titrating solution tank 31 by the sampling pump 4 , thoroughly mixed , then led to a mixer 34 together with an iron ion - containing solution as given above under ( b - 2 ), sampled from a titrating solution tank 33 by the sampling pump 4 , thoroughly mixed , and subjected to reaction . then , the resulting solution was led to the main electrode chamber 35 &# 39 ; of a complexing agent concentration detection cell 35 , where a difference in potential was detected between a platinum electrode 27 &# 39 ; and a silver - silver chloride electrode 9 &# 34 ; by means of the controller 10 . numeral 11 &# 39 ;&# 39 ;&# 39 ; is a membrane . when the detected potential was larger than the preset potential in the controller , a signal was transmitted to a makeup pump 36 to supply a makeup solution as given above under ( e ) to the plating tank 1 from a makeup tank 37 for adjusting the concentration of complexing agent through a valve 38 and the mixer 3 until the measured potential became smaller than the preset potential . the sampled solution leaving the main electrode chamber 27 &# 39 ; was thrown away . the concentration of cupric ions and the concentration of complexing agent could be thus automatically controlled for a continuation of 116 hours , where the sampling rate of the sampling pump 4 was 50 ml / l , the temperature of detected plating solution was about 25 ° c . owing to the cooler 5 , the preset potential for the ph of the plating solution was - 0 . 260 v , the preset potential for the concentration of cupric ions was 0 . 100 v , and the preset potential for the concentration of complexing agent was 0 . 150 v . under these conditions , the ph could be automatically controlled to 12 . 3 ± 0 . 04 , the concentration of cupric ions to 13 . 1 ± 0 . 53 g / l , and the concentration of complexing agent to 40 ± 0 . 7 g / l . automatic control of the same chemical plating solution as in example 1 was carried out in a system as shown in fig4 by measuring ph and the concentration of cupric ions in the same manner as in examples 1 and 5 , then by measuring the concentration of the reducing agent , and then by measuring the concentration of the complexing agent in the same manner as in example 5 . the ph control was carried out in the same manner as in example 1 , and control of the concentrations of cupric ions , the reducing agent and the complexing agent was carried out with automatic analyzing solutions , electrodes , and makeup solutions for adjusting the concentrations as given below under ( a ) to ( h ). ______________________________________cuso . sub . 4 . 5h . sub . 2 o 14 . 107 ghcoona 64 g12 n hydrochloric acid 30 mlwater to make total volume 1 l______________________________________ ______________________________________na . sub . 2 so . sub . 4 50 gedta - 2na 15 gnaoh 4 gna . sub . 2 so . sub . 3 4 . 593 gwater to make total volume 1 l______________________________________ ______________________________________ki 40 gi . sub . 2 5 . 076 gwater to make total volume 1 l______________________________________ ______________________________________ triethylenetetramine 100 ml12 n hydrochloric acid 164 mlwater to make total volume 1 l______________________________________ ______________________________________fe . sub . 2 ( so . sub . 4 ). sub . 3 ( nh . sub . 4 ). sub . 2 so . sub . 4 . 24h . sub . 2 o 25 . 130 gwater to make total volume 1 l______________________________________ ( d ) electrodes for measuring the concentrations of cubric ions , reducing agent and complexing agent ______________________________________cuso . sub . 4 . 5h . sub . 2 o 250 gwater to make total volume 1 l______________________________________ ______________________________________37 % formalin 200 mlwater to make total volume 1 l______________________________________ ______________________________________edta - 2na 100 gwater to make total volume 1 l______________________________________ ( h ) standard solution : 0 . 1 n hydrochloric acid - the control system isshown in fig4 . at first , the ph control and the control of the cupricion concentration and the complexing agent were carried out by members 1to 30 in fig4 in the same manner as in examples 1 and 5 . in the presentembodiment , the sampled solution leaving the cupric ion concentrationdetection cell 26 was devided into two streams , and one stream was led tothe main electrode chamber 7 &# 39 ; of the complexing agent detection cell 20 , whereas the other stream was led to a mixer 32 , after the flow rate wasadjusted by the sampling pump 4 , together with a sulfite ion - containingsolution as given above under ( b - 1 ), sampled from a titrating solutiontank 31 by the sampling pump 4 , thoroughly mixed , then led to a mixer 34together with an iodine - containing solution , as given above under ( b - 2 ), sampled from a titrating solution tank 33 by the sampling pump 4 , thoroughly mixed , and subjected to reaction . then , the stream was led toa main electrode chamber 35 &# 39 ; of a reducing agent detection cell 35 , wherea difference in potential was detected between a platinum electrode 27 &# 39 ; and a silver - silver chloride electrode 9 &# 39 ;&# 39 ;&# 39 ; by means of the controller10 . numeral 11 &# 39 ;&# 39 ;&# 39 ; is a membrane . when the detected potential was smallerthan the present potential in the controller , a signal was transmittedfrom the controller to a makeup pump 36 to supply a makeup solution , asgiven above under ( f ), to the plating tank 1 from a makeup tank 37 foradjusting the reducing agent through a valve 38 and the mixer 3 until thedetected potential exceeded the present potential . the sampled solutionleaving the main electrode chamber 35 &# 39 ; was thrown away . - on the otherhand , a standard solution , as given above under ( h ), leaving thereference electrode chamber 20 &# 39 ; of the complexing agent concentrationdetection cell 20 was led to a reference electrode chamber 9 &# 39 ;&# 39 ;&# 39 ; of thereducing agent concentration detection cell 35 to obtain a stablepotential from the silver - silver chloride electrode 9 &# 39 ;&# 39 ;&# 39 ; in the referenceelectrode chamber 35 &# 39 ;&# 39 ;, and then thrown away . the ph , the cupric ionconcentration , the reducing agent concentration and the complexing agentconcentration of the chemical copper plating solution could be thusautomatically controlled for a continuation of 100 hours , where thesampling rate of the sampling pump was 50 ml / l , the detection temperatureof sampling plating solution was about 25 ° c . owing to the cooler5 , the present potential for the ph of the plating solution was - 0 . 260 v , the present potential for the cupric ion concentration was 0 . 100 v , thepresent potential for the reducing agent concentration was 0 . 050 v , andthe present potential for the complexing agent concentration was 0 . 150 v . under these conditions , the ph could be automatically controlled to12 . 3 ± 0 . 04 , the cupric ion concentration to 13 ± 0 . 52 g / l , thereducing agent concentration to 3 ± 0 . 15 ml / l , and the complexing agentconcentration to 40 ± 0 . 8 g / l with high controlling exactness . - sincethe ph of the plating solution could be measured stably with goodexactness for a prolonged time by means of a copper oxide electrode , theph of the plating solution could be adjusted with good exactness in thepresent embodiment . as a result , a titration error due to a ph change wassmall in the titration for measuring the concentration of cupric ions , reducing agent and complexing agent , and these concentrations could beadjusted with improved exactness . furthermore , since a change in the phof the plating solution was small , no precipitation of the titratingsolutions took place in conduits , and thus the control system had animproved reliability . - in the present example , a non - soluble electrodesuch as electrodes of gold , tungsten , carbon , palladium , etc . can be usedin place of platinum as the main electrode for measuring theconcentration of the reducing agent with similar results . | 2 |
the amphoteric substance used to treat the polyene resins is selected from the group consisting of silicated magnesium oxide , basic aluminum oxide , silica gel , magnesium oxide , magnesium hydroxide , calcium oxide , calcium hydroxide , barium oxide and barium hydroxide . the average particle size of the amphoteric substance is preferably in the range of about 2 microns to about 200 microns . a particularly preferred amphoteric agent is magnesol ® polysorb 30 / 40 hydrated silicated magnesium oxide , which has a particle size range of from about 2 to about 200 microns and an average particle size of 50 microns . contact time with the polyene resin will vary depending upon the temperature employed and the moisture content and viscosity of the resin . the time should be for sufficient time to reach a cl - content of less than 1 . 0 ppm , preferably to 0 . 5 ppm or less , or for sufficient time to improve the shelf life of a thiolene composition prepared by mixing the polyene with a polythiol after the amphoteric treating agent has been separated from the polyene . the treatment can also be used to reduce sodium and potassium levels below 1 ppm , suitably 0 . 5 or less . typical contact times will be between 1 hour and 3 days . treatment efficiency can be improved , lessening necessary contact time , if the polyene has a small moisture content , suitably , 0 . 01 %- 1 . 0 %. when a dry resin is used and moisture can readily be removed subsequent to treatment , e . g . by vacuum stripping , it may be desirable to add moisture to the treatment mixture . contact temperatures will also vary depending on viscosity of the polyene . effective ion removal can be obtained at temperatures between 0 ° c . and 100 ° c . provided that the polyene is sufficiently non - viscous at the temperature employed to allow for good agitation of the mixture . the amphoteric treating agent must be removed from the polyene resin prior to formulation into a curable composition , such as a thiol - ene composition . separation can be accomplished by filtration but in some cases where the amphoteric treating agent has a clay - like consistency addition of a filter aid such as celite ® to the treatment mixture prior to filtration is necessary for effective filtration . addition of the filter aid does not appear to influence the effectiveness of the amphoteric treating agent in removing ionic species or in improving shelf - life stability of thiolene compositions produced from the treated resin . the plural norbornene functional compounds useful in the invention are known from u . s . pat . no . 4 , 808 , 638 , incorporated herein by reference , and have recently also been described in jacobine et al , &# 34 ; photoinitiated cross - linking of norbornene resins with multifunctional thiols &# 34 ;, chapter 13 of radiation curing of polymeric materials , acs symposium series # 417 , american chemical society , 1990 , and u . s . pat . no . 5 , 167 , 882 , also incorporated herein by reference . particularly preferred norbornene compounds are norbornenemethyl norbomenecarboxylate and norbornene carboxylate esters of polyols such as 1 , 6 - hexanediol , trimethylolpropane , ethoxylated bisphenol a , poly ( tetramethyleneoxide ) and mixtures thereof . the polythiol component of the inventive compositions may be any compound having two or more thiol groups per molecule . suitable polythiols are described in u . s . pat . no . 3 , 661 , 744 at col . 8 , in 76 - col . 9 , in 46 ; in u . s . pat . no . 4 , 119 , 617 , col . 7 , ins 40 - 57 ; u . s . pat . no . 3 , 445 , 419 ; and u . s . pat . no . 4 , 289 , 867 . especially preferred are polythiols obtained by esterification of a polyol with an α or β - mercaptocarboxylic acid such as thioglycolic acid , or β - mercaptopropionie acid . particularly preferred polythiols are pentaerythritol tetramercaptoacetate and pentaerythritol tetrakis - β - mercaptopropionate ( petmp ). the ratio of the polyene to the polythiol component can be varied widely . generally it is preferred that the ratio of thiol to ene groups be between 0 . 7 : 1 and 1 . 3 : 1 , but ratios outside this range may occasionally be usefully employed without departing from the invention hereof . while a curable composition using norbornene functional compounds of the invention may include both difunctional norbornenyl compounds and difunctional thiol compounds , it will be understood that at least a portion of at least one of these components should contain more than two functional groups per molecule to produce a crosslinked product when cured . that is , the total of the average number of norbornene groups per molecule of norbornene functional compound and the average number of coreactive thiol groups per molecule of the thiol functional compound should be greater than 4 when a crosslinked cured product is desired . this total is referred to as the &# 34 ; total reactive functionality &# 34 ; of the composition . the initiator used in the curable thiol - ene formulations is suitably a free radical photoinitiator . examples of free radical photoinitiators include benzoin and substituted benzoin compounds , benzophenone , michler &# 39 ; s ketone , dialkoxybenzophenones , dialkoxyacetophenones , peroxyesters described in u . s . pat . nos . 4 , 616 , 826 and 4 , 604 , 295 , etc . the photoinitiator is employed in an amount effective for initiating cure of the formulation upon irradiation with uv light , suitably 0 . 1 - 10 %, typically 0 . 5 - 5 %. the formulations also preferably include a stabilizer . preferred stabilizers are described in ep 428 , 342 . such stabilizers are non - acidic nitroso compounds , particularly n - nitrosoarylhydroxylamines and salts thereof . particularity suitable stabilizer compounds are the ammonium and aluminum salts of n - nitrosophenylhydroxylamine which may be usefully employed at levels between about 10 ppm and 2 %, preferably 10 - 5 , 000 ppm . as described in u . s . pat . no . 5 , 208 , 281 , triiodide and other polyiodides are useful shelf - life stabilizers for thiol - ene formulations . the invention is illustrated by reference to the following non - limiting examples . dinorbornene resins were produced by dieis - alder cycloaddition of cyclopentadiene to ethoxylated bisphenol a . the same lot of acrylate starting material was used in both the control and the treated samples . resins were filtered at 50 ° c . through a course frit celite ® c bed after synthesis . the treated sample was mixed with 2 wt % magnesol ® polysorb 30 / 40 silicated magnesium oxide , stirred three hours at 45 ° c . and allowed to sit overnight . celite ® filter aid , 3 wt % was added , mixed for one hour at 45 ° c . and then the mixture filtered at 70 ° c . using a 1μ filter pad . the dinorbornene resins were then formulated into thiol - ene formulations using equivalent weights of pentaerythritol tetramercaptopropionate , 2 wt % darocure ® 1173 photoinitiator and 1000 ppm aluminum n - nitrosophenylhydroxylamine . samples of the formulations were then stored at room temperature and at 5 ° c . under nitrogen . viscosities of the formulations were taken at periodic intervals to ascertain their relative storage stability . results are given in table i . table i______________________________________ formulation viscositiesstorage interval ( cumulative change )( temperature ) example 1 control______________________________________ 0 7178 6864 7 days ( rt *) 7904 ( 10 %) 8024 ( 17 %) 28 days ( rt ) 8595 ( 20 %) 10441 ( 52 %) 90 days ( rt ) 8985 ( 25 %) 14728 ( 115 %) 180 days ( rt ) 10218 ( 42 %) 21627 ( 215 %) 180 days ( 5 ° c .) 7520 ( 5 %) 9809 ( 43 %) ______________________________________ * rt = room temperature ( approximately 21 ° c .). the procedure of example 1 was repeated using the same batch of norbornene resin for both control and treated samples . results are shown in table ii . table ii______________________________________ formulation viscositiesstorage interval ( cumulative change )( temperature ) example 2 control______________________________________ 0 7187 7204 7 days ( rt ) 8418 ( 17 %) 53520 ( 643 %) 28 days ( rt ) 9714 ( 36 %) 69865 ( 870 %) 90 days ( rt ) 14431 ( 101 %) 92660 ( 1186 %) 180 days ( rt ) 15302 ( 113 %) 104348 ( 1348 %) 180 days ( 5 ° c .) 8808 ( 23 %) 33213 ( 361 %) ______________________________________ analysis for selected ions in the norbornene resins used in this example gave the following results : untreated control : 11 . 8 ppm cl - ; & lt ; 0 . 5 ppm br - ; 6 . 4 ppm na + ; 1 . 5 ppm k + . treated resin : & lt ; 0 . 5 ppm cl - ; & lt ; 0 . 5 ppm br - ; & lt ; 1 ppm na + & lt ; 1 ppm k + . the treated norbornene resin used in example 2 was spiked with 7 . 2 ppm cl - , as nacl in a methanol solution using an equivalent weight of 18 - crown - 6 to assure transfer of the salt into the resin . the spiked resin was then formulated as per example ii . after 7 days , the viscosity of the formulation had increased 44 %, more than double the viscosity increase of the formulation made from the treated , unspiked resin . the procedure of example 2 was repeated except that the norbornene monomer used was hexanediol dinorbornene carboxylate and the viscosity was monitored for only seven days at room temperature . results are given in table iii . table iii______________________________________ formulation viscositiesstorage interval ( cumulative change )( temperature ) example 4 control______________________________________0 215 2107 days ( rt ) 330 ( 53 %) 917 ( 337 %) ______________________________________ treatment of triallyl - 1 , 3 , 5 - triazine - 2 , 4 , 6 ( 1h , 3h , 3h )- trione in the manner of example i gave a reduction of chloride content from 5 . 2 ppm to 0 . 2 ppm . the treatment did not affect storage stability of a thiol - ene formulation prepared from this resin but the reduction in chloride content was considered desirable for electrical insulating and corrosion resistance properties of the formulation . samples of the untreated dinorbornene resin used in example 2 were treated in the same manner as in that example except that the 2 wt % magnesol ® polysorb 30 / 40 and 3 wt % celite ® filter aid , respectively , were replaced with , 2 wt % basic aluminum oxide and 1 wt % celite ®; 2 wt % silica gel and 1 wt % celite ®; and 3 wt % magnesol ® polysorb 30 / 40 and no celite ®. hydrolyzable ion content was determined by ion chromatography on two trials for each sample and results are shown in table iv . table iv__________________________________________________________________________ potassiumsample treatment chloride ( ppm ) bromide ( ppm ) sodium ( ppm ) ( ppm ) __________________________________________________________________________none 9 . 8 none detected 7 . 5 1 . 7 11 . 7 none detected 9 . 3 2 . 02 wt % basic aluminum 0 . 1 none detected & lt ; 0 . 2 none detectedoxide and 1 wt % celite ® & lt ; 0 . 1 none detected & lt ; 0 . 2 none detected2 wt % silica gel and 1 0 . 1 none detected & lt ; 0 . 2 none detectedwt % celite ® 0 . 1 none detected & lt ; 0 . 2 none detected3 wt % magnesol ® & lt ; 0 . 1 none detected & lt ; 0 . 2 none detectedpolysorb 30 / 40 and no & lt ; 0 . 1 none detected & lt ; 0 . 2 none detectedcelite ® __________________________________________________________________________ estimated detection limits for bromide were 0 . 5 ppm and for potassium were 0 . 2 ppm . | 2 |
a configuration of a dielectric filter according to a first embodiment of the present invention will be described below by referring to fig1 to 4 . in fig1 dielectric rods 1 and 2 are disposed orthogonally to each other and grooves 7 are provided at the intersection . a dielectric rod complex made up of such a plurality of dielectric rods combined is disposed in an outer conductive member 6 to form a dielectric resonator 10 . in fig1 there is also shown an external coupling element 5 . fig2 a shows an elevation and a right - hand side view of the external coupling element shown in fig1 which includes a first coupling portion 51 and a second coupling portion 52 . the first coupling portion 51 is connected to the central conductor of a signal input / output connector 4 at one end and the second coupling portion 52 is connected to the inner surface ( ground ) of the outer conductive member 6 at one end . the first coupling portion 51 and the second coupling portion 52 are continuous . the central conductor of the input / output connector 4 , the external coupling element 5 , and the outer conductive member 6 form a loop . since the first coupling portion 51 is disposed in parallel with the axial direction of the dielectric rod 1 and the second coupling portion 52 is disposed in parallel with the axial direction of the dielectric rod 2 , the first coupling portion 51 and the dielectric rod 1 are magnetically coupled and the second coupling portion 52 and the dielectric rod 2 are magnetically coupled . the resonator made up of the dielectric rod 2 is also coupled with the resonator made up of the dielectric rod 1 since the grooves 7 are formed at the intersection of the dielectric rod 1 and the dielectric rod 2 . the resonator made up of the dielectric rod 1 may be considered the first resonator in a multistage filter and the resonator made up of the dielectric rod 2 may be considered the second - stage resonator . on the other hand , the resonator made up of the dielectric rod 1 may also be the last resonator and in that case , the resonator made up of the dielectric rod 2 may be the resonator disposed one stage before . the conditions are the same in both cases . fig1 also shows instantaneous electric - field vectors at the same time generated in the external coupling element and the dielectric rods . when the electric - field vectors e1 and e2 generated in the dielectric rods 1 and 2 are in phase , the electric - field vectors eq1 and eq2 corresponding to the first coupling portion 51 and the second coupling portion 52 of the external coupling element 5 appear as shown in the figure and the sections are coupled with the corresponding dielectric rods in phase , respectively . fig2 b shows an elevation and a right - hand side view of another similar external coupling element , in which a step is formed between the portions 51 and 52 . in fig2 a and 2b , the outer conductive member or casing 6 is made from a metallic panel and the input / output connector 4 is mounted on the casing 6 . one end of the external coupling element 5 is soldered to the central conductor of the input / output connector 4 and the other end is soldered to the inner surface of the outer conductive member 6 . in the external coupling element shown in fig2 a , as the length l1 and the width w1 of the first coupling portion 51 and the height h1 from the outer conductive member 6 become larger , the coupling level with the resonator made up of the dielectric rod 1 shown in fig1 increases . as the length l2 of the second coupling portion 52 and the height h1 from the outer conductive member 6 become larger , the coupling level with the resonator made up of the dielectric rod 2 shown in fig1 increases . in this way , the coupling level between the external coupling element and the first ( or the last ) resonator and the coupling level between the external coupling element and the second ( or the stage immediately before the last stage ) resonator can be set independently . in the external coupling element shown in fig2 b , by forming a step between the portions 51 and 52 , the height h2 of the second coupling portion 52 is set lower than the height h1 of the first coupling portion 51 , so that the coupling level between the second coupling portion 52 and the resonator made up of the dielectric rod 2 shown in fig1 is set relatively low . in this way , the coupling level between the external coupling element and the first ( or the last ) resonator and the coupling level between the external coupling element and the second - stage ( or the stage immediately before the last stage ) resonator can be set independently , simply by changing h1 and / or h2 respectively . fig3 is an equivalent circuit diagram of the dielectric filter shown in fig1 . when the coupling between the input / output coupling inductor generated by the external coupling element and the first ( or the last ) resonator is in phase with the coupling between the first ( or the last ) resonator and the second - stage ( or the stage immediately before the last stage ) resonator , the coupling between the input / output inductor and the second - stage ( or the stage immediately before the last stage ) resonator is also in phase due to the external coupling element configured as described above . with this configuration , an attenuation maximum is generated at the higher - frequency side of the transmission band as shown in fig4 . fig1 shows a single tm double - mode dielectric resonator . by arranging tm double - mode dielectric resonators having the same configuration and sequentially coupling specified resonators , a third - order or higher - order dielectric filter having three or more resonators can be configured . or , a dielectric filter including two resonators can be configured by providing , in addition to the input / output connector 4 and the external coupling element 5 , another external coupling element which couples with another input / output connector and with the resonator made up of the dielectric rod 2 in the configuration shown in fig1 . a configuration of a dielectric filter according to a second embodiment of the present invention will be described below by referring to fig5 to 7 . in fig5 dielectric rods 1 and 2 are disposed orthogonally to each other and grooves 7 are provided at the intersection , forming a dielectric rod complex , which is disposed in an outer conductive member 6 . in fig5 there is also shown an external coupling element 5 which includes a first coupling portion 51 and a second coupling portion 52 . the first coupling portion 51 is connected to the central conductor of a signal input / output connector 4 at one end and the second coupling portion 52 is connected to the inner surface ( ground ) of the outer conductive member 6 at one end . the first coupling portion 51 and the second coupling portion 52 are continuous . the central conductor of the input / output connector 4 , the external coupling element 5 , and the outer conductive member 6 form a loop . since the first coupling portion 51 is disposed in parallel with the axial direction of the dielectric rod 1 and the second coupling portion 52 is disposed in parallel with the axial direction of the dielectric rod 2 , the first coupling portion 51 and the dielectric rod 1 are magnetically coupled and the second coupling portion 52 and the dielectric rod 2 are magnetically coupled . the resonator made up of the dielectric rod 2 is coupled with the resonator made up of the dielectric rod 1 since the grooves 7 are formed at the intersection of the dielectric rod 1 and the dielectric rod 2 . the resonator made up of the dielectric rod 1 will be considered to be the first resonator and the resonator made up of the dielectric rod 2 will be considered the second - stage resonator . fig5 shows instantaneous electric - field vectors at the same time generated in the external coupling element and the dielectric rods . when the electric - field vectors e1 and e2 generated in the dielectric rods 1 and 2 are in phase , the electric - field vectors eq1 and eq2 corresponding to the first coupling portion 51 and the second coupling portion 52 of the external coupling element 5 appear as shown in the figure . the dielectric rod 1 is coupled with the first coupling portion 51 in phase and the dielectric rod 2 is coupled with the second coupling portion 52 in reverse phase . fig6 is an equivalent circuit diagram of the dielectric filter shown in fig5 . when the coupling between the input / output coupling inductor generated by the external coupling element and the first resonator is in phase with the coupling between the first resonator and the next - stage resonator , the coupling between the input / output inductor and the next - stage ( the second - stage ) resonator is in reverse phase due to the external coupling element configured as described above . with this configuration , an attenuation maximum is generated at the lower - frequency side of the transmission band as shown in fig7 . in fig8 a , a second coupling portion 52 is provided near the central conductor of the input / output connector 4 and a first coupling portion 51 is connected to the inner surface of the outer conductor at one end . when this external coupling element 5 is substituted for the external coupling element shown in fig1 the same characteristics as those of the dielectric filter shown in the first embodiment are obtained . in fig8 b , instead of using a metallic plate , a rod - or wire - shaped metallic member is bent to form a first coupling portion 51 and a second coupling portion 52 . in fig8 c , a rod - or wire - shaped metallic member is used in the same way . one end of a first coupling portion 51 is connected to the central conductor of the input / output connector 4 , and one end of a second coupling portion 52 is connected to the inner surface of the outer conductor . in fig8 d and 8e , a first coupling portion 51 is connected to the central conductor of the input / output connector 4 at one end , and is connected to the inner surface of the outer conductor at the other end . in addition , a second coupling portion 52 protrudes from the first coupling portion 51 toward a side and is connected to the inner surface of the outer conductor at one end . in fig8 f , one end of a first coupling portion 51 is connected to the central conductor of the input / output connector 4 , and a second coupling portion 52 protruding from the other end of the first coupling portion 51 toward a side is connected to the inner surface of the outer conductor at one end . when such an external coupling element is used in the configuration shown in fig1 the first coupling portion 51 is coupled with the resonator made up of the dielectric rod 1 , and the second coupling portion 52 is coupled with the resonator made up of the dielectric rod 2 . in fig8 g , 8h , and 8i , one end of a first coupling portion 51 is connected to the central conductor of the input / output connector 4 and the other end is connected to the inner surface of the outer conductor . toward a side of the first coupling portion 51 , a second coupling portion 52 protrudes , and one end of the second coupling portion 52 is left open . fig9 a is a perspective view , fig9 b is an elevation and right - hand side view showing a fourth embodiment of the invention . in this embodiment , the external coupling element 5 does not have a distinct first coupling portion and second coupling portion , as described above . rather , the whole loop formed by the external coupling element and the outer conductor is slanted . when this external coupling element is substituted for the external coupling element shown in fig1 the device is coupled with both the resonator made up of the dielectric rod 1 and the resonator made up of the dielectric rod 2 . the coupling levels between the external coupling element 5 and the two resonators change according to the slant angle θ shown in fig9 b of the external coupling element 5 . in other words , when angle θ decreases , the coupling level between the external coupling element and the first resonator ( dielectric rod 1 ) increases and the coupling level between the external coupling element and the next - stage resonator ( dielectric rod 2 ) decreases . in contrast , when angle θ increases , up to 90 degrees , the coupling level between the external coupling element and the first resonator decreases and the coupling level between the external coupling element and the next - stage resonator increases . as the length l1 , the width w1 , and the height h1 of the external coupling element become larger , the coupling level between the external coupling element and the first resonator and the coupling level between the external coupling element and the next - stage resonator become larger . in this configuration , the coupling level between the external coupling element and the first resonator and the coupling level between the external coupling element and the next - stage resonator cannot be independently specified . by taking these relationships into consideration , the dimensions of each section and the mounting angle need to be specified . fig1 shows a configuration of an external coupling element used for a dielectric filter according to a fifth embodiment of the present invention . a rod - or wire - shaped metallic member is used to form an external coupling element , instead of a metallic plate . the other configurations are the same as those used in fig9 a . therefore , also in this case , by specifying the slant angle θ , the length l1 , and the height h1 of the external coupling element 5 , the coupling level between the external coupling element and the first ( or the last ) resonator and the coupling level between the external coupling element and the next - stage ( or the stage immediately before the last ) resonator are specified . a configuration of a dielectric filter according to a sixth embodiment of the present invention will be described below by referring to fig1 and 12 . fig1 is a perspective view showing the configuration of the main section of a dielectric filter . in the figure , there are shown dielectric rods 1 , 2 , and 3 disposed orthogonally to each other and grooves 7 provided at the intersections . a dielectric rod complex made up of such a plurality of dielectric rods is disposed in an outer conductive member 6 . in fig1 , there is also shown an external coupling element 5 which includes a first coupling portion 51 and a second coupling portion 52 . the first coupling portion 51 is connected to the central conductor of a signal input / output connector 4 at one end and the second coupling portion 52 is connected to the inner surface ( ground ) of the outer conductive member 6 at one end . the first coupling portion 51 and the second coupling portion 52 are continuous . the central conductor of the input / output connector 4 , the external coupling element 5 , and the outer conductive member 6 form a loop . since the first coupling portion 51 is disposed in parallel with the axial direction of the dielectric rod 1 and the second coupling portion 52 is disposed in parallel with the axial direction of the dielectric rod 2 , the first coupling portion 51 and the dielectric rod 1 are magnetically coupled and the second coupling portion 52 and the dielectric rod 2 are magnetically coupled . the resonator made up of the dielectric rod 3 is not coupled with the first coupling portion 51 or the second coupling portion 52 . the resonator made up of the dielectric rod is coupled with the resonator made up of the dielectric rod 1 since the grooves 7 are formed at the intersection of the dielectric rod 1 and the dielectric rod 2 . since the grooves 7 are also formed at the intersection of the dielectric rod 2 and the dielectric rod 3 , the resonator made up of the dielectric rod 3 is coupled with the resonator made up of the dielectric rod 2 . therefore , the resonator made up of the dielectric rod 1 serves as the first resonator , the resonator made up of the dielectric rod 2 serves as the second - stage resonator , and the resonator made up of the dielectric rod 3 serves as the third - stage resonator . fig1 shows instantaneous electric - field vectors at the same time generated in the external coupling element and the dielectric rods . when the electric - field vectors e1 and e2 generated in the dielectric rods 1 and 2 are in phase , the electric - field vectors eq1 and eq2 corresponding to the first coupling portion 51 and the second coupling portion 52 of the external coupling element 5 appear as shown in the figure and the sections are coupled with the dielectric rods 1 and 2 in phase . fig1 is an equivalent circuit diagram of the dielectric filter shown in fig1 . when the coupling between the input / output coupling inductor generated by the external coupling element and the first resonator is in phase with the coupling between the first resonator and the next - stage resonator , the coupling between the input / output inductor and the next - stage ( the second - stage ) resonator is also in phase due to the external coupling element configured as described above . with this configuration , an attenuation maximum is generated at the higher - frequency side of the transmission band as shown in fig4 . a configuration of an antenna duplexer according to a seventh embodiment of the present invention will be described below by referring to fig1 to 19 . fig1 is a perspective view showing components of an antenna duplexer , other components not being shown in this view . in fig1 , there are shown casings 15a , 15b , 15c , and 15d which are connected to form a unit with cross - shaped dielectric rod complexes disposed inside and which have outer conductors formed at the outer surfaces . coupling windows 61a and 61b are formed at surfaces opposing each other of the cavities 15a and 15b . in the same way , coupling windows 61c and 61d are formed at surfaces opposing each other of the cavities 15c and 15d . four tm double - mode dielectric resonators 10a , 10b , 10c , and 10d are arranged in this way . as will be described later , metallic panels to which external coupling elements are mounted are placed at the upper and lower surfaces of the cavities 15a , 15b , 15c , and 15d and are soldered through grounding plates . fig1 is a plan view showing the components illustrated in fig1 . the relationship between dielectric rods and external coupling elements , which are shown in phantom in the figure . external coupling elements 5a and 5d and a coupling device 8 for connection to the antenna are mounted to the upper metallic panel . fig1 a and 15b are cross sections of an assembled antenna duplexer . fig1 a is a cross section taken on a line passing through the coupling device 8 for connection to the antenna , and fig1 b is a cross section taken on a line passing through the external coupling elements 5a , 5d . in fig1 a and 15b , there is shown an upper metallic panel 16 and a lower metallic panel 17 . an input / output connector 4bc serving as an antenna terminal , an input / output connector 4a serving as a tx - in terminal , and an input / output connector 4d serving as an rx - out terminal are mounted to the upper metallic panel 16 . at the inner surface of the upper metallic panel 16 , the coupling device 8 at the antenna side and the external coupling elements 5a and 5d are mounted . fig1 a is a plan view and fig1 b is a bottom view showing a configuration of the coupling device 8 . coupling loops 81 and 82 form loops together with the central conductor 41 of the input / output connector and the upper metallic panel 16 . the tip of the central conductor 41 of the input / output connector is threaded and the coupling loops 81 and 82 are secured to the tip with a nut 42 . as clearly understood from fig1 to 16b , the coupling loop 81 is magnetically coupled with the dielectric rod 1b of the dielectric resonator 10b , and the coupling loop 82 is magnetically coupled with the dielectric rod 1c of the dielectric resonator 10c . as shown in fig1 b , phase - adjustment electrodes 9 generate the specified capacitance with the upper metallic panel 16 to adjust the phases of the signals induced by the coupling loops 81 and 82 . fig1 a is an elevation , fig1 b is a left - hand side view , and fig1 c is a bottom view showing a configuration of the external coupling elements 5a and 5d shown in fig1 a and 15b . since the devices have substantially the same shapes , only one of them is shown in fig1 a - 17c . as shown , an external coupling element mainly includes a first coupling portion 51 and a second coupling portion 52 . one end of the first coupling portion 51 is connected and secured with a nut 42 to the central conductor of the input / output connector protruding from the upper metallic panel 16 , and one end of the second coupling portion 52 is soldered to the upper metallic panel 16 . by providing two of such external coupling elements 5a and 5d , the dielectric rod 1a of the dielectric resonator 10a and the first coupling portion 51a are magnetically coupled , and the dielectric rod 2a and the second coupling portion 52a are magnetically coupled , all of these elements being shown in fig1 . in addition , the dielectric rod 1d of the dielectric resonator 10d and the first coupling portion 51d are magnetically coupled , and the dielectric rod 2d and the second coupling portion 52d are magnetically coupled . as shown in fig1 , since a groove 7a is formed at the intersection of the dielectric rods 1a and 2a in the dielectric resonator 10a , when the instantaneous electric - field vectors in phase generated by the two resonators made up of the dielectric rods 1a and 2a are shown by hollow arrows in fig1 , the coupling between the first coupling portion 51a and the dielectric rod 1a is in phase and the coupling between the second coupling portion 52a and the dielectric rod 2a is in reverse phase as shown by the solid arrows . since a groove 7d is formed at the intersection of the dielectric rods 1d and 2d in the dielectric resonator 10d , when the instantaneous electric - field vectors in phase generated by the two resonators made up of the dielectric rods 1d and 2d are shown by hollow arrows in fig1 , the coupling between the first coupling portion 51d and the dielectric rod 1d is in phase and the coupling between the second coupling portion 52d and the dielectric rod 2d is in reverse phase as shown by the solid arrows . fig1 is an equivalent circuit diagram of the antenna duplexer . fig1 shows the characteristics of a transmission filter and a receiving filter . as shown in fig1 , since the coupling between the tx - in input / output coupling inductor and the second - stage resonator is in reverse phase , an attenuation maximum is generated at the lower - frequency side of the transmission band as shown in fig1 a . with this attenuation maximum , signal components in the receiving band are more steeply cut . since the coupling between the rx - out input / output coupling inductor and the resonator at the stage immediately before the last stage is in phase , an attenuation maximum is generated at the higher - frequency side of the transmission band as shown in fig1 b . with this attenuation maximum , transmission - signal components are steeply cut . fig2 a shows an equivalent circuit diagram of a dielectric filter according to an eighth embodiment of the present invention . in the above described embodiments , an external coupling element is provided which is magnetically coupled with both of the first and the next - stage resonators , or an external coupling element is provided which is magnetically coupled with both resonators disposed at the last stage and the stage immediately before the last stage . in fig2 a , there are a first external coupling element which is magnetically coupled with both of the first and the next - stage resonators , and a second external coupling element which is magnetically coupled with the resonators disposed at both the last stage and the stage immediately before the last stage . an external coupling element of the type shown in fig1 or fig5 is provided for the dielectric resonator including the first resonator and the dielectric resonator including the last resonator . fig2 a is an equivalent circuit diagram of the dielectric filter and fig2 b to 20e show the characteristics of the filter . when the coupling indicated in fig2 a by i and the coupling indicated by o are set to be in phase ( indicated by +), two attenuation maximums are generated at the higher - frequency side of the transmission band as shown in fig2 b . when the coupling indicated in fig2 a by i and the coupling indicated by o are set to be in reverse phase ( indicated by -), two attenuation maximums are generated at the lower - frequency side of the transmission band as shown in fig2 e . when the coupling i and the coupling o are respectively set to be + and -, or - and +, an attenuation maximum is generated at each of the lower - frequency side and the higher - frequency side of the transmission band as shown in fig2 c and 20d . although the present invention has been described in relation to particular embodiments thereof , many other variations and modifications and other uses will become apparent to those skilled in the art . the present invention is not limited by the specific disclosure herein . | 7 |
a vehicle vision system and / or driver assist system and / or object detection system and / or alert system operates to capture images exterior of the vehicle and may process the captured image data to display images and to detect objects at or near the vehicle and in the predicted path of the vehicle , such as to assist a driver of the vehicle in maneuvering the vehicle in a forward ( or rearward ) direction . front facing vehicular cameras include optical elements that constitute the camera . these elements are typically mounted in a vehicular camera housing , such as a windshield electronics module housing or the like , such as shown in fig1 and 2 ( and such as a housing that utilizes aspects of the vision systems described in u . s . pat . nos . 7 , 526 , 103 ; 7 , 480 , 149 ; 7 , 188 , 963 ; 6 , 824 , 281 ; 6 , 341 , 523 ; 6 , 250 , 148 ; 6 , 516 , 664 and / or 6 , 968 , 736 , which are hereby incorporated herein by reference in their entireties ). as can be seen with reference to fig1 and 2 , the housing may extend forward of the camera lens aperture and includes a stray light cone or shroud which serves to insulate the camera lens aperture from stray light that arises from reflections off the dashboard and / or windshield . such housings are typically relatively bulky compared to the optical elements of the camera and thus the housing may occupy a considerable amount of windshield real estate or space . it thus may be desirable to eliminate the housing , or at least minimize the extent of the camera housing , so as to free up space on the windshield . this would not only provide better aesthetics , but also increased visibility through the windshield for the driver of the vehicle . as shown in fig3 , the present invention proposes to eliminate the stray light cone or shroud and minimize the camera housing so that the housing only contains the optical elements of the camera and any necessary interfacing elements . at the very least , the present invention seeks to eliminate the stray light cone or shroud so that there is a minimum of the camera housing projecting forward of the camera lens aperture . instead of a stray light cone or shroud , the camera or vision system 10 of the present invention includes a camera 12 , with an angular filter 14 placed on or near the windshield 16 forward of the camera 12 and the camera lens aperture ( and not part of or incorporated in a camera housing of a windshield electronics module or the like ). the angular filter 14 comprises a transparent ( or substantially transparent or light transmitting ) or see - through film , which limits or substantially precludes reflection of light through an angular range corresponding to the stray light that would otherwise impinge the camera lens aperture . the angular filter 14 may comprise any suitable materials . for example , a suitable film material may be found on the likes of computer notebook screens and other types of display monitors and are commercially available from the 3m company and other suppliers . in some embodiments , the filter may be placed directly on the windshield , and in other embodiments ( and such as shown in fig3 ) the filter may be spaced apart from the windshield surface on a plane just below the camera lens aperture , in which case the filter may be mounted on a transparent substrate ( not shown ) or the like . optionally , the filter may be provided in the form of anti - reflective coating on the windshield , which acts to prevent reflections from the windshield . with the proposed structure , the designer of the camera system or vision system is afforded a great deal of design flexibility . in particular , and as can be seen with reference to fig3 , it will be appreciated that the printed circuit board 18 and other electronic components may be housed and disposed rearward of the camera optical elements and placed higher up on or along or near the windshield or even hidden all together under the vehicle roof liner . optionally , and as shown in fig3 , a flexible coupling 20 may also be provided between the small camera 12 and the printed circuit board 18 . with such a flexible coupling ( which electrically connects circuitry of the circuit board with circuitry of the camera to power and / or control the camera and to receive image data from the camera ), the present invention may provide a universal or substantially universal solution to many vehicles which may all have different windshield rake angles . for example , and as can be seen with reference to fig3 , the flexible coupling 20 may flex to allow the camera 12 to be arranged generally horizontally when the circuit board 18 is mounted along ( and generally parallel to ) the windshield 16 , such as , for example , along a windshield that has a rake angle of about 20 degrees , and the flexible coupling 20 may be adjusted or flexed to allow the camera 12 to be arranged generally horizontally when the circuit board 18 is mounted along a different windshield 16 ′, such as , for example , along a windshield that has a rake angle of about 40 degrees . the flexible electrical connector thus flexes to allow a viewing angle of the camera to be adjusted relative to a mounting angle of the circuit board , depending on the particular vehicle application of the camera system . thus , a common camera assembly or system 10 may be provided that may readily be adapted or configured for application to vehicles with different windshield angles ( with the flexible coupling or flex connection allowing for adjustment of the angular tilt or relative angles between the camera and lens axis and the circuit board ), without requiring additional mounting bracketry and the like to adapt the assembly to the particular vehicle . the camera or sensor may comprise any suitable camera or sensor . optionally , the camera may comprise a “ smart camera ” that includes the imaging sensor array and associated circuitry and image processing circuitry and electrical connectors and the like as part of a camera module , such as by utilizing aspects of the vision systems described in u . s . provisional application ser . no . 61 / 565 , 713 , filed dec . 1 , 2011 ; and / or ser . no . 61 / 563 , 965 , filed nov . 28 , 2011 , which are hereby incorporated herein by reference in their entireties . the vehicle may include any type of sensor or sensors , such as imaging sensors or radar sensors or lidar sensors or ultrasonic sensors or the like . the imaging sensor or camera may capture image data for image processing and may comprise any suitable camera or sensing device , such as , for example , an array of a plurality of photosensor elements arranged in 640 columns and 480 rows ( a 640 × 480 imaging array ), with a respective lens focusing images onto respective portions of the array . the photosensor array may comprise a plurality of photosensor elements arranged in a photosensor array having rows and columns . the logic and control circuit of the imaging sensor may function in any known manner , such as in the manner described in u . s . pat . nos . 5 , 550 , 677 ; 5 , 877 , 897 ; 6 , 498 , 620 ; 5 , 670 , 935 ; 5 , 796 , 094 and / or 6 , 396 , 397 , and / or u . s . provisional applications , ser . no . 61 / 615 , 410 , filed mar . 26 , 2012 ; ser . no . 61 / 613 , 651 , filed 2012 ; ser . no . 61 / 607 , 229 , filed mar . 6 , 2012 ; ser . no . 61 / 605 , 409 , filed mar . 1 , 2012 ; ser . no . 61 / 602 , 878 , filed feb . 24 , 2012 ; ser . no . 61 / 602 , 876 , filed feb . 24 , 2012 ; ser . no . 61 / 600 , 205 , filed feb . 17 , 2012 ; ser . no . 61 / 588 , 833 , filed jan . 20 , 2012 ; ser . no . 61 / 583 , 381 , filed jan . 5 , 2012 ; ser . no . 61 / 579 , 682 , filed dec . 23 , 2011 ; ser . no . 61 / 570 , 017 , filed dec . 13 , 2011 ; ser . no . 61 / 568 , 791 , filed dec . 9 , 2011 ; ser . no . 61 / 567 , 446 , filed dec . 6 , 2011 ; ser . no . 61 / 559 , 970 , filed nov . 15 , 2011 ; ser . no . 61 / 552 , 167 , filed oct . 27 , 2011 ; ser . no . 61 / 540 , 256 , filed sep . 28 , 2011 ; ser . no . 61 / 513 , 745 , filed aug . 1 , 2011 ; ser . no . 61 / 511 , 738 , filed jul . 26 , 2011 ; and / or ser . no . 61 / 503 , 098 , filed jun . 30 , 2011 , which are all hereby incorporated herein by reference in their entireties . the system may communicate with other communication systems via any suitable means , such as by utilizing aspects of the systems described in pct application no . pct / us10 / 038477 , filed jun . 14 , 2010 , and / or u . s . patent application ser . no . 13 / 202 , 005 , filed aug . 17 , 2011 , now u . s . pat . no . 9 , 126 , 525 , and / or u . s . provisional applications , ser . no . 61 / 567 , 150 , filed dec . 6 , 2011 ; ser . no . 61 / 565 , 713 , filed dec . 1 , 2011 ; and / or ser . no . 61 / 537 , 279 , filed sep . 21 , 2011 , which are hereby incorporated herein by reference in their entireties . the imaging device and control and image processor and any associated illumination source , if applicable , may comprise any suitable components , and may utilize aspects of the cameras and vision systems described in u . s . pat . nos . 5 , 550 , 677 ; 5 , 877 , 897 ; 6 , 498 , 620 ; 5 , 670 , 935 ; 5 , 796 , 094 ; 6 , 396 , 397 ; 6 , 806 , 452 ; 6 , 690 , 268 ; 7 , 005 , 974 ; 7 , 937 , 667 ; 7 , 123 , 168 ; 7 , 004 , 606 ; 6 , 946 , 978 ; 7 , 038 , 577 ; 6 , 353 , 392 ; 6 , 320 , 176 ; 6 , 313 , 454 and 6 , 824 , 281 , and / or international publication no . wo 2010 / 099416 , published sep . 2 , 2010 , and / or pct application no . pct / us10 / 47256 , filed aug . 31 , 2010 , and / or u . s . patent application ser . no . 12 / 508 , 840 , filed jul . 24 , 2009 , and published jan . 28 , 2010 as u . s . pat . publication no . us 2010 - 0020170 ; and / or u . s . provisional applications , ser . no . 61 / 511 , 738 , filed jul . 26 , 2011 ; and / or ser . no . 61 / 503 , 098 , filed jun . 30 , 2011 , which are all hereby incorporated herein by reference in their entireties . the camera or cameras may comprise any suitable cameras or imaging sensors or camera modules , and may utilize aspects of the cameras or sensors described in u . s . patent application ser . no . 12 / 091 , 359 , filed apr . 24 , 2008 ; and / or ser . no . 13 / 260 , 400 , filed sep . 26 , 2011 , and / or u . s . pat . nos . 7 , 965 , 336 and / or 7 , 480 , 149 , which are hereby incorporated herein by reference in their entireties . the imaging array sensor may comprise any suitable sensor , and may utilize various imaging sensors or imaging array sensors or cameras or the like , such as a cmos imaging array sensor , a ccd sensor or other sensors or the like , such as the types described in u . s . pat . nos . 5 , 550 , 677 ; 5 , 670 , 935 ; 5 , 760 , 962 ; 5 , 715 , 093 ; 5 , 877 , 897 ; 6 , 922 , 292 ; 6 , 757 , 109 ; 6 , 717 , 610 ; 6 , 590 , 719 ; 6 , 201 , 642 ; 6 , 498 , 620 ; 5 , 796 , 094 ; 6 , 097 , 023 ; 6 , 320 , 176 ; 6 , 559 , 435 ; 6 , 831 , 261 ; 6 , 806 , 452 ; 6 , 396 , 397 ; 6 , 822 , 563 ; 6 , 946 , 978 ; 7 , 339 , 149 ; 7 , 038 , 577 ; 7 , 004 , 606 and / or 7 , 720 , 580 , and / or u . s . patent application ser . no . 10 / 534 , 632 , filed may 11 , 2005 , now u . s . pat . no . 7 , 965 , 336 ; and / or pct application no . pct / us2008 / 076022 , filed sep . 11 , 2008 and published mar . 19 , 2009 as international publication no . wo / 2009 / 036176 , and / or pct application no . pct / us2008 / 078700 , filed oct . 3 , 2008 and published apr . 9 , 2009 as international publication no . wo / 2009 / 046268 , which are all hereby incorporated herein by reference in their entireties . the camera module and circuit chip or board and imaging sensor may be implemented and operated in connection with various vehicular vision - based systems , and / or may be operable utilizing the principles of such other vehicular systems , such as a vehicle headlamp control system , such as the type disclosed in u . s . pat . nos . 5 , 796 , 094 ; 6 , 097 , 023 ; 6 , 320 , 176 ; 6 , 559 , 435 ; 6 , 831 , 261 ; 7 , 004 , 606 ; 7 , 339 , 149 and / or 7 , 526 , 103 , which are all hereby incorporated herein by reference in their entireties , a rain sensor , such as the types disclosed in commonly assigned u . s . pat . nos . 6 , 353 , 392 ; 6 , 313 , 454 ; 6 , 320 , 176 and / or 7 , 480 , 149 , which are hereby incorporated herein by reference in their entireties , a vehicle vision system , such as a forwardly , sidewardly or rearwardly directed vehicle vision system utilizing principles disclosed in u . s . pat . nos . 5 , 550 , 677 ; 5 , 670 , 935 ; 5 , 760 , 962 ; 5 , 877 , 897 ; 5 , 949 , 331 ; 6 , 222 , 447 ; 6 , 302 , 545 ; 6 , 396 , 397 ; 6 , 498 , 620 ; 6 , 523 , 964 ; 6 , 611 , 202 ; 6 , 201 , 642 ; 6 , 690 , 268 ; 6 , 717 , 610 ; 6 , 757 , 109 ; 6 , 802 , 617 ; 6 , 806 , 452 ; 6 , 822 , 563 ; 6 , 891 , 563 ; 6 , 946 , 978 and / or 7 , 859 , 565 , which are all hereby incorporated herein by reference in their entireties , a trailer hitching aid or tow check system , such as the type disclosed in u . s . pat . no . 7 , 005 , 974 , which is hereby incorporated herein by reference in its entirety , a reverse or sideward imaging system , such as for a lane change assistance system or lane departure warning system or for a blind spot or object detection system , such as imaging or detection systems of the types disclosed in u . s . pat . nos . 7 , 720 , 580 ; 7 , 038 , 577 ; 5 , 929 , 786 and / or 5 , 786 , 772 , and / or u . s . patent application ser . no . 11 / 239 , 980 , filed sep . 30 , 2005 , now u . s . pat . no . 7 , 881 , 496 , and / or u . s . provisional applications , ser . no . 60 / 628 , 709 , filed nov . 17 , 2004 ; ser . no . 60 / 614 , 644 , filed sep . 30 , 2004 ; ser . no . 60 / 618 , 686 , filed oct . 14 , 2004 ; ser . no . 60 / 638 , 687 , filed dec . 23 , 2004 , which are hereby incorporated herein by reference in their entireties , a video device for internal cabin surveillance and / or video telephone function , such as disclosed in u . s . pat . nos . 5 , 760 , 962 ; 5 , 877 , 897 ; 6 , 690 , 268 and / or 7 , 370 , 983 , and / or u . s . patent application ser . no . 10 / 538 , 724 , filed jun . 13 , 2005 and published mar . 9 , 2006 as u . s . publication no . us - 2006 - 0050018 - a1 , which are hereby incorporated herein by reference in their entireties , a traffic sign recognition system , a system for determining a distance to a leading or trailing vehicle or object , such as a system utilizing the principles disclosed in u . s . pat . nos . 6 , 396 , 397 and / or 7 , 123 , 168 , which are hereby incorporated herein by reference in their entireties , and / or the like . optionally , the circuit board or chip may include circuitry for the imaging array sensor and or other electronic accessories or features , such as by utilizing compass - on - a - chip or ec driver - on - a - chip technology and aspects such as described in u . s . pat . no . 7 , 255 , 451 and / or u . s . pat . no . 7 , 480 , 149 ; and / or u . s . patent application ser . no . 11 / 226 , 628 , filed sep . 14 , 2005 and published mar . 23 , 2006 as u . s . publication no . us - 2006 - 0061008 , and / or ser . no . 12 / 578 , 732 , filed oct . 14 , 2009 and published apr . 22 , 2010 as u . s . publication no . us - 2010 - 0097469 , which are hereby incorporated herein by reference in their entireties . optionally , the vision system may include a display for displaying images captured by one or more of the imaging sensors for viewing by the driver of the vehicle while the driver is normally operating the vehicle . optionally , for example , the vision system may include a video display device disposed at or in the interior rearview mirror assembly of the vehicle , such as by utilizing aspects of the video mirror display systems described in u . s . pat . no . 6 , 690 , 268 and / or u . s . patent application ser . no . 13 / 333 , 337 , filed dec . 21 , 2011 , now u . s . pat . no . 9 , 264 , 672 , which are hereby incorporated herein by reference in their entireties . the video mirror display may comprise any suitable devices and systems and optionally may utilize aspects of the compass display systems described in u . s . pat . nos . 7 , 370 , 983 ; 7 , 329 , 013 ; 7 , 308 , 341 ; 7 , 289 , 037 ; 7 , 249 , 860 ; 7 , 004 , 593 ; 4 , 546 , 551 ; 5 , 699 , 044 ; 4 , 953 , 305 ; 5 , 576 , 687 ; 5 , 632 , 092 ; 5 , 677 , 851 ; 5 , 708 , 410 ; 5 , 737 , 226 ; 5 , 802 , 727 ; 5 , 878 , 370 ; 6 , 087 , 953 ; 6 , 173 , 508 ; 6 , 222 , 460 ; 6 , 513 , 252 and / or 6 , 642 , 851 , and / or european patent application , published oct . 11 , 2000 under publication no . ep 0 1043566 , and / or u . s . patent application ser . no . 11 / 226 , 628 , filed sep . 14 , 2005 and published mar . 23 , 2006 as u . s . publication no . us - 2006 - 0061008 , which are all hereby incorporated herein by reference in their entireties . optionally , the video mirror display screen or device may be operable to display images captured by a rearward viewing camera of the vehicle during a reversing maneuver of the vehicle ( such as responsive to the vehicle gear actuator being placed in a reverse gear position or the like ) to assist the driver in backing up the vehicle , and optionally may be operable to display the compass heading or directional heading character or icon when the vehicle is not undertaking a reversing maneuver , such as when the vehicle is being driven in a forward direction along a road ( such as by utilizing aspects of the display system described in pct application no . pct / us2011 / 056295 , filed oct . 14 , 2011 and published apr . 19 , 2012 as international publication no . wo 2012 / 051500 , which is hereby incorporated herein by reference in its entirety ). optionally , the vision system ( utilizing a forward and / or rearward facing camera and other cameras disposed at the vehicle with exterior fields of view ) and / or the camera or cameras as part of a vehicle vision system comprising or utilizing a plurality of cameras ( such as utilizing a rearward facing camera and sidewardly facing cameras and a forwardly facing camera disposed at the vehicle ), may provide a display of a top - down view or birds - eye view of the vehicle or a surround view at the vehicle , such as by utilizing aspects of the vision systems described in pct application no . pct / us10 / 25545 , filed feb . 26 , 2010 and published on sep . 2 , 2010 as international publication no . wo 2010 / 099416 , and / or pct application no . pct / us10 / 47256 , filed aug . 31 , 2010 and published mar . 10 , 2011 as international publication no . wo 2011 / 028686 , and / or pct application no . pct / us11 / 62834 , filed dec . 1 , 2011 and published jun . 7 , 2012 as international publication no . wo 2012 - 075250 , and / or u . s . patent application ser . no . 13 / 333 , 337 , filed dec . 21 , 2011 , now u . s . pat . no . 9 , 264 , 672 , and / or u . s . provisional applications , ser . no . 61 / 615 , 410 , filed mar . 26 , 2012 ; ser . no . 61 / 588 , 833 , filed jan . 20 , 2012 ; ser . no . 61 / 570 , 017 , filed dec . 13 , 2011 ; ser . no . 61 / 568 , 791 , filed dec . 9 , 2011 ; ser . no . 61 / 559 , 970 , filed nov . 15 , 2011 ; ser . no . 61 / 540 , 256 , filed sep . 28 , 2011 , which are hereby incorporated herein by reference in their entireties . optionally , the video mirror display may be disposed rearward of and behind the reflective element assembly and may comprise a display such as the types disclosed in u . s . pat . nos . 5 , 530 , 240 ; 6 , 329 , 925 ; 7 , 855 , 755 ; 7 , 626 , 749 ; 7 , 581 , 859 ; 7 , 446 , 650 ; 7 , 370 , 983 ; 7 , 338 , 177 ; 7 , 274 , 501 ; 7 , 255 , 451 ; 7 , 195 , 381 ; 7 , 184 , 190 ; 5 , 668 , 663 ; 5 , 724 , 187 and / or 6 , 690 , 268 , and / or in u . s . patent application ser . no . 12 / 091 , 525 , filed apr . 25 , 2008 , now u . s . pat . no . 7 , 855 , 755 ; ser . no . 11 / 226 , 628 , filed sep . 14 , 2005 and published mar . 23 , 2006 as u . s . publication no . us - 2006 - 0061008 ; and / or ser . no . 10 / 538 , 724 , filed jun . 13 , 2005 and published mar . 9 , 2006 as u . s . publication no . us - 2006 - 0050018 , which are all hereby incorporated herein by reference in their entireties . the display is viewable through the reflective element when the display is activated to display information . the display element may be any type of display element , such as a vacuum fluorescent ( vf ) display element , a light emitting diode ( led ) display element , such as an organic light emitting diode ( oled ) or an inorganic light emitting diode , an electroluminescent ( el ) display element , a liquid crystal display ( lcd ) element , a video screen display element or backlit thin film transistor ( tft ) display element or the like , and may be operable to display various information ( as discrete characters , icons or the like , or in a multi - pixel manner ) to the driver of the vehicle , such as passenger side inflatable restraint ( psir ) information , tire pressure status , and / or the like . the mirror assembly and / or display may utilize aspects described in u . s . pat . nos . 7 , 184 , 190 ; 7 , 255 , 451 ; 7 , 446 , 924 and / or 7 , 338 , 177 , which are all hereby incorporated herein by reference in their entireties . the thicknesses and materials of the coatings on the substrates of the reflective element may be selected to provide a desired color or tint to the mirror reflective element , such as a blue colored reflector , such as is known in the art and such as described in u . s . pat . nos . 5 , 910 , 854 ; 6 , 420 , 036 and / or 7 , 274 , 501 , which are hereby incorporated herein by reference in their entireties . optionally , the display or displays and any associated user inputs may be associated with various accessories or systems , such as , for example , a tire pressure monitoring system or a passenger air bag status or a garage door opening system or a telematics system or any other accessory or system of the mirror assembly or of the vehicle or of an accessory module or console of the vehicle , such as an accessory module or console of the types described in u . s . pat . nos . 7 , 289 , 037 ; 6 , 877 , 888 ; 6 , 824 , 281 ; 6 , 690 , 268 ; 6 , 672 , 744 ; 6 , 386 , 742 and 6 , 124 , 886 , and / or u . s . patent application ser . no . 10 / 538 , 724 , filed jun . 13 , 2005 and published mar . 9 , 2006 as u . s . publication no . us - 2006 - 0050018 , which are hereby incorporated herein by reference in their entireties . changes and modifications to the specifically described embodiments may be carried out without departing from the principles of the present invention , which is intended to be limited only by the scope of the appended claims as interpreted according to the principles of patent law . | 1 |
embodiments of the invention will now be described , by way of example , not limitation . it is to be understood that the invention is of broad utility and may be used in many different contexts . the example of a search process as described herein below can be modelled by a searcher presenting to a search system a query and receiving a response ( search results ) indicating the one or more “ hits ” found . a query can be in the form of a search query string comprising one or more tokens delimited by delimiters or parsing rules . in addition to varying a search based on variations of the search query string , context might be also taken into account . for example , the querier might have previously set constraints on the search , such as to return only age - appropriate hits , prior searches might be taken into account , and a querier identity ( such as the yahoo ! id currently associated with the web browser client submitting the search query string ) and settings set by the user . other contexts might be the time of day , the computer being used , the location of the computer ( e . g ., ip address , physical location , etc .). the response need not be limited to search results . for example , a searcher might transmit a query and receive a web page in response that includes sponsored search results , search results independent of sponsorship , directory listings , alternative corpus search results , advertisements , links and possibly other elements . one or more of such elements might be dependent on the query and / or search results , but some elements might be independent of the query and search results . for example , a searcher might enter a query string q and receive in response a web page containing some hits corresponding to q from one search database , hits corresponding to q from another search database , presentations corresponding to q , advertising corresponding to q , advertising that is independent of q , page elements that are independent of q ( such as a greeting specific to the user , page elements that always appear on each results page , etc .). when a query is received by a search system , the search system processes the search and returns one or more “ hits ”, where a “ hit ” is the atomic unit handled by the search system . likewise , a presentation system processes the search and returns one or more hits . the search system and presentation system can be the same system , different systems , distinct instances of similar systems using different corpuses , etc . for example , a querying system might include a search system that takes in a query and returns a set of hits that correspond to elements in a search corpus deemed to satisfy the query based on content of the query and those elements , and the querying system might also include a presentation system that takes in a query and returns a set of hits that correspond to presentations selected from a set of presentations ( such as a presentations database ) that are selected based on some presentation criteria or rules . one example of presentation criteria would have the presentations associated with elements of the query , possibly independent of the content of the presentation , such that a presentation is likely to be returned as part of the response when the query contains a particular term . the search system corpus can be free - form text , files , database records , web pages , data object or the like . where the search corpus is a structured database , the hits are records from the structured database . where the search system manages documents , such as text documents , image and text documents , image documents , html documents , pdf documents , or the like , the hits are documents . it should be understood that the present invention is not limited to any particular atomic unit , but by way of example , much of this disclosure describes searching using the document as the atomic unit . in general terms , a query is sent to a query system , which applies the query and / or other contexts to one or more systems and receives responses of one or more hits ( or no hits , in some cases ), back from those systems and supplies that collection of responses ( or less than all of the responses if too many responses are provided ) to the querier as a response to the query . in some cases , the returned hits are a function of the content of those hits , but in other cases the returned hits might be independent of the content of those hits . as an example of the latter , advertisements might be returned because the system rules are that a particular advertisement is to be returned in response to particular query terms even if the advertisement does not contain the query term . of course , with targeted advertising , an advertiser will generally want to limit the presentation of a particular advertisement to users that have an interest in what is being advertised and that is often determined from the user &# 39 ; s intent for a search as evidenced by the query string presented . it should be understood that the search system need not provide all hits or only hits that match the query and that a presentation system need not provide all hits that match presentation rules . for example , the search system might limit the number of hits returned to some number , might apply other limitations to the query term , such as omitting hits that match the query , ignore duplicate hits , etc . the search system might also expand the search results to include hits that almost match the query , hits that are designated to be included in searches , such as special topic hits , advertising hits , etc . some expansion or contraction might be dependent on the size or content of the search results prior to such expansion or contraction . for example , the search engine might add hits that are close if no hits would otherwise be returned and might remove hits if too many hits would have been returned , such as by deleting common words from queries prior to completing the search results . a searcher can be a human user , such as a person typing in search terms into a browser window to query a search engine via the web , but can also be an automated process , such as a computer program capable of sending queries to search engines in the form expected by the search engine . for example , a computer program might generate queries and form http messages directed at a web server coupled to a search engine . in many of the examples shown herein , the search engine searches among a set of documents ( a corpus ) for hits that match the criteria defined by the query . it should be understood that the term “ document ” is generally used to refer to units of the corpus being searched . a document can be a document , such as a contract , a file , a story , a writing , or the like , but might also be a snippet of text , data that might be considered part of a document in other contexts , program code , image data , a stored file , or the like . therefore , the term need not be narrowly construed . referring now to the figures and using the above definitions , an exemplary search and presentation system will now be described . fig1 is a block diagram of a query system 100 according to embodiments of the present invention . using query system 100 , a querier issues a search request to a search server using a search client , such as a web browser client . as shown in fig1 , a human user 103 or a computer process 105 issues a query using search client 110 . the search query , typically in the form of a search query string , is sent to a search server 120 , which returns search results responsive to the search query to search client 110 along with zero or more presentations . in other variations , the search query and / or presentation come from one system and the results are routed to another system . search server 120 is shown coupled to a search engine 130 and a presentation server 132 , which is in turn coupled to a presentation details database ( pdd ) and a presentation manager 136 . the interconnections between various systems need not be described in detail , as such methods of interconnections can be accomplished using well - known techniques . search client 110 might be a personal computer running an http client , such as a web browser client , and communicating with an http server running at search server 120 , interconnected over a network such as the global internet . it should be understood that other embodiments also fall within the scope of the invention . for example , search client 110 might be implemented as a handheld device , a computer with no human user interface , a dedicated device , a kiosk , etc . also , the clients and servers need not use http , but might use a different protocol for making requests for pages and objects , for responding to those requests and for combining search results with other presentations . in operation , and as described in further detail below , search client 110 sends a search query string to search server 120 , possibly also including context data ( other query state ) such as a yahoo ! id of the yahoo ! user sending the request , location of the search client , etc . presentation server 132 might also use the context data to determine which presentations to return . fig2 illustrates elements of a search server in greater detail . as shown there , the search server includes a page constructor 200 , and storage for search results 210 , matching ads 212 , matching inserts 214 , sponsored links 216 and a query log 220 . from a received query , the search server obtains search results 210 , either by performing a search itself or by requesting results from another search engine . typically , a search is performed using an index to the corpus being searched , such as a keyword index . in that case , the search results 210 are the hits that are generated based on the index . elements 212 , 214 and 216 are , in this example , presentations returned by a presentation server . other page elements , such as globally used or static presentations might also be involved . page constructor 200 then generates a page from elements in storage 210 - 216 and sends the page as a response to the search query . a query log might be maintained of queries made and the results , as well as some indication of subsequent selections that the user makes from the results . for example , if a user issues a query q , receives a set of results r , and selects a link s associated with one of the results in the set of results r , the association of q with s can be stored in a query log . an example of a page 300 constructed by page constructor 200 is shown in fig3 . in this example , the search string was “ camera ”. page 300 includes information organized into different page layout areas 302 , 304 , 306 , 308 , 310 , 312 and 314 . the top of page 300 includes an indication of the search , a dialog box in which another search can be initiated , and clickable links for help , home page , etc . simple search results , such as search results from a web index for “ camera ”, are listed in layout area 308 . in this example , upon a search query using the query string “ camera ”, the search server populates storage 210 with web search results , and possibly other results . the presentation server , in response to the particular terms of the query string ( and possibly other state ), generates advertisements , inserts and sponsored links associated with the search terms . layout area 308 includes links that represent hits responsive to the search term and are preferably independent of who sponsors links . layout area 310 is provided for insertion of an advertisement determined by the presentation server . it should be understood that presentations are not limited to advertisements . in some cases , public interest announcements might be used as presentations . for example , if a user enters a search query “ skiing mountaintop resort tickets ” and there is currently an emergency alert for that resort , a weather advisory might be presented upon a match to those search terms . while non - advertisements such as those might be used as presentations , many of the examples herein will use advertisements as the type of presentation being selected and presented . layout area 312 and 214 provide additional matching inserts returned by the presentation server or are generated by the search server . in this example , layout area 312 contains links for executing alternative searches and layout area 314 contains links for other searches . while it is more typically the case that an advertiser pays for a keyword in layout area 310 ( e . g ., the advertiser gets its advertisement presented in layout area 314 in search results pages resulting from searches that use the keywords that the advertiser paid for ), an advertiser might also or instead pay for the right to have presented their message in other layout areas . for example , an interested search service might pay to be the alternative in layout area 314 for some search terms . this might be useful where the interested search service is topic - specific and the terms used are also topic - specific . thus , if a chemical compounds search system provides detailed searches into its chemical compounds database of interest to only a few searchers using search server 120 , then searches that use terms that would likely only be used by someone in that narrow field might result in a results page wherein the narrow interest search engine is presented in layout area 314 . layout area 302 displays matching inserts 214 . in this example , those matching inserts are “ inside yahoo !” links that relate to the search term . layout area 304 displays directory matches , which are matches from the yahoo ! directory , a hierarchical arrangement of topics and links associated with those topics at various levels in the hierarchy . layout area 306 displays sponsored matches , which are hits provided to the user based on sponsorship of particular keywords . fig4 illustrates aspects of the invention wherein search terms are canonicalized before being presented to a presentation processor . as shown there , a search server 400 comprises , among other elements not shown , a search processor 402 that couples to a search engine 404 , a presentation processor 406 that couples to a presentation server 408 , a canonicalizer 410 and rule bases 412 that are interfaced with plug - ins of canonicalizer 410 . other connections exist , but are not shown , such as connections to components that receive the presentations to be presented and the search results . canonicalizer 410 takes in a query string and outputs a reformed query string , wherein terms from the query string are replaced with their canonical forms . of course , for some query strings , if none of the terms of the query string met a canonicalization criteria , the reformed query string would be identical to the input query string . with canonicalization , distinct terms that convey identical user intent , or nearly identical user intent , can be matched such that identical or nearly identical user intent results in a common reformed query string , thereby simplifying and / or improving search results . in preferred embodiments , the input to a presentation processor is the same for different search strings that canonicalize to the same base canonicalization . canonicalization also allows for improved keyword - based presentation selection , so that one presentation that is to be shown when a searcher indicates a particular intent can be shown over distinct searches . for example , suppose a presentation p is targeted to searchers that intend to search for telephone calling rates . presentation p might be associated in a presentation database with the keywords “ telephone call rate ”. with canonicalization , “ phone ” is reformed to its canonical form “ telephone ” ( one word usage to another ), “ calling ” to its canonical form “ call ” ( suffix removal ) and “ rates ” to its canonical form “ rate ” ( plurals to singular ), and spelling errors can also be eliminated using canonical forms . thus , the query string “ fone calling rates ” would be reformed to “ telephone call rate ” and would result in presentation p being presented , regardless of the fact that none of the original query terms are directly associated with presentation p . matching is a process of checking two or more search phrases , words or portions of search phrases to determine if they canonically represent the same input despite being different strings . two approaches to matching might be done . in one approach , inputs are converted before any operations ( storing , filtering , forwarding , etc .) into a base canonical form . in that approach , matching is done by checking for an exact match between the canonical forms . in another approach , inputs are represented in their original form , but when two or more inputs are compared , they pass through a canonicalizer and the outputs of the canonicalizer are tested to find identity . a parallel canonicalization process might be done for search results , as well as for presentation decisions , but it might also not be done , or a different canonicalization process used . thus , the query might be canonicalized to one reformed search query string for application to a search engine and canonicalized to another reformed search query string for application to a presentation search engine . examples of canonicalization are described herein , but it should be understood that the invention is not limited to using just these canonicalizations or using all of these canonicalizations . these canonicalizations can be included or excluded on the fly through the use of plug - ins to a canonicalizer . each plug - in might have a rule base to indicate the rules for when two distinct words or strings are canonically equal . alternatively , the plug - ins might provide the canonical form for an input string . in that case , the equivalence of two distinct words or phrases can be determined by passing both through the canonicalizer and checking whether the canonical forms for both inputs are equal . examples of canonicalizations ( the underlying rules define what is canonical ) are shown in table 1 . search history canonicalization uses a history of user search patterns ( such as a log of millions of queries performed using yahoo ! search engines ) to identify patterns , such as common acronyms ( lol and “ laugh out loud ”), common spelling mistakes , and compound words such as “ online shopping ” and “ on line shopping ”). search results canonicalization is based on common search results being selected when shown in response to distinct queries . a decision as to when to canonicalize might be based on query logs , possibly including at least partial clickstreams . for example , suppose one large set of users searches using search string a and receives hits h 1 , h 2 , h 3 in response , while another large set of users searches using search string b and receives hits h 4 , h 5 , h 6 in response and there is some overlap of the set of hits between the two results . if it turns out that many users in both sets are selecting a common hit from the search results even though they received that hit using different search strings , then those two search strings might be flagged as being of the same base canonical form . thus , if the web page for “ northern europe pedalling tour guides ” shows up in search results for the search string “ danish biking ” and in search results for the search string “ scandinavian bicycling ” and searchers for both search strings frequently select the “ northern europe pedalling tour guides ” web page from either search string , the phrases “ danish biking ” and “ scandinavian bicycling ” might be canonicalized such that they reduce to the same base canonicalization . of course , for this example , using just word - based or term - based canonicalization , “ danish ” and “ scandinavian ” might canonicalize together and “ biking ” and “ bicycling ” might canonicalize together , yielding the same results anyway . canonicalizations can be applied in varying order or always in the same order for possibly greater consistency . canonicalizations might also have exceptions and customizations , which can be handled in the same way as other canonicalizations . for example , exceptions might be that “ colour ” can be canonical with “ color ” and “ telephone ” can be canonical with “ phone ”. exceptions or custom rules can be made to be applied exclusively without any other rules . this exception handling mechanism allows , for example , a product manager or producer to create a custom canonicalization , for example , for a different language . in addition to word - based canonicalization , term - based canonicalization can also be performed . these two can be used to gather and even recursively . for example , word - based canonicalization might canonicalize “ united states of america air force ” to “ united state of america air force ”, then term - based canonicalization might canonicalize it to “ usa air force ”, then “ usa af ” and then term - based canonicalization might further canonicalize the phrase to “ usaf ”. the rules and dictionaries , as needed , can be stored in an efficient data structure . a computer implementation for storing the rules and dictionaries for use by a web server or any number of web servers , or for use with any number of computer processes to share , can be used to achieve a highly scalable architecture , which can grow with traffic increases without requiring software and data redesign . one process for generating a dictionary is described here . in this example , a set of nouns are collected , such as from a standard dictionary file . a standard dictionary file is likely to have considerable “ noise ”, so some refinement should be done . first , compound words are be removed from the dictionary . then , an inflection process is used to convert singular nouns from the set of nouns to plural nouns . an invert mapping of the inflection process is done to convert plural nouns to singular nouns and check for cyclic mappings , wherein the output of the inverted mapping step is compared to the singular nouns input to the inflection process . singular nouns that do not pass the cyclic mapping check can be flagged , removed or processed specially . nouns that do not have corresponding plurals in the set of nouns are then removed ( e . g . actinomeris , baccharis , qatari , etc .). some plural forms can be mapped to multiple singular forms ( e . g ., bases -& gt ; basis or base ), so multiples are removed . many short nouns are abbreviations and their plural forms are real words with completely different meanings ( e . g ., wa is an abbreviation for washington state , and the apparent plural “ was ” is an unrelated word ). some singular forms are themselves plural forms , which have their singular forms ( e . g ., algaes -& gt ; algae -& gt ; alga ), so the various transitive mappings should be consolidated into one ( e . g ., algaes -& gt ; alga ). other types of conversions might also be included , such as changing dialects ( e . g ., british english “ colour ” to american english “ color ”, or vice versa ), popular short forms (“ telephone ” to “ phone ”) and singular nouns that have multiple plural forms (“ antennae ” and “ antennas ” are both plural forms of “ antenna ”). fig5 illustrates a presentation manager 500 that might be used to populate a pdd 506 and arbitrate bids from competing advertisers or other presenters for keyword allocation . in one aspect of the present invention , keyword and phrase canonicalization that occurs in canonicalizer 410 ( fig4 ) also occurs in a canonicalizer within the presentation manager . a prospective presenter might interact with presentation manager 500 using a presenter system 502 . in some implementations , the interaction is performed by a sales agent for the operator of the search and presentation system , but in other implementations , the bidding process can be “ self - serve ”, wherein prospective presenters interact directly with presentation manager 500 to select keywords and other criteria for a presentation campaign , identify which keywords are available and unavailable and under what conditions , pay for the presentation services , and provide the presentation or a reference to the presentation . once a bid is finalized , a closed bid 504 is stored in pdd 506 , providing the presentation server access to the particular campaign details . an example of a closed bid 510 is shown . the elements shown are a keyword , alternates , the winning bidder &# 39 ; s id , a campaign date range , and a pointer to a desired presentation . of course , bids might have fewer fields or more fields than shown . it is not necessary for closed bid 504 to contain payment details , if presentation manager 500 handles those details . in an example of usage of the system shown in fig5 , suppose a presenter decides to submit bids for a sponsored link to the presenter &# 39 ; s car dealership . the presenter might decide the present each time someone searches for “ car dealers ”. since the user intent is arguably the same for a search for “ car dealer ” and “ car dealers ”, the same presentation might be shown to each . rather than require the bidder to bid on each variation , the bidder can bid on the canonical form , or any variation that maps to a canonical form . if the canonical forms are determined on the fly , then the bidder has the advantage that later developed variations ( such as unexpected misspellings ) would also be include in the bid . the presenter might pick a date range for the campaign , a number of hits , number of clicks , or other limitation on the exposure . if that does not overlap with already promised and closed bids , it can be granted to the presenter . as part of the process , the presenter provides the presentation or a reference to a presentation . for example , the presenter might provide a banner advertisement image and associated click - through links , which could then be stored in pdd 506 . alternatively , the presenter might just provide a url that points to a server managed by the presenter , thus allowing the presenter to more closely monitor the number of presentations that are occurring . this self - service aspect of the presentation manager allows individual presenters to “ browse ” available campaigns and to choose among the available slots without requiring an intermediate sales step . however , in some cases , such as for complex campaigns and new users , a sales agent might intermediate to ensure that the presenter is able to get the most satisfactory campaign . some campaigns might be quite complex , such as a campaign to have a minimum of 10 , 000 page views on search results where “ car dealer ” or any of its variations that would canonicalize to “ car dealer ” appears in a search query between 8 am and 5 pm on a business day for searches within the yahoo ! business property , nonexclusive to other presenters using that same keyword , and exclusive of other presenters using that same keyword within the yahoo ! yellow pages property on weekends . canonicalization has a number of benefits . it allows a presenter to reach an intended target audience even if members of the audience enter variations of the purchased keyword . it also allows a presenter to preclude others from bidding and winning on variations of the presenter &# 39 ; s trademarks without the presenter having to separately bid on all the possible variations of the trademark . another advantage is that a presenter would not have to guess ahead of time which of several valid variations might be used the most . canonicalization of search phrases either increases the relevant information found or reduces the complexity of finding relevant information for users . in the ever - increasing web space , this process has become more and more critical . presentation manager 500 canonicalizes the bids , so that the presenter winning the bid for “ car dealers ” also gets to present for searches on “ car dealer ” ( singular vs . plural ), “ car , dealer ” ( punctuation canonicalization ) and “ car deeler ” ( spelling canonicalization ). fig6 shows a networked system in which a plurality of search clients can access a search system to apply queries to a corpus of documents . in this system , one or more ( but possibly thousands or more ) client systems 902 make requests via the internet 904 . the requests flow to servers 908 via an http server 906 , but it should be understood that multiple http servers might be present and other protocols might be used instead of , or in addition to , http . a server 908 sends the query to a query process 910 , which might be an instantiation of a software object in server 908 or elsewhere , or might include hardware components . the query processes 910 then parse the search query strings and obtain documents , references to documents , links , or other indications of hits , from one or more corpuses 912 . in generating results , query processes 910 might send their query terms to a presentation server that will return presentations to be included with the search results , such as advertisements , alerts , messages , notices , links and the like . in some embodiments , corpuses 912 are complete copies of the entire corpus , but in other embodiments , the corpuses 912 are subsets of the complete corpus . in the latter case , server 908 or server process 910 can determine , from the query and possibly other information , which corpus to use . note that in some cases , one query process 910 might access more than one corpus 912 , even for a single query . in fig6 , multiple instances of objects are differentiated by a parenthetical index , such as 902 ( 1 ) for a specific instance of a client system 902 . for various objects , the terminal index is some unspecified number , such as “ 602 ( n 1 )”. where the number of objects is not required to be the same , the terminal indices are indicated with distinct variables . thus , while exactly three servers 980 and three corpuses 912 are shown in fig6 , there are n 2 ( an indeterminate number ) servers and n 6 ( another indeterminate number ) corpuses 912 implied by fig6 , so a one - to - one correspondence of servers to corpuses is not required . unless otherwise specified , different terminal indices can have the same or different values ranging from one to numbers larger than one . the invention has now been described with reference to the preferred embodiments . alternatives and substitutions will now be apparent to persons of skill in the art . accordingly , it is not intended to limit the invention except as provided by the appended claims . | 8 |
referring to fig1 there is shown a schematic block diagram illustrating the main functionalities of the method and system of the invention . the shown processing system 1 receives an input video signal 6 represented by the components y ′ uv according to the known yuv model for representing a colour image , where the y component represents the luminance ( brightness ) of the individual pixels p of the image and u and v represent the chrominance ( colour ) components , mapping each representable colour into a two - dimensional uv - space . the shown embodiment of the system 1 according to the invention comprises an inference system 2 for carrying out the histogram and chrominance processing according to the invention . this system 2 provides output variables 9 , 10 , 11 and 12 relating to saturation , brilliance , contrast and gamma that by means of the display controlling system 3 , which also receives the original y ′ uv video signal 6 , provide the final output signal 8 to the display means 4 . according to a specific embodiment of the invention , the inference system ( or specifically the histogram processing means as will be described in detail below ) is furthermore provided with an output signal from an ambient light sensor that senses the intensity ( or other related quantity ) of the ambient light . histogram and chrominance processing can be viewed as an inference system , which affects various parameters via modifications of the incoming video signal . the modification is based on the properties of the incoming video signal and ( according to a specific embodiment of the invention ) an ambient light sensor . the resulting parameters may be based on both global properties ( the entire image field ) and local properties . with reference to fig2 , the inference system 2 consists basically of two consecutive modules 13 and 14 , with the main functionalities described below . the input is typically a component signal i . e . luminance and colour difference signals . this is generally denoted y ′ uv , with y ′ being the luminance component , and u , v the colour difference components . the first module is the histogram processing block 13 , by means of which a luminance transfer function t ( k ) and a chrominance scaling factor or chrominance gain g c 16 is determined . the second module is the chrominance processing block 14 , carrying out selective chroma adjustment ( global chroma adjustment is carried out in block 17 , cf . below ). the original input video signal ( y ′ uv ) in 6 results by the processing carried out in the modules 13 and 14 in the output signal ( y ′ uv ) out1 15 that after scaling of the chrominance components u and v by the chrominance gain g c as shown in the functional block 17 results in the final output video signal ( y ′ uv ) out2 18 . in the following a detailed description of the processing actually carried out in the functional blocks 13 and 14 will be given in the histogram processing , the black level is set according to a measure of the lowest level present in the image , and a function dependent on the average image level . the transfer function of the histogram processing block 2 is also modulated according to the input 5 of an ambient light sensor . if the ambient light intensity is high , the image dynamics are increased for the low image levels , and vice versa . in addition , the histogram processing block 2 provides a chrominance scaling value , the chrominance gain g c . the chrominance scaling is based on the ratio of a linear transfer function with offset , and the total transfer function derived by the processing . the global chrominance scale value is calculated at the average level of the unprocessed image , using only the black level offset . thus , as the processing is likely to increase / decrease the luminance at the average level , the chroma components are multiplied by the scale value to achieve a similar increase / decrease . this approximately preserves the saturation of the image . with reference to the flow charts shown in fig3 ( a ), ( b ) and ( c ) a more detailed description of the steps carried out in an embodiment of the invention will be given . initially a histogram ( ref , number 19 ) of luminance values of the incoming video signal y ′ uv ( reference number 6 of fig1 and 2 ) is formed . this is done by dividing the total range of the luminance signal into n non - overlapping subranges ( denoted bins ). the bins can have any distribution , and can be of equal size , or the sizes may grow e . g . exponentially . each sample ( or , if the signal is subsampled , less than that ) of the signal then adds to the count of the samples in the respective bin . this produces a histogram of luminance sample values , with an appropriate resolution . the histogram of luminance values of the image field is denoted as : h ( k )= n k , where k denotes the bin number , and n k denotes the number of samples in the field falling within the levels represented by bin k . in the following description ‘ histogram ’ denotes the normalised histogram ( ref . number 20 ): p ( k )= n k / n , where n is the total count of the histogram — i . e . p ( k ) is the percentage of counts that fall within bin k . the normalised histogram 20 is used for calculation of the average luminance level ( ref . number 21 ): where α ( k ) is the average level represented by bin k . the calculated average is used subsequently in the algorithm . the histogram p ( k ) is according to one specific embodiment of the invention in functional block 22 weighted by a power function k α such that : p 1 ( k )= p ( k ) k α , kε { 0 , . . . , n − 1 }, where α is a constant . subsequently p 1 ( k ) is normalised ( ref . number 23 ) such that it should be noted that weighting of the histogram p ( k ) by a power function k α is only one specific example of a weighting function that can be applied in the histogram processing according to the invention . generally the histogram p ( k ) can according to the invention be weighted by a weight function w ( k ) that can exhibit other and possibly more complicated functional relationships with the parameter k ( the bin number ) than the power function described above . the power function weighted luminance histogram is then clipped ( ref . number 24 ) by thresholding each bin at a particular maximum level such that : p 2 ( k )= min [ p 1 ( k ), c ( k )], kε { 0 , . . . , n − 1 } where c ( k ) is a function setting the clipping level for bin k . after these modifications a cumulative histogram is calculated ( ref . number 25 ): a second cumulative luminance histogram ( ref . number 26 ) is also formed from the un - modified histogram : the cumulative luminance histogram p c ( k ) is used ( ref . number 27 ) for detecting the luminance level , for which the cumulative proportion exceeds a small but fixed percentage of the sample counts . the level found from this , denoted bl 1 , is used as an offset for the signal , which by subtraction moves the lowest signal level ( occurring within some time period ) to the lowest valid signal level . additionally the offset is increased in relation to the average luminance of the image . this additional offset , bl 2 , is found ( ref . number 28 ) from a scaled power - function relation : bl 2 = c 1 y avg p where c 1 , β are constants . with reference to block 29 the total offset , bl , is the sum of the two offsets bl 1 , bl 2 , thresholded at a maximum offset b max as : bl = min [ bl 1 + bl 2 , b max ] the total offset value bl is temporally filtered ( ref . number 30 ) by a general finite impulse response filter , typically with a low - pass characteristic to avoid large fluctuations . referring to block 31 of fig3 ( b ) an additional step of the algorithm according to this embodiment of the invention partially establishes the transfer function of the histogram processing block 2 based on the ambient light level 5 . taking as reference an identity mapping : t ( k )= k , which is transformed by the total offset described above such that the transfer function is : t ( k )→ t ( k )= k − bl , the effect of the ambient light level is to transform this by a power function relation using two functions : which are weighted to produce a transfer function by the relation : { circumflex over ( t )} ( k )= τ t 1 ( k )+( 1 − τ ) t 2 ( k ), τε [ 0 , 1 ], kε { 0 , . . . , n − 1 } the parameter τ reflects the ambient light intensity , e . g . by having a linear relation with a particular light intensity range . using a β which does not deviate much from 1 , the relation for { circumflex over ( t )}( k ) can produce an approximately linear transfer function for some particular τ . if the ambient light intensity is high the t 1 ( k ) function will receive the largest weight , and vice versa . this has the effect of increasing the dynamics for the low signal levels at high ambient light intensity , and vice versa . this results in a mapping , which provides a better utilisation of the available dynamic range , in accordance with human contrast sensitivity . referring to block 32 after these transformations a weighted summation of p 3 ( k ) and { circumflex over ( t )}( k ) is formed as : t ( k )= s ( p 3 ( k )+ c 2 { circumflex over ( t )}( k )), where s is a scaling parameter , which normalises t ( k ) to utilise the maximum signal output range . the parameter c 2 controls the relative weighting of the two transfer functions , and thereby the weighting of histogram equalisation versus ambient light adaptation . the transfer function t ( k ) provides the desired input - output mapping . thus , t ( k ) represents the transfer function from the input signal y ′ uv ( reference numeral 6 ) to the output signal of the histogram processing block 13 in fig2 . since the luminance mapping is changed by this transfer function , a global chrominance gain , g c is calculated as : g c = t ( y avg )/ t ( y avg ) as shown in block 33 . thus , if at the average level , the luminance has increased , the chrominance signals will be multiplied by an equal factor and vice versa . the g c value is bounded within an interval of unity gain . if it falls outside this interval , it is set at the interval minimum / maximum . the global chrominance scaling effected by g c is applied after the chrominance processing described below in connection with fig3 ( c ). if the signal range has been quantized to a lower resolution for histogram processing , the resulting transfer function can be scaled to the proper range by using an interpolation method the subsequent chrominance processing 14 according to the invention is described below with reference to fig3 ( c ). the chrominance processing represents a selective chroma adjustment . the processing considers each individual pixel : p =( y p , u p , v p ). the pixel chrominance co - ordinates : p c =( u p , v p ) are used for calculating a local ( i . e . individual for each pixel ) chrominance gain . the chrominance components can be used as indices for e . g . a table 34 containing the gain values . alternatively the gain could be calculated from a mathematical function 35 . regardless of method , a function g ( u p , v p ) provides the local gain value for each individual pixel . the chrominance scaled pixel is then given by : p s =( y ′ p , g ( u p , v p ) u p , g ( u p v p ) v p ), forming the output 15 from the chrominance processing block 14 . referring again to fig2 after application of the global chrominance gain g c , derived by the above luminance histogram processing the output ( y , u , v ) co - ordinates of the pixel become : p s =( y ′ p , g c g ( u p , v p ) u p , g c g ( u p , v p ) v p ). the gain from the chrominance processing , i . e . g ( u p , v p ), will typically be greater than or equal to one , thus maintaining or increasing the saturation of the pixel . an illustrative example of such a gain function , where the gain is represented by the grey tone value , where black indicates unity gain and white indicates a gain value & gt ; 1 , is given in fig4 , where ( u , v )=( 0 , 0 ) is located at the centre . for this gain function , most of the ( u , v ) plane has a homogeneously decreasing gain as a function of ( u , v ) magnitude . a specific region 37 is set at unity gain , having a smooth transition to the surrounding gain values . in the figure , black indicates unity gain , and white indicates the maximum gain value in the table . having the gain dependent on the pixel co - ordinates in this way allows selective processing , such that e . g . pixels within a specific region of the ( u , v ) plane , will be unaltered . this is desirable in e . g . the ( u , v ) region representing typical skin colour . the magnitude of the scaling will in general depend on the magnitude of the ( u , v ) vector , in such a way that small magnitudes will receive a relatively large scaling and vice versa . referring again to fig1 , the four shown parameters : saturation 9 , brilliance 10 , contrast 11 and gamma 12 are related to various of the quantities determined as described above and shown in the flowchart in fig3 . thus , saturation 9 is primarily influenced by the chrominance gain g c which is the direct scaling of the chrominance components u p , v p resulting from the histogram processing . the chrominance processing furthermore influences the chrominance components u p , v p of the individual pixels by multiplication by a constant ( per pixel ) being typically larger than or equal to unity . this furthermore either maintains or increases the saturation 9 . brilliance 10 is primarily influenced by the total off - set bl that improves the black level . contrast 11 is primarily influenced by the quantity p 3 ( k ) being included in the expression t ( k )= s ( p 3 ( k )+ c 2 { circumflex over ( t )}( k )) in that utilisation of p 3 ( k ) alone would have provided approximate histogram equalisation . this would , however , lead to a rather drastic effect on the image , which is according to this embodiment of the invention counteracted by using the two transfer functions in the expression for t ( k ). the parameter gamma 12 is directly influenced by the second term in the above expression , i . e . c 2 { circumflex over ( t )}( k ), i . e . the transfer function formed based on the intensity of the surrounding light . the quantities t 1 ( k ) and t 2 ( k ) in { circumflex over ( t )}( k ) can reduce or increase , respectively , the gamma value of the system and the effect hereof is a change of the dynamics of the image . for the parameter saturation 9 the effect can thus be described for each individual pixel , in that the chrominance signal is changed relative to the luminance signal . for the remaining of the four parameters shown in fig1 , i . e . brilliance 10 , contrast 11 and gamma 12 , it is only relevant to regard the effect for the entire image , as the effect results from the signal values being stretched over the interval of these values in order to attain a new distribution of signal values . calculation of the global chrominance gain g c is in the following illustrated by a specific ( and simplified ) numerical example of histogram processing according to the invention . t ( k )= s ( p 3 ( k )+ c 2 { circumflex over ( t )} ( k )) in the following example , it will be assumed that the number of input levels have been quantizised into ten bins ( in an actual implementation this number will typically be larger ). it is furthermore assumed that the values of p 3 ( k ) and { circumflex over ( t )}( k ) for each bin number are as given in table 1 below : if it is furthermore assumed that c 2 = 8 the values for the sum of p 3 ( k ) and c 2 { circumflex over ( t )}( k ) given in table 2 below will be obtained : assuming furthermore that the final transfer function concerns an 8 - bit video signal ( 256 levels , all levels used as valid signal data ), the constant ( scale factor ) s is used for scaling the output appropriately , in this example yielding : s = 255 / 9 . the values of the total transfer function t ( k ) given in table 3 below are then obtained : for the data shown above , an interpolated mapping for 8 - bit signal input - output is given in fig5 . this mapping will add dynamics to the low signal levels , at the expense of decreased dynamics for the higher image levels . after interpolation t ( k ) is now defined for the desired input levels . in this example for kε { 0 , 1 , . . . , 255 }. assuming now that y avg = 140 , then t ( y avg )= t ( 140 )= 162 . t ( k ) is in this example an identity mapping minus the offset bl , i . e . t ( k )= k − bl . assuming that bl = 1 , t ( 140 )= 139 . the average luminance has thus been increased by the histogram processing method according to the invention and the chrominance components should be scaled accordingly by g c . | 7 |
the present invention identifies potential collision with traffic in sufficient time to allow the crew to take corrective action . the present invention also ensures that nuisance alerts or lost alerts are minimized . the present invention does not rely on the availability of map data for the airport . fig1 shows an exemplary system 20 located on an ownship ( e . g ., aircraft , airport ground vehicle ) 18 for providing a crew of the ownship ample early warning of a potential ground operations collision . the system 20 includes a processor 24 that is in signal communication with a data communication device 28 , memory 30 ( i . e ., database ), an output device 32 , a navigation / position device 34 ( e . g ., gps , ins , etc .) and an interface ( if ) device 36 . the processor 24 receives the following data from existing avionic systems on the ownship 18 : geographic position ( latitude and longitude from the positioning device 34 ); heading ( from the heading reference system 38 ( e . g ., gyro , compass , inertial navigation system ( ins )); speed ( from the positioning device 34 ); and wingspan information ( from the memory 30 ). the processor 24 receives the following data from other aircraft or vehicles ( the “ traffic ”): an example of the data communications device 28 includes an automatic dependent surveillance - broadcast ( ads - b ) data link system . the processor 24 also receives from the memory 30 , or some external source , some constant values , such as those previously defined in various publications ( e . g ., rtca do - 322 ). examples of constant values include : flight crew reaction time t r ( seconds )— time to alert notice and evaluation ; flight crew action time t a ( seconds )— time of decision making and starting a braking action ; aircraft “ standard ” deceleration a ( meters / second )— rate of deceleration while braking following an alert . using all or a portion of the received data , the processor 24 determines if a collision - alert condition exists . if a collision - alert condition is determined to exist , the processor 24 outputs an alert signal to the output device 32 . fig2 shows a first taxiing aircraft 50 that has determined that a potential collision condition exists with a second taxiing aircraft 54 . in response to the potential collision condition determination , the first taxiing aircraft 50 activates lights 40 ( e . g ., landing lights ) that provide illumination in the direction of the second taxiing aircraft 54 , thus alerting the second aircraft &# 39 ; s flight crew of an alert condition . fig3 shows a flow diagram of an exemplary process 60 performed by the system 20 . first , at a decision block 64 , the processor 24 determines if the ownship is on the ground . if the ownship is a ground vehicle , then this condition is always true . if the ownship is an aircraft , then the processor 24 determines this condition to be true , based on an on - ground indicator ( e . g ., weight - on - wheels signal ) received from a databus via the if device 36 , ownship position and altitude information , airport / geographic information ( i . e ., altitude ), or some other criteria . after the ownship is determined to be on the ground , the processor 24 receives information from other proximate grounded vehicles at process 68 . then , the process 60 determines if the ownship is moving , see decision block 70 . if the ownship is determined to be moving , the process 60 determines if a potential collision condition exists , based on the received target information and the ownship information , see decision block 72 . if the potential collision condition does not exist , then the process 60 returns to decision block 64 after a delay ( block 74 ). if the potential collision condition exists , then , at a block 76 , a distance to the traffic , when the traffic will pass the ownship after an estimated ownship stopping position , is determined . next , at a decision block 80 , it is determined if the determined distance to the traffic is less than or equal to a predetermined safe - distance value . if the distance to traffic is not less than or equal to the predetermined safe - distance value , then the process 60 returns to decision block 64 . if the distance to traffic is less than or equal to the predetermined safe - distance value , then , at a block 82 , a potential collision alert condition exists and warning of the traffic is performed by illuminating an exterior light 40 of the ownship . the illuminated exterior light of the ownship provides a warning to the flight crew of the traffic that a collision threat exists . at a decision block 86 , after a delay the process 60 determines if the potential collision alert condition still exists . if the potential collision alert condition still exists , then at a block 88 , the illumination of the exterior light ( s ) is changed ( e . g ., steady to flashing ; slow flashing to fast flashing ). if the potential collision alert condition is determined to not exist after the delay , then at a block 90 , the exterior light ( s ) is extinguished . the exterior light is one designated exclusively for this purpose or is an existing light ( s ) of the ownship ( e . g . landing lights ). in one embodiment , the first time the exterior light ( s ) is illuminated , it is illuminated in a predefined pattern . an example of the predefined pattern includes steady on at various levels of intensity . another example of the predefined pattern includes flashing at a first rate . when the exterior light ( s ) illumination is changed , various aspects of the illuminating exterior light ( s ) are changed either separately or in combination . for example , the light intensity changes , the rate of flashing changes or if there are more than one landing light , then the lights alternately flash . if the potential collision alert condition still existed after the delay without adequate resolution , it would be assumed that a collision is more imminent . in this situation , the exterior light illumination is changed in order to impart a more immediate need to take action . increasing the flash rate or intensity of the exterior light ( s ) are exemplary ways of imparting a need to take action . in one embodiment , the outputted alerts include graphical highlighting of areas or traffic on a cockpit map display , are text messages presented on a display , or are aural messages provided to the crew via cockpit loudspeaker or headset . tactile alert systems may also be used . the solution of the potential traffic collision detection is built on the following conditions : ownship is aware about the traffic position ( e . g ., from traffic ads - b data or another source ); ownship is aware about the traffic heading ( e . g ., from traffic ads - b data or another source ); ownship is aware about the traffic speed ( e . g ., from traffic ads - b data or another source ); and ownship is aware about the traffic size category ( e . g ., from traffic ads - b data or another source ). wingspan of the traffic is determined according to information about the size category of the traffic aircraft , e . g ., from the traffic ads - b data and a database stored in the memory 30 . for each size category , the processor 24 uses the higher value of wingspan range stored in the memory 30 . the processor 24 uses the following constants when determining the full - stop location : flight crew reaction time ( t r ( sec )); flight crew action time ( t a ( sec )); and aircraft deceleration ( a (′ s 2 )). based on speed of the ownship ( os ) the braking distance ( d brake ) and time to full stop ( t stop ) are calculated from following formulas : where ( t s ) is time of ownship deceleration to full stop from ( v os ) ( actual speed of ownship ) without consideration of crew reaction or action time . equation ( 3 ) represents the assumption that , after alert triggering , the speed of ownship remains constant during the time period ( t r + t a ) and after this time ownship starts deceleration with deceleration rate ( a ) ( ownship decelerates until v os = 0 ). the processor 24 calculates “ safe distance ”. d safe , which represents minimum distance between ownship and traffic ( tr ), in which ownship and traffic shall pass each other . w span — tr — wingspan of the traffic ; w span — os — wingspan of the ownship ; ( retrieved from ownship parameters database ( the memory 30 )). the processor 24 recalculates the position of traffic ( x tr ; y tr ) to a “ local ” coordinate system relative to the position of ownship ( fig4 ). current position of ownship and traffic in the local coordinate system ( expressed in feet ) is as follows : os position ( x os ; y os ): ( 0 ; 0 ) tr position [ x tr ; y tr ]: ( x tr gps − x os gps ; y tr gps − y os gps ) the processor 24 evaluates whether the traffic represents a potential threat to ownship . evaluation is based the following values : the current distance between ownship and traffic is expressed as follows : d curr =√{ square root over (( x tr − x os ) 2 +( y tr − y os ) 2 )}{ square root over (( x tr − x os ) 2 +( y tr − y os ) 2 )} ( 5 ) calculation is running in the local coordinate system x os = y os = 0 ; thus , equation ( 5 ) is rewritten as : d curr =√{ square root over (( x tr 2 + y tr 2 )} ( 6 ) the distance between ownship and traffic is written as a function of time . in the local coordinate system the position of ownship and traffic in time ( t ) is written as follows : y os ( t ) = y os + v os · t · cos γ os = v os · t · sin γ os ( 7 ) where : os = 90 − ownship heading tr = 90 − traffic heading ( os and tr represent the angle of ownship and traffic heading measured in local coordinate system ). function of distance between the ownship and traffic is expressed as follows : d ( t ) =√{ square root over ( a · t 2 + b · t + c )} ( 10 ) where : a = v tr 2 − 2 ·( v tr · cos γ tr · v os · cos γ os + v tr · sin γ tr · v os · sin γ os )+ v os 2 b = 2 ·[ x tr ·( v tr · cos γ tr − v os · cos γ os )− y tr ·( v tr · sin γ tr − v os · sin γ os )] c = x tr 2 + y tr 2 equation ( 10 ) indicates parabolic running of function d ( t ) . as an example , fig5 shows running of the function d ( t ) in the interval t [− 5 , 30 ]. in this example , d ( t ) is depicted under the following conditions : ownship heading : 50 ° ownship speed : 30 knots traffic coordinates ( foot ): [ 755 . 6 ; − 101 . 99 ] traffic heading : 340 ° traffic speed : 30 knots from fig5 it is seen that , in a certain time , ownship and traffic will be at a minimum distance from each other ( d ( t ) reaches its minimum ). minimum of d ( t ) shows in distance and time when ownship and traffic will pass each other if both airplanes maintain constant actual speed and heading . if the traffic is about to collide with ownship , the minimum of d ( t ) will be less than “ safe distance ” ( d safe ). if first derivative of function d ( t ) is equal to zero , the time in which the distance between ownship and traffic will be minimum can be calculated . substituting t min to the equation ( 10 ) the minimum value of d ( t ) is obtained . the minimum value of d ( t ) is the distance in which ownship and traffic pass each other ( or “ collide ”). d min =√{ square root over ( a · t min 2 + b · t min + c )} ( 14 ) if d min is less than d safe , the traffic may represent a potential future threat . then , the processor 24 calculates the distance in which traffic will pass ownship after ownship stops ( d stop ), if an alert is triggered at the current time . calculation is done in the local coordinate system ( x os = y os = 0 ). using equation ( 3 ) the position of ownship in time is written as follows : in the same time , under the assumption of constant speed and heading of traffic , the traffic is determined to be at the following position : for the condition above , the distance by which traffic is predicted to pass the ownship can be obtained from equation ( 9 ). for this case equation ( 10 ) is expressed as follows and distance by which traffic will pass the stationary ownship is calculated : d * ( t ) =√{ square root over (( x * tr + v tr · t · cos γ tr ) 2 +( y * tr + v tr · t · sin γ tr ) 2 )}{ square root over (( x * tr + v tr · t · cos γ tr ) 2 +( y * tr + v tr · t · sin γ tr ) 2 )} d * ( t ) =√{ square root over ( a *· t 2 + b *· t + c * )} a *= v tr 2 b *= 2 · v tr ·( x * tr · cos γ tr − y * tr · sin γ tr ) c *= x * tr 2 + y * tr 2 d stop represents the expected distance by which traffic will pass the ownship if alert is triggered at present time and ownship is stopped under the assumption of equation ( 3 ). if the value of d stop is greater than the “ safe distance ” value ( equation ( 4 )), traffic is evaluated as “ safe ”. if the value of d stop is less than the “ safe distance ” value ( equation ( 4 )), traffic is evaluated as a threat and an alert is triggered . in one embodiment , the processor 24 continuously evaluates the distance between ownship and traffic and the predicted separation distance d stop between ownship and traffic if ownship stops . if this distance is equal to or less than the safe distance , the alert is triggered . fig4 shows an example of two aircraft on crossing taxiways . while the preferred embodiment of the invention has been illustrated and described , as noted above , many changes can be made without departing from the spirit and scope of the invention . accordingly , the scope of the invention is not limited by the disclosure of the preferred embodiment . instead , the invention should be determined entirely by reference to the claims that follow . | 6 |
the detailed description set forth below in connection with the appended drawings is intended as a description of the presently preferred embodiment of the invention , and is not intended to represent the only form in which the present invention may be constructed or utilized . it is to be understood , however , that the same or equivalent functions may be accomplished by different embodiments that are also intended to be encompassed within the spirit and scope of the invention . with reference now to fig1 , a cross sectional view of the earth &# 39 ; s surface is shown . atmosphere 30 is shown with clouds 32 releasing precipitation 34 , falling towards the ground 50 . as is well understood , ground 50 is comprised of top soil layer 52 . underneath top soil layer 52 is clay layer 54 , and underneath that is sand lens 56 . aquifer 60 is a layer of water , and can exist in permeable rock , permeable mixtures of gravel , and / or sand , or fractured rock 58 . precipitation 34 falls on top soil layer 52 , and is gradually filtered of impurities by the varying layers of sand , soil , rocks , gravel , and clay as it moves through the same by gravitational force , eventually reaching aquifer 60 . in the context of the above natural features , the present invention will be described . referring now to fig2 , a first embodiment of the present inventive concrete paving system 100 is shown . situated above clay layer 54 is an aggregate leach field 82 comprised of sand and gravel particles . above aggregate leach field 82 is a pavement layer 80 , which by way of example only and not of limitation , is concrete composed of portland cement and an aggregate . pavement layer 80 may be reinforced with any reinforcement structures known in the art such as rebar , rods and so forth for increased strength . preferably , the reinforcement structure has the same coefficient of thermal expansion as the pavement material , for example , steel , where concrete is utilized , to prevent internal stresses in increased temperature environments . by way of example only and not of limitation , pavement layer 80 has reinforcement bars 90 . it will be appreciated by one of ordinary skill in the art that the pavement layer 80 need not be limited to architectural concrete , and asphalt and other pavement materials may be readily substituted without departing from the scope of the present invention . extending from the top surface to the bottom surface of pavement layer 80 are one or more surface drains 84 . due to the fact that non - porous concrete , that is , concrete having aggregate mixed into the cement , permits little water to seep through , surface drains 84 expedite the water flow into aggregate leach field 82 . typically , by way of example only and not of limitation , surface drains 84 are filled with rocks to prevent large debris such as leaves and trash from clogging the same . within aggregate leach field 82 are one or more leach lines 86 , which assist the transfer of fluids arriving through surface drains 84 . by way of example only , leach lines 86 are in direct fluid communication with surface drains 84 . leach lines 86 have a higher porosity than the surrounding leach field 82 to enable faster transmission of fluids . leach field 82 is also capable of absorbing water , and in fact , certain amounts are absorbed from leach lines 86 . additional water flowing from surface drains 84 is also absorbed into leach field 82 . in this fashion , water is distributed across the entire surface area of leach field 82 , resulting in greater replenishment of the aquifer . a person of ordinary skill in the art will recognize that the leach field 82 acts as a filter by gradually removing particulates from precipitation , and resulting in cleaner water in the aquifer . as is well understood in the art , clay has a lower porosity as compared to an aggregate of , for example , sand , gravel , or soil . in order to expedite the transmission of water into the aquifer , aggregate drains 88 extend from aggregate leach field 82 , through clay layer 54 , and into sand lens 56 . therefore , a minimal amount of water is absorbed into the clay layer 54 , and the replenishment process is expedited . after the water flows from leach field 82 into sand lens 56 via aggregate drains 88 , it is dispersed throughout sand lens 56 , trickling through to the aquifers in the vicinity . the water in the aquifer is thus replenished through largely natural means , namely the filtration process involved in absorbing precipitation through aggregate leach field 82 and sand lens 56 , despite the existence of a non - porous material such as concrete overlying the ground surface in the form of pavement layer 80 . the aquifer replenishment system as described above is generally formed over previously undeveloped land , or any land that has been excavated to a clay layer 54 . thus , surfaces that have been previously paved by other means must first be removed so that the natural water absorption mechanisms of the earth are exposed . after this has been completed , aggregate drains 88 are drilled from the exposed clay surface 54 into sand lens 56 . after filling the aggregate drains 88 with aggregate , a generally planar aggregate leach field 82 is formed . contemporaneously , leach lines 86 are formed , and is encapsulated by the aggregate which constitutes leach field 82 . after leach field 82 is constructed , concrete reinforcements 90 are placed , and uncured concrete is poured to create pavement layer 80 . with respect to the formation of surface drains 84 , any conventionally known methods of creating generally cylindrical openings in concrete may be employed . for example , before pouring the uncured concrete , hollow cylinders may be placed and inserted slightly into leach field 82 to prevent the concrete from flowing into the opening . yet another example is pouring the concrete and forming a continuous layer , and drilling the concrete after curing to form surface drain 84 . it is to be understood that any method of forming surface drain 84 is contemplated as within the scope of the present invention . with reference to fig3 , a second embodiment of the aquifer replenishing system 200 is shown , including an elevated curb section 192 , a gutter section 196 , and a road pavement section 190 . road pavement section 190 is comprised of a pavement layer or pavement surface 195 , which by way of example only and not of limitation , is architectural concrete , asphalt concrete , or any other paving material known in the art , and is supported by base course 194 . base course 194 is generally comprised of larger grade aggregate , which is spread and compacted to provide a stable base . the aggregate used is typically ¾ inches in size , but can vary between ¾ inches and dust - size . in accordance with the present invention , gutter section 196 has a porous concrete gutter 184 in which the top surface thereof is in a substantially co - planar relationship with the top surface of pavement surface 195 . optionally , porous concrete gutter 184 is supported by base 185 which is composed of similar aggregate material as base course 194 . furthermore , extending from optional base 185 into aquifer 60 is a rock filled bore 188 . as a person of ordinary skill in the art will recognize , a bore filled with rocks will improve the channeling of water due to its increased porosity as compared with ordinary soil . optional base 185 and porous concrete gutter 184 is laterally reinforced by cut off walls 183 and elevated curb section 192 . the cut off walls 183 are disposed on opposing sides of the porous concrete gutter 184 and the base 185 between the elevated curve section 192 and the pavement surface 195 . it is expressly contemplated that the cut off walls 183 may be pre - cast or cast in place . when precipitation falls upon road pavement section 190 , the water is channeled toward gutter section 196 . porous concrete gutter 184 permits the precipitation to trickle down to aquifer 60 . when optional base 185 and rock filled bore 188 is in place , there is an additional filter effect supplementing that of the porous concrete gutter 184 . a similar result can be materialized where the water drains from the upper surface of elevated curb section 192 , or precipitation directly falls upon porous concrete gutter 184 . please note a large surface drain may be used in lieu of the porous concrete gutter . this embodiment is particularly beneficial where retrofitting the gutter is a more desirable solution rather than re - paving the entire road surface . in a conventional road pavement as shown in fig4 , pavement surface 195 and base course 194 extend to abut elevated curb section 192 . in preparation for retrofitting gutter section 196 , a section of pavement surface 195 and base course 194 is excavated as shown in fig5 , leaving a hole 197 defined by the exposed surfaces of elevated curb section 192 , base course 194 , and pavement surface 195 . this is followed by the optional step of pouring and curing a cut - off wall 183 as illustrated in fig6 , which , as discussed above , serves to reinforce the gutter section 196 . one or more bores 188 are drilled down to aquifer 60 , and filled with rocks , as shown in fig7 . an optional base of aggregate 185 is formed above rock filled bore 188 , and compacted by any one of well recognized techniques in the art . finally , a volume of porous concrete mixture , that is , a concrete without sand or other aggregate material , is poured and cured , forming porous concrete gutter 184 . while recognizing the disadvantages of using porous concrete , namely , the reduced strength of the resultant structure , a person of ordinary skill in the art will also recognize that gutter section 196 sustains less stress thereupon in normal use as compared to road pavement section 190 . the above description is given by way of example , and not limitation . given the above disclosure , one skilled in the art could devise variations that are within the scope and spirit of the invention disclosed herein . further , the various features of the embodiments disclosed herein can be used alone , or in varying combinations with each other and are not intended to be limited to the specific combination described herein . thus , the scope of the claims is not to be limited by the illustrated embodiments . | 4 |
referring to fig1 of the drawings , 1 denotes an outfeed portion , in its entirety , of a unit 2 for overwrapping packets of cigarettes 3 in leaves or sheets 4 of transparent material , for example polypropylene . such packets 3 are rectangular and prismatic in shape , referable to a longitudinal axis denoted 5 , presenting two larger side faces 6 parallel one with another and with the longitudinal axis 5 , two smaller or flank faces 7 disposed parallel to the longitudinal axis 5 and at right angles to the larger faces 6 , and two end faces 8 disposed transversely to the longitudinal axis 5 . the outfeed portion 1 of the unit 2 includes a feed conveyor 9 ( part of which visible in fig1 ) set in rotation clockwise , as viewed in fig1 , about an axis denoted 10 , by which successive packets 3 are advanced with their axes 5 disposed parallel to the axis 10 of the conveyor , each enveloped in part by a sheet 4 of transparent material , toward a feed station 11 . also forming part of the outfeed portion 1 is a transfer wheel 12 set in rotation anticlockwise , as viewed in fig1 , about an axis 13 parallel to the axis 10 of the conveyor 9 , interposed between the feed station 11 and a release station 14 serving a substantially horizontal outfeed conveyor belt 15 of which one end is looped about a return pulley coinciding with the transfer wheel 12 . the sheets 4 are wrapped around the respective packets 3 by the conveyor 9 in conventional manner , not illustrated , so that each is formed into a tubular wrap 4 ′ ( see fig5 ) centered on an axis coinciding with the longitudinal axis 5 , that is , a wrap 4 ′ clinging to the four side faces 6 - 6 and 7 - 7 of the packet 3 and secured along one flank face 7 by a sealed seam 16 uniting two overlapped edges of the sheet 4 . the feed conveyor 9 is equipped peripherally with a plurality of assemblies 17 , equispaced one from another and pivotable about axes 18 disposed parallel to the axis 10 of rotation , each affording a holder 19 proportioned to accommodate a single packet 3 wrapped in a relative sheet 4 . the holder 19 is delimited by a back wall 20 designed to make contact with one flank 7 of the packet 3 , and two side walls 21 and 22 designed to engage the two larger side faces 6 of the packet . the front part of the holder 19 , opposite the back wall 20 , remains open . as discernible from fig3 , and for reasons that will become clear in due course , the holder 19 is proportioned in such a way that the two ends of the packet 3 project one on either hand , together with the two ends of the tubular wrap 4 ′. with reference to fig5 , each end of the tubular wrap 4 ′ comprises two appendages denoted 23 and 24 projecting from the two larger side faces 6 , an appendage 25 projecting from the flank face 7 offered to the back wall 20 , and an appendage 26 projecting from the flank face 7 along which the sealed seam 16 is applied . one portion 27 of the side wall denoted 21 ( which advances forwardmost in the direction of rotation of the conveyor 9 ) is mounted pivotably to a hinge pin 28 parallel with the axis 10 of the conveyor , coupled to actuator means ( not illustrated ), and capable thus of combining with the opposite side wall 22 to function as gripping means by which the packet 3 is retained internally of the holder 19 . as illustrated in fig1 and 2 , the transfer wheel 12 comprises a drum 29 mounted to a shaft 30 of which the axis coincides with the axis 13 of the wheel . the drum 29 is equipped at the right hand end , as viewed in fig2 , with a cylindrical flange 29 a centered on the axis 13 and carrying a number of shafts 31 centered on respective axes 31 ′ and extending toward the opposite end of the drum 29 . the shafts 31 are equispaced angularly around and parallel to the axis 13 of the wheel , and serve to carry respective gripper assemblies 32 each affording a holder 33 such as will accommodate a packet 3 disposed with its axis 5 parallel to the aforementioned axis 13 . each assembly 32 comprises two mutually parallel arms 34 anchored at respective ends to the opposite ends of a single shaft 31 . the free end presented by each arm 34 of the gripper assembly 32 serves to carry a respective shaft 35 of which the axis 35 a is disposed parallel to the axis 13 of the wheel 12 . the two shafts 35 are axially aligned one with another and carry the holder 33 between their respective ends . both sets of shafts 31 and 35 are coupled to actuator means ( not illustrated ) such as will cause the arms 34 to pivot on the respective axes 31 a relative to the drum 29 , and the holders 33 to rotate about the respective axes 35 a relative to the arms 34 , during the rotation of the transfer wheel 12 about its axis 13 . in the example illustrated , the single holder 33 comprises two l - shaped elements denoted 36 , each mounted to the end of a respective shaft 35 . the elements 36 in question present two first portions 36 a lying in a common plane , parallel to the axis 13 of the wheel and combining to establish a back wall 37 of the holder 33 such as will engage the flank face 7 of the packet 3 occupying the open front of the holder 19 afforded by each assembly 19 of the conveyor 9 . the elements 36 also present two portions 36 b normal to the first portions 36 a , disposed mutually parallel and separated by a distance substantially equal to the longitudinal dimension of a single packet 3 , of which the free ends are fashioned with a rounded profile . the two parallel portions 36 b establish two further walls of the holder 33 , and more exactly two side walls 38 by which the two corresponding appendages 26 of the tubular wrap 4 ′ are folded at the moment when the packet 3 is directed into the holder 33 . as illustrated in fig6 , the step of folding each appendage 26 has the effect of forming two triangular folds 26 ′, doubled against the innermost surfaces of the adjoining appendages 23 and 24 . each shaft 35 of the gripper assembly 32 is ensheathed by a tubular element or sleeve 39 that carries gripping means 40 a comprising two jaws 40 and 41 of width substantially matching the width of the packet 3 , pivotable about respective axes 42 and 43 extending mutually parallel and transverse to the shaft axis 35 a . the gripping means 40 a in question constitute means 44 by which to pinch the packet 3 across the opposite endmost edges of the larger side faces 6 , and are capable of movement induced by actuator means ( not illustrated ) between an open position , illustrated in fig1 , and a closed position illustrated in fig1 and 3 . the jaws denoted 40 , uppermost as illustrated in fig3 , present a free gripping end of width substantially identical to that of the packet 3 and are equipped on the side farthest from the back wall 37 with a drag tooth 45 designed to engage one of the flank faces 7 of the packet 3 when released from the conveyor 9 to the transfer wheel 12 . as illustrated in fig4 , it will be seen that with the pinching means 44 in the closed position , the two fold - making longitudinal corner edges 46 of each side wall 38 engage substantially in contact with a gripping face 47 of the corresponding jaw 40 and 41 . consequently , as illustrated in fig6 and 8 , each edge 26 a of a relative folded appendage 26 , coinciding with one side of the relative triangular fold 26 ′ and overlapping part of the corresponding corner edge of a respective end face 8 , will be pinned between the corner edge 46 of the wall 38 and the face 47 of the jaw together with a part 48 of the edge of the appendage 23 or 24 projecting from the respective larger side face 6 of the packet 3 . as illustrated in fig1 and 4 , the unit 2 further comprises heating means denoted 49 , located along the two opposite longitudinal corner edges 46 of each fold - making side wall 38 and consisting , for example , in electrical resistance elements . similarly , the unit 2 comprises heating means 50 located on an area 47 ′ of the gripping face 47 presented by each jaw 40 and 41 , positioned to coincide with the aforementioned corner edges 46 . the outfeed conveyor belt 15 , which advances in the direction denoted f 1 , is equipped with slats 51 delimiting pockets 52 each designed to accommodate a relative packet 3 . 53 denotes a horizontal guide element positioned above the top branch of the belt 15 at a distance substantially equal to the depth of one packet 3 . 54 denotes one of two second fold - making side walls ( one only being visible in fig1 ) by which the two appendages 25 of the tubular wrap 4 ′ opposite to the appendages denoted 26 are flattened against the end faces 8 ( see fig8 ). 55 and 56 denote two helical fold - making elements by which the remaining appendages 23 and 24 of the tubular wrap 4 ′ extending on either side from the two larger faces 6 of the packet 3 are flattened against the end faces 8 , overlapping one another ( see fig8 and 9 ). 57 denotes one of two heat - seal devices , one only being visible in fig1 , by which the two appendages 23 and 24 are bonded one to another over a substantially central area of the end face 8 , excluding the aforementioned edges 26 a and 48 , to complete the ends 8 ′ of the overwrapping . in operation , each holder 19 of the conveyor 9 containing a single packet 3 approaches the entry to the feed station 11 , which extends through an arc of predetermined length , and draws alongside a holder 33 of the transfer wheel 12 , the two holders being substantially aligned at this juncture on an axis transverse to the longitudinal axis 5 of the packet 3 . during this step , the packet 3 will be actively restrained by the aforementioned gripping means 22 and 27 of the one holder 19 , whilst the gripping means 40 a of the other holder 33 are spread , thus allowing interpenetration of the two holders to the point at which the flank face 7 of the packet 3 presenting the sealed seam 16 registers against the back wall 37 , and the ends projecting from the first gripping means 22 and 27 are caused to locate between the jaws 40 and 41 of the second gripping means 40 a . at this point , the jaws 40 and 41 are caused by respective actuator means to close and the gripping means 22 and 27 are spread , allowing the teeth 45 to draw the packet 3 from the holder 19 at the exit end of the feed station 11 . restrained between the jaws 40 and 41 , with the transfer wheel 12 , the arms 34 and the holders 33 rotating anticlockwise ( as viewed in fig1 ), the packet 3 arrives at the release station 14 turned through an angle of some 180 ° from the position in which it had left the holder 19 of the conveyor 9 . on entering the release station 14 , accordingly , the packet 3 will assume a position in which the larger side face 6 engaging the bottom jaw 40 lies substantially in the same plane as that occupied by the top branch of the conveyor belt 15 . at this stage , the gripping means 40 a are spread , and the flank face 7 opposite to that presenting the sealed seam 16 on the tubular wrap 4 ′ is engaged by a slat 51 passing between the two pairs of jaws 40 and 41 , through the gap that separates the aforementioned portions 36 a of the two l - shaped elements denoted 36 . as the packet 3 advances along the belt 15 , the two projecting appendages 25 are flattened by the second fold - making side walls 54 against the respective end faces 8 , whereupon the remaining appendages 23 and 24 are flattened by the helical fold - making elements 55 and 56 likewise against the end faces 8 , one overlapping the other . finally , the two appendages 23 and 24 are secured one to another by the heat - seal devices 57 to complete the closure of the overwrapping 4 . it will be seen that the step of transferring the packet 3 from the feed conveyor 9 to the transfer wheel 12 , during which the respective holders 19 and 33 are caused to interlock , comprises the step of stabilizing the appendages denoted 26 . this stabilizing action , applied along respective lines denoted 58 in the drawings , is generated by the combined action of the aforementioned edges 26 a and 48 of stabilizing means afforded by the longitudinal corner edges 46 of each side wall 38 and the contact areas 47 ′ of the gripping faces 47 . the stabilizing means 46 and 47 ′ in question might operate applying compression alone , or with the aid of the aforementioned heating means 49 and 50 . either solution will ensure that the folded appendage 26 remains stably in place during the remainder of the transfer steps described above . to advantage , moreover , and as discernible from fig9 , the heat - seal 57 ′ applied to each pair of appendages 23 and 24 by the heat - seal devices 57 is located in an area of the relative end 8 ′ not occupied by the stabilization lines 58 . it will be seen from the foregoing that there is no need to equip the unit 2 with mechanisms serving specifically to retain the first appendages 26 in the position assumed following the folding steps . in effect , such mechanisms are replaced by the aforementioned stabilizing means 46 and 47 ′, which are one and the same as the means serving to fold the appendages 26 and remain active during the relative folding step and / or during the step of transferring the packets 3 from the feed station 11 to the release station 14 . | 1 |
the present invention will now be described more fully with reference to the accompanying drawings in which alternate embodiments of the invention are shown and described . it is to be understood that the invention may be embodied in many different forms and should not be construed as limited to the illustrated embodiments set forth herein . rather , these embodiments are provided so that this disclosure may be thorough and complete , and will convey the scope of the invention to those skilled in the art . with reference initially to fig1 , one embodiment of the includes a golf swing training device 10 having an elongate shaft 12 with a proximal end portion 14 for holding the device by a user , an opposing distal end portion 16 , and an intermediate portion 18 therebetween . a grip 20 may be affixed at the proximal end portion 14 . a first coupling 22 is affixed to the shaft 12 generally within the proximal end portion 14 , but may be located as desired along the shaft length . a second coupling 24 is affixed the shaft 12 within the intermediate portion 18 , by way of example for the embodiment herein described . a stop 26 is attached to the shaft 12 at the distal end portion 16 , herein illustrated at an extreme end 28 of the shaft . the shaft 12 carries a first sliding element 30 for movement between the first coupling 22 and the second coupling 24 , and a second sliding element 32 for movement between the second coupling 24 and the stop 26 . the sliding elements 30 , 32 have sufficient weight for responding to centrifugal forces during the swinging of the shaft 12 by a user when holding the grip 20 in simulating a golf swing . with continued reference to fig1 , the first sliding element 30 is initially coupled to the first coupling 22 and the second sliding element 32 is coupled to the second coupling 24 prior to a swinging of the shaft in a training exercise . as will be further detailed later in this section , the first sliding element 30 is released from the first coupling 22 by a first centrifugal force generated by the swinging of the shaft 12 during a first swinging motion ( known in golfing as a backswing ). the first sliding element 30 accelerates toward the second coupling 24 and makes a first distinctive sound upon contact with a back surface 34 of the second coupling . the second sliding element 32 , initially coupled to the second coupling 24 , remains coupled during the backswing and is released during a second swinging motion ( known in golfing as a downswing ) by a second centrifugal force generated during the second swinging motion of the shaft 12 . the second sliding element 32 accelerates toward the stop 26 and makes a second distinctive sound when contacting the stop . for the embodiment of the device 10 , herein described with reference to fig1 , the shaft 12 comprises a circular cross section , and has a constant cross section along lengths of the shaft having the sliding element movements . with reference to fig2 , 2 a , and 3 , one embodiment of the grip 20 , herein described by way of example , includes a plurality of protrusions 36 that extend outwardly from a longitudinal axis 38 of the grip and are arranged for receiving multiple finger webs 40 biased against them in guiding a hand 42 of the user 44 , as illustrated with reference to fig4 - 6 , for gripping the shaft 12 proximal end portion 14 , earlier described with reference to fig1 . in one embodiment , the grip 20 may comprise three protrusions 46 for receiving the hand 42 that for a right - handed golfer will be the top hand on the shaft 12 positioned at a proximal portion 20 p of the grip , as illustrated by way of example with reference to fig7 . the three protrusions 46 extend from a first side 48 of the grip 20 for receiving three webs 40 between four fingers of the top hand . with reference again to fig2 , 2 a , and 3 , and to fig7 and 7a , another protrusion 52 for receiving a web 54 between fingers of the bottom hand 56 of the user 44 along a distal portion 20 d of the grip 20 . in one desired arrangement , and as illustrated with reference to fig8 , the longitudinal axis 38 of the grip 20 ( coincident with the axis of the shaft 12 ) and an a centerline 58 through a palm of the top hand 42 form approximately a forty five degree angle 60 . as further illustrated with reference again to fig5 , the protrusions 46 are aligned such that a line 47 extending through the protrusions along common points 46 a , 45 b , and 46 c on each of the protrusions 46 forms a non - zero angle 47 a with the longitudinal axis 38 . each protrusion 46 a , 46 b , 46 c of the protrusions 46 is thus offset from an adjacent one protrusion along a circumference of the grip 20 . with reference again to fig2 - 4 , a fourth protrusion 62 extends from a second side 64 radially offset from the first side 48 for receiving a thumb 66 of the top hand 42 , as illustrated with reference again to fig5 , by way of example . further , an indentation 68 is provided on the second side 64 for receiving a thumb of the bottom hand 56 . a second indentation 69 is also provided on the grip second side 64 for use by the thumb of the top hand 52 while the thumb is biased against the protrusion 62 . with reference again to fig1 , the couplings 22 , 24 and the sliding elements 30 , 32 may have various embodiments within teachings of the present invention . by way of example , and with reference to fig9 - 11 , the couplings 22 , 24 and the sliding elements 30 , 32 may be magnetically coupled with both being magnetized , one having a magnet and the other metallic , or the like . for the embodiment herein described by way of example , the sliding element comprises a plastic body 70 with a metallic ring 72 on a coupling side of the element . the sliding elements 30 , 32 may be modified in weight by adding ballast material to the plastic body , by way of example , or by selecting a desired weighted element . the couplings 22 , 24 are magnetized for the embodiment herein described . alternatively , and as will come to those of skill in the art now having the benefit of the teachings of the present invention , friction or latching connections 25 may be used , such as an adhesive or velcro , illustrated with reference again to fig1 . by way of example for the embodiment herein described for the gold training device 10 , a first coupling force between the first coupling 22 and the first sliding element 30 is less than a second coupling force between the second coupling 24 and the second sliding element 32 , thus less centrifugal force is required for releasing the first sliding element than for releasing the second sliding element . with continued reference to fig9 - 11 , for the embodiment herein described , the first and second sliding elements 30 , 32 comprise the body 70 having a bore 74 extending therethrough and dimensioned for sliding along the shaft 12 . it may be desirable to modify the friction between the first and second sliding elements 30 , 32 and the shaft 12 . one embodiment for modifying the frictional force may include having each sliding element 30 , 32 formed from two parts 70 a , 70 b and having the shaft 12 slidably received therebetween . by compressing the shaft 12 between the two parts 70 a , 70 b using connecting screws 76 , a desired sliding friction between the sliding elements and the shaft is achieved . as a result and by way of example when simulating a golfing swing , the releasing of the sliding elements and the sliding along the shaft may be modified to accommodate a desired circumstance or user characteristic . the coupling forces between the first coupling and the first sliding element and between the second coupling and the second sliding element may be preset for a desired swinging movement . yet further with regard to training a swing , and with reference again to fig1 , an alignment element 78 may be carried by the shaft 12 , which element may have a shape of a golf club head for the golf training device 10 herein described by way of example . in addition , a rod 80 may be carried within the shaft and longitudinally extendable from the proximal end portion 14 for viewing by the user during a swinging movement for identifying a swing plane therefor , desirable in one training exercise for a golf swing . by way of example , one method of use may include the training of a full golf swing . with reference now to fig1 and 13 , during one desired swing , two impact or percussion sounds will be heard . with reference to fig1 and to swing locations points a - f , the first sound is heard during the backswing at point e in the backswing as the first sliding element 30 contacts the second coupling 24 . in order for the user to hear the noise associated with the backswing ( the first sound ), the user will need to “ set ” the club properly . for the example herein described , the first sliding element 30 will begin to leave the first coupling 22 near swing point d . this may require a cocking of the wrists and a slight increase in tempo during the backswing , illustrated by way of example with reference to angles α and β for swing points d and e , respectively . with reference again to fig1 , the second impact sound is desirably heard at point j . this is created when a desired tempo is used . by way of example , imagine a cracking of a whip . this allows the second sliding element 32 to be released from the second coupling 24 , as illustrated at about point 1 , to slide down the shaft 12 and hit the stop 26 . typically , an un - cocking of the wrists as illustrated with angles β to α in the downswing will cause a desired release of the second sliding element 32 . the desired setting of the club going back and the desired releasing , or un - cocking , on the downswing provides a desirable maximum club head acceleration . as earlier described with reference to fig9 - 11 , not every golfer swings with the same speed or force . with this in mind , the first and second slidable elements 30 , 32 will be adjustable so that the beginner , as well as the seasoned professional will be allowed to train using the device 10 . by way of example for one embodiment herein describe , the first sliding element 30 may require less centrifugal force to allow it to break free from its starting position . the second sliding element 32 may be set to require significantly more centrifugal force to be applied during the downswing to allow it to break free and contact the stop 26 at the end of the shaft 12 . as illustrated with reference to fig1 , an alternate embodiment of the device 10 , identified as device 11 may include a tapered golf shaft 12 and the two sliding elements 30 , 32 to move freely after they have been released from their respective starting positions 82 , 84 . as above described with reference to fig1 , the stop 26 is carried at the shaft distal end 14 opposite the grip 20 . the stop 26 prevents the first and second sliding elements 30 , 32 from coming loose from the shaft 12 and provides a distinct sound at the time of the second impact portion of the swing creating the sound made during the downswing . the second sliding element 32 stops the first sliding element 30 when the user makes the desired backswing . the first sound is made when the first element 30 hits the second element 32 during the backswing . a release mechanism 86 ( a friction barrier by way of example ) described with reference to fig1 - 17 holds the first sliding element 30 in place during the completion of the backswing and releases both the first and second slidable elements for moving toward the stop 26 when sufficient force is applied during the downswing . as illustrated by way of example with reference to fig1 , one embodiment may include the sliding element 30 , 32 having the bore 74 forced into a taper of the tapered shaft 12 varying the frictional contact by pushing the element to a first , second , third indicator mark 88 made on the shaft . as illustrated with reference to fig1 , notches 90 and tabs 92 may be carried by the shaft 12 , whether tapered or not , and by the surface of the bore 74 , with a degree of releasing force countering a centrifugal force based on the number of notches engaged . yet further , a friction sleeve 94 may be employed for establishing a preset frictional contact 95 between the element 30 , 32 and the shaft 12 , as illustrated by way of example with reference to fig1 . as above described , during a desired swing , two impact or percussion sounds are heard . with reference to fig1 and 18 , the first sound is heard during the backswing at point e . as above described , in order for the user to hear the noise associated with the backswing ( the first sound ), the user will need to “ set ” the club properly . this may require a cocking of the wrists and a slight increase in tempo during the backswing , by way of example . the second impact sound is heard at point j as illustrated with reference to fig1 . the sliding elements 30 , 32 slide down the shaft 12 together and hit the stop 26 . this will be when the wrists un - cock in the downswing . the desired setting of the club going back and the desired releasing , or un - cocking , on the downswing permits achieving maximum club head acceleration . as above described , not every golfer swings with the same speed or force . therefore , frictional contact of the first and second sliding elements 30 , 32 with the shaft 12 may be adjustable so that the beginner , as well as the seasoned professional will be allowed to practice with this device . many modifications and other embodiments of the invention will come to the mind of one skilled in the art having the benefit of the teachings presented in the foregoing descriptions and the associated drawings . therefore , it is to be understood that the invention is not to be limited to the specific embodiments disclosed , and that modifications and alternate embodiments are intended to be included within the scope of the appended claims . | 0 |
the disposable protective garment of the applicant &# 39 ; s invention allows simplified manufacture by side to side orientation of the protective garments along a dispensing strip . the garments produced are then secured to the front of the user by a top adhesive strip and a bottom adhesive section . in reference to fig1 a user is shown removing a disposable protective garment 10 from dispensing box 30 . the strips of disposable protective garments are contained within dispensing box 30 on roll 36 . the back side of disposable garment 10 has a liquid impermeable laminate 20 covering the entire back side of the disposable protective garment 10 . the disposable garments may be separated from one another by tearing along perforation line 28 . this allows the user to tear off each individual disposable protective garment for individual use . on the reverse side of the disposable protective garment 10 is liquid absorbent material 22 . attached onto liquid impermeable laminate 20 are adhesive strips 14 , 16 . adhesive strip 14 is positioned at the top of the garment and runs along the side to side length of the garment . adhesive bottom strip 16 is shown as a shorter length of adhesive positioned near the bottom at the center of the side to side width of the garment . fig2 shows a schematic of the manufacturing process for producing disposable protective garments shown in fig1 . the process begins by unrolling a continuous sheet of liquid absorbent material 22 from master roll 100 . the continuous sheet of liquid absorbent material may be comprised of porous paper , non - woven cotton , or various multiple layered absorbent materials . as the continuous sheet is unrolled it is directed by rollers into printing system 110 . in printing system 110 the sheet of liquid absorbent material is rolled between first set of printing drums 112 and second set of printing drums 114 . these drums contact the sheet of liquid absorbent material 22 and are able to transfer printing to the sheet of absorbent material by thermal transfer printing , applied on - line ink transfer , or other known printing methods . it is also possible that an electrostatic printhead could be used in place of pairs of printing drums 112 , 114 . the printer applies decorative indicia in repetitive patterns onto one side of the sheet of liquid absorbent material . although the printing system is illustrated as occurring before the lamination , it is also possible to print after lamination has occurred . the material after passing through printing system 110 is transferred into lamination system 120 . in lamination system 120 the sheet is rolled between lamination drums 122 . as sheet of liquid absorbent material 22 is rolled between lamination drums 122 , an even coating of laminate is applied to one side of the sheet . this can be effected by unrolling laminate roll 126 onto lamination drum 122 . as laminate roll 126 unrolls , it is in contact with adhesive reservoir 124 such that the unrolling roll of laminate is coated with an adhesive . as the adhesive coated laminate comes in contact with sheet of liquid absorbent material 22 , the two sheets bond together such that one sheet is formed having a liquid absorbent material layer 22 and a liquid impermeable laminate layer 20 . although it is possible to use as a laminate material various plastic , rubberized or polymeric materials it is preferred to use a polyethylene film web that is 0 . 5 millimeter thick . the preferred adhesives used to bond the sheet of absorbent material 22 to the liquid impermeable layer 20 are water based . the laminated sheet then moves from lamination system 120 into drying tunnel 130 . in drying tunnel 130 heat is applied such that the water - based adhesive dries bonding the two layers 20 , 22 of the sheet together . the sheet is then rewound onto roll 50 . the laminated sheet then passes from drying tunnel 130 into processing system 140 . processing system 140 is further illustrated in fig3 and 3a . finally the roll is rewound onto product roll 150 . product roll 150 allows the system to maintain a dynamic tension such that the sheet is firmly held against the drums of the production system . product roll 150 can then be further processed into individual rolls which are packaged either individually in shrink - wrap or in dispensing boxes . the processing system 140 of fig2 is further illustrated in fig3 . in this system the laminate absorbent material is unrolled from roll 50 . this processing system performs the final steps in making the disposable garment . these steps include application of the adhesive strips onto the laminated sheet , as well as dicing and perforating the laminated sheet into individual strips of garments . in the processing system , rolls of adhesive tape 52 are unrolled and adhesive strip 14 is applied by pressure roller 53 onto the liquid impermeable laminate sheet 20 . the rolls of adhesive tape 52 unroll onto the length of sheet 20 . each of the rolls of adhesive tape 52 is spaced apart at discrete distances along the width of the sheet 20 . this separation distance is the top to bottom length of one strip of protective garments . in a similar manner , rolls of adhesive tape 54 are also positioned in a parallel orientation separated by a distance such that they dispense adhesive onto liquid impermeable laminate 20 . roll of adhesive tape 54 has a tape cut out 55 such that adhesive strip 16 is not continuously dispensed onto the liquid impermeable laminate 20 but instead is dispensed at regular intervals on liquid impermeable laminate 20 . alternatively a continuous strand of adhesive tape may be dispensed by roll of adhesive tape 54 such that the tape extends along the length of laminate sheet 20 . the positioning of roll of adhesive tape 52 and roll of adhesive tape 54 is such that the rolls of tape are separated by a length equal to the desired length of the garment . when the roll is subsequently cut , the tapes are positioned such that one length of adhesive extends across the top of each garment that is formed and the other adhesive strip is positioned on the bottom of the garment formed with both of the adhesives applied to the laminated back side of the garment . a number of adhesives are adaptable to the present invention . the preferred adhesive is a roll of double - sided tape with plastic release liner . one side of the tape adheres to liquid impermeable laminate 20 . the other side of the double - sided adhesive tape is covered by a plastic release liner . this liner may be subsequently removed exposing the sticky surface of the adhesive tape . the adhesive tape is selected such that it is adhesive to clothing without staining the clothing . alternative adhesives , such as removable pressure sensitive adhesives may also be used . this type of adhesive would be applied in the desired strip by a roller in contact with the adhesive reservoir . several sticky , removable pressure - sensitive adhesives are known . after the adhesive is applied , the sheet is next passed such that it presses against dye cut roller 60 . dye cut roller 60 has at regular intervals , dye cut blade 65 . dye cut blade 65 has an arc blade 64 and a straight edge blade 63 . the blades are positioned perpendicularly to the axis of rotation . dye cut roller 60 also has a perforating blade 62 positioned parallel to the axis of rotation . as dye cut roller rolls , it contacts the moving sheet of laminated material . arc blade 64 cuts this sheet such that arcs are formed in the sheet at regular intervals . blade straight edge 63 cuts the material such that the material sheet is divided into discrete widths each width being the width of a single strip of disposable protective garments . perforating blade 62 then makes a perforating cut 28 at regular intervals along the sheet . the dye cut blades result in the production of protective garments with a top scoop cut 25 and a bottom straight line cut 27 . a small arc of material is removed from the sheet in this production process . bottom straight line cut 27 separates the sheet of material into individual rolls of protective garments 32 , 33 , 34 . an alternative processing system is shown in fig3 a . again roll 50 unrolls the base sheet of material . adhesive tape rolls 52 again unroll tape 14 at regular intervals . tape 14 adheres to liquid impermeable laminate 20 when it is pressed onto this material by roller 53 . at the far edge of the sheet , edge roll of adhesive tape 56 has a tape arc cut out 57 which applies an arc of tape to the edge of the sheet . dye cut roller 60 has at regular intervals dye cut blade 65 . dye cut blade 65 has an arc blade 64 that at regular patterns cuts a scoop arc through the material along the length of the material as the material is drawn past the rotating blade . because the blade is positioned on a cylinder , the cylinder may be rotated such that the blade cuts a pattern at a regular interval into the material . dye cut blade 65 and roll of adhesive tape 52 are positioned such that the arc cut by dye cut blade 65 cuts through adhesive tape 14 . this leaves a small arc of adhesive tape 13 cut away from strip of adhesive tape 14 . the cut made by dye cut blade 65 also separates one disposable protective garment from another along the width of the sheet of laminated material . this again results in individual rolls of disposable protective garments 32 , 33 and 34 . fig3 b shows an individual disposable protective garment made by the process shown in fig3 a . the liquid impermeable laminate 20 is shown having running across the top an adhesive top strip 14 . an arc has been cut from adhesive top strip 14 . on the bottom of the garment is arc of adhesive tape 13 . fig3 a illustrates how using one roll of adhesive tape and a single dye cut both top and bottom adhesive strip can be added to the disposable protective garment further simplifying the production of the disposable protective garments . the blade which cuts through the strip of adhesive tape also separates the sheet of laminated material into individual strips of disposable protective garments 32 , 33 , 34 . fig4 illustrates the back side of disposable protective garment . liquid impermeable laminate 20 covers the entirety of the back side . extending across the top of the disposable protective garment from side to side is adhesive strip 14 . centrally located on the bottom of the back side of the disposable protective garment is adhesive bottom strip 16 . arrows 4 indicate a cross - sectional cut illustrated in fig5 . fig5 illustrates the cross - sectional cut of a section of the disposable protective garment including a cross section of the top adhesive strip 14 . as shown liquid absorbent material 22 has been laminated onto liquid impermeable laminate 20 . on top of liquid impermeable laminate 20 is adhesive top strip 14 . adhesive top strip 14 is composed of a plastic release liner 12 and a length of two - sided adhesive tape 15 positioned between plastic release liner 12 and liquid impermeable laminate 20 . plastic release liner 12 may be peeled away exposing an adhesive layer of two - sided adhesive tape 15 . because each side of two - sided adhesive tape 15 has adhesive properties , one side may adhere to liquid impermeable laminate 20 while the other side may adhere to the wearer of the disposable protective garment . the reverse side of the disposable protective garment shown in fig4 is seen in fig6 . this front side is comprised of liquid absorbent material 22 . printed onto liquid absorbent material 22 is printing 17 . this side of the garment would be visible when the garment is secured to the user by adhesive strip 14 , 16 . | 8 |
exemplary embodiments of the present invention are described with reference to the accompanying drawings in detail . the same reference numbers are used throughout the drawings to refer to the same or like parts . detailed description of well - known functions and structures incorporated herein may be omitted to avoid obscuring the subject matter of the present invention . fig1 is a block diagram illustrating a configuration of a wireless communication system according to an embodiment of the present invention . referring to fig1 , the wireless communication system of this embodiment includes a ue 10 , an enhanced node b ( enb ) 20 , an mme 30 , a serving gateway ( s - gw ) 40 , and a packet data network gateway ( p - gw ) 50 . the ue 10 may be fixed or mobile . the ue 10 can be a normal ue for performing normal communication function or a machine type communication ( mtc ) ue for performing mtc function . here , mtc technology can be applied to smart metering for automated communication between the power company server and electric meter reader and alarm system for automated communication between the security company server and an illegal intrusion alarm . the enb 20 manages a cell . at this time , the enb 20 is a macro enb , and the cell is a macro cell as a cell of a typical cellular system . here , the terms “ enb ” and “ cell ” can be interchangeably used in the same meaning . the enb 20 connects to the ue 10 through a radio channel and controls radio resource . for example , the enb generates and broadcasts system information necessary for control within the cell and allocates radio resource for transmitting / receiving packet data or control information to / from the ue 10 . the system information is capable of including carrier information ( plmn id ), enb cell global id ( ecgi ), and tracking area id ( tai ) of each cell . the enb is capable of collecting channel measurement result information for the serving and neighbor cells to make a handover decision and command handover . in order to achieve this , the enb 20 is provided with the control protocol such as radio resource control protocol related to the radio resource management . the mme 30 manages ue 10 in idle mode and selects the s - gw 40 and the p - gw 50 . the mme 30 is responsible for roaming and authentication functions . the mme 30 also processes bearer signals generated by the ue 10 . in order to achieve this , the mme 30 allocates identity information to the ue 10 and manages the connection with the ue 10 using the identity information . at this time , the mme 30 can be a normal mme for supporting the normal ues or a mtc mme for supporting the mtc ues . here , the mme 30 is cable of having a unique entity id which allows for identifying the normal mme and mtc mme . the mme 30 connects to the enb 20 through a radio channel and connects to the ue 10 via the enb 20 . here , the mme 30 connects to the enb via s1 - mme interface . at this time , the mme 30 communicates with the ue 10 using non access stratum ( nas ) message . the mme 30 supports a plurality of tracking areas and is connected with a plurality of enbs 20 providing respective tracking area information . that is , a plurality of enbs 20 providing the same tracking area information can be connected with the mme 30 . it is also possible for the plural enbs 20 proving different tracking area informations to connect to the respective mmes 30 . it is also possible for the plural enbs 20 supporting different tracking areas to be connect to the same mme 30 . the s - gw 40 connects to the enb 20 and the mme 30 through radio channels . here , the s - gw 40 connects to the enb 20 through s1 - u interface . the s - gw 320 is responsible for the ue mobility control function . that is , when the ue 10 performs handover between enbs or roams across 3gpp radio network networks , the s - gw 40 acts as a mobility anchor of the ue 10 . the p - gw 50 connects to the s - gw 40 through a radio channel . here , the p - gw 50 connects to the s - gw via s5 interface . the p - gw 50 connects to the internet protocol ( ip ) network 60 . the p - gw 50 is responsible for ip address allocation to the ue 10 and packet data - related functions . that is , the p - gw 50 delivers the packet data received through the ip network 60 to the ue 10 via the s - gw 40 and the enb 20 . when the ue moves between the 3gpp radio network and non - 3gpp radio network , the p - gw 50 acts as the mobility anchor of the ue 10 . the p - gw 50 also determines the bearer bandwidth for the ue 10 and performs packet data forward and routing function . the wireless communication system is capable of further including a home subscriber server ( hss ) ( not shown ). the hss stores the subscriber information per ue . when the ue 10 attempts attachment to the network , the hss provides the mme 30 with the information related to the ue 10 for use in controlling the ue 10 . once it has connected to the enb 20 of the wireless communication system , the ue 10 connects to the ip network 60 through a data path consisting of the enb 20 , the s - gw 40 , and the p - gw 50 so as to exchange packet data . the ue 10 is also capable of transmitting a nas request to the mme 30 via the enb 20 . the nas message is capable of including request including at least one of attach request , tracking area update request , or service request . upon receiving the nas request message , the enb 20 selects mme 30 according to the network node selection function ( nnsf ) and sends the nas request message to the selected mme 30 . this is because the enb 20 is capable of being connected to a plurality of mmes 30 individually through s1 - mme interface . in this embodiment , although the description is directed to the case where the ue 10 is an mtc ue , the enb 20 is connected to the respective normal mme and mtc mme , the present invention is not limited thereto . that is , although the normal ue is replaced by mtc ue implemented with a specific function and the mme is replaced by mtc mme implemented to support other type of ue , the present invention is applicable . fig2 is a signaling diagram illustrating a connection procedure in the wireless communication system according to the first embodiment of the present invention . referring to fig2 , the connection procedure between the mtc ue 11 and mtc mme 330 starts in such a way that the mtc ue 11 establishes an rrc connection with the enb 20 . when it attaches to the radio network initially or enters the cell supporting the tracking area information , the mtc ue 11 is capable of performing initial rrc connection to the enb 20 to establish the connections to the mmes 30 , 31 , and 33 . the mtc ue 11 sends the enb 20 an rrc connection request message at step 111 . since it is the initial connection to the enb 20 , the mtc ue 11 sends the ue id in the form of a random value through in the rrc connection request message . upon receipt of the rrc connection request message , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 113 . upon receipt of the rrc connection setup message , the mtc ue 11 sends the enb 20 an rrc connection setup complete message at step 115 . at this time , the mtc ue 11 transmits the nas request message to the mtc mme 33 in the rrc connection setup complete message . here , the mtc ue 11 is capable of transmitting the rrc connection request message or the rrc connection setup complete message with an mtc indicator for indicating that the ue is the mtc ue . the mtc ue 11 is also capable of inserting the entity id of the mme entity 30 , 31 , or 33 to which it has connected previously in the rrc connection setup complete message . once the connection has been established with the mtc ue 11 , the enb 20 selects one of a plurality of mmes 30 , 31 , and 33 at step 117 . at this time , the enb 20 determines whether the rrc connection setup complete message includes an entity id . if an entity id is included , the enb selects the mme identified by the entity id . if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if it has no s1 - mme interface connection with the mme identified by the entity id , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . here , the enb 20 is capable of determining whether the rrc connection request message or the rrc connection setup complete message includes the mtc indicator . if no mtc indicator is included , the enb 20 selects the normal mme 31 . otherwise , if the mtc indicator is included , the enb 20 selects the mtc mme 33 . once the mtc mme 33 has been selected , the enb 20 sends the mtc mme 33 an initial ue message for the mtc ue 11 at step 119 . at this time , the enb 20 transmits the rrc connection setup complete message in the nas request message . upon receipt of the initial ue request message , the mtc mme 33 sends the mtc ue 11 an initial ue response message at step 121 via the enb 20 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . the mtc mme 33 also transmits the nas response message in the nas message . the mtc mme 33 is capable of transmitting global unique temporary id ( guti ) as the identity information for the mtc ue 11 in the nas response message . here , the guti includes the information on the carrier supported by the enb 20 connected currently to the mtc mme 33 , mme group id of the mme 33 , entity id of the mtc mme 33 , and mme - temporary mobile subscriber id ( m - tmsi ) which the mtc mme 33 allocates to the mtc ue 11 ; and the sae temporary mobile subscriber id consists of the entity id and m - tmsi . meanwhile , the mtc ue 11 is capable of re - attempting rrc connection with the enb 20 . that is , when it transitions from the idle mode to the active mode or enters a cell supporting the tracking area information that has been identified already , the mtc ue 11 is capable of attempting rrc connection to the enb 20 for re - establishing the connection to the mme 30 , 31 , or 33 to which it has connected . that is , the mtc ue 11 sends the enb 20 the rrc connection request message at step 141 . since it is a retry for connection to the enb 20 , the mtc ue 11 includes the s - tmsi as the ue id in the rrc connection request message . upon receipt of the rrc connection request message , the enb 20 sends the mtc ue 11 the rrc connection setup message at step 143 . upon receipt of the rrc connection setup message , the mtc ue 11 sends the enb 20 the rrc connection setup complete message at step 145 . at this time , the mtc ue 11 transmits the nas request message for the mtc mme 33 in the rrc connection setup complete message . once the mtc ue 11 has connected , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 147 . at this time , the enb 20 determines whether the rrc connection setup complete message includes the entity id . if the entity id is included , the enb 20 selects the mme identified by the entity id . that is , the enb 20 checks the entity id with s - tmsi included in the rrc connection request message and selects the entity matched with the entity id . if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . in case that it has not s1 - mme interface connection with the mme identified by the entity id , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . once the mtc mme 33 has been selected , the enb 20 sends the mtc mme 33 an initial ue request message for the mtc ue 11 at step 149 . at this time , the enb 20 transmits the nas request message carried in the rrc connection complete message . upon receipt of the initial ue request message , the mtc mme 33 sends the mtc ue 11 an initial ue response message via the enb 20 at step 151 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . the mtc mme 33 transmits the nas message including the nas response message . the operation procedure between the mme 30 , 31 , and 33 and the enb 20 according to an embodiment of the present invention is described hereinafter . fig3 is a flowchart illustrating the operation procedure of the mme 30 , 31 , or 33 of fig2 . referring to fig3 , if a nas request message is received from the ue 10 or 11 , the mme 30 , 31 , or 33 detects this at step 161 and determines whether to assign guto to the ue 10 or 11 at step 163 . that is , the mme 30 , 31 , or 33 determines whether the guti has been assigned to the ue 10 or 11 . if it is determined that the guti has not been assigned to the ue 10 or 11 at step 163 , the mme 30 , 31 , or 33 assigns a guti to the ue 10 or 11 at step 165 . the mme 30 , 31 , or 33 also sends the ue 10 or 11 the nas response message including the corresponding guti at step 167 . otherwise , if it is determined that the guto has been assigned to the ue 10 or 11 , the mme 30 , 31 , or 33 sends the ue 10 or 11 the nas response message via the enb 20 . fig4 is a flowchart illustrating the operation procedure of the enb 20 of fig2 . referring to fig4 , the enb 20 of the present embodiment establishes an rrc connection with the ue 10 or 11 at step 181 . if a nas request message is received from the ue 10 or 11 , the enb 20 detects the message and selects an mme 30 , 31 , or 33 at step 185 . if an entity ie is received along with the nas request message , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . if no entity id is received , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if an mtc indicator is received along with the nas request message , the enb 20 selects the mtc mme 33 . otherwise , if no mtc indicator is received , the enb 20 selects the normal mme 31 . the enb 20 sends the mme 30 , 31 , or 33 the nas request message at step 187 . if the nas response message is received from the mme 30 , 31 , 33 , the enb 20 detects this at step 189 and delivers the nas response message to the ue 10 or 11 at step 191 . although the above description has been directed to the exemplary case where the enb 20 selects the mtc mme 33 for the mtc ue 11 in initial rrc connection with the mtc ue 11 in the first embodiment of the present invention , the present invention is not limited thereto . that is , when selecting an mme 30 , 31 , or 33 arbitrarily , although the enb 20 selects the normal mme 31 , the present invention can be implemented . such examples are described in the second to sixth embodiments of the present invention . fig5 is a signaling diagram illustrating a connection procedure in the wireless communication according to the second embodiment of the present invention . referring to fig5 , the connection establishment procedure between the mtc ue 11 and the mtc mme 33 according the present embodiment starts in such a way that the mtc ue 11 attempts to establish an rrc connection to the enb 20 . when it attempts initial attachment to the radio network or enters a cell supporting the tracking area information , the mtc ue 11 is capable of establishing the initial rrc connection to the enb 20 to connect to a new mme 30 , 31 , or 33 . the mtc ue 11 sends the enb 20 an rrc connection request message at step 211 . since it is the initial connection to the enb 20 , the mtc ue 11 transmits a random value of the ue id in the rrc connection request message . if the rrc connection request message is received , the enb 20 sends an rrc connection setup message to the mtc ue 11 at step 213 . in response to the rrc connection setup message , the ue 11 sends an rrc connection complete message to the enb 20 at step 215 . at this time , the mtc ue 11 transmits an nas request message for the mtc mme 33 in the rrc connection complete message . here , the mtc ue 11 is capable of inserting the entity id of the mme 30 , 31 , or 33 to which it has connected in the rrc connection complete message . if the mtc ue 11 has connected , the enb 20 selects one of a plurality of mmes 30 , 31 , and 33 at step 217 . at this time , the enb 20 determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme 30 , 31 , or 33 identified by the entity id . otherwise , if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if there is no connection with the mme 30 , 31 , or 33 through the s1 - mme interface , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if the selected mme is the normal mme 31 , the enb 20 sends the normal mme 31 an initial ue request message for the mtc ue 11 at step 219 . at this time , the enb 20 transmits the nas request message carried in the rrc connection complete message . if the initial ue request message in received , the normal mme 31 checks that the nas request message is transmitted from the mtc ue 11 in the initial ue request message at step 221 . for example , the enb 20 delivers the mtc indicator received from the mtc ue 11 to the normal mme 31 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the normal mme 31 to identify the mtc ue 11 based on the mtc indicator included in the subscriber information of the mtc ue 11 which is transmitted by the hss . also , it is possible for the normal mme 31 to identify the mtc ue 11 based on the random value selected in the range allowed for normal ue as ue id . next , the normal mme 31 sends a guti allocation request message to the mtc mme 33 at step 223 . that is , the normal mme 31 requests the mtc mme 33 for the guti of the mtc ue 11 . in response to the guti allocation request message , the mtc mme 33 sends the normal mme 31 a guti allocation response message at step 225 . that is , the mtc mme 33 provides the normal mme 331 with the guti as the identity information for the mtc ue 11 . here , the guti includes the information on the carrier supported by the enb 20 connected currently to the mtc mme 33 , mme group id of the mme 33 , entity id of the mtc mme 33 , and mme - temporary mobile subscriber id ( m - tmsi ) which the mtc mme 33 allocates to the mtc ue 11 ; and the s - tmsi consists of the entity id and m - tmsi . if the guti allocation response message is received , the normal mme 31 is capable of transmits ue context of the mtc ue 11 to the mtc mme 33 at step 227 . next , the normal mme 31 sends the mtc ue 11 an initial ue response message via the enb 20 at step 229 . at this time , the normal mme 31 generates the nas response message by processing the request data included in the nas request message . the normal mme 31 also includes the guti for the mtc ue 11 in the nas response message . meanwhile , the mtc ue 11 is capable of retries rrc connection to the enb 20 . that is , when it wakes up and transitions from the idle mode to the active mode or enters the cell supporting the tracking area information that has been identified already , the mtc ue 11 is capable of retrying rrc connection to the enb 20 for reconnection to the mme 30 , 31 , or 33 . that is , the mtc ue 11 transmits the rrc connection request message to the enb 20 at step 241 . since it is the retry for connection , the mtc ue 11 transmits the rrc connection request message configured with the s - tmsi as the ue id . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 the rrc connection setup message at step 243 . if the rrc connection setup message is received , the mtc ue 11 sends the rrc connection complete message to the enb 20 at step 245 . at this time , the mtc ue 11 transmits the nas request message for the mtc mme 33 in the rrc connection complete message . once the mtc ue 11 has connected , the enb 20 selects one of the plural mmes 30 , 31 , or 33 at step 247 . at this time , the enb 20 determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme identified by the entity id . that is , the enb 20 checks the entity id based on the s - tmsi included in the rrc connection request message and selects the mme 30 , 31 , or 33 matched to the entity id . if not entity id is included , the enb selects an mme 30 , 31 , or 33 arbitrarily . if there is no connection with the mme 30 , 31 , or 33 matched to the entity id through s1 - mme interface , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . once the mtc mme 33 has been selected , the enb 20 sends the mtc mme 22 the initial ue request message for the mtc ue 11 at step 249 . here , the enb 20 transmits the nas request message in the rrc connection complete message . if the initial ue request message is received , the mtc mme 33 is capable of sending the normal mme 31 a ue context request message for the mtc ue 11 at step 251 . if the ue context request message is received , the normal mme 31 is capable of sending the mtc mme 33 a ue context response message including the ue context at step 253 . afterward , the mtc mme 33 sends the mtc ue 11 the initial ue response message via the enb 20 at step 255 . at this time , the mtc mme 33 generates the nas message by processing the request data included in the nas request message . the mtc mme 33 also transmits the nas response message in the nas message . descriptions are made of the operation procedures of the normal mme 31 and mtc mme 33 hereinafter . since the operation procedure of the enb 20 in the present embodiment is similar to that of the first embodiment of the present invention , detailed description thereon is omitted herein . fig6 is a flowchart illustrating the operation procedure of the normal mme 31 of fig5 . referring to fig6 , if an nas request message is received from the ue 10 or 11 , the normal mme 31 detects this at step 261 and determines whether to allocate guti to the ue 10 or 11 at step 263 . that is , the normal mme 31 determines whether the ue 10 or 11 has been assigned the guti already . if it is determined to allocate guti at step 263 , the normal mme 31 determines whether the ue 10 or 11 is the mtc ue 11 at step 265 . if it is determined that the ue 10 or 11 is the mtc ue 11 at step 265 , the normal mme 31 sends the mtc mme 33 a guti allocation request message at step 267 . afterward , if a guti allocation response message is received from the mtc mme 33 , the normal mme 31 detects this at step 269 and sends the ue 10 or 11 a nas response message including the corresponding guti at step 271 . otherwise , if it is determined that the ue 10 or 11 is not the mtc ue 11 at step 265 , the normal mme 31 allocates a guti to the ue 10 or 11 at step 270 . next , the normal mme 31 sends the ue 10 or 11 the nas response message including the guti at step 271 . if it is determined that there is no need to allocate guti to the ue 10 or 11 at step 263 , the normal mme 31 sends the ue 10 or 11 a nas response message via the enb 20 at step 275 . fig7 is a flowchart illustrating the operation procedure of the mtc mme 33 of fig5 . referring to fig7 , if a guti allocation request message is received from the normal mme 31 , the mtc mme 33 detects this at step 281 and sends the normal mme 31 a guti allocation response message at step 283 . if no guti allocation request message is received but a nas request message is received from the ue 10 or 11 , the mtc mme 33 detects this at step 285 and sends the ue 10 or 11 the nas response message via the enb 20 at step 287 . although the description has been directed to the case where the normal mme 31 and mtc mme 33 communicate to each other directly in the second embodiment of the present invention , the present invention is not limited thereto . that is , even when the normal mme 31 and the mtc mme 33 are not communication directly , the present invention can be implemented . such an example is described in the third embodiment of the present invention hereinafter . fig8 is a signaling diagram illustrating a connection procedure in the wireless communication system according to the third embodiment of the present invention . referring to fig8 , the connection procedure between the mtc ue 11 and the mtc 33 according to the third embodiment starts in such a way that the normal mme 31 retains the list of gutis , i . e . mtc gutis , as the identity information that can be allocated by the mtc mme 33 at step 311 . at this time , the mtc mme 33 sends the list of the mtc gutis directly to the normal mme 31 such that the normal mme 31 stores the mtc guti list . the mtc mme 33 registers the mtc guti list with an operation and management ( o & amp ; m ) server ( not shown ) which provides the normal mme 31 with the mtc guti such that the normal mme 31 is capable of storing the list of the mtc gutis . here , the guti includes the information on the carrier supported by the enb 20 connected currently to the mtc mme 33 , mme group id of the mme 33 , entity id of the mtc mme 33 , and mme - temporary mobile subscriber id ( m - tmsi ) which the mtc mme 33 allocates to the mtc ue 11 ; and the s - tmsi consists of the entity id and m - tmsi . next , the mtc ue 11 attempts the rrc connection to the enb 20 . when it attempts initial attachment to the radio network or enters the cell supporting the tracking area information , the mtc ue 11 is capable of attempting the initial rrc connection to the enb 20 to establishing connection to the mme 30 , 31 , or 33 . that is , the mtc ue 11 sends the enb 20 an rrc connection request message at step 313 . since it is the initial attachment to the enb 20 , the mtc ue 11 sends a random value as the ue id in the rrc connection request message . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 315 . in response to the rrc connection setup message , the mtc ue 11 sends the enb 20 an rrc connection complete message at step 317 . at this time , the mtc ue 11 transmits a nas request message for the mtc mme 33 in the rrc connection complete message . here , the mtc ue 11 is capable of further including the entity id of the mme 30 , 31 , or 33 to which it has connected previously in the rrc connection complete message . once the mtc ue 11 has connected , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 319 . at this time , the enb 20 determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . otherwise , if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if it is not connected to the mme 30 , 31 , or 33 match with the entity id through s1 - mme interface , the enb selects an mme 30 , 31 , or 33 arbitrarily . if the normal mme 31 is selected , the enb 20 sends the normal mme 31 an initial ue request message addressed to the mtc ue 11 at step 321 . at this time , the enb 20 transmits the nas request message carried in the rrc connection complete message . if the initial ue request message is received , the normal mme 31 checks that the nas message carried in the initial ue request message has been transmitted by the mtc mme 11 at step 323 . for example , the enb 20 transmits the mtc indicator received from the mtc ue 11 to the normal mme 31 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the hss to transmit the mtc indicator in the subscriber information of the mtc ue 11 to the normal mme 31 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the mtc ue 11 uses a random value selected in the range discriminated from that for the normal ue such that the normal mme 31 identifies the mtc ue 11 . the normal mme 31 determines the guti for the mtc ue 11 from the mtc guti list and marks the guti as being used at step 324 . the normal mme 31 is capable of transmitting the ue context of the mtc ue 11 to the mtc mme 33 at step 325 and then checking that the guti for the mtc ue 11 is not used from the mtc guti list at step 326 . next , the normal mme 31 sends the mtc ue 11 an initial ue response message via the enb 20 at step 327 . at this time , the normal mme 31 generates a nas response message by processing the request data in the nas request message . the normal mme 31 transmits the nas response message in the nas message . the normal mme 31 is also capable of transmitting the guti selected from the mtc guti list in the nas response message . the mtc ue 11 is capable of retrying the rrc connection to the enb 20 . after wake - up from the idle mode when it transitions from the idle mode to the active mode or enters the cell supporting the tracking area information that has been identified already , the mtc ue 11 is capable of retrying the rrc connection to the enb 20 to reestablish the connection to the mme 30 , 31 , or 33 to which it has connected previously . that is , the mtc ue 11 sends the enb 20 an rrc connection request message at step 341 . since it is the retry of the connection to the enb 20 , the mtc ue 11 transmits the rrc connection request message with the 5 - tmsi as the ue id . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 343 . in response to the rrc connection setup message , the mtc ue 11 sends the enb 20 an rrc connection complete message at step 345 . at this time , the mtc ue 11 transmits the nas request message for the mtc mme 33 in the rrc connection complete message . if the mtc ue 11 has connected , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 347 . at this time , the enb determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme 30 , 31 , or 33 matched with entity id . that is , the enb 20 checks the entity id based on the s - tmsi included in the rrc connection request message and selects the mme 30 , 31 , or 33 matched with the entity id . if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . also , if it has not connected to the mme 30 , 31 , or 33 matched with the entity id through s1 - mme interface , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . once the mtc mme 33 has been selected , the enb 20 sends the mtc mme 33 an initial ue request message for the mtc ue 11 at step 349 . here , the enb 20 transmits the nas request message carried in the rrc connection complete message . if the initial ue request message is received , the mtc mme 33 is capable of transmitting a ue context request message for the mtc ue 11 to the normal mme 31 at step 351 . if the ue context request message is received , the normal mme 31 sends the mtc mme 33 a ue context response message including the ue context at step 353 and marks the guti for the mtc ue 11 as not being used in the mtc guti list at step 354 . although not depicted , when the ue context request message is received , the normal mme 31 is capable of checking the guti for the mtc ue 11 as being not used in the mtc guti list and then transmits the ue context response message . afterward , the mtc mme 33 sends the mtc ue 11 an initial ue response message via the enb 20 at step 355 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . the mtc mme 33 transmits the nas response message in the nas message . a description is made of the operation procedure of the normal mme 31 according to this embodiment hereinafter . since the operation procedures of the enb 20 and the mtc mme 33 according to this embodiment are similar to those in the first embodiment , detailed descriptions thereon are omitted herein . fig9 is a flowchart illustrating the operation procedure of the normal mme 31 of fig8 . referring to fig9 , the normal mme 31 retains the mtc guti list in the embodiment at step 361 . at this time , the normal mme 31 also stores a list of gutis that the normal mme 31 can allocate , i . e . normal guti list in addition to the mtc guti list . if a nas request message is received from the ue 10 or 11 , the normal mme 31 detects this and determines whether to allocate guti to the ue 10 or 11 at step 363 . that is , the normal mme 31 determines whether it has allocated a guti to the ue 10 or 11 previously . if it is determined to allocate a guti to the ue 10 or 11 at step 365 , the normal mme 31 determines whether the ue 10 or 11 is an mtc ue 11 at step 367 . if it is determined that the ue 10 or 11 is the mtc ue 11 at step 367 , the normal mme 31 allocates an guti selected from the mtc guti list to the ue 10 or 11 . afterward , the normal mme 31 sends the ue 10 or 11 a nas response message including the corresponding guti at step 371 . otherwise , if it is determined that the ue 10 or 11 is not the mtc ue 11 at step 367 , the normal mme 31 allocates the guti selected from the normal guti rest to the ues 10 or 11 at step 370 . next , the normal mme 31 sends the ue 10 or 11 the nas response message including the corresponding guti at step 371 . if it is not necessary to allocate a guti to the ue 10 or 11 at step 365 , the normal mme 31 sends the ue 10 or 11 the nas response message via the enb 20 at step 375 . although the description has been directed to the case where normal mme 31 delivers the guti allocated by the mtc mme 33 to the mtc ue 11 in the initial rrc connection between the mtc ue 11 and the enb 20 in the second and third embodiments , the present invention is not limited thereto . that is , the present invention can be implemented in such a way that the mtc mme 33 is capable of allocating and transmitting the guti for the mtc ue 11 . such an example is described hereinafter in the fourth embodiment of the present invention . fig1 is a signaling diagram illustrating a connection procedure in the wireless communication system according to the fourth embodiment of the present invention . referring to fig1 , the connection procedure between the mtc ue 11 and the mtc mme 33 according to the this embodiment starts in such a way that the mtc ue 11 attempts rrc connection to the enb 20 . at this time , when it tries initial attachment to the radio network or enters the cell supporting the tracking area information , the mtc ue 11 is capable of initial rrc connection to the enb 20 to establish the connection to a new mme 30 , 31 , or 33 . that is , the mtc ue 11 sends the enb 20 the rrc connection request message at step 411 . since it is the initial attachment , the mtc ue 11 transmits a random value as the ue id in the rrc connection request message . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 413 . if the rrc connection setup message is received , the mtc ue 11 sends an rrc connection complete message to the enb 20 at step 415 . at this time , the mtc ue 11 transmits a nas request message for the mtc mme 33 in the rrc connection complete message . here , the mtc ue 11 is capable of further including the entity id of the mme 30 , 31 , or 33 to which is has connected previously in the rrc connection complete message . once the mtc ue 11 has connected , the enb 20 selects one of a plurality of mmes 30 , 31 , and 33 at step 417 . at this time , the enb 20 determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . also , if it has not connected to the mme 30 , 31 , or 33 matched with the entity id via s1 - mme interface , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . once the normal mme 31 has been selected , the enb 20 sends the normal mme 31 an initial ue request message for the mtc ue 11 at step 419 . at this time , the enb 20 transmits the nas request message carried in the rrc connection complete message . if the initial ue request message is received , the normal mme 31 determines whether the nas request message carried in the initial ue request message is transmitted by the mtc ue 11 at step 421 . for example , the enb 20 transmits the mtc indicator received from the mtc ue 11 to the normal mme 31 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the hss to transmit the mtc indicator in the subscriber information of the mtc ue 11 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the mtc ue 11 to use a random value selected in the range discriminated from that for the normal ue such that the normal mme 31 identifies the mtc ue 11 . next , the normal mme 31 sends the mtc mme 33 an initial ue request message for the mtc ue 11 at step 423 . here , the normal mme 31 is capable of transmitting the initial ue request message using the tunneling technique . if the initial ue request message is received , the mtc mme 33 is capable of transmitting to the normal mme 31 a ue context request message for the mtc ue 11 additionally at step 425 . if the ue context request message is received , the normal mme 31 is capable of transmitting a ue context response message including the ue context to the mtc mme 33 at step 427 . here , the mtc mme 33 and the mtc ue 11 are capable of perform nas communication via the enb 20 and the normal mme 31 at step 429 . that is , the mtc mme 33 and the mtc ue 11 are capable of generating and exchanging nas messages . here , the normal mme 31 is capable of exchanging the nas messages with the mtc mme 33 using the tunneling technique . next , the mtc mme 33 sends the normal mme 31 an initial ue response message at step 431 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . here , the mtc mme 33 is capable of transmitting the nas response message using the tunneling technique . the mtc mme 33 is capable of transmitting the guti allocated as identity information of the mtc ue 11 in the nas response message . afterward , if the initial ue response message is received , the normal mme 31 transmits the initial ue response message to the mtc ue 11 via the enb 20 at step 433 . meanwhile , the mtc ue 11 is capable of retrying rrc connection to the enb 20 . after wake - up from the idle mode , when it transitions from the idle mode to the active mode or enters the cell supporting the tracking area information which has been known already , the mtc ue 11 is capable of retrying the rrc connection to the enb 20 for reestablishing the connection to the mme 30 , 31 , or 33 to which the mtc mme has connected previously . that is , the mtc ue 11 sends the enb 20 the rrc connection request message at step 441 . since it is reconnection to the enb 20 , the mtc ue 11 transmits the rrc connection request message in which the ue id is set to the s - tmsi . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 443 . if the rrc connection setup message is received , the mtc ue 11 sends the enb 20 an rrc connection complete message at step 445 . at this time , the mtc ue 11 transmits the nas request message for the mtc mme 33 in the rrc connection complete message . once the mtc terminal 11 has connected , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 447 . at this time , the enb 20 determines whether the rrc connection complete includes an entity id . if an entity id is included , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . that is , the enb 20 checks the entity id from the s - tmsi of the rrc connection request message and selects the mme 30 , 31 , or 33 matched with the entity id . otherwise , if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . also , if it has not connected to the mme 30 , 31 , or 33 matched with the entity id , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . once the mtc mme 33 has been selected , the enb 20 sends the mtc mme 33 an initial ue request message for the mtc ue 11 at step 449 . here , the enb 20 transmits the nas request message carried in the rrc connection complete message . if the initial ue request message is received , the mtc mme 33 sends the mtc ue 11 an initial ue response message via the enb 20 at step 451 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . the mtc mme 33 transmits the nas response message in the nas message . a description is made of the operation procedure of the normal mme 31 according to this embodiment hereinafter . since the operation procedures of the enb 20 and the mtc mme 33 according to this embodiment are similar to those of the first embodiment of the present invention , detailed descriptions thereon are omitted herein . fig1 is a flowchart illustrating the operation procedure of the normal mme 31 of fig1 . referring to fig1 , if an nas request message is received from the ue 10 or 11 , the normal mme 31 detects this at step 461 and determines whether to allocate a guti to the ue 10 or 11 at step 463 . that is , the normal mme 31 determines whether the ue 10 or 11 has been allocated a guti already . if it is determined that the ue 10 or 11 has been allocated a guti already at step 463 , the normal mme 31 determines whether the ue 10 or 11 is the mtc ue 11 at step 465 . if it is determined that the ue 10 or 11 is the mtc ue 11 at step 465 , the normal mme 31 sends the mtc mme 33 a nas request message at step 467 . afterward , if an nas response message including the guti for the ue 10 or 11 is received , the normal mme 31 detects this at step 469 and delivers the nas response message including the corresponding guti to the ue 10 or 11 at step 471 . otherwise , if it is determined that the ue 10 or 11 is not the mtc ue 11 at step 465 , the normal mme 31 allocates a guti for the ue 10 or 11 at step 470 . the normal mme 31 delivers the nas response message to the ue 10 or 11 at step 471 . at this time , the normal mme 31 transmits the nas response message including the corresponding guti . if it is determined that there is no need to allocate a guti to the ue 10 or 11 at step 463 , the normal mme 31 sends the ue 10 or 11 the nas response message via the enb 20 . although the description is directed to the case , when the enb 20 selects the mme 30 , 31 , or 33 for the mtc ue 11 , the mme 30 , 31 , or 33 performs operation for allocating guti to the mtc 11 in the second to fourth embodiments of the present invention , the present invention is not limited thereto . that is , the present invention is capable of being implemented in such a way that , as well as the mme 30 , 31 , or 33 , the enb 20 performs the operation for allocation guti to the mtc ue 11 . such examples are described in the fifth and sixth embodiments of the present invention hereinafter . fig1 is a signaling diagram illustrating the connection procedure in the wireless communication system according to the fifth embodiment of the present invention . referring to fig1 , the connection procedure between the mtc ue 11 and the mtc mme 33 according to this embodiment starts in such a way that the mtc ue 11 attempts rrc connection to the enb 20 . when it attempts initial connection to the radio network or enters a cell supporting the tracking area information which has not been recognized , the mtc ue 11 is capable of attempting initial rrc connection to the enb 20 to establish the connection to a new mme 30 , 31 , or 33 . that is , the mtc ue 11 sends the enb 20 an rrc connection request message at step 511 . since it is the attempt for initial attachment t 0 the enb 20 , the mtc ue 11 transmits the rrc connection request message including a random value set as the ue id . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 513 . if the rrc connection setup message is received , the mtc ue 11 sends the enb 20 an rrc connection complete message at step 515 . at this time , the mtc ue 11 transmits the nas request message for the mtc mme 33 in the rrc connection complete message . here , the mtc ue 11 is capable of transmitting the rrc connection complete message including the entity id of the mme 30 , 31 , or 33 to which it has connected previously . once the mtc ue 11 has connected , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 517 . at this time , the enb determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme entity 30 , 31 , or 33 matched with the entity id . if no entity id is included , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . also , if it has not connected to the mme 30 , 31 , or 33 matched with the entity id via s1 - mme interface , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if the normal mme 31 has been selected , the enb 20 sends the normal mme 31 an initial ue request message for the mtc ue 11 at step 519 . at this time , the enb 20 transmits the nas request message carried in the rrc connection complete message . here , the enb 20 is capable of storing the initial ue request message or the nas request message . if the initial ue request message is received , the normal mme 31 checks that the nas request message carried in the initial ue request message has been transmitted by the mtc ue 11 at step 521 . for example , the enb 20 is capable of transmitting the mtc indicator received from the mtc ue 11 to the normal mme 31 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the hss to transmit the mtc indicator in the subscriber information of the mtc ue 11 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the mtc ue 11 to use a random value selected in the range discriminated from that for the normal ue such that the normal mme 31 identifies the mtc ue 11 . next , if the mtc ue 11 has been identified , the normal mme 31 sends the enb 20 an mme reselection request ( ue redirect request ) message at step 523 . at this time , the normal mme 31 in capable of transmitting the mme reselection request message including the information on the mtc mme 33 , e . g . entity id . here , the normal mme 31 is capable of transmitting the nas request message of the mtc ue 11 in the mme reselection request message . next , if the mme reselection request message is received , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 525 . at this time , the enb selects the mtc mme 33 . herein , the enb 20 determines whether the mme reselection request message includes an entity id . if an entity id is included , the enb 20 selects the mtc mme 33 matched to the entity id . otherwise , if no entity id is included , the enb 20 selects an mtc mme 33 arbitrarily . also , if it has not connected to the mme 33 matched with the entity id via s1 - mme interface , the enb 20 selects the mtc mme 33 arbitrarily . next , if the mtc mme 33 has been selected , the enb 20 sends the mtc mme 33 an initial ue request message for the mtc ue 11 at step 527 . the mtc mme 33 sends the mtc ue 11 an initial ue response message via the enb 20 at step 529 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . the mtc mme 33 transmits the nas response message in the nas message . the mtc mme 33 is also capable of transmitting the nas response message including the guti allocated as the identity information of the mtc ue 11 . the mtc ue 11 is capable of retrying rrc connection to the enb 20 . that is , after wake - up from the idle mode , when it transitions from the idle mode to the active mode or enters a cell supporting the tracking area information which has not been recognized until then , the mtc ue 11 is capable of retrying rrc connection to the enb 20 to reestablish the connection to the mme 30 , 31 , or 33 to which it has connected previously . next , the mtc ue 11 is capable of attempting connection to the mtc mme 33 via the enb 20 . since the connection procedure between the mtc ue 11 and the mtc mme 33 is similar to steps 441 to 451 of fig1 , detailed description thereon is omitted herein . descriptions are made of the operation procedures of the normal mme 31 and the enb 20 according to the present embodiment hereinafter . since the operation procedure of the mtc mme 33 according to this embodiment is similar to that of the first embodiment of the present invention , detailed description thereon is omitted herein . fig1 is a flowchart illustrating the operation procedure of the normal mme 31 of fig1 . referring to fig1 , if the nas request message is received from the ue 10 or 11 , the normal mme 31 detects this at step 561 and determines whether to allocate a guti to the ue 10 or 11 at step 563 . that is , the normal mme 31 determines whether the ue 10 or 11 has been allocated a guti already . if it is determined to allocate a guti to the ue 10 or 11 at step 563 , the normal mme 31 determines whether the ue 10 or 11 is the mtc ue 11 at step 565 . if it is determined that the ue 10 or 11 is the mtc ue 11 , the normal mme 31 sends the enb an mme reselection request message at step 567 . otherwise , if it is determined that the ue 10 or 11 is not the mtc ue 11 at step 565 , the normal mme 31 allocates a guti to the ue 10 or 11 at step 569 . next , the normal mme 31 sends the ue 10 or 11 a nas response message at step 571 . at this time , the normal mme 31 transmits the nas response message including the corresponding guti . if it is determined not to allocate a guti to the ue 10 or 11 at step 563 , the normal mme 31 sends the ue 10 or 11 a nas response message via the enb 20 at step 573 . fig1 is a flowchart illustrating the operation procedure of the enb 20 of fig1 . referring to fig1 , the enb 20 tries to establish rrc connection with the ue 10 or 11 at step 581 . afterward , if a nas request message is received from the ue 10 or 11 , the enb 20 detects this at step 583 and selects an mme 30 , 31 , or 33 at step 585 . at this time , if an entity id is received in the nas request message , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . if no entity id is received , the enb selects an mme entity 30 , 31 , or 33 arbitrarily . if an mtc indicator is received in the nas request message , the enb 20 selects the mtc mme 33 . if no mtc indicator is received , the enb 20 selects the normal mme 31 . the enb 20 delivers the nas request message to the mme 30 , 31 , or 33 at step 587 . next , if an mme reselection request message is received from the mme 30 , 31 , or 33 , the enb 20 detects this at step 589 and reselects an mme 30 , 31 , or 33 at step 591 . at this time , the enb 20 selects the mtc mme 33 . at this time , if an entity id is received in the mme reselection request message , the enb 20 selects the mtc mme 33 matched with the entity id . if no entity id is received , the enb 20 selects the mtc mme 33 arbitrarily . the enb 20 delivers the nas request message to the reselected mme 30 , 31 , or 33 at step 593 . afterward , if a nas response message is received from the mme 30 , 31 , or 33 , the enb detects this at step 595 and delivers the nas response message to the ue 10 or 11 at step 597 . although the description is directed to the case where the enb 20 retransmits the nas request message in the fifth embodiment of the present invention , the present invention is not limited thereto . that is , the present invention can be implemented in such a way that the mtc ue 11 retransmits the nas request message . such an example is described in the sixth embodiment of the present invention of the present invention . fig1 is a signaling diagram illustrating a connection procedure in the wireless communication system according to the sixth embodiment of the present invention . referring to fig1 , the connection procedure between the mtc ue 11 and the mtc mme 33 starts in such a way that the mtc ue 11 attempts rrc connection to the enb 20 . at this time , when it attaches to the network initially or enters a cell supporting the tracking information which has not been recognized yet , the mtc ue 11 is capable of trying initial rrc connection to the enb 20 to establish a connection to a new mme 30 , 31 , or 33 . that is , the mtc ue 11 sends an rrc connection request message to the enb 20 at step 611 . since it is the initial connection attempt to the enb 20 , the mtc ue 11 transmits a random value as a ue id in the rrc connection request message . if the rrc connection request message is received , the enb 20 sends the mtc ue 11 an rrc connection setup message at step 613 . if the rrc connection setup message is received , the mtc ue 11 sends the enb 20 an rrc connection complete message at step 615 . at this time , the mtc ue 11 transmits a nas request message for the mtc mme 33 in the rrc connection complete message . here , the mtc ue 11 is capable of transmitting the entity id of the mme 30 , 31 , or 33 to which it has connected previously in the rrc connection complete message . next , if the mtc ue 11 has connected , the enb 20 selects one of a plurality of mmes 30 , 31 , and 33 at step 617 . at this time , the enb 20 determines whether the rrc connection complete message includes an entity id . if an entity id is included , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . if no entity id is included , the enb 20 selects an mme 30 , 31 , or 31 arbitrarily . also , if it has not connected with the mme 30 , 31 , or 33 matched with the entity id through s1 - mme interface , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . once the normal mme 31 has been selected , the enb 20 sends the normal mme 31 an initial ue request message for the mtc ue 11 at step 619 . at this time , the enb 20 delivers the nas request message carried in the rrc connection complete message . if the initial ue request message is received , the normal mme 31 checks that the nas request message carried in the initial ue request message has been transmitted by the mtc ue 11 . for example , the enb 20 transmits the mtc indicator received from the mtc ue 11 to the mme 31 such that the mme 31 identifies the mtc ue 11 . also , it is possible for the hss to transmit the mtc indicator in the subscriber information of the mtc ue 11 to the normal mme 31 such that the normal mme 31 identifies the mtc ue 11 . also , it is possible for the mtc ue 11 to use a random value selected in the range discriminated from that for the normal ue as the ue id such that the normal mme 31 identifies the mtc ue 11 . next , if the mtc ue 11 has been identified , the normal mme 31 sends the enb 20 a mme reselection request message at step 623 . at this time , the normal mme 31 is capable of the information or the mtc mme 33 , i . e . entity id , in the mme reselection request message . afterward , the normal 31 delivers the nas retransmission request message to the mtc ue 11 at step 625 . at this time , the normal mme 31 is capable of the nas retransmission request message through nas communication via the enb 20 . if the nas retransmission request message is received , the mtc ue 11 retransmits the nas request for the mtc mme 33 at step 627 . at this time , the mtc ue 11 is capable of transmitting the nas request message through nas communication . next , if the retransmitted nas request message is received , the enb 20 selects one of the plural mmes 30 , 31 , and 33 at step 629 . at this time , the enb 20 selects the mtc mme 33 . here , the enb 20 determines whether the mme reselection request message includes an entity id . if an entity id is included , the enb selects the mtc mme 33 matched with the entity id . otherwise , if no entity id is included , the enb 20 selects the mtc mme 33 arbitrarily . also , if it has not connected to the mtc mme 33 matched with the entity id through the s1 - mme interface , the enb selects the mtc mme 33 arbitrarily . once the mtc mme 33 has been selected , the enb 20 sends the mtc mme 33 an initial ue request message for the mtc ue 11 at step 631 . the mtc mme 33 sends the mtc ue 11 an initial ue response message via the enb 20 at step 633 . at this time , the mtc mme 33 generates the nas response message by processing the request data in the nas request message . the mtc mme 33 transmits the nas response message in a nas message . the mtc mme 33 is also capable of transmitting the nas response message including a guti allocated as the identifier information of the mtc ue 11 . the mtc mme 11 is capable of retrying the rrc connection to the enb 20 . that is , when it wakes up , i . e . transitions from the idle mode to the active mode or enters the cell supporting the tracking area information which has been recognized previously , the mtc ue 11 is capable of retrying the rrc connection to the enb 20 to reestablish the connection to the mme 30 , 31 , or 33 to which the mtc ue 11 has connected previously . the mtc ue 11 is capable of trying to connect to the mtc mme 33 via the enb 20 . since the connection procedure between the mtc ue 11 and the mtc mme 33 is similar to steps 441 to 451 of fig1 that has been described above , detailed description thereon is omitted herein . the operation procedures of the normal mme 31 and the enb 20 according to the present invention embodiment are described hereinafter . since the operation procedure of the mtc mme 33 according to the present embodiment is similar to that of the first embodiment of the present invention , detailed description thereon is omitted herein . fig1 is a flowchart illustrating the operation procedure of the normal mme 31 of fig1 . referring to fig1 , if a nas request message is received from the ue 10 or 11 , the normal me 31 detects this at step 661 and determines whether to allocate a guti to the ue 10 or 11 at step 663 . that is , the normal mme 31 determines whether the ue 10 or 11 has been allocated a guti already . if it is determined to allocate a guti to the ue 10 or 11 at step 663 , the normal mme 31 determines whether the ue 10 or 11 is the mtc ue 11 at step 665 . if it is determined that the ue 10 or 11 is the mtc ue 11 at step 665 , the normal mme 31 sends the enb 20 an mme reselection request message at step 667 . next , the normal mme 31 sends the mtc ue 11 a nas retransmission request message via the enb 20 at step 669 . otherwise , if it is determined that the ue 10 or 11 is no the mtc ue 11 at step 665 , the normal mme 31 allocates a guti to the ue 10 or 11 at step 671 . the normal mme 31 sends the ue 10 or 11 a nas response message at step 673 . at this time , the normal mme 31 transmits the nas response message including the corresponding guti . if it is determined that there is no need to allocate a guti to the ue 10 or 11 at step 663 , the normal mme 31 sends the ue 10 or 11 the nas response message via the enb 20 at step 675 . fig1 is a flowchart illustrating the operation procedure of the enb 20 of fig1 . referring to fig1 , the enb 20 establishes an rrc connection with the ue 10 or 11 at step 681 . if a nas request message is received from the ue 10 or 11 , the enb 20 detects this at step 683 and selects an mme 30 , 31 , or 33 at step 685 . at this time , if an entity id is received along with the nas request message , the enb 20 selects the mme 30 , 31 , or 33 matched with the entity id . if no entity id is received , the enb 20 selects an mme 30 , 31 , or 33 arbitrarily . if an mtc indicator is received along with the nas request message , the enb 20 selects the mtc mme 33 . if no mtc indicator is received , the enb 20 selects the normal mme 31 . the enb 20 delivers the nas request message to the mme 30 , 31 , or 33 at step 687 . next , if an mme reselection request message is received from the mme 30 , 31 , or 33 , the enb 20 detects this at step 689 . afterward , if a nas retransmission request message is received from the mme 30 , 31 , or 33 , the enb 20 detects this at step 691 and delivers the nas retransmission request message to the mtc ue 11 at step 693 . if a nas request is received , the enb 20 detects this at step 695 and reselects an mme 30 , 31 , or 33 at step 697 . at this time , the enb 20 selects the mtc mme 33 . here , if an entity id is received in the mme reselection request message , the enb 20 selects the mtc mme 33 . otherwise , if not entity id is received , the enb selects the mtc mme 33 arbitrarily . the enb 20 delivers the nas request message to the reselected entity 30 , 31 , or 33 . if a nas response message from the mme 30 , 31 , or 33 , the enb 20 detects this at step 701 and delivers the nas response message to the ue 10 or 11 at step 703 . according to the above - described embodiments , it is possible to connect the mtc ue 11 to the mtc mme 33 efficiently in the wireless communication system . that is , the mtc ue 11 can connect to the mme 33 efficiently through cooperation between enb 20 and normal mme 31 or normal mme 31 and mtc mme 33 . although the description is directed to the connection procedure between mtc ue 11 and the mtc mme 33 in the wireless communication system , the present invention is not limited thereto . that is , the present invention also can be implemented by connecting the normal ue to the normal mme 31 efficiently through cooperation between the enb 20 and the normal mme 31 or the normal mme 31 and mtc mme 33 . in the wireless communication system , it is possible for connecting the ue 10 or 11 to the mme 30 , 31 , or 33 corresponding to the supplementary function efficiently . that is , the ue 10 or 11 is capable being connected to the mme 30 , 31 , or 33 efficiently through cooperation between the enb 20 and the mme 30 , 31 , or 33 or among the mmes 30 , 31 , and 33 supporting different supplementary functions . although the descriptions have been directed to the case where the connection between the ue and the mme is established in association with a specific supplementary function , the present invention is not limited thereto . that is , the present invention can be implemented in such a way that the connection between the ue and the mme is established according to the load status of the mme . for example , if the enb request for the identity information of a ue , the mme checks the current load status . at this time , the mme determines whether the current load is greater than a predetermined threshold value , i . e . whether overload occurs . if it is determined that the current load is not greater than the threshold value , i . e . no overload occurs , the mme is capable of allocating the identity information to the ue . otherwise , if it is determined that the current load is greater than the threshold value , i . e . overload occurs , the mme requests another mme for the identity information of the ue . that is , if overload occurs , the mme suspends the connection of the ue and request another mme for the identity information . in this way , the other mme is capable of allocating identity information to the ue . here , the mme is capable of transmitting the identity information to the ue via the other mme . furthermore , the ue is capable of trying connection to another mme using the corresponding identity information . according to the present invention , it is possible to connect a ue to an mme efficiently in the wireless communication system . that is , the ue is capable of being connected to an mme efficiently through cooperation between the enb and the mme or among the mmes . at this time , the mmes is capable of cooperating among each other according to the supportable supplementary function or load status . although exemplary embodiments of the present invention have been described in detail hereinabove with specific terminology , this is for the purpose of describing particular embodiments only and not intended to be limiting of the invention . while particular embodiments of the present invention have been illustrated and described , it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention . | 7 |
the invention includes several large components which are assembled on the horse . these components are shown laid out flat in fig . 1 . main wrap 10 is sized to pass around a horse &# 39 ; s mid section . it is made of a flexible and elastic fabric material . it will stretch when placed under tension . each end features a rolling stay 18 , which is a semi - rigid bar ( made of material which is substantially more rigid that the elastic material of the main wrap ) slipped into a stitched pocket . these rolling stays allow a user to easily grasp an end of the main wrap at a single point . the device could function without the rolling stays , but would be more cumbersome to handle . their operation will be more fully described subsequently . each end of the main wrap also features a bridging strap 26 extending outward . these will be used to temporarily secure the main wrap to the horse while the other components are positioned . ventral window 22 is located in the middle of the main wrap . the window is flanked by a pair of window stays 20 . these are similar to the rolling stays , except that they maybe affixed permanently . mesh panel 24 covers the open portion of the ventral window . the main wrap is configured to be wrapped around the middle portion of a horse . turning briefly to fig . 11 , the reader will observe the main wrap installed on a horse . the wrap includes a large elastic panel having a dorsal region and a ventral region . the dorsal region is of course configured to fit over the dorsal region of the horse while the ventral region of the elastic panel is configured to fit over the ventral region of the horse . the dorsal region of the elastic panel is broken by a gap ( which is spanned by the two bridging straps 26 in the view ). the ventral region of the elastic panel includes the ventral window ( which can simply be an opening in the elastic panel or a second gap in the elastic panel bridged by two or more straps ). returning now to fig . 1 , the next major component is saddle bridge 12 , which attaches over the dorsal region of the horse in the position customarily occupied by a saddle . ventral window cover 14 attaches over the horse &# 39 ; s ventral region and covers ventral window 22 . saddle bridge 12 and ventral window cover 14 are preferably made of the same material as main wrap 10 . they are both flexible and elastic . the final major component is brace 16 . it is a series of straps joined together in the configuration shown . a pair of lower wings 90 is connected to a pair of upper wings 94 by sternal bridge 92 . the brace is also made of elastic and flexible material . fig . 17 shows all the components installed on a horse . by briefly studying this view , the reader may gain a helpful general understanding of where each component will ultimately be placed . main wrap 10 passes around the horse &# 39 ; s mid section . saddle bridge 12 spans the top and bridges the gap in the dorsal region of the elastic panel of the main wrap ( it is shown in a stretched state ). ventral window cover 14 passes around the horse &# 39 ; s ventral region . brace 16 passes around the two front legs . fig . 2 shows the main wrap , saddle bridge , and ventral window cover in a folded state so that the reader may understand the nature of the material employed to make them . main wrap 10 features inner surface 28 and outer surface 30 . inner surface 28 is smoothly textured . it will bear against the horse &# 39 ; s hide , so it is preferably comfortable to a horse . outer surface 30 is covered in fine velcro ® loop material . (“ velcro ”® is a trademark of velcro industries , b . v . of the netherlands . the trademark refers to mating pieces of fabric having hooks on one piece and loops on the other piece . when the two pieces are pressed together , the hooks mechanically interlock with the loops , thereby forming a relatively weak attachment between the two pieces ). those skilled in the art will know that some modem velcro ® loop fabrics are quite fine . the outer surface is preferably such a fine loop . ideally the loop structure will be tight enough to prevent the unwanted capture of lint , hairs , and dirt . both the inner and outer surfaces must be able to stretch significantly . since the characteristics of the inner and outer surfaces of the main wrap must be different , it is preferable to construct the main wrap as a laminate of two different materials — one for the inner surface and one for the outer surface . saddle bridge 12 and ventral window cover 14 are made the same way . the saddle bridge has inner surface 32 and outer surface 34 , while the ventral window cover has inner surface 36 and outer surface 38 . the outer surfaces of all three components are covered in velcro ® loop material . this loop material is designed to engage with various velcro ® hook patches in the present invention . as an example , the two bridging straps 26 on the main wrap contain velcro ® hook patches . if the two free ends of the main wrap are pulled toward one another ( forming the main wrap into a loop ), each bridging strap can be pressed against outer surface 30 on the opposite side of the gap to hold the main wrap in a loop . this will in fact be the procedure by which the main wrap is placed on the horse ( described in more detail subsequently ). the inner surfaces will not engage the velcro ® hook patches . thus , it is important to place the inner surfaces toward the horse and the outer surfaces away from the horse . color coding may be helpful to one installing the device . as an example , the inner surfaces can be white , while the outer surfaces can be blue . fig2 b shows the installation of the aforementioned rolling stays 18 in the main wrap . a stay pocket 97 is formed on each end of the main wrap . it is possible to slide a rolling stay 18 in and out of each stay pocket . the rolling stays are preferably semi - rigid . they can be made of a hard plastic , such as extruded abs , or even thin aluminum bars . an important feature of the main wrap is its ventral access window . fig . 3 shows this component in more detail . the main wrap is preferably made of two separate elastic panels which are broken by a second gap in the ventral region . this second gap is bridged by front strap 40 and rear strap 46 . as for the balance of the main wrap , the front and rear straps are made of elastic material . the two window stays 20 remain in place to prevent the middle portion of the window opening from bowing outward when tension is placed on the main wrap ( such as when it is stretched around a horse &# 39 ; s abdomen ). they are attached along the two lateral ventral edges ( first lateral ventral edge 21 and second lateral ventral edge 23 ) that define the gap in the main wrap . the reader will therefore note that the boundary of ventral window 22 is defined by a first lateral ventral edge ( proximate the first window stay ), front strap 40 , a second lateral ventral edge ( proximate the second window stay ), and rear strap 46 . mesh panel 24 covers the opening . it has a hook tab 42 at each of its four comers . when it is placed over the opening , the velcro ® hooks on the four hook tabs stick to the velcro ® loops covering outer surface 30 . the mesh panel is preferably made of a fine mesh material — as fine as or finer than window screen . a relatively coarse depiction for the mesh is shown in the view . this is intended to be merely representational of the mesh material . once the mesh panel is affixed , middle strap 44 is placed over the mesh panel to reinforce the opening . it has a hook tab 48 on each end . these also engage the velcro ® loops on outer surface 30 . the middle strap is preferably made of elastic material as well , so that it can be stretched snugly across the opening . fig . 4 shows how the mesh panel and middle strap can be opened . while both these pieces can be removed in their entirety , it is often convenient to detach only one side and roll them back as shown . this provides good access to opening 50 . fig . 5 shows inner surface 36 of ventral window cover 14 . a dart seam 52 is provided at both the anterior and posterior extremes of central portion 64 . this allows the panel to assume the contoured shape shown ( where the two side edges curve ). those skilled in the art will realize that the dart seams allows the ventral window cover to more accurately follow the convex shape of a horse &# 39 ; s chest and abdomen . the dart seams are created by laying out a flat pattern , then cutting out two vee - shaped darts , then sewing the sides of the darts together ( or otherwise bonding them together ). the result is a slightly concave surface ( when viewed from the perspective of fig5 ) that can curve in two planes . the two dart seams are preferably asymmetric , since the horse &# 39 ; s abdomen will be smaller than its chest . thus , it is important to put the device in the correct orientation . hence , it is helpful to provide the printed graphic (“ head ”) to help the user properly orient the device . each lateral side of the ventral window cover has three tabs — front tab 58 , middle tab 60 , and rear tab 62 . the outer extreme of each tab includes a hook panel 54 and a lanyard 56 . the hook panels are positioned to engage the velcro ® loops on outer surface 30 of main wrap 10 . the lanyards are used to pull the window cover taut before the velcro ® features are engaged . fig6 shows inner surface 32 of saddle bridge 12 . it also includes a pair of dart seams 68 at both the anterior and posterior extremes of central portion 66 . these allow the panel to be curved in two planes , as for the ventral window cover . however , given the physiology of the concave shape of a horse &# 39 ; s back , it is not so important to make the device asymmetric . thus , the two darts may be the same . each lateral side of the saddle bridge has three tabs — front tab 76 , middle tab 78 , and rear tab 80 . the outer extreme of each tab includes a hook panel 70 and a lanyard 72 . the hook panels are positioned to engage the velcro ® loops on outer surface 30 of main wrap 10 . the lanyards are used to pull the window cover taut before the velcro ® features are engaged . a loop panel 74 is also located proximate each of the six tabs . these are small patches of velcro ® loop material . they allow the six tabs to be folded in and temporarily attached in a folded state ( with each hook panel 70 being attached to a loop panel 74 ). fig . 7 shows the saddle bridge with the tabs in the folded and locked state . it will remain in this position until the tabs are pulled free . this folded state can be helpful in the installation process , which will be described shortly . fig . 8 shows more detail regarding brace 16 . all its components have an inner surface 84 and an outer surface 86 . outer surface 86 is covered in fine velcro ® loop material . four hook panels 88 are provided to attach the brace . these hook panels are completely detachable from the brace . this feature allows the user to trim the length of the upper and lower wings . if a wing is too long , the user pulls its hook panel 88 loose , then cuts it to the desired length . the user then presses the hook panel back against outer surface 86 . a portion of each hook panel should cover the end of a wing and a portion should be positioned to extend beyond the wing . the velcro ® hooks on this extended portion will be used to engage the velcro ® loops on the outer surface of the main wrap , the saddle bridge , and / or the ventral window cover . fig8 b shows the same brace with the angles defining the joints between the components being altered somewhat . such alterations may need to be made to accommodate varying equine physiology . however , the brace shown in fig8 b functions int he same manner as the brace shown in fig8 . having described the components in detail , the application of the device to a horse will be explained . the device will typically be installed after some type of abdominal surgery on the horse . fig9 shows two components ready for installation . saddle bridge 12 has been placed in the configuration shown in fig7 ( though it is inverted from the orientation of fig7 ). the two ends of main wrap 10 have been rolled into two rolls 96 flanking ventral window 22 , so that the main wrap is now compact and easy to handle . fig1 shows the horse , which will typically be held by an attendant using a halter around the horse &# 39 ; s head . two more people then stand beside the horse on opposite sides of the horse &# 39 ; s withers . the main wrap is passed under the horse &# 39 ; s abdomen , with inner surface 28 facing the horse . the ventral access window is centered over the horse &# 39 ; s abdomen . each roll 96 is then unrolled up the horse &# 39 ; s two sides . the rolling stays 18 help hold the rolls fairly rigid so that they are easy to manipulate . fig1 shows the main wrap after the two rolls 96 have been completely unrolled . the elastic panel comprising the main wrap has a gap in its dorsal region . the panel actually terminates in a first lateral dorsal edge 25 ( visible to the viewer in fig1 and also labeled in fig1 ) and a second lateral dorsal edge 27 on the other side of the horse ( also labeled in fig1 ). the two lateral dorsal edges are proximate the pockets used to house the two rolling stays . at this point , each of the two attendants flanking the horse pulls a bridging strap 26 over the horse &# 39 ; s back and presses the velcro ® hooks on the underside of each bridging strap against the velcro ® loop material on outer surface 30 . the gap in the dorsal region of the elastic panel is thereby temporarily secured . the bridging straps can be left in place while the users place the next component . fig1 shows saddle bridge 12 placed over the horse &# 39 ; s back and spanning the gap in the main wrap . because the six tabs on the saddle bridge are folded under and secured , it does not “ stick ” to anything . the user may therefore manipulate the saddle bridge and obtain the desired position . the saddle bridge is preferably used to tighten the main wrap in a controlled fashion . the tightening sequence will be dictated by the particular horse &# 39 ; s anatomy , and the user &# 39 ; s preferred approach ( the users will often be directed by a veterinarian ). thus , the following should be viewed as exemplary , rather than indicating the only method of application . the user will often want to secure the two middle tabs 78 , since these will tighten the main wrap around the horse &# 39 ; s largest circumference . one person on each side pulls the lanyard on the two middle tabs 78 to unfold the middle tabs and pull them outward . the two people then pull the lanyards out and down ( making sure that the hook panels 70 remain clear of the velcro ® loop material on the main wraps outer surface ) until the desired tension is reached ( the tabs will stretch considerably ). they then press the two middle tabs against the main wrap , whereupon the velcro ® interface will secure the two middle tabs . this action effectively tightens the middle of the main wrap around the largest circumference of the horse . next , the two people detach the two front tabs 76 and stretch and attach these tabs to secure the main wrap around the portion of the horse that is customarily occupied by a saddle girth . finally , the two people detach , adjust , and secure the two rear tabs 80 to secure the main wrap around the horse &# 39 ; s abdomen . fig1 shows the saddle bridge with all three sets of tabs attached to the main wrap . while it may be possible to create the desired profile of tension in the main wrap on initial installation , it may often be necessary to adjust the tabs through several iterations . this may easily be done by using a lanyard to pull a particular tab loose . the tension provided by that tab is then modified and the tab is reattached . the independent nature of the six tabs , in combination with the elastic nature of the material used , allows the assembly to accommodate many variations is equine anatomy . the reader will observe in fig1 that the three tabs facing the viewer have been independently adjusted to different lengths . at some point in the installation process ( generally after the saddle bridge has been installed ), it may be desirable to remove the two rolling stays 18 . the reader will recall from fig2 b that the two rolling stays may be pulled out of the two rolling stay pockets . fig1 shows this operation . the rolling stay pockets are located high enough that the rolling stays are free to slide out over the horse &# 39 ; s rump . they should then be stored for future use . fig1 shows the installation of the ventral window cover . it is passed under the horse &# 39 ; s abdomen and the three sets of tabs are then sequentially pulled taut and attached by pressing hook panels 54 ( see fig5 ) against the velcro ® loop material on the outer surface of the main wrap . like the saddle bridge , it may have to be iteratively tightened until the desired fit is achieved . finally , brace 16 should be installed . fig1 shows this step . sternal bridge 92 is passed between the horse &# 39 ; s front legs . the two lower wings 90 are then positioned over the lower chest , while the two upper wings 94 are posited over and beyond the shoulders . the wings are drawn taut and the four hook panels 88 are then pressed against the outer surface of the main wrap , saddle bridge , and or ventral window cover ( depending on the position desired ). fig1 shows the brace installed . the two upper wings 94 should pass over the point of the shoulder 100 , while the sternal bridge should lie below carotid notch 102 . in this location , the brace will be stabilized by the horse &# 39 ; s own anatomy . it prevents the main wrap from migrating rearward . with the installation complete , the horse is free to move about without fear of dislodging the wrap . thus , the horse need not be confined during the recuperation process . one of the invention &# 39 ; s main features is the inclusion of the ventral access window . this allows access to the horse &# 39 ; s ventral region while the bandage remains in place . fig1 and 19 show the access process . in fig1 , the three nearside tabs on the ventral window cover have been detached , allowing the window cover to drop open . the user next grasps hook tab 48 and pulls the near end of middle strap 44 loose . finally , the user grasps the near side of mesh panel 24 and pulls it free . fig1 shows the resulting configuration , with one side of the mesh panel and the middle strap dropped open . opening 50 then provides unfettered access to the horse &# 39 ; s abdomen . an old dressing can then be removed . sutures or staples can be inspected and cleaned . a new dressing 104 can then be slipped into position . the mesh panel , middle strap , and ventral window cover are then replaced in sequence . the ventral window cover can be retightened as desired . during this process , abdominal support is still provided by the balance of the main wrap . there is only a brief period where the wound site itself is unsupported . this period ends when the ventral window is closed . those skilled in the art will realize that the ventral window cover need not be completely removable from the rest of the main wrap . it could be stitched down one side , leaving the other side removable . however , providing a completely removable ventral window cover is the preferred embodiment . although the preceding description contains significant detail , it should not be viewed as limiting the invention but instead as providing illustrations of the preferred embodiments of the invention . as an example , buckles and clasps could be substituted for the use of the velcro ® interfaces without altering the basis structure of the invention . these would certainly be less convenient , but they could be used in the same fashion . thus , the scope of the present invention should thus be defined by the following claims rather than any specific examples given . | 0 |
throughout the following description , specific details are set forth in order to provide a more thorough understanding of the invention . however , the invention may be practiced without these particulars . in other instances , well known elements have not been shown or described in detail to avoid unnecessarily obscuring the invention . accordingly , the specification and drawings are to be regarded in an illustrative , rather than a restrictive , sense . fig1 shows a portion of the frame 10 of a typical wood - framed structure . frame 10 comprises wooden studs 11 covered on the exterior by sheathing 12 . frame 10 includes an aperture 13 surrounded by wooden framing members 14 for receiving a window unit 15 . window unit 15 includes a window frame 16 , which may be made from any suitable material , and a glass panel 18 . window unit 15 is illustrated as being four - sided . the invention may also be used with construction units having other shapes such as triangular , round , semi - circular , polygonal etc . window frame 16 includes a flange 20 which projects in a lateral direction around the periphery of window frame 16 . aperture 13 is smaller than the outer dimension of flange 20 and is dimensioned to receive window frame 16 while flange 20 bears against the exterior surface of sheathing 12 . this invention provides clips 30 . each clip 30 has an exterior end 32 adapted to engage window frame 16 and an interior end 34 adapted to be fastened to building frame 10 from the inside of building frame 10 . clips 30 are used by affixing one or more clips 30 to each side of window frame 16 . in the example shown in fig1 , two clips 30 are affixed to each side of window frame 16 . for larger window units , three or more clips 30 might be affixed to each side of window frame 16 . in most cases , two or more clips 30 will be affixed to each side of window frame 16 . in the illustrated embodiment of the invention clips 30 attach to flange 20 . fig2 shows a clip 30 in greater detail . clip 30 is formed from a strip of any suitable material , such as steel , strong plastic , or the like . the material of clip 30 is preferably resilient . in some embodiments , clip 30 may be coated with a coating layer ( not shown ) which is thermally non - conductive relative to the material of clip 30 . for example , such a coating layer may comprise rubber , plastic , vinyl , fiberglass or the like . such a coating layer may help to reduce or prevent condensation on the surface ( s ) of clip 30 . in some embodiments , a coating layer may be provided on the contact surface ( s ) of clip 30 . interior end 34 of clip 30 comprises one or more apertures 36 which can receive fasteners , such as screws or nails , to affix interior end 34 to building structure 10 . apertures 36 constitute one possible means for affixing interior end 34 to a building structure . exterior end 32 of clip 30 is bent to define a deep groove 38 . as shown in fig3 , groove 38 is deep enough to receive flange 20 of window frame 16 . the portions 39 a and 39 b of clip 30 on either side of groove 38 are preferably ( but not necessarily ) resiliently biased toward one another , so that clip 30 tends to grip flange 20 . inwardly - angled teeth 40 ( fig2 ) may optionally be provided on one or both sides of groove 38 . after flange 20 is received in groove 38 , teeth 40 bite into flange 20 and resist any forces which might tend to pull flange 20 out of groove 38 . an outer side 42 of groove 38 may be tapered so that it is easy to guide flange 20 into groove 38 . as flange 20 is introduced into side 42 of groove 38 , it tends to wedge portions 39 a and 39 b apart so that flange 20 is held securely in groove 38 . clip 30 is preferably ( but not necessarily ) bent at a location intermediate ends 32 and 34 . the bend defines a fulcrum 44 . as shown in fig3 , when end 34 is fastened to structure 10 , clip tends to pivot about fulcrum 44 so that end 32 is biased into even firmer engagement with flange 20 . clip 30 is preferably resiliently flexible . as end 34 is fastened to building structure 10 by fasteners , such as nails 46 , clip 30 is straightened . providing a bend in clip 30 also facilitates affixing clip 30 to building structure 10 with fasteners ( for example nails or screws ) which are angled in an inward direction . when such fasteners are tightened , clips 30 are drawn inwardly and pull window frame 16 firmly into the aperture . fig4 a , 4 b and 4 c illustrate a number of alternative configurations for interior end 34 . in each of fig4 a , 4 b and 4 c , end 34 includes a number of projections 48 which project from clip 30 and which may be driven into framing members 14 ( fig1 ) when clip 30 is affixed to a window frame 16 . in the illustrated embodiments , projections 48 are integral with the material of the body of clip 30 and are formed by bending flaps of the material of clip 30 . projections 48 may be triangular , as shown in fig4 a and 4b , or may have more elongated shapes , as shown in fig4 c , or may have other shapes . the embodiments of fig4 a and 4c comprise both apertures 36 and projections 48 . projections 48 may project at right angles to end 34 of clip 30 . in alternative embodiments , projections 48 capable of use for affixing end 34 to building structure 10 could comprise separate elements affixed to end 34 in any suitable manner . for example , suitable projections 48 could be spot - welded to end 34 . projections affixed to end 34 provide an alternative means for affixing end 34 to a building structure 10 . in the embodiment of fig4 c , projections 48 are located near the ends of flexible fingers 49 . projections 48 are not necessarily large enough to permanently affix ends 34 to a building structure 10 . in some embodiments , projections 48 may be used to temporarily hold ends 34 to the building structure until screws or nails are inserted through apertures 36 . fig5 a and 5b illustrate a clip 30 according to another embodiment of the invention . in the embodiment of fig5 a and 5b , clip 30 comprises a protuberance 33 which projects upwardly from a surface of middle portion 31 . when window unit 15 is mounted in a building aperture 23 using clips 30 of the type shown in fig5 a and 5b , protuberances 33 create a gap 37 between the uppermost edge 14 a of framing members 14 and a lower edge 16 a of window frame 16 . gap 37 extends between adjacent clips 30 on the same side of window unit 15 . gap 37 may be used to facilitate the exchange of gas and / or moisture between the exterior and interior of a building , and to facilitate the escape of gas and / or moisture from between the layers of a building wall . although fig5 b depicts clip 30 in use on a lower side of window unit 15 , it will be appreciated that clips incorporating protuberance 33 may be used to create gaps 37 on other sides of window unit 15 . protuberance 33 depicted in fig5 a and 5b represents one possible embodiment of a protuberance that will create a gap 37 between window frame 16 and framing members 14 . some alternative embodiments comprise a plurality of protuberances on each clip 30 . some alternative embodiments comprise one or more protuberances that project in the opposing direction from an opposite surface of middle portion 31 ( i . e . towards framing members 14 ). in other alternative embodiments , clip 30 comprises one or more protuberances which project in an interior direction from a surface of portion 39 b to provide a gap between window flange 20 ( and portion 39 b of clip 30 ) and the exterior surface of sheathing 12 . such a gap may communicate with gap 37 to facilitate the exchange of gas and / or moisture . in still other alternative embodiments , the relative thickness of middle portion 31 ( and / or portion 39 b ) of clip 30 are increased , so that clip 30 can act as a spacer to provide gaps between a window frame and adjacent structures . fig6 a and 6b are respectively cross - sectional and isometric views of a clip 130 according to a further alternative embodiment of the invention . clip 130 comprises a plurality of pieces , which include exterior piece 130 a , interior piece 130 b and thermal isolation coupling 137 . as shown in fig6 a and 6b , exterior piece 130 a preferably comprises exterior end 132 , including portions 139 a , 139 b which define deep groove 138 . interior piece 130 b preferably comprises interior end 134 and middle portion 131 . thermal isolation coupling 137 couples interior piece 130 b to exterior piece 130 a and provides thermal insulation therebetween . thermal isolation coupling 137 is fabricated from a material ( or materials ) that are thermally insulating relative to the material of exterior and interior pieces 130 a , 130 b . for example , exterior and interior pieces 130 a , 130 b may comprise steel or some other metallic alloy ., while thermal isolation coupling 137 may comprise rubber , plastic , vinyl , fiberglass or the like . thermal isolation of interior piece 130 b from exterior piece 130 a reduces the possibility of moisture condensing on interior piece 130 b due to cold temperatures experienced by exterior piece 130 a . in the illustrated embodiment ; thermal isolation coupling 137 comprises grooves 141 a , 141 b for respectively receiving the ends of exterior and interior pieces 130 a , 130 b . preferably , thermal isolation coupling 137 is fabricated from a resilient material , such that when exterior and interior pieces 130 a , 130 b are inserted into grooves 141 a , 141 b , the deformation of grooves 141 a , 141 b acts to hold the ends of exterior and interior pieces 130 a , 130 b in - place ( i . e . to couple the ends of exterior and interior pieces 130 a , 130 b to thermal isolation coupling 137 ). in alternative embodiments , adhesive , rivets and / or other suitable fasteners may be used to help couple the ends of exterior and interior pieces 130 a , 130 b to thermal isolation coupling 137 . thermal isolation coupling 137 may be molded in place around the ends of pieces 130 a , 130 b . exterior and interior pieces 130 a , 130 b may be coated with a coating layer ( not shown ) which is thermally non - conductive relative to the material of exterior and interior pieces 130 a , 130 b . such a coating layer may also help reduce or prevent condensation on the surface ( s ) of exterior and interior pieces 130 a , 130 b . it can be appreciated that the use of this invention can significantly simplify the installation of prefabricated construction units in a building , especially where one would need a ladder , scaffold , man lift or the like to reach the locations where - the construction units will be installed from the exterior of the building . a worker can affix clips 30 according to the invention to a construction unit and then , from inside the structure , orient the construction unit at an angle to the aperture in which the construction unit will be installed and pass the construction unit through the aperture to the outside of the structure . still working from inside the structure , the worker can then draw the construction unit into place in the aperture and fasten the construction unit in place by affixing interior ends 34 of clips 30 to the structure . if necessary , shims may be installed around the frame of the construction unit to properly align the construction unit in the aperture . a further advantage of the invention is realized in situations where a waterproofing membrane or the like is applied to the exterior of building frame 10 . prior art systems for securing construction units to building structures typically require the membrane to be punctured by nails or screws in the area adjacent to aperture 13 . in some cases building codes prohibit fastening the lower sides of construction units in ways which result in the membrane being punctured . sometimes windows are installed with no fasteners on their lower sides for this reason . the result can be that the lower sides of the windows can move , especially in windy weather . the use of clips 30 according to the invention allows the membrane to remain intact and still permits securing the lower side of window units and other construction units by way of one or more clips 30 . it can be appreciated that clips 30 having an exterior end 32 as described above can be affixed to a construction unit frame with minimal tools and without the need to drill holes in the frame or to modify the window or door frame in other respects . where a component ( e . g . a member , tab , fastener etc .) is referred to above , unless otherwise indicated , reference to that component ( including a reference to a “ means ”) should be interpreted as including as equivalents of that component any component which performs the function of the described component ( i . e ., that is functionally equivalent ), including components which are not structurally equivalent to the disclosed structure which performs the function in the illustrated exemplary embodiments of the invention . as will be apparent to those skilled in the art in the light of the foregoing disclosure , many alterations and modifications are possible in the practice of this invention without departing from the spirit or scope thereof . for example : while the above detailed description relates primarily to window units , it is to be understood that clips according to the invention may equally be used to secure other types of construction units , such as door units , vent units , sunlight units and the like , into appropriately sized apertures in a building frame . in some embodiments , a layer of deformable , elastomeric material ( not shown ) may be attached to one ( or both ) of the surfaces of middle portion 31 of clip 30 . such deformable , elastomeric layer ( s ) may make clip 30 more malleable , thereby facilitating installation of clip 30 and preventing clip 30 from accidentally damaging window unit 15 or frame 10 . such deformable , elastomeric layer ( s ) may also help to accommodate warpage in the shape of the edges of window unit 15 and / or framing members 14 . similar deformable , elastomeric layer ( s ) may be used with all of the above - discussed clip embodiments . in some embodiments , thermal isolation coupling 137 may have a different shape than the one depicted in fig6 a and 6b and may be coupled to exterior and interior pieces 130 a , 130 b in a different manner than that depicted in fig6 a and 6b . fig7 a and 7b respectively depict cross - sectional views of window mounting clips according to still further embodiments of the invention . clip 130 of fig7 a comprises an exterior piece 130 a and an interior piece 130 b . pieces 130 a , 130 b are coupled to one another by a thermal isolation coupling 137 ′ that is t - shaped in cross section , with flanges 150 a , 150 b that extend over pieces 130 a , 130 b . thermal isolation coupling 137 ′ may be coupled to exterior and interior pieces 130 a , 130 b using adhesive , rivets and / or other suitable fasteners ( not shown ). those skilled in the art will appreciate that t - shaped thermal isolation coupling 137 ′ may be inverted ( relative to pieces 130 a , 130 b ) such that flanges 150 a , 150 b extend under pieces 130 a , 130 b . in the embodiment of fig7 b , exterior and interior pieces 130 a , 130 b are coupled together by a relatively flat - shaped thermal isolation coupling 137 ″. thermal isolation coupling 137 ″ comprises exterior and interior ends 152 a , 152 b , which extend respectively over pieces 130 a , 130 b . thermal isolation coupling 137 ″ may be coupled to pieces 130 a , 130 b using adhesive , rivets and / or other suitable fasteners ( not shown ). those skilled in the art will appreciate that flanges 152 a , 152 b of thermal isolation coupling 137 ″ may alternatively extend below pieces 130 a , 130 b or both above and below pieces 130 a , 130 b . thermal isolation couplings 137 ′, 137 ″ are preferably thermally non - conductive relative to the material of exterior and interior pieces 130 a , 130 b . accordingly , the scope of the invention is to be construed in accordance with the substance defined by the following claims . | 4 |
embodiments of the present invention allow a user ( e . g ., hunter , sports spectator , camper , hiker , bird watcher , and the like ) to use an all - terrain seat that is adjustable to fit any type of terrain . by individually adjusting the legs of the all - terrain seat , users are able to use the all - terrain seat on terrains of any incline . moreover , the all - terrain seat may be used near obstructions such as trees , buildings , and the like , so that a hunter or other user can sit in very close proximity to the obstruction . the following detailed description of exemplary embodiments of the invention makes reference to the accompanying figures , which show the exemplary embodiment by way of illustration and its best mode . while these exemplary embodiments are described in sufficient detail to enable those skilled in the art to practice the invention , it should be understood that other embodiments may be realized and that logical and mechanical changes may be made without departing from the spirit and scope of the invention . thus , the following detailed description is presented for purposes of illustration only and not of limitation . for example , the steps recited in any of the method or process descriptions may be executed in any order and are not limited to the order presented . turning now to the figures , fig1 shows a perspective view of an embodiment of the all - terrain seat 100 of the present invention . the illustrated embodiment of all - terrain seat 100 includes a seat assembly 110 and leg members 120 , 130 , and 140 that support seat assembly 110 . each leg member comprises an upper and lower leg section . leg member 120 comprises upper leg section 125 and lower leg section 127 . leg member 130 comprises upper leg section 135 and lower leg section 137 . leg member 140 comprises upper leg section 145 and lower leg section 147 . the upper and lower leg sections are removably attached such that each lower leg section 127 , 137 , 147 is configured to slide into and traverse the inside of the respective upper leg section 125 , 135 , 145 . in this manner , the upper and lower sections for each leg member are individually adjustable . that is , the user may adjust only one , two , or all three leg members , depending on the incline and other characteristics of the surface . alternatively , in accordance with other embodiments of the present invention , the lower leg sections could be configured to traverse the outside of the respective leg section . in addition , leg caps 150 , 160 , and 170 may be attached to one end of lower leg sections 127 , 137 , 147 respectively , such that the leg caps make contact with the surface or terrain and may be used to further stabilize seat 100 . it will be appreciated that leg caps 150 , 160 , 170 distribute the load so that seat 100 may be used on any type of surface , including soft surfaces . in accordance with another aspect of the present invention , and with reference to fig1 and 3 , the adjustable leg sections of each leg member have push buttons 128 , that allow the leg sections to easily attach , detach , and adjust for height . thus , the legs may be individually adjusted so that the user can sit on any surface . at the touch of a push button , the legs may be detached and attached to seat assembly 110 for easy transport as illustrated in fig3 . in accordance with another aspect of this embodiment , seat assembly 110 also comprises a quiet ball bearing raceway that enables the seat assembly to swivel 360 degrees . in accordance with another aspect of this embodiment , the legs may be adjusted to at least 20 inches in height , and lightweight seat ( approximately 3 . 0 pounds ) 100 is capable of supporting an individual weighing more than 350 pounds . fig2 shows a perspective view of another embodiment of an all - terrain seat 200 of the present invention . the illustrated embodiment of all - terrain seat 200 includes a seat assembly 210 , channels 222 , 224 , 226 and leg members 220 , 230 , and 240 that support seat assembly 210 . each leg member comprises an upper and lower leg section . leg member 220 comprises upper leg section 225 and lower leg section 227 . leg member 230 comprises upper leg section 235 and lower leg section 237 . leg member 240 comprises upper leg section 245 and lower leg section 247 . seat assembly 210 has channels 222 , 224 , 226 that are approximately parallel and extend through the seat assembly . in this manner , leg members 220 , 230 , 240 may be stored in the channels for easy transport as described below . the upper and lower leg sections are removably attached such that each lower leg section 227 , 237 , 247 is configured to slide into and traverse the inside of the respective upper leg section 225 , 235 , 245 . in this manner , the upper and lower sections for each leg member are individually adjustable . that is , the user may adjust only one , two , or all three leg members , depending on the incline and other characteristics of the surface . alternatively , in accordance with other embodiments of the present invention , the lower leg sections could be configured to traverse the outside of the respective leg section . in addition , leg caps 250 , 260 , and 270 may be attached to one end of lower leg sections 227 , 237 , 247 respectively , such that the leg caps make contact with the surface or terrain and may be used to further stabilize seat 200 . it will be appreciated that leg caps 250 , 260 , 270 distribute the load so that seat 200 may be used on any type of surface , including soft surfaces . in accordance with another aspect of the present invention , and with reference to fig2 and 4 , the adjustable leg sections of each leg member have push buttons 228 , that allow the leg sections to easily attach , detach , and adjust for height . thus , the legs may be individually adjusted so that the user can sit on any surface . at the touch of a push button , the legs may be detached and slide into channels 222 , 224 , 226 on seat assembly 210 for easy transport . in accordance with another aspect of this embodiment , seat assembly 210 also comprises a quiet ball bearing raceway that enables the seat assembly to swivel 360 degrees . in accordance with another aspect of this embodiment , the legs may be adjusted from at least 16 . 5 inches to at least 23 . 5 inches in height , and seat 200 is capable of supporting an individual weighing more than 500 pounds . the seat is made from light weight , high impact strength plastic and thus the seat , in this embodiment , may weigh less than 5 pounds . in accordance with another embodiment of the present invention , and with reference to the accompanying figures , a “ spike seat ” model comprises a very lightweight adjustable leg seat that has individually adjustable legs that may extend up to 18 inches in height . the lower leg sections of this embodiment may optionally have spikes such that the seat can securely sit on various types of terrain . in accordance with one aspect of this embodiment , the seat weighs approximately three pounds due to the use of lightweight , high impact strength plastic . it will be appreciated that all - terrain seat 100 , 200 has , inter alia , the following advantages : individually adjustable legs — can be used on grass , in the woods , on the beach , and is designed for use on sloped or uneven surfaces . lightweight — made from high impact strength plastic . exceptionally portable — attaches to belt on waist , fit inside a backpack , or easily hand carried . oversized leg caps — distributes the load so the seat can be used on all surfaces . benefits , other advantages , and solutions to problems have been described above with regard to specific embodiments . however , the benefits , advantages , solutions to problems , and any element ( s ) that may cause any benefit , advantage , or solution to occur or become more pronounced are not to be construed as critical , required , or essential features or elements of any or all the claims . as used herein , the terms “ comprises ”, “ comprising ”, or any other variation thereof , are intended to cover a non - exclusive inclusion , such that a process , method , article , or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process , method , article , or apparatus . further , no element described herein is required for the practice of the invention unless expressly described as “ essential ” or “ critical ”. | 0 |
with initial reference to fig1 and 2 , a dishwasher constructed in accordance with the present invention , is generally indicated at 2 . dishwasher 2 includes an outer support body 4 which is positioned below a kitchen countertop 6 along side a plurality of cabinets 8 . as shown , cabinets 8 include drawers 9 - 12 and a door 13 . as further shown , dishwasher 2 includes an upper washing unit or drawer 16 , as well as a lower washing unit or drawer 18 . as each washing unit 16 , 18 is similarly constructed , a detailed description will be made with respect to upper washing unit 16 with an understanding that lower washing unit 18 includes corresponding structure . upper washing unit 16 includes a front wall 20 , a rear wall 21 , a bottom wall 22 and opposing side walls 23 and 24 that collectively define an upper washing chamber 28 . a dishrack 30 is positioned within upper washing chamber 28 to support kitchenware , indicated generally at 31 , which may include plates , cups or the like . upper washing unit 16 is slidably supported within outer support body 4 through a pair of extensible drawer glides , one of which is indicated at 33 . finally , dishwasher 2 is shown to include a lid 37 that is selectively shiftable relative to washing chamber 28 as drawer 16 is moved into and out of outer support body 4 . dishwasher 2 selectively performs a washing operation in washing chamber 28 during which sprays or jets of washing fluid are directed onto kitchenware 31 by a lower wash arm 47 , as well as an upper washing mechanism 50 . in the embodiment shown , upper washing mechanism 50 is positioned at an upper portion of rear wall 21 . as best shown in fig2 and 3 , upper washing mechanism 50 includes a water delivery portion 56 having an inlet conduit 58 which directs a flow of washing fluid towards a spray bar 60 . in accordance with the invention , inlet conduit 58 includes a first end section 63 that extends to a second end section 64 through an intermediate section 65 . first end section 63 is preferably domed - shaped so as to receive an inlet nozzle 69 therein ( see fig4 ) as will be discussed more fully below . as further shown in fig3 , spray bar 60 includes a first end portion 90 that extends to a second end portion 91 through an intermediate portion 92 that defines a central trough 97 . first and second end portions 90 and 91 actually define support members in a manner that will be detailed more fully below . in any event , spray bar 60 is actually fluidly connected to second end section 64 of inlet conduit 58 so as to receive a flow of washing fluid from inlet nozzle 69 . the flow of washing fluid is directed outward from central trough 97 through a plurality of nozzles 104 - 111 . actually , trough 97 is divided into first and second lateral sections or zones 114 and 115 by a central support member 112 , with nozzles 104 - 107 being positioned in first lateral zone 114 and nozzles 108 - 111 being positioned in second lateral zone 115 . upper washing mechanism 50 also includes a paddlewheel member 119 rotatably supported within trough 97 of spray bar 60 . paddlewheel member 119 actually includes a first paddle support 121 having a first end section 122 that extends to a second end section 123 through an intermediate section 124 . first paddle support 121 is arranged within first lateral zone 114 of trough 97 . arranged alongside first paddle support 121 , in second lateral zone 115 , is a second paddle support 129 . in a manner similar to that described above , second paddle support 129 includes a first end section 130 , a second end section 131 and an intermediate section 132 . first and second paddle supports 121 and 129 are rotatably supported upon a central rod 135 that extends substantially the entire length of trough 97 . towards that end , central rod 135 includes first and second outer bearing elements 137 and 138 that are rotatably supported upon first and second end sections 90 and 91 of spray bar 60 , as well as a central bearing / support portion 139 that rests upon central support member 112 . in any case , as each paddle support 121 , 129 is substantially , identically constructed , a detailed description will be made with respect to first paddle support 121 with an understanding that second paddle support 129 is correspondingly constructed . first paddle support 121 includes a plurality of disk - shaped deflector members 145 - 147 positioned adjacent nozzles 104 , 106 and 107 respectively , as well as a paddle - shaped deflector member 150 positioned is adjacent to nozzle 105 . with this arrangement , a jet of washing fluid exiting nozzle 105 impacts paddle - shaped deflector member 150 causing first paddle support 121 to rotate about an axis defined by central rod 135 . as first paddle support 121 rotates , additional jets of washing fluid emanating from nozzles 104 , 106 and 107 impact disk - shaped deflector members 145 - 147 respectively , causing the jets of washing fluid to diverge into streams of washing fluid which are directed onto kitchenware supported upon dishrack 30 . as discussed above , washing fluid is introduced into upper washing mechanism 50 through inlet nozzle 69 illustrated in fig4 . in accordance with the invention , inlet nozzle 69 includes a main body portion 160 having a base section 162 , provided with a circular flange 163 , which extends through an intermediate section 164 to a tapered or nozzle section 165 . nozzle section 165 is provided with a plurality of openings , one of which is indicated at 167 , as well as a diffuser 169 . diffuser 169 includes an aperture 171 that receives a mechanical fastener 174 ( see fig3 ) which secures upper washing mechanism 50 to washing chamber 28 . in addition to mechanical fastener 174 , upper washing mechanism 50 is also retained against rear wall 21 by a mounting bracket 184 . in further accordance with the invention , mounting bracket 184 includes a main body 186 having a ring portion 188 from which extends an intermediate or planar portion 189 before terminating in a support portion 190 . support portion 190 includes first and second ear elements 192 and 193 , each provided with a corresponding tab element 196 , 197 that snap - fittingly engages inlet conduit 58 . as will be discussed more fully below , mounting bracket 184 is secured against rear wall 21 of washing chamber 28 through circular flange 163 of inlet nozzle 69 . as best shown in fig5 and 6 , inlet nozzle 69 is connected to and receives a flow of washing fluid through an inlet feed member 206 extending through rear wall 21 of washing chamber 28 . inlet feed member 206 includes a conduit portion 208 and a base portion 210 . conduit portion 208 includes a main body section 214 having a base section 215 from which extend an inlet nipple 216 and an outlet nipple 217 . main body section 214 also includes a flange 222 having a pair of mounting ears , one of which is indicated at 225 . as will be discussed more fully below , flange 222 acts as an interface between conduit portion 208 and base portion 210 . outlet nipple 217 includes a hollow interior portion 228 that leads into base section 215 and fluidly connects to inlet nipple 216 . outlet nipple 217 also includes a plurality of external threads 231 which , as best shown in fig6 , engage with inlet nozzle 69 . more specifically , outlet nipple 217 extends through rear wall 21 of washing chamber 28 and ring portion 188 of mounting bracket 184 . once in place , inlet nozzle 69 is secured to inlet feed member 206 through threads 231 , with circular flange 163 trapping mounting bracket 184 against rear wall 21 . finally , inlet nipple 217 is shown to include a pair of outer rings 235 and 236 which provide a positive engagement for a hose 238 that is secured through a clamp 239 ( see fig7 ). with this arrangement , inlet feed member 206 receives a flow of washing fluid from a pump ( not shown ) through inlet nipple 216 . the flow of washing fluid is thereafter is redirected outward through outlet nipple 217 into inlet nozzle 69 and into spray bar 60 . as stated above , conduit portion 208 is supported upon a base portion 210 through flange 222 . towards that end , base member 210 is provided with a main housing 245 that includes a mounting member 247 and a cover 248 . mounting member 247 is provided with a pair of supports 260 and 261 that align with mounting ears 225 . supports 260 and 261 are adapted to receive mechanical fasteners , one of which is shown at 265 , to secure conduit portion 208 to base portion 210 . mounting member 247 further includes a central opening 267 that leads into main housing 245 . a seal 269 extends about central opening 267 and engages with flange 222 of conduit portion 208 . in addition , cover 248 is pivotally connected to mounting member 247 through a hinge 270 and secured through a tab member 273 . actually , main housing 245 serves as an enclosure for electronic circuitry 280 ( see fig7 ) associated with a flow sensor 283 , such as a diaphragm positioned across central opening 267 . sensor 283 senses the flow of washing fluid through conduit portion 208 during an overall washing operation . reference will now be made to fig8 in describing an alternative embodiment of the present invention . as shown , an upper wash mechanism 350 includes a water delivery portion 356 having an inlet conduit 358 that is connected to a spray bar 360 . spray bar 360 includes a first end section 390 that extends to a second end section 391 through an intermediate section 392 . actually , arranged at intermediate section 392 is a “ t ” member 394 that directs a flow of washing fluid into a first lateral zone 360 and a second lateral zone 361 . each lateral zone 360 , 361 includes a plurality of nozzles 404 - 406 and 407 - 409 respectively . jets of washing fluid emanating from nozzles 404 - 409 impact upon a paddlewheel member 419 that is rotatably mounted to a pair of laterally spaced first and second support members 421 and 429 . actually , paddlewheel member 419 is provided with a pair of bearings , one of which is indicated at 438 , that provide smooth rotation as paddlewheel 419 is impacted and rotated by jets of washing fluid emanating from nozzles 404 - 409 . in addition , paddlewheel member 419 is provided with a slight twist or spiral which ensures continued exposure to the jets of washing fluid . thus , in accordance with the embodiment shown , paddlewheel member 419 constitutes an overall deflector member 445 that causes the jets of washing fluid to diverge into a plurality of streams which subsequently impact upon kitchenware supported upon dishrack 30 during an overall washing operation . at this point , it should be readily understood that the present invention provides for an efficient upper washing mechanism for directing water to an upper portion of a washing chamber in a drawer - type dishwasher . more particularly , mounting the upper washing mechanism to a wall of the wash chamber advantageously provides protection to various wash system components arranged within outer housing 4 . more specifically , the particular positioning of the upper washing mechanism ensures that any residual water remaining within the wash system drops directly into the washing chamber and not onto various components carried within outer housing 4 as would be the case with a wash arm mounted to , for example , lid 37 . in addition , the paddlewheel configuration establishes an extremely efficient and is effective washing fluid distribution arrangement that creates streams of washing fluid sprayed randomly about the washing chamber . in any case , although described with reference to preferred embodiments of the invention , it should be readily understood that various changes and / or modifications can be made to the invention without departing from the spirit thereof . for instance , the overall shape , angular orientation , number and spacing of the deflector members can vary in accordance with the present invention . in general , the invention is only intended to be limited by the scope of the following claims . | 0 |
for purposes of the present invention , an antioxidant is a compound , component or mixture of compounds or components , some of which are capable of reacting with free radicals to inhibit free radical chain reactions . consequently , an antioxidant of the present invention has the effect of improving at least one chemical or physical characteristic of the oil upon exposure of the oil to elevated temperature , including , for example , the stability of the oil to oxidative degradation , inhibiting the formation of undesirable oxides and peroxides , inhibiting molecular weight reduction of the oil molecules , inhibiting formation of crosslinks in the oil that can lead to the presence of sludge , and inhibiting the formation of undesirable and / or unpleasant taste and odor bodies . such antioxidants include natural and synthetic food acids and herbs , for example citric acid and rosemary extract , as well as other compounds and components identified herein and elsewhere in the art as exhibiting at least one of the above characteristics . generally , useful herbs and herbal extracts include those such as turmeric , rosemary , oregano , sage , garlic , ginger , peppermint , purslane , bilberry , milk thistle , grape seed , green tea , maritime pine and st . john &# 39 ; s wort ( also known as hypericum ). a useful listing can be found on the internet at www . ars - grin . gov / duke / comprising phytochemical and ethnobotanical databases maintained by dr . j . duke , incorporated herein by reference to the extent permitted . therefore , in the context of the present invention , the use of an antioxidant stabilizes or improves the stability of hot oil used for cooking or frying in the sense that such oil can be used for a longer period of time before the quality of the oil or food cooked therein becomes unacceptable due to color , taste and / or odor . at least some of the benefits of the present invention are achieved by the addition of an aqueous composition , that is by the addition of water as a component . although not wishing to be bound by theory , it is believed that the water of the composition , particularly in the form in which it is introduced according to the present invention , facilitates removal of volatile , odor forming species from used cooking oil , e . g ., physically by a process analogous to steam distillation , or otherwise . compositions of the present invention comprising ( a ) water , and ( b ) at least one antioxidant , preferably a food acid , can typically be prepared by dissolving or dispersing the antioxidant in water . in a preferred embodiment , antioxidant is present in an amount of from about 5 % to about 60 % by weight , preferably from about 10 % to about 40 % by weight . more preferably , the composition , prior to addition to the oil , forms a solution , dispersion or suspension . the composition , upon addition to the cooking oil preferably forms a solution with the oil ; alternatively , it forms a dispersion , a suspension or each of these conditions ( solution , dispersion , suspension ) can occur simultaneously to varying degrees . compositions of the present invention comprising ( a ) water , ( b ) at least one water - soluble or water - dispersible emulsifier , and ( c ) at least one antioxidant , preferably a food acid , can typically be prepared by dissolving or dispersing the emulsifier and antioxidant in water . in a preferred embodiment , the water - soluble or water - dispersible emulsifier is present in an amount of about 0 . 00001 wt . % to about 5 wt . %, preferably from about 0 . 0001 wt . % to about 2 wt . % and the antioxidant is present in an amount from about 5 wt . % to about 60 wt . %, preferably from about 10 wt . % to about 40 wt . %. in a preferred embodiment , the characteristics of the emulsifier include one or more of the following : non - ionic , non - toxic regarding its suitability for human consumption , and low or non - foaming . more preferably , the composition , prior to addition to the oil , forms a solution , dispersion or a suspension . the composition , upon addition to the cooking oil disperses as a dilute emulsion . forming an emulsion when the composition is introduced to the oil can be desirable since an emulsion enhances uniform dispersion of antioxidant ingredients and water throughout the cooking oil and prevents the coalescence of water droplets . this may aid in control of , or inhibit the rate of release of antioxidant composition . generally , the cooking oil is at a temperature in a range from about 300 ° f . to 385 ° f . when the composition is added to the oil , and typically from about 325 ° f . to about 360 ° f . water - soluble or water dispersible emulsifiers are generally known in the art . examples of water - soluble or water dispersible emulsifiers include , but are not limited to mono and diglycerides of fat forming fatty acids , carboxylic acids and fatty acids esters of glycerol . as used herein , “ food acid ” includes , but is not limited to citric acid , tartaric acid , malic acid , lactic acid , acetic acid , fumaric acid , ascorbic acid or vitamin c , isoascorbic acid , succinic acid , adipic acid , hydrochloric acid , and phosphoric acid , as well as glycerol esters of the above listed acids , ethylenediamine tetraacetic acid and fatty acids as well as permutations , combinations and mixtures thereof . the composition optionally further comprises a food compatible agent , such as acetic acid and / or chelating agent that reduces the hardness of the water , as the use of hard water can be counterproductive to inhibiting degradation reactions in the cooking oil . alternatively , demineralized water , or water with reduced concentrations of minerals , can be used . compositions of the present invention preferably comprise at least one antioxidant selected from the group consisting of citric acid , ascorbic acid , ascorbyl palmitate and natural antioxidants derived from the turmeric or rosemary . advantages of the present invention are achieved by adding a minor concentration of a composition of the present invention , for example , ( a ) a composition comprising a minor concentration of at least one water soluble or water dispersible antioxidant which may be a food acid , water and , optionally , at least one water - soluble or water dispersible emulsifier , and ( b ) introducing the composition into a major concentration of a cooking oil . in a particularly preferred embodiment , the cooking oil is at a temperature in a range of from about 315 ° f . to about 360 ° f . the aqueous composition is preferably introduced into cooking oil without using either a solid mineral carrier or a liquid oil carrier . the mixture is more preferably introduced into the cooking oil at a slow , controlled rate over a period of time so as not to create a hazard by rapidly converting the liquid water to steam . this is achieved by controlling the rate of introduction of the aqueous composition to that comparable to the dehydration and migration of water from the surface of food cooking or frying in hot oil . all food contains water . generally , foods contain about 40 % to about 70 % water . supplementary water and antioxidants may be added by choice of an appropriate physical device for introduction of aqueous composition . the composition may be added as a fine spray or mist over the surface of the oil or by a single or multiple orifices so introduction of the composition causes an acceptable level of effervescence without splattering hazard . the aqueous composition may be added to the oil in a fine stream , preferably as a fog or mist of liquid droplets ; such droplets or stream are preferably aerated . when added in the form of droplets , the size of the droplets is typically about 0 . 1 mm diameter to about 3 . 0 mm diameter ; preferably from about 0 . 5 mm to about 2 . 5 mm . alternatively , a fine stream of the composition can be about 0 . 05 mm to about 6 mm in diameter ; preferably about 1 mm to about 2 mm . the aqueous composition can be introduced into or onto the surface of the oil using various application devices . for example , it is convenient to use containers such as plastic squeeze bottles that are equipped with covers or caps that are capable of generating a fine stream or mist when the bottle is squeezed . such containers are well known . alternatively , application containers can be hand held containers of the type that generate a fine mist or fog based on the use of a dip tube , spray nozzle and squeeze handle that draws the liquid from the container and forces it through the nozzle when the user squeezes or depresses the handle . furthermore , containers that utilize a pump dispenser can be employed as well as syringes equipped with a fine bore capillary , needle or tube . these and other convenient containers , devices and methods for dispensing a fine stream , mist or fog are similarly well known in the art and can be selected by the artisan based on such factors as cost and convenience . the applicator device , including nozzle configuration , is preferably selected so as to generate an aerated liquid stream and / or aerated liquid particles or droplets . such an applicator is available from delta manufacturing ( pa ). in circumstances where it may be desirable to limit the amount of air introduced into the oil , e . g ., a commercial frying operation conducted for extended periods at elevated temperature , inert gas such as nitrogen , carbon dioxide or mixtures thereof , can be used in place of or in combination with air . consequently , for purposes of the present invention , the term aeration should be understood to refer to the incorporation of small bubbles of a gas in a liquid droplet or stream where the gas can be air or an inert gas or mixtures thereof . preferably , the composition is applied as a conical shaped spray of appropriate size droplets deposited on the surface of the hot oil over a wide area , for example an oval or circular shape having a major diameter of from about 3 inches to about 9 inches . preferably , the area covered by the spray or mist is in a circular pattern about 5 inches in diameter or an oval pattern about 5 inches by about 9 inches . alternatively , the mist or fog is sprayed above the surface of the fryer so that it covers from about 15 % to about 70 % of the surface area of the fryer ; for example , from about 30 % to about 50 %. the specific area covered is not considered to be critical , provided that the composition reaches the surface of the oil and is carried into the overall oil composition . a further alternative embodiment or method of applying the composition to the oil , particularly preferred for use with large frying equipment , such as used by manufacturers of cooked food products , is illustrated in fig1 . in this embodiment , the composition may be introduced from a reservoir ( 5 ) containing the composition through strategically placed multiple orifices beneath ( 3 ) and / or above ( 6 ) the surface of the oil by use of a control valve ( 7 ) in order to introduce a stream or a “ fog ” or a mist of small droplets of about 0 . 1 mm diameter to about 3 . 0 mm diameter , for example , about 0 . 5 mm to about 2 . 5 mm diameter . preferably the composition is introduced below the surface of the oil as , for example , droplets having preferred sizes of from about 1 . 0 mm to about 1 . 5 mm diameter . the rate of addition of the composition can be controlled , for example , by the use of a metering pump ( 4 ). this is preferably accomplished at fixed intervals of time , for example , after the oil is at elevated or cooking temperature , after fixed intervals of cooking or as determined by periodic measurement of oil properties and / or visual observation of food appearance and internal temperature of the food ( cooking performance of the oil ). the rate of introduction may be varied by a review of the measured or observed properties of the oil and the food . the metering input of the composition may also be varied automatically by sensing key properties of the oil such as free fatty acids ( ffa ), peroxide or polar content . such time intervals are conveniently selected by those skilled in the field of cooking , and particularly in the field of preparing fried foods , after limited experimentation or experience using the methods taught herein . consequently , the amount of aqueous antioxidant composition comprising , for example , at least one food acid and / or at least one herbal extract and water can be added in an amount that compensates for the loss of or degradation of antioxidant that occurs over the selected time period or to adjust the quality of the cooking oil composition to a predetermined value of a test measurement carried out by an automated or manual test result . the composition of the present invention comprising at least one antioxidant , e . g ., food acid , and water , and , optionally , at least one emulsifier , can be prepared by mixing , such mixing optionally comprising processes such as solubilizing , dispersing or suspending , the recited components , and other optional , beneficial cooking oil additive ( s ) with one another . the mixing sequence is not critical and an appropriate operation can be determined with limited experimentation . emulsifiers are generally known in the art . for purposes of the present invention , emulsifiers include both oil - soluble and water - soluble or water - dispersible emulsifiers . in carrying out this aspect of the invention , the antioxidant , e . g ., food acid , additive in liquid or particulate form is dispersed or dissolved in the water or emulsifier / water mixture and the mixture is delivered to the hot cooking oil . examples of such emulsifiers include , but are not limited to mono and diglycerides of fat forming fatty acids and / or other food compatible acids , and ascorbyl palmitate . in a particularly preferred embodiment , the emulsifier is selected from the group consisting of water - soluble or water - dispersible and oil - soluble emulsifiers and the antioxidant additive is in a form selected from the group consisting of solid particulates , liquids , aqueous solutions and aqueous dispersions . the antioxidant additives include antioxidant food acids described above as well as other antioxidants such as glycerol ester of citric acid and fat forming fatty acids derived from sunflower oil or canola oil , ascorbic acid , ascorbyl palmitate , turmeric and rosemary extract . in a particularly preferred embodiment ascorbyl palmitate is used , alone or in combination with other antioxidants and / or emulsifiers , in order to take advantage of both its antioxidant and emulsifier characteristics . useful food additive materials also exhibiting both antioxidant and emulsifier characteristics include citric acid and fatty acid esters of glycerol ; sodium , potassium and calcium lactates ; sodium and potassium tartrates ; sodium , calcium and potassium citrates ; sodium , potassium , calcium , ammonium and magnesium phosphates ; and lecithin . consequently , such materials can be used alone in order to provide both antioxidant and emulsifier characteristics or they can be used in combination with other antioxidant and emulsifier materials already described in order to enhance the performance of the compositions . furthermore , such dual function materials can be used in combination or mixture with one another . the process of reducing the rate of oil degradation reactions or stabilizing the composition of hot cooking oil is preferably performed by controlling the rate of introduction of the solutions , dispersions , slurries or suspensions of the antioxidants and / or other beneficial food additive , e . g . water , food acid , or other antioxidant or emulsifier additives , aqueous or nonaqueous , into the hot cooking oil . the rate is preferably one that permits and enhances safe dispersion and diffusion , more preferably without the use of supplementary “ foreign ” carrier materials such as porous minerals or oil emulsions . in a preferred example , a water soluble antioxidant solution may be furnished as a safe “ concentrated additive solution ” to reduce shipping and packaging costs in contrast to a product using oil or porous mineral as a delivery carrier . when the compositions of the present invention are added to the cooking oil , antioxidant previously depleted from the cooking oil is replenished fully or partially by at least one added antioxidant . the compositions also can be added in order to supplement at any time the antioxidant present in the cooking oil . the compositions of the present invention can be effectively delivered to the hot cooking oil by various methods . such methods are applicable to restaurant fryers as well as factory process fryers . for example , the composition containing a food acid , antioxidant and other additive can be delivered to the hot cooking oil using a fine bore or narrow diameter pipe or line . various devices for delivering the composition of the present invention are illustrated in fig1 - 8 . devices for delivering a fine stream include , e . g ., the squeeze bottles of fig2 , 3 and 5 , each including a small diameter opening through which the composition is delivered . a hypodermic syringe as illustrated in fig6 , or small diameter tubing with an appropriate limiting discharge orifice , from which the composition can be delivered onto and / or under the surface of the oil . alternatively , other dispersion or delivery devices comprising a pump or trigger mechanism in combination with a fine orifice or spray nozzle may be used to introduce the compositions of the present invention into the hot oil , such as in the form of a spray or a fine stream , as small diameter droplets , a fog or a “ mist ” of the additive solution over the surface of hot oil ; see fig4 , 7 and 8 . referring to fig2 , 201 is a squeeze bottle , 202 the cap and 203 tip , including small diameter exit hole 204 from which the composition exits when it is extended up from the retracted position in the surface , as illustrated , to about a vertical or 90 ° position relative to the cap surface . referring to fig3 , 301 is a squeeze bottle , 302 a protrusion or tip that is integral with the bottle cap and 303 a small diameter opening from which the composition exits the bottle when the bottle is squeezed ; typically , the bottle cap includes a removable cover for the tip in order to seal it when the bottle is not in use . fig4 illustrates a pump - type dispenser bottle 401 wherein when the pump mechanism 402 is depressed , the liquid within the bottle is drawn up through a dip tube ( not shown ) connected to the pump mechanism and exits through a small diameter orifice 403 in the form of a fog , mist or as small droplets , depending on the diameter or configuration of the orifice . fig5 is a squeeze bottle 501 in which the cap 502 includes an integral cover 503 that , when open , reveals a protrusion 504 and small diameter exit orifice 505 . fig6 is a typical hypodermic syringe comprising a small diameter needle or extension 601 from which the composition exits when the plunger 602 is depressed within the body of the syringe 603 . if desired , the body of the syringe can be volumetrically calibrated to facilitate use of desired amount of the composition with each depression of the plunger . additionally , the syringe can be refilled from a supply of the composition . similarly , calibration and the ability to be refilled are characteristics that are common to each of the devices for adding the composition of the present invention to the hot oil . fig7 illustrates a squeeze - type spray device including a squeeze handle mechanism 702 in which a dip tube ( not shown ) is connected , typically press - fit , internally to the spray head mechanism within the bottle 701 . the composition exits the device through the small diameter opening 704 in the adjustable flow control cap 703 . the squeeze handle mechanism , including the dip tube , is separable from the bottle and typically is attached to it by a screw cap 705 . a universal dip tube and spray mechanism is illustrated in fig8 . the dip tube includes a filter 802 at the pickup end of the tube 801 ; the tube passes through a cap 803 that can be attached to the composition reservoir by , e . g ., a snap or screw fit . as in mechanisms of this type , when the handle 804 is squeezed , it creates a vacuum in the reservoir or bottle resulting in fluid being drawn up the dip tube from which it exits through the adjustable nozzle 805 at the orifice 806 . adjustment of the nozzle opening allows the composition to exit in the form of a fine mist or fog , as small droplets or in the form of a fine stream . an alternative sprayer illustrated in fig9 comprises a dip tube 901 , spray nozzle 902 and squeeze handle 903 arrangement similar to that in fig7 . as in the device illustrated in fig7 , the spray head mechanism is adjustable by rotating the nozzle clockwise or counterclockwise to obtain more or less of a fine stream . additionally , the device illustrated in fig9 also introduces aeration , the extent of which is adjustable by similar rotation of the spray head nozzle . still alternatively , the additive solution , dispersion or concentrate may be introduced continuously , intermittently or at fixed or regular intervals from a storage container where the introduction tube is fixed at a safe point in the fryer and the flow rate is set to meet the needs of the cooking demand during the day . for example , dispersion and diffusion of the aqueous food acid solution into hot cooking oil can take the form of a metering pump with volume and / or time control to introduce the fluid through a manifold containing orifices located beneath , and / or above , the surface of the oil . furthermore , sensors can be used to continuously monitor the technical condition of the oil , e . g ., according to polymerized triglycerides content , polar content , free fatty acid level or peroxide level . various tests to measure oil quality are disclosed in the article by c . gertz , et al ., in the european j . lipid sci . technol . cited hereinabove as well as in u . s . pat . nos . 4 , 349 , 353 and 4 , 731 , 332 . commercial versions of the tests referred to in the latter patents are available from miroil division of oil process systems inc . ( allentown , pa .). these references , including descriptions of various test methods , are incorporated by reference to the extent permitted . an oil quality sensor to dispense and disperse the additive composition to the oil may activate the metering pump . the use of an emulsifier in the composition of the present invention further facilitates efficient dispersion of the composition upon contact with the hot cooking oil , such that the water present in the composition is effectively dispersed so that when it is converted to steam the water droplets are small enough to avoid dangerous splattering of the hot oil . for purposes of the present invention , it is preferred that the aqueous antioxidant food acid or additive should be used in hot cooking oil , e . g ., at or above about 250 ° f ., more preferably at or above about 275 ° f ., still more preferably , the oil temperature is about 300 ° f . to about 375 ° f ., still more preferably about 315 ° f . to about 360 ° f . if the oil is not sufficiently hot , the aqueous composition can sink to a “ cold zone ” at the bottom of the fryer and remain in the form of a warm water composition that is not hot enough to change the water to steam in order to facilitate dispersion and / or diffusion of the water in the aqueous composition and its constituent ingredients into the cooking oil . generally , cooking oils are triglycerides , i . e ., the esterification product of glycerol with three molecules of saturated , unsaturated , or a mix of saturated and unsaturated carboxylic acids . preferably , the cooking oils include vegetable derived , animal derived , and marine source derived fats and fatty oils that are liquids at the particular temperature that is necessary for the desired cooking effect . examples of vegetable oil include canola oil , coconut oil , comgerm oil , cotton seed oil , olive oil , palm oil , peanut oil , rapeseed oil , safflower oil , sesame seed oil , soy bean oil , sunflower oil or mixtures thereof . examples of animal derived oil include lard and tallow ( e . g ., beef , sheep fat ). cooking oil also includes any mixture of the vegetable derived , animal derived , and marine source derived fats . a test of the present invention was conducted in which an aqueous composition containing 20 wt . % antioxidant was sprayed into hot , used cooking oil that had degraded to the point of having an undesirable odor . immediately upon contact of the composition spray with the hot cooking oil a “ froth ” or boiling effect was observed , but undesirable splattering of the hot oil did not occur . the composition was added to the cooking oil from above the surface of the oil using a squeeze handle type spray device of the type illustrated in fig9 , thereby introducing the composition in the form of small diameter aerated droplets . after the oil became quiescent , the cooking odor previously present was no longer noticeable . the composition continued to be applied at approximately 6 hour intervals , thereby appreciably extending the useful life of the cooking oil . various publications , including research reports and the patents , are cited throughout the present application and the contents of these publications , as well as the documents cited in these publications are incorporated herein by reference to the extent permitted . furthermore , any range of numbers recited in the specification or paragraphs hereinafter describing various aspects of the invention , such as that representing a particular set of properties , units of measure , conditions , physical states or percentages , is intended to literally incorporate expressly herein by reference or otherwise , any number falling within such range , including any subset of numbers or ranges subsumed within any range so recited . the term “ about ” when used as a modifier for , or in conjunction with , a variable , is intended to convey that the numbers and ranges disclosed herein are flexible and that practice of the present invention by those skilled in the art using temperatures , concentrations , amounts , contents , carbon numbers , properties such as particle size , surface area , diameter , volume , bulk density , etc ., that are outside of the range or different from a single value , will achieve the desired result , namely , provide an additive and the ability to deliver it to hot oil in order to improve the stability and performance of the oil for frying foods at elevated temperature . although the invention herein has been described with reference to particular embodiments , it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention . it is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the summary of the invention or the appended claims . | 0 |
while the present invention is susceptible of embodiment in various forms , there is shown in the drawings and will hereinafter be described a presently preferred embodiment with the understanding that the present disclosure is to be considered an exemplification of the invention and is not intended to limit the invention to the specific embodiment illustrated . it should be further understood that the title of this section of this specification , namely , “ detailed description of the invention ”, relates to a requirement of the united states patent office , and does not imply , nor should be inferred to limit the subject matter disclosed herein . all patents referred to herein , are hereby incorporated herein by reference , whether or not specifically do so within the text of this disclosure . in the present disclosure , the words “ a ” or “ an ” are to be taken to include both the singular and the plural . conversely , any reference to plural items shall , where appropriate , include the singular . referring now to the figures and in particular to fig1 and 2 , there is shown a print head , for example , an ink jet print head having a positive air system 12 in accordance with the principles of the present invention . the positive air system 12 reduces the potential for dust and debris interfering with the print head jetting pattern and reduces the potential for dust and debris fouling the print head 10 . the system 12 effectively envelopes the environment e around the jetted fluid to prevent the ingress of dust and debris to the local environment e , and minimally , if at all , interferes with the pattern of the jetted fluid . in a very basic form , a printing system 14 includes a conveyor 16 along which boxes b or the like are conveyed past the print head 10 . the print head 10 jets a fluid , such as ink , onto the box b to , for example , provide a bar code , a description of the package contents , a mailing address , or the like . those skilled in the art will recognize the various arrangements by which a print head is mounted near a conveyor for such . the air system 12 , as shown in fig1 and 2 includes air knives or air curtains 18 , to define an enclosure 20 around the print head 10 . as illustrated , three air knives 18 are positioned such that , along with the conveyor 16 , they envelope the print head 10 . each air knife 18 is formed as a wall 19 having a plurality of orifices 22 , formed in a linear array 24 , through which air is exhausted or vented . as illustrated , one air knife 18 is positioned above the print head 10 ( air knife 18 a ), with the array 24 generally parallel to the direction d of conveyance of the box b . a pair of opposing knives 18 b , 18 c are positioned on either side of the print head 10 , with their respective arrays 24 generally perpendicular to the direction d of conveyance of the box b . an air supply 26 supplies clean , debris - free air to the air knives . referring now to fig3 there is shown a cross - sectional view of an exemplary air knife 18 . one of the novel features of the present positive air system 12 is the ability to maintain the “ cleanliness ” of the environment enveloping the print head ; that is , the area between the print head and the boundaries defined by the air knives 18 a , b , c , e . g ., the local environment e . the present positive air system 12 controls this environment , i . e ., maintains a positive pressure to reduce or eliminate the ingress of dust and debris , while at the same time , preventing interference with the fluid jetting patterns . an air path 28 is formed in each knife 18 that branches from a main or common branch 30 to each of the orifices 22 . the path 28 is configured such that the pressure drop ( or the ultimate pressure ) at each orifice 22 is equal to the pressure at each other orifice 22 . in this manner , there are no unaccounted for , or undetermined , air flow patterns . rather , by balancing the pressure drop , the air flow pattern is predictable so as to prevent interference with the fluid jet pattern . in a present air knife 18 , the primary branch 30 is divided into three secondary branches 32 . each of the secondary branches 32 is further divided into three tertiary branches 34 which in turn are divided into paired orifice feed branches 36 . each of the orifice feed branches 36 is about the same length as each other orifice feed branch 36 . as such , the pressure drop across each of the orifice feed branches 36 is about equal as well . however , the secondary 32 and tertiary branches 34 are not of equal length ; thus , the pressure drop could differ between branches ( that is among the secondary branches 32 or among the tertiary branches 34 ). in order to assure that the pressure drop across each of the branches 32 , 34 is about equal , a diverter 38 is positioned at about the branch 32 or 34 junctures . in this manner , the diverter directs or diverts air flow into the various branches 32 and 34 to effect an equal pressure drop ( and thus outlet pressure ) at each of the orifices 22 . in addition to the diverters 38 , a pin 40 can be positioned at the entrance to each of the shortest of the secondary 32 and tertiary 34 branches . the pin 40 further assists in balancing the pressure drops through the various branches to effect a balanced pressure at the orifices 22 . optionally , a restrictor such as that indicated at 42 , can be positioned at about each of the orifices 22 . the restrictor 42 is configured so as to assist in effecting an equal pressure drop ( e . g ., equal pressure at the orifices ), and to further limit the velocity and pressure of the air exiting the orifices . unlike known positive pressure systems which use relatively high air pressures , the present system 12 uses air at a pressure of about 1 psig to about 5 psig . it has been found that an air pressure of about 1 psig is advantageous over known high pressure systems in that the air pressure is sufficiently low so that there is little to no adverse effect on the jetted fluid . that is , the air does not move the jetted fluid from the path that the fluid would other traverse toward the media ( e . g ., box b ) onto which it is applied . an alternate embodiment of an air path 128 for an air knife 118 is shown in fig4 . in this embodiment , the air path 128 is formed different from that of the embodiment 28 in fig3 . the path 128 includes a main or primary branch 130 that divides into three secondary branches 132 . each of the three secondary branches 132 in turn divides into three tertiary branches 134 which in turn divide into three orifice feed branches 136 . again , pins 140 , diverters 138 and restrictors 142 can be used ( if desired ) to facilitate the balancing or equalizing or air pressure at each of the orifices 122 . additionally , a restriction 144 ( as a decrease in diameter or a restrictor ) can be formed at about the primary branch 130 to further facilitate pressure balancing . as seen in fig4 the orifices 122 a at about the edge of the knife 118 can be angled outward . in this manner ( because the knives 118 are angled outward and / or upward relative to the print head 10 , as best seen in fig1 - 13 ), any gaps in air flow that may otherwise occur at the “ corners ” where the upper and side knives meet , are “ filled ”. still other embodiments of the air knife or air curtain are shown in fig6 - 9 . in these embodiments , rather than a plurality of pathways , a relatively large , contained chamber 220 provides a pressurized air reservoir 223 . air is directed out of the reservoir 223 through a plurality of small orifice - like openings 222 in the body of the chamber 220 ( fig6 ), or through an elongated , narrow orifice - like slot 228 in the chamber 220 or in a cover plate 226 ( fig8 ) for the chamber 220 , overlying the reservoir 223 . in still another embodiment 318 as seen in fig9 a thin spacer plate 330 ( about { fraction ( 1 / 1000 )} inch or 1 mil ) having a notched or etched portion 332 is positioned between the chamber body 320 and the cover plate 326 . the notch 332 is open to the reservoir 323 so that air exits the reservoir 323 from between the chamber body 320 and the cover plate 326 through the an elongated orifice - like slot 322 that is defined by the notch 332 . this arrangement provides a continuous restricted flow path or continuous restriction , and as such , provides for a controlled flow ( and pressure ) along the length of the slot 322 . an exemplary cross - section of the air knife embodiments 218 , 318 is illustrated in fig7 . as can be seen , an entrance 234 , 334 to the reservoir 223 , 323 , formed in the chamber body 220 , 320 is relatively small ( thus defining a restriction ) compared to the size of the reservoir 223 , 323 . as such the pressure drop at any of the orifices 222 is about equal to the pressure drop at any of the other orifices 222 and , likewise , the pressure drop at any location along the elongated slot 228 , 322 is about equal to the pressure drop at any other location along the slot 228 , 322 . similar to the angled orifices 122 a of the embodiment 118 illustrated in fig4 the spacer plate 330 can have an angled edge ( as indicated at 333 ) to direct air outwardly , at an angle , to account for the angled orientation of the knives 318 . this prevents “ gaps ” at the corners or junctures of the upper and side knives 318 . in conjunction with the novel use of a low pressure system , as seen in fig1 , the present positive air system 12 uses angled curtains or knives 18 to facilitate directing the deflected air away ( indicated by the arrow at 44 in fig8 ) from the print head 10 . that is , rather than the orifices 22 , 122 , 222 ( or slots 228 , 322 ) directing air perpendicular to the box surface s onto which the indicia is printed , the orifices 22 , 122 , 222 ( or slots 228 , 322 ) direct the air at an angle relative to the surface s . in this manner , the air that deflects off of the surface s is directed away from the print head 10 , rather than toward the print head 10 . it has been observed that this arrangement blows the dust and debris away from the local environment e to maintain the print head 10 and environment e contaminant free . this arrangement also prevents the formation of eddy currents within the local environment e ( e . g ., immediately around the print head i 0 ), that could otherwise adversely impact the fluid droplet path . also as seen in fig1 - 13 , the positive air system 12 can include a supplemental box cleaner knife 46 positioned upstream of the print head 10 and its associated knives / curtains 18 , 118 , 218 , 318 . this supplemental knife 46 facilitates maintaining the local environment e contaminant - free by removing any dust or debris that may be present on the box b before the box b is presented at the print head 10 . an alternate embodiment of the positive air system 50 is illustrated in fig1 - 16 . in this embodiment , the print head 10 is disposed within an enclosure 52 that essentially forms a tunnel 54 . as such , the air flows through the tunnel 54 , including around the print head 10 , and out a forward end 56 of the tunnel , past the print head 10 . to prevent over - pressurization of the tunnel 54 , as when the box b moves passed the tunnel front 56 , a flapper valve 58 is positioned in one of the enclosure walls 60 that provides communication between the tunnel 54 and the outside environment . the flapper valve 58 is closed during normal operation , thus isolating all but the tunnel front 56 . when a box b passes in front of the tunnel 54 , moving passed the print head 10 , the flapper valve 58 opens to relieve any pressure increase in tunnel 54 . in this manner , the air that is supplied through the tunnel 54 does not adversely effect the operation of the print head 10 ( i . e ., effect the fluid droplet path ). again , air is supplied from a clean , debris - free air supply 62 . from the foregoing it will be observed that numerous modifications and variations can be effectuated without departing from the true spirit and scope of the novel concepts of the present invention . it is to be understood that no limitation with respect to the specific embodiments illustrated is intended or should be inferred . the disclosure is intended to cover by the appended claims all such modifications as fall within the scope of the claims . | 1 |
a heat exchanger 1 according to the invention for an air conditioning unit of a motor vehicle , particularly for a low - consumption vehicle , with a plurality of flat tubes 2 which are arranged parallel to one another and through which a heat transfer medium flows and with rib sets 3 arranged between the flat tubes 2 , has electrically operated heating elements 4 as additional heating which can be connected as required . the flat tubes 2 are connected to a system 133 for circulating a first heat transfer medium through each of the flat tubes 2 , schematically depicted in fig1 . the heating elements 4 , consisting of a resistance wire 4 ′ and of an insulation layer 4 ″, are held by means of the holding elements 5 , in the first exemplary embodiment by means of a holding grid 6 which is soldered on a narrow side of each flat tube 2 . the holding grid 6 is produced from a metal sheet which is provided by means of a forming operation with beads 7 serving for subsequent soldering , in which case soldering may take place simultaneously with the soldering of the remaining heat exchanger , since the heating elements 4 cannot , as a rule , be exposed to the soldering operation . the mounting of the heating elements 4 is illustrated in detail in fig1 . the left part of fig1 shows the positioning of the heating element 4 on the holding element 5 soldered to the flat tube 2 , the forming of the holding element 5 is illustrated in the middle and the heating element 4 ready - fixed with the aid of the holding element 5 is illustrated on the right . in this case , the ends 8 of the holding grid 6 are crimped shut . the beads 7 on the one hand , serve for positioning the holding grid 6 and the heating elements 4 and , on the other hand , form a heat - conducting connection to the heat exchanger 1 , in order to utilize part of the rib surface of the latter for the transfer of heat to the air flowing through . depending on the electrical resistance , on - board voltage and desired electrical heating power , the individual heating elements 4 may be connected by means of a parallel and / or series connection in a way not illustrated in any more detail . for power regulation , a pulse - width modulation method is used , but other methods for power regulation are also possible . three very similar exemplary embodiments are described below with reference to fig2 to 4 . in these and all the following exemplary embodiments , elements not described in any more detail are identical to those of the first exemplary embodiment described above . according to the exemplary embodiment illustrated in fig2 , heating elements 14 , consisting of a resistance wire 14 ′ and of an insulation layer 14 ″, are pressed directly into projecting rib sets 13 which are configured in such a way that they project sufficiently far beyond the flat tubes 12 , in the present case , conventional beaded tubes , so that they themselves form the holding elements 15 . if required , the heating elements 14 may additionally be surrounded by a metallic casing and be secured between the ribs , for example by means of adhesive bonding . in this case , the heating elements 14 have a sheet - like configuration such that their thicknesses correspond approximately to the thickness of the flat tubes 12 . at the same time , in the present instance , the heating elements 14 consist of two individual heating conductors , so that current inward and return routing is provided within a heating element 14 . in the other two exemplary embodiments illustrated in fig3 and 4 , there are provided for the heating elements 24 and 34 , special holding elements 25 and 35 which are themselves pressed into projecting rib sets 23 and 33 and , if appropriate , additionally secured . in these instances , too , the flat tubes 22 and 32 are conventional beaded tubes . alternatively , in a similar way to the first exemplary embodiment , the holding elements 25 and 35 may be soldered in at the same time as the manufacture of the heat exchanger without heating elements 24 and 34 and be provided with the heating elements 24 and 34 thereafter . according to the fifth exemplary embodiment illustrated in fig5 , for better thermal coupling of rib surfaces to the heating elements 44 , a folding strip 45 ′ consisting of a solder - plated aluminum strip is provided , which is pushed into the flat tubes 42 , which are again beaded tubes , before and after the bundling and before the soldering , is fixed and is also soldered . furthermore , the holding element 45 in the form of a holding grid 46 is tacked on to the bundled heat exchanger 41 in a similar way to fig1 , without the heating element 44 and insulation , by means of a wire connection or welding , and is also soldered . according to the first exemplary embodiment , the heating elements 44 are inserted and crimped in after soldering . in the present exemplary embodiment , only every second row of flat tubes 42 is equipped with heating elements 44 , but any other desired variants are also possible . fig6 to 8 show exemplary embodiments with modified flat tubes 52 , 62 and 72 , to which a heating element 54 , 64 and 74 is fastened by means of a holding element 55 , 65 and 75 . according to the sixth exemplary embodiment ( cf . fig6 ), the holding element 55 comprises a flat - designed end of the flat tube 52 , while , according to the seventh exemplary embodiment ( cf . fig7 ), the end of the flat tube 62 is of open design and receives the holding element 65 . according to the eighth exemplary embodiment ( fig8 ), the holding element 75 is mounted laterally on the flattened flat tube 72 , that side of the holding element 75 which is located opposite the common side being in alignment with the corresponding side of the flat tube 72 . according to the ninth exemplary embodiment illustrated in fig9 , the holding element 85 provided is a holding grid 86 and the heating element 84 provided is a heating grid 84 ′ which is illustrated , stretched out , in fig1 , fig1 illustrating at the top the length which corresponds essentially to the length of the heat exchanger 81 , that is to say to the tube length . for assembly , the holding grid 86 is bent in such a way that it can receive the correspondingly folded heating element 84 . for this purpose , said holding grid is pushed between two rib sets 83 , fixed in a known way , that is to say , for example , introduced before the soldering process and also soldered , and the heating element 84 is subsequently pushed or pressed into the open grooves . this is essentially a heat exchanger of conventional type of construction , in which the gilled corrugated rib is replaced by a deeper rib , with the result that the rib projects beyond the flat tube 82 in order to receive the holding grid 86 and the heating grid 84 ′ embedded in the latter . the holding grid may also be formed by individual u profiles which are not interconnected or by correspondingly pre - bent sheet metal strips . the heating grid is produced , for example , by stamping and subsequent forming from one piece , a combination of parallel - connected and series - connected regions being possible in the present instance ( cf . fig1 , in the present instance in each case three parallel - connected regions are connected in series ), but a straightforward parallel connection or a straightforward series connection is also possible . to avoid short circuits between the heating grid 84 ′ and the holding grid 86 , the heating grid 84 ′ is provided with an insulation layer 84 ″. this insulation layer 84 ″ is formed by an insulating lacquer . so that the width b of the current supply and current distributor strips of the heating grid of fig1 can be made narrower , it is possible to reinforce these with an attached electrically conductive bar . a heating grid with a busbar 99 according to this variant is illustrated in fig1 . in this case , the busbar 99 also increases the mechanical dimensional stability of the heating grid and makes it easier to push it into the u - shaped receptacles of the holding grid . according to a further tenth exemplary embodiment , a heating grid 104 ′ serving as a heating element 104 is designed in such a way that it can be pushed in directly on the air outflow side between rib sets 103 projecting on the end face beyond the coolant - carrying flat tubes , without the risk of damage to the insulation layer and of a short circuit possibly resulting from this . according to the exemplary embodiment , the insulation layer is formed by a teflon coating , but it may also be formed , for example , by correspondingly suitable lacquers , in particular stoving lacquers with sufficient temperature resistance , or the like . additional protection is afforded by a slight forming of the projecting ribs in the region of their corners , so that an introduction slope for the heating grid 104 ′ is obtained . forming may take place before the soldering of the heating body block or else thereafter , as illustrated in fig1 a . in this case , a special forming tool ( indicated at the top in fig1 a ) is introduced between the respective rib sets 103 in the introduction direction of the heating grid 104 ′, so that the corners of the individual ribs are formed and thereby sloped . after the forming operation , as illustrated in fig1 b , the correspondingly bent heating grid 104 ′ is introduced on the end face with respect to the flat tubes between the projecting rib sets 103 serving as a holding element 105 . in the present instance , a heating section of the heating grid 104 ′ is arranged between two adjacent rib sets in each case , but other variants are also possible , in which not every interspace between two rib sets receives a heating section of the heating grid . the individual heating sections of the heating grid 104 ′ are connected by means of connecting webs and auxiliary connecting webs , as is evident from fig1 . fig1 shows the heating grid 104 ′, there being provided between the individual heating sections , which run parallel to the flat tubes in the assembled state , connecting webs arranged on the end face and narrow auxiliary connecting webs which , in the assembled state , run beyond the end faces of the rib sets . the arrangement of the heating sections and connecting webs is meander - like , as also in the exemplary embodiment described above with reference to fig1 . fig1 shows a variant of the heating grid of fig1 , but in a stretched - out illustration , wider connecting webs being provided , which are folded round in order to double the material thickness , as indicated by arrows at the bottom of fig1 . it can also be seen from fig1 that , in the middle of the heating sections , a predetermined bending line is provided by means of perforations , which at the same time prevents the axial current flow and consequently the generation of heat in the region of the contact point with the narrow sides of the flat tubes . the width of the remaining material between the individual perforations is dimensioned such that a sufficient elastic force can be applied so that the flanks of the heating sections are pressed against the rib sets . alternatively , slots may also be provided , as illustrated in fig1 . if an additional holding grid is provided , pressing takes place against the latter . the heating grid according to the variant is stamped out from a heating conductor band material . by the doubling of material , tripling , etc . also being possible , the current density in this region can be lowered and therefore local heating at the connecting webs can be reduced , without an additional current conducting bar mounted at a later stage being necessary . the auxiliary connecting webs between the heating sections serve merely for improved handling during mounting and are severed after assembly has taken place . in the case of a holding grid without a current conducting function , the severance of the auxiliary connecting webs may be dispensed with . by a folding in , if appropriate even multiple folding in of edge zones , for example also sheet edge zones , the material thickness and therefore the current - conducting cross section is enlarged . the same may , of course , also be achieved correspondingly by a use of what are known as tailored blanks as base material for the stamped sheets , and in these the edge zones assigned to connecting webs are of thicker design . fig1 illustrates an eleventh embodiment , according to which a polymeric ptc plastic element , designated below as a cutout s , is interposed centrally in the heating section ( heating element 114 which is formed by a heating grid ) which runs in a meander - like manner in a web of a holding grid ( holding element 115 ) of u - shaped design . this cutout s serves for overheating protection and ensures that , at too high a temperature , no or only minimal current flows through the corresponding heating section and overheating is thereby prevented . for this purpose , the cutout element is designed in such a way that it likewise bears in a sheet - like manner against the flanks of the holding grid and consequently likewise discharges its lost heat to the latter . the holding grid and / or the heating grid are insulated relative to one another by means of a largely electrically non - conductive layer between them . the function of the holding grid is to absorb over a large area the heat discharged by the heating grid and to transfer the latter to the rib blocks adjacent thereto ( see fig1 ). for this purpose , the entire structure of the heating elements is divided into a plurality of and consequently higher - impedance parallel heating circuits which are protected individually by means of more cost - effective overheating cutouts based , for example , on polymeric ptc elements . thus , it is possible , inter alia , to prevent the electrical connecting bridges between individual heating sections from being overheated . various circuits are illustrated in fig1 a to 16 c . fig1 a shows a circuit in which all the webs of the heating grid are connected in parallel , each web being equipped with a series - connected overheating cutout . in this case , the individual webs must be of correspondingly high - impedance design , this preferably being achieved by means of the meander - shaped design , as illustrated in fig1 . by use of other circuits , as illustrated , for example , in fig1 b and 16 c , the current flowing in the heating sections can be adapted to the current carrying capacity of the overheating cutout by an adaptation of the resistance . intermediate cooling of the current bridges 131 by heat contact with the rib sets may take place in that , according to fig1 , the current bridges 131 are designed with an additional bead 130 as an intermediate cooling bead , said beads engaging into the free interspaces between the rib sets . in this case , however , heating sections of the heating grid are arranged only between every second rib set . it may be noted that the holding grid 115 is not illustrated in perspective in fig1 . alternatively to the illustration in fig1 , any other desired arrangements are possible , for example heating section , bead , bead , heating section . by the increase in the resistance by means of a meander structuring of the heating grid , the current flow through a section can be markedly reduced . this affords the possibility of keeping the loss heat occurring in the current bridges between the individual heating sections so low that the latter do not overheat , even without direct contact with the rib blocks . according to a twelfth exemplary embodiment illustrated in fig1 , a heating grid ( heating element 124 ) lies as a composite structure directly in a holding grid ( holding element 125 ). according to the present exemplary embodiment , this is possible due to the use of a composite structure consisting wholly of a plastic ptc structure and of an electrically conducting contact band . in this case , the current flow is routed from the inner electrode (+ pole ) through the polymeric ptc structure outward to the holding grid which at the same time constitutes the other electrode ( ground ). the entire heat exchanger is in this case at a potential of the voltage source , preferably at ground potential . to coordinate the resistance with the desired heating capacity , the specific resistance and also the area and thickness of the polymeric ptc material employed may be used and / or the resistance is adapted by means of circuitry measures . for this purpose , for example , the voltage may be supplied at first portions of middle electrodes . according to fig1 and 20 which illustrate a thirteenth exemplary embodiment , the current is in this case routed from the middle electrode to the holding grid and from there back to a second portion of the middle electrode . the holding grid is in this case at an intermediate potential and has to be insulated electrically from the heating body . advantageously , the polymeric ptc material consists of a film which is laid in a u - shaped manner around the middle electrode and under light pressure stresses just fills the space within the holding grid , or it is designed as an extruded profile . in this thirteenth exemplary embodiment with a middle electrode for contacting a polymeric ptc layer as a continuous heating element within a holding grid , a metallic heating conductor is dispensed with completely . as a result of the ptc characteristic , the heating structure itself is safe and requires no additional overheating protection . the heating grid and / or holding grid may be bent according to the cross sections illustrated in fig2 a to 21 f . the relatively angular u - profile illustrated in fig2 a and 21 b offers the largest contact surface and therefore the best heat transfer . the u - profile illustrated in fig2 c and 21 d and having a v - shaped design at the bottom offers tolerance compensation as a result of a resilient bearing contact of the flanks . the same also applies correspondingly to the u - profile illustrated in fig2 e and 21 f which is dented from below , in this case a longer bearing contact of the flanks and consequently better heat transfer being afforded . by virtue of the configuration according to fig2 a to 21 f , a planar bearing contact of the heating grid flanks against the flanks of the holding grid is ensured , even in the case of a slightly variable thickness of the electric insulating layer . | 5 |
fig1 shows the system architecture of an avatar network including devices of the present invention . the avatar network includes multiple video acquisition devices 3 ( only one is shown in the figure for simplification ), multiple remote computers 2 ( only one is shown in the figure for simplification ), a server 1 which is located in the internet and has a public ip address , and a communication network 4 . the communication network 4 may be the combination of the internet , wired lan and wireless lan . the video acquisition devices 3 are located in locales where content is provided , and the remote computers 2 are in front of remote users . the video acquisition devices 3 are connected with the server 1 through the communication network 4 including wireless lan and the internet . the remote computers 2 are connected with the server 1 through the communication network 4 including the wired lan and the internet . by the aid of the server 1 , according to the process described by fig2 , the remote computers 2 and the video acquisition devices 3 can be connected through the communication network 4 for transmitting video data and haptic data . the remote computers 2 may have the private ip address of lan , and are connected with the internet through routers which have public ip address . remote computers 2 are in front of users , and are equipped with joysticks 21 . users obtain the locale video information through the screen of remote computers 2 , and give haptic information through joysticks 21 according to the intention of users . the haptic information will affect the speed and the position of video acquisition devices 3 . the video information acquired by video acquisition devices 3 is changed due to the movement of video acquisition devices 3 . therefore , viewed from the locale content , the remote users interacts with the locale dynamically , and viewed from the users , video acquisition devices 3 can be regarded as avatars of users . as an avatar of a user , it is unnecessary for a video acquisition device 3 to have the public ip address . the video acquisition device 3 may have a private ip address of wireless lan , and be connected with the internet through wireless gateways . the video acquisition device 3 includes an video input unit 31 , a computing unit 32 for processing video data and haptic data , an electromechanical unit 33 for moving according to the haptic data , and a communication unit ( not shown ) for transmitting the video data and haptic data . the electromechanical unit 33 can be regarded as “ feet ” of the avatar . the electromechanical unit 33 includes wheels , a driving mechanism , a dc motor for driving the wheels and a stepper motor , a power electronic device for controlling the motor and a battery serving as a power source . for example , the power electronic device can receive pwm signals from the computing unit 32 , and determine the speed of the dc motor , and then control the speed of wheels according to the duty ratio of pwm signals . the pwm signals are generated according to the haptic data . the video input unit 31 can be regarded as “ eyes ” of the avatar . the video input unit 31 includes a ccd camera or a cmos camera , a video capture card and a pan unit . for example , the video capture card can be connected with the computing unit 32 through the pci bus . the computing unit 32 can send instructions related to video capture to the video capture card . the video input unit 31 can be equipped with multiple cameras , in order to acquire video information from a plurality of views or achieve three - dimensional effect . the computing unit 32 and the communication unit of the video acquisition device process and transmit video data and haptic data which are related to the “ feet ” or “ eyes ” of the avatar . they can be realized with the industrial computer and the wlan card . for example , the video frame information from the video input unit 31 can be compressed into a plurality of data packets less than 1 kb , and be sent to the remote computer 2 . data packets from the remote computer 2 containing haptic data are converted into pwm signals , and then are inputted into the electromechanical unit 33 of the video acquisition device 3 . fig2 shows a flowchart of the method according to the present invention . the flowchart illustrates the process of the method according the present invention . the whole process relates to the local video acquisition devices 3 , the remote computers 2 and the server 1 located in the internet , which are shown in fig1 . after a video acquisition device 3 is powered up , at least two udp channels between a video acquisition device 3 and a nearest router with a public ip address should be maintained . the first udp channel is used to transmit video data from the video acquisition device 3 to the remote computer 2 , and the second udp channel is used to transmit haptic data from the remote computer 2 to the video acquisition device 3 . additional udp channels can be used to transmit haptic data from the video acquisition device 3 to the remote computer 2 , or used to transmit audio data . to this end , in step 100 , the video acquisition devices send the data packet containing register signaling and avatar information ( such as nickname or id numbers of the video acquisition devices ) to register the video port number of the devices on the server 1 . if the video acquisition devices haven &# 39 ; t received the request signaling from remote computers 2 , the video acquisition devices 3 regularly repeat the registration . in order to maintain the first udp channel between the video acquisition devices 3 and the nearest routers with public ip address , the intervals between the registrations are less than or equal to 3 minutes . and the server 1 records the router &# 39 ; s ip address and video port number for the first udp channel . in step 200 , the video acquisition devices 3 send data packets containing the register signaling and avatar information , in order to register the haptic port number of the devices on the server 1 . if the video acquisition devices haven &# 39 ; t received the request signaling from remote computers , the video acquisition devices 3 regularly repeat the registration . in order to maintain the second udp channel between the video acquisition devices 3 and the nearest routers with public ip address , the interval between the registrations are less than or equal to 3 minutes . and the server 1 records the router &# 39 ; s ip address and port number for the second channel . the order of the step 100 and step 200 may be changed . after receiving data packets containing different kinds of register signaling , the server 1 sends data packets for confirmation to the video acquisition devices 3 respectively . after the registration , the server deems the video acquisition devices corresponding to the avatar information online . a user inputs an instruction for connecting avatar into remote computers , and the instruction contains parameters , such as avatar information and username ( if necessary , the instruction contains a password , and the username may be retrieved from a configuration file ). similarly , at least two udp channels between the remote computer 2 and the nearest router with a public ip address should be established . the first udp channel of the remote computer is used to transmit video data from the video acquisition device 3 to the remote computers 2 , and the second udp channel of the remote computers 2 is used to transmit haptic data from the remote computer 2 to the video acquisition device 3 . an additional udp channel of the remote computer 2 may be used to transmit haptic data from the video acquisition device 3 to the remote computer 2 , and may also be used to transmit audio data . in step 300 , the remote computer sends a data packet containing the register signaling and the username to register the video port number of the user on the server . the server records the router &# 39 ; s ip address and port number for the first udp channel of the remote computer . in step 400 , the remote computer sends the data packet containing the register signaling and the username , in order to register the haptic port number of the user on the server . the server records the router &# 39 ; s ip address and port number for the second udp channel of the remote computer . the order of the step 300 and step 400 can be changed . after receiving data packets containing different kinds of register signaling , the server sends data packets for confirmation to the remote computer respectively . after the registration , the server deems the user who corresponds to the username and is front of the remote computer online . after the remote computer 2 registers video port number and haptic port number on the server 1 , in step 500 , according to the video acquisition device &# 39 ; s information ( also called avatar information ) inputted by the user , the remote computer 2 sends a request signaling including the information about the video acquisition device to the server 1 . at this time , the server has recorded video port numbers , haptic port numbers and public ip addresses corresponding to multiple online video acquisition devices 3 . according to an avatar nickname or an id in the request signaling , the server searches the related record of the video acquisition device to be connected to the remote computer 2 . if necessary , the server 1 may check whether the user corresponding to the remote computer 2 has the permission to connect to the requested video acquisition device 3 . and the server 1 can also check whether the requested video acquisition device 3 is connected to another remote computer . if the requested video acquisition device is offline , or if it is connected to another remote computer , or if the user hasn &# 39 ; t the enough permission , the server 1 returns the request failure information , and the whole process ends . if the requested video acquisition device is online and is idle , and if the user has the permission to connect , then in step 600 , the server 1 returns a data packet for confirming the request , which contains a public ip address , video port number and haptic port number corresponding to the video acquisition device . in step 700 , according to the public ip address and port numbers corresponding to the video acquisition device , the server 1 forwards the user &# 39 ; s request signaling to the video acquisition device , and finds out the public address and port numbers corresponding to the remote computer 2 which sends the request , and notifies the video acquisition device of them . after the remote computer 2 and the video acquisition device have known their opposite &# 39 ; s address information , two channels between the remote computer 2 and the video acquisition device 3 should be established to transmit video data and haptic data respectively . to this end , the remote computer 2 sends test packets to the public ip address and video port number corresponding to the video acquisition device through its first udp channel , and sends test packets to the public ip address and haptic port number corresponding to the video acquisition device through its second udp channel . similarly , the video acquisition device 3 sends test packets to the ip address and video port number corresponding to the remote computer 2 through its first udp channel , and sends test packets to the ip address and haptic port number corresponding to the remote computer 2 through its second udp channel . the test packets may not arrive at the remote computer 2 or the video acquisition device 3 . but with the aid of the test packets , the first udp channel of the remote computer 2 , the first udp channel of the video acquisition device and the route of the internet are connected and form the first channel for transmitting video data . the second udp channel of the remote computer 2 , the second udp channel of the video acquisition device , and the route of the internet are connected and form the second channel for transmitting haptic data . for more details about establishing channels , please refer to the well - known p2p technology . in step 800 , the video acquisition device 3 confirms that it has received the request from the user by using the first channel , and waits for the acknowledgement from the remote computer . once receiving the confirmation , the video acquisition device 3 starts to transmit video data to the remote computer through the first channel , and waits for haptic data from the remote computer in the second channel . after receiving the confirmation through the first channel , the remote computer sends a data packet for acknowledging to the video acquisition device 3 in step 900 . and in step 1000 , the remote computer sends a data packet to the server , in order to confirm the established connection . thereafter , the remote computer waits for video data from the video acquisition device 3 in the first channel , and sends haptic data to the video acquisition device 3 through the second channel . the haptic data are a set of sample values of motion state . for example , the haptic data may be a set of sample values of tilt angle of a joystick , namely a set of sample values of given movement speed . the remote computer 2 processes the video data received from the first channel , and presents the processed video data to the user . the user determines the next motion state of the avatar ( namely the video acquisition device ) according to the video information , and generates haptic information with the joystick . the haptic information is transmitted to the video acquisition device 3 through the second channel . the video acquisition device 3 processes the received haptic information . then according to the user &# 39 ; s intention , the video acquisition device 3 “ moves ” as user &# 39 ; s avatar , and send video information which is “ seen ” by the avatar to the user through the first channel . when the user doesn &# 39 ; t want to continue to be connected with his avatar , the user inputs a disconnecting instruction : to the remote computer 2 . after receiving this instruction , the remote computer 2 stops receiving video data in the first channel . and it stops sending haptic data in the second channel . in step 1100 , the remote computer 2 sends a data packet containing a disconnecting signaling to the server 1 . after the server 1 receives this data packet , the flag of the video acquisition device 3 is set idle by the server 1 . if necessary , the server 1 calculates the duration of the connection between the user and the avatar , which is used to the subsequent processing such as billing . in addition , in step 1200 , the remote computer 2 sends a data packet containing a disconnecting signaling to the video acquisition device 3 . after receiving the data packet , the video acquisition device 3 stops sending video data in the first channel . and it stops receiving haptic data in the second channel and registers video port number and haptic port number on the server regularly . the server deems the video acquisition device 3 online . when the video acquisition device 3 is online and idle , with a remote computer having access to the internet , another user can transform the video acquisition device 3 into his avatar . 100 video acquisition devices register visual address information on the server 200 video acquisition devices register haptic address information on the server 300 the remote computer registers visual address information on the server 400 the remote computer registers haptic address information on the server 800 the video acquisition device confirms request signaling for computer 1200 the remote computer sends disconnecting signaling to the video acquisition device while the invention has been described above by reference to various embodiments , it is intended that the foregoing detailed description be regards as illustrative rather than limiting . it should be understood that many changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims . | 7 |
other characteristics and advantages of this invention shall become clear with the following description as well as with the sketches found in the appendix , designed to illustrate various possible configurations with no limitative intent . to simplify , we shall consider that the lines appearing on the cross - sections represent the cell material . in order to take into account the known descriptions arising out of the previous art , the spaces that are contained within these lines can be assumed to represent male mandrels or molds . the spaces which are outside the lines can be assumed to represent female molds . the dotted lines as well as the dots indicating the longitudinal axes do not represent any material . they are used to show the boundaries of the partially virtual envelopes , most often in the description relating to the cell body , or to locate the cell with respect to its longitudinal axis . when the description refers to a cell in its natural state , we mean a cell whose position and shape are identical to those of the cell still in the mold prior to its release . therefore , a cell can be in its natural state when the support is being assembled . in a completed support , a cell in its natural state shall be assumed filled with a fluid , the volume of which is equal to the volume of the male mandrel used to manufacture the cell , and not subjected to any external mechanical strain , except the ambient pressure . fig1 is a bird &# 39 ; s eye view of an upper sheet made of roughly identical expansible cells , such as those shown on fig6 , 9 , 10 and 11 . fig2 : cross section of the side walls of the body of a cell in its natural state , in the shape of an eight branch star . fig3 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly circular and about octagonal , with eight randomly distributed crevices of various shapes and at least as many flat segments as there are crevices on the outer perimeter . fig4 a : cross section of the side walls of the body of a cell in its natural state with four branches ending at the four corners of a square , mostly derived from the previous art . fig4 b : detail of a rib of an expansible cell according to the previous art and the current invention . fig5 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring four crevices on the sides of the square and at least as many flat segments on the outer perimeter . fig6 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring four diagonal crevices and at least as many flat segments on the outer perimeter . fig7 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring four diagonal crevices , the walls of these crevices being not parallel and the crevices being larger at the distal end of the cell or draft and featuring at least as many flat segments as there are crevices on the outer perimeter . fig8 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly octagonal , featuring eight crevices on the eight faces of the octagon and two concentric inner perimeters , and having at least as many flat segments on the outer perimeter as there are crevices . fig9 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly circular , featuring four crevices and having at least as many flat segments on the outer perimeter as there are crevices . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring four diagonal crevices whose walls are not parallel , the crevices being larger towards the center of the cell or against draft , and having at least as many flat segments on the outer perimeter as there are crevices . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly circular , featuring four crevices with draft and at least as many flat segments on the outer perimeter as there are crevices . fig1 : cross section of the side walls of the body of a cell in its natural state in the shape of a five branch star , each branch ending at the corners of a pentagon . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly pentagonal , featuring five crevices on the five sides of the pentagon and as many flat segments on the outer perimeter as there are crevices . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly pentagonal , featuring five crevices on the five sides of the pentagon , three sides being curved , continuous on three sections between four of the crevices , the two other sides being flat , and having at least as many flat segments on the outer perimeter as there are crevices . fig1 a : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring five crevices , two crevices being located on the half diagonal lines of the square , at the end points of a given side , one crevice being located at the midpoint of the side opposite to the side between the two crevices on the half diagonal lines , the last two crevices being located on the outer envelope , roughly at the two - third point on the last two sides , between the first three crevices , and said cell featuring at least as many flat segments on the outer perimeter as there are crevices . fig1 b : detail of the rib of a cell exhibiting at least three sides . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly pentagonal , featuring ten crevices , five of which are on the sides of the pentagon , the five others being on the apexes of the pentagon , and two concentric inner perimeters , and featuring at least as many flat segments on the outer perimeter as there are crevices . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly circular , featuring five crevices and at least as many flat segments on the outer perimeter as there are crevices . fig1 : bird &# 39 ; s eye view of a support consisting of an upper sheet made of roughly identical expansible cells , such as those shown on fig6 , 9 , 10 and 11 , attached to a lower sheet . fig1 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring five crevices , two crevices being located on the half diagonal lines of the square , at the end points of a given side , one crevice being located at the midpoint of the side opposite to the side between the two crevices on the half diagonal lines , the last two crevices being located on the outer envelope , roughly at the two - third point on the last two sides , between the first three crevices , these two crevices presenting each a concave wall and a convex wall , said cell featuring at least as many flat segments on the outer perimeter as there are crevices . fig2 : cross section of the side walls of the body of a cell in its natural state with four branches , each branch ending at the corner of a square according to previous art and in which the ribs are as fine as possible . fig2 : cross section of the side walls of the body of a cell in its natural state whose external envelope is roughly square , featuring four crevices on the four sides of the square , these crevices being as narrow as possible , and featuring at least as many flat segments on the outer perimeter as there are crevices . this invention pertains to the design of mattresses , cushions , padding for medical use , reusable packaging for fragile items and dampening support . one creates a support or padding which consists of an upper sheet 1 , generally flexible and formed as needed , consisting of expansible cells 3 which can be interconnected and which can expand when filled with a fluid , characterized by the fact that the cross section of the body of a cell in its natural state is delimited by at least two partially virtual perimeters , inner 6 and outer 7 , which are concentric and inscribed on envelopes of various shapes , square 16 , pentagonal 19 , octagonal 17 , circular 18 , irregular 15 and 20 , where the slits , crevices or cracks are mostly created by more or less closely spaced side walls , which are parallel 4 or not , with draft 8 or against draft 9 , straight 21 , concave 10 , convex 11 or in the form of jagged lines 12 a and 12 b , which connect the outer perimeter 7 to the inner perimeter 6 . without any limitative intent , the use of a jagged line 14 to connect to a point 22 on the perimeter 7 to a point 23 of the center area 6 more or less near the axis 24 of the balloon or cell ( fig3 / fig2 / fig1 ) offers a definite advantage in that the part of the cell side wall connecting two points located on separate concentric perimeters 6 and 7 can be a definite straight line on its centripetal path if , between two other points 28 being the same as the first one located on the outer perimeter 7 at the junction or exit point from a crevice . all the points on the flat section 29 are further away from the center 24 of the cell than the other points which are not on the flat section 29 and form the envelope 7 on its path between two points 28 located at the junction of successive crevices 4 . one sees ( fig1 ) a shaped upper sheet 1 , made of inflated cells 3 . having cells rigidly attached to each other via sheet 1 offers all kinds of benefits to the fabrication process . the sheet 1 being assembled with sheet 2 ( fig1 ), it is nevertheless sometime possible to assemble a single cell or a cluster of interconnected cells originating from a sheet 1 on sheet 2 independently from the rest of the support . the perimeter of the cell being equal to the sum of the apparent lengths of the exterior on the sides of the concentric sheaths plus the lengths repeated as many times of the walls of the fissures connecting these concentric sheaths . the shape of the cells as described in the present invention is characterized by the fact that unlike the cells known in the prior art and which comprise branches in straight lines ( fig4 b ) the cells purpose of the present invention possess walls whose sides have a wider surface ( fig1 b ) and which show slits , clefts or fissures . as described in the prior art a cell 3 ( fig1 and fig1 ) comprises from apex to bottom along the longitudinal axis 24 an apex 25 in the shape of a dome or a cupola when the cell is filled with fluid and when the cell is in a resting state the walls on the exterior sheath generally rejoin gently the central point of that apex preferably situated along the longitudinal axis : a body 26 purpose of the invention , a base 27 of indifferent shape , uniform or not with the body in a resting state , one may for example have a cell body 26 in a square section ( fig6 ) and a base 27 in a round , octagonal or square section , of a greater or smaller size in height and width . the bottom of the fissures of a cell in a resting state generally rejoin gently the exterior wall 7 above the joined plane of sheets 1 and 2 so as to also allow for the expansion of the fissures at that level . according to the invention , fissures possess walls perceptibly more or less close , parallel or perceptibly 4 , concave 10 , convex 11 , broken 12 a and 12 b the walls of the fissures are not necessarily symmetrical in relation to the sagittal plane of the fissure ( fig3 ) and are not necessarily radiad ( fig1 ). according to the invention and the description of the fissures , the cell &# 39 ; s wings and branches are comprised and defined between two contiguous and successive fissures as we shall define them later ; they are at a minimum triangular in shape generally , but can also be quadrilateral ( fig5 ) or other , with an interior apex . one must note that graebe in u . s . pat . no . 4 , 005 , 236 and u . s . pat . no . 5 , 052 , 068 described shapes of cells with several wings uncommon and not defined outside notably of what results from his invention described in u . s . pat . no . 4 , 541 , 136 and described again for parties in u . s . pat . no . 5 , 052 , 068 ; roux in his application fr 95 / 08972 described different forms one after another without being able to describe them as in the present invention in a global manner and the irrefutable differences in relation to the prior art . by comparison with the products known in the prior art , where the first ( fig2 ) is described as a star formed of eight branches 5 joined to a central virtual element 6 and contained in an exterior sheath 7 and the second ( fig4 a ) as a star with four branches ending at the four corners of a squared sheath , one sees that from the distal extremity of the branches to the proximal part the walls of the branches 5 are in a straight line 13 . the advantage of the present invention by comparison is in the replacement of these straight walls ( fig2 fig4 a , fig1 ), the straight line being the shortest path from one point to another , by longer cell walls for example in a jagged line 14 between points 22 and 23 located each on one of the concentric perimeters 7 and 6 , portions of the cell walls which follow in their centripetal path the path of the exterior sheath and shown in their distal path on at least a part of the exterior sheath 7 between the two points 28 and a flat part 29 ( fig4 b ) and in their proximal path slits or fissures 4 between two contiguous parts of proximal walls of said portions of the walls , fissures 4 with walls more or less perceptibly closer whose sagittal plan is here radial on the path of these jagged line 14 , in the proximity of the center 24 named proximal path , the sagittal plane of a fissure is the plane located generally at mid point between the posing walls of a fissure as we shall see further on this plane is not necessarily radial . one sees that according to the invention the gain in perimeter of the cell inflated with fluid is perceptibly from 10 % to 25 % in practice , and as much as 40 % in theory as we shall demonstrate further on , in the case of a cell presenting a section with four fissures on the lateral sides ( fig5 ) having wings with several sides in relation to a cell in the shape of a cross ( fig4 a ) having wings with two sides , just like a star with eight branches ( fig2 ) has a perimeter which is inferior to a cell with eight fissures ( fig3 ). the process is identical between a star with five branches ( fig1 ) in a relation to a pentagon with five fissures ( fig1 ). in theory considering that figs . ( 20 ) and ( 21 ) represent the section of cell bodies inscribed in squared sheaths of the same dimension as in examples pushed to the extreme in representations of figs . ( 4 a ) and ( 5 ) respectively where the wings are as thin as possible and the fissures the narrowest : knowing that “ d ” is the length of half of the diagonal of the square in the case of a cell meeting the criteria of fig . ( 20 ) the perimeter of the cell would be eight times “ d ”, in the case of a cell meeting the criteria of fig . ( 21 ) the perimeter would be equal to sixteen times “ d ”, which is divided by the square root of two if the square root of two is perceptibly equal to the fraction seven fifths , the theoretical perimeter of the cell ( fig2 ) would be approximately eleven and a half times “ d ”. consequently , the theoretical perimeter of the cell in fig . ( 21 ) is superior by about 40 % to that of the cell in fig . ( 20 ), more simply by comparing the wings or branches ( fig4 a ) in the prior art and the ones ( fig1 b ) according to the invention , the supplement in length according to the invention is perceptibly the difference between the lengths of the exterior side ( fig1 b ) and the thickness of the wing in the prior art ( fig4 b ), in the case where the thickness of the wing is very low or in the case of a wing is very low or in the case of a wing with parallel walls ( fig4 b ) the presence of a flat part 29 according to the invention on perimeter 7 concerning this wing indicative of the given advantage . graebe at first in his first patents and then in u . s . pat . no . 4 , 541 , 136 , followed by benguigui in u . s . pat . no . 5 , 553 , 220 described cells whose wings have parallel walls and also depression notably lateral in the case of cells with four branches all of them possessing , for graebe as well as for benguigui , an axis of symmetry and at least two planes of symmetry , the cell described in u . s . pat . no . 4 , 541 , 136 ( fig4 a ) itself having four planes of symmetry . in all cases , the wings with parallel walls induce depression which can never themselves possess parallel walls , although already in request fr / 9508972 the disposition of the wings and of the fissures allows that the walls of a same fissure could be parallel for all the fissures of the cell . however , in the case of cells possessing very many wings or of a very small dimension , the practical need to smooth down the rough angles protruding notably at the level of the exterior perimeter 7 requires of one to specify the difference and the advantage of the present invention . according to the invention the space included between two points 28 and two fissures 4 in succession on the exterior perimeter 7 must imperatively include a flat part 29 ( fig4 b ) ( fig3 , 6 , 7 , 8 , 9 , 10 , 11 , 12 , 13 , 14 , 15 , 16 , 17 , 19 , 21 ). as an example for fig . ( 4 b ) which one considers the flat part 29 as a tangent or as a cord in relation to the exterior limit of the prior art between two points 28 does not create any problem in the framework of the present invention since whatever the shape of a cell may be one must take into account only its real sizes at the starting point either the sizes and volume empty in a resting state , it appears that for size outside all of a given cell according to the prior art and the dimensions outside all according to the invention , it is according to this latter invention that the volume contained in a cell in a resting state is the most important , according to the invention , all the points constituting a flat plane 29 on the tract of the exterior sheath 7 between two points 28 at the junction of two successive fissures 4 are further away from the center 24 than the other points of the sheath 7 between the points 28 not constituting of a straight line or flat part 29 . the accomplishment of the invention allows one to see during the expansion of a cell beyond its resting position and therefore by the increase in the perimeter of the cell to obtain a decrease in the density of the cells per surface unit of support while keeping an optimum efficiency — having consequently as an advantage a gain in matter , energy such that for the drying , polymerization , vulcanization , by a better venting of the upper sheet generally obtained by dipping of the mandrels or male molds in a dip of liquid matter : latex , polyvinyl - chloride or other , which will coat them with uniform matter , which could be a very important gain particularly when the support cells such as mattresses possess heights ranging from 10 to 40 centimeters and consequently : time for the production of the upper sheet and generally all of all of these advantages plus , for the assembly of the upper sheet in its form and of the lower sheet to obtain the finished product , by the presence of plane joints of a greater surface area , due to the larger spacing of the cells of the two contiguous rows due to the invention and consequently a better assembly of sheet 1 and 2 . according to a preferred example in realization , one sees ( fig1 ) a support made of an upper sheet where the cells 3 are placed and a lower sheet 2 , the flat base ( fig1 ) or shaped ( fig1 ) ( to be eventually laid itself on a foundation in place made of semi rigid polyurethane foam for example ) and made of the assembly of sheets 1 and 2 ; one can also as in some cases in the prior art make supports composed of two sheets of the shape 1 , the first one keeping the upper position ( fig1 ) and the second one being reversed so that the apexes 25 of its cells be down and base 27 at the apex , all of it presenting a symmetry in relation to the plane joint : one can also depending on the support remove cells of the sheet of shape 1 as to leave an empty space between the remaining cells or any other exploitable combination in cell height . the communication system between the cells being indifferent and known by the prior art . according to the preferred examples of the best mode of realization all of the sharp angles protruding and on the cells and therefore the shape of the molds used in their manufacture will be blunted or rounded off . the walls of the fissures can be parallel 4 , with draft 8 or counterdraft 9 , in a straight line 21 , concave 10 , convex 11 , or even jagged 12 a and 12 b . the distribution of the fissures between the concentric perimeters , with a minimum number of two , can be random , that is to say that a fissure with walls in the shape of a jagged line can be contiguous with a fissure with parallel walls . according to the best methods of realization the exterior virtual sheath 7 outside or irregular section shapes will possess in order of preference a square section 16 or rectangular , circular 18 , pentagonal 19 , octagonal 17 . the number of fissures is limited by their width at the level of the interior concentric perimeter , by the thickness of the wings at that level and by the length of the interior concentric perimeter . the greater the number of fissures , the more this allows to meet the objective of the density of cells per unit of surface of support , however for purposes of realization and manufacture of the supports or padding for medical use we can limit the number of fissures as described further on . in the extreme case where a cell would have very many wings , the difference between the prior art and the invention is demonstrated as follows . according to the invention the schematic shape of the wing of a male mandrel being used for the manufacture of cells by soaking far example , and consequently this cell wing in a resting state is the part between two successive or contiguous fissures , and often shown as a triangle ( fig3 ) ( fig6 ) ( fig7 ) ( fig9 ) ( fig1 ) ( fig1 ) ( fig1 a ) ( fig1 ) or by a shape perceptibly triangular whose apex is located on the side of the interior sheath and the base on the side of the exterior sheath . we say that according to the invention a cell &# 39 ; s wing in a resting state possesses at least three sides with at least two sides coming each from the walls of the two successive fissures and at least are side following the path of the exterior sheath , this third side possesses at least a flat part 29 on part of its path along the exterior sheath 7 . the cells meeting the description of figs . ( 6 )-( 7 )-( 9 )-( 10 )-( 11 ) would be more efficient by corner expansion according to the diagonals by avoiding support cavities at the intersection of the intercellular rows , offering therefore a most uniform surface of support ; these rows correspond to the assembly zones ( gluing , seam or other ) of the upper sheets 1 and lower ones 2 . the external virtual sheath 7 for supports against bedsores can have a transverse section of about ten to one hundred millimeters , the walls of the fissures can be about two to twenty millimeters apart , the thickness of the wall of a cell can vary from half to about two millimeters . one can have as a support against bedsores or a padding an even number of fissures between about four , eight , ten , the central longitudinal axis could be an axis of symmetry . one can have as a support against bedsores or a padding an odd number of fissures between at least three and approximately nine , the eventual plane of symmetry going by the central axis . one can note that it is absolutely not necessary to have symmetry in the cells for better efficiency of the support . as one can understand the invention can be adapted to all shapes of cells , of which we retain mainly and for the purpose of example , cells having a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in its resting state whose section of body 26 one sees in a transverse section ( fig3 ) of the walls , the irregular external sheath 7 perceptibly circular 15 for one half semi octagonal for the other possessing eight fissures of different shapes , one fissure between both halves made of a straight wall 21 and the other convex 10 and at the opposite in relation to the center 24 of a fissure 24 made of a straight wall 21 and one convex 11 these first two fissures presenting a counter draft , half - way between the first two fissures on the semi octagonal side of a fissure with straight walls 21 with draft , on the opposite side of fissure with straight walls 21 with counter draft , between the first fissure named and the fissure with the straight walls and draft a fissure with a straight wall 21 and the other one in an jagged line 12 a opposite a fissure with a straight wall and the other angled 12 b between the second fissure named and the fissure with straight walls and draft a fissure with straight walls 21 perceptibly parallel 4 and on the opposite a fissure with a straight wall 21 and the other concave 10 , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in s resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls , with external sheath 7 irregular perceptibly pentagonal 20 possessing five fissures 4 with walls perceptibly pentagonal 20 possessing five fissures 4 with walls perceptibly parallel on the five lateral sides of this pentagon , three sides being in the shape of a continuous are on three section located between four fissures , the two other sides being flat the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig6 ) of the walls , with external sheaths 7 perceptibly squared 16 possessing four fissures 4 with walls perceptibly parallel on the diagonals of that square , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig7 ) of the walls , with external sheath 7 perceptibly squared 16 possessing four fissures 8 on the diagonals of that square , the fissures having walls which are not parallel are under at the distal extremity of the fissure or draft , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig8 ) of the walls , with external sheath 7 perceptibly octagonal 17 possessing eight fissures 4 with walls perceptibly parallel on the eight lateral faces of this octagon and two internal concentric perimeters , each proximal extremity or bottom of successive fissures ending alternatively at the level or each internal concentric perimeter , the cell possessing one flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig9 ) of the walls , with external sheath 7 perceptibly circular 18 possessing four fissures 4 perceptibly parallel , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat part 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls , with external sheath 7 perceptibly squared 16 possessing four fissures 9 on the diagonals of that square , the fissures having walls which are not parallel are wider at the proximal extremity of the fissure or bottom or counter draft , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls , with external sheath 7 perceptibly circular 18 possessing four fissures 8 with draft , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls , with external sheath 7 perceptibly pentagonal 19 possessing five fissures 4 with walls perceptibly parallel on the five lateral sides of this pentagon at an equidistant of the extremities on each side , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls , with external sheath 7 irregular perceptibly pentagonal 20 possessing five fissures 4 with walls perceptibly pentagonal 20 possessing five fissures 4 with walls perceptibly parallel on the five lateral sides of this pentagon , three sides being in the shape of a continuous are on three section located between four fissures , the two other sides being flat the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 a ) of the walls , with external sheath 7 perceptibly squared 16 possessing five fissures 4 with perceptibly parallel walls two fissures of which are located at the level of the superior angles of that square , two other on the lateral sides of the square and at two thirds of these sides closer to the base of the square and the fifth one at the middle of the base of the square , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls , with external sheath 7 perceptibly pentagonal 19 possessing ten fissures 4 five of the fissures on the five lateral sides of this pentagon , the other five at the five apexes of this pentagon and two internal concentric perimeters , the bottom of the contiguous fissures ending at the level of each perimeter or internal sheath , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls with external sheath 7 perceptibly circular 18 possessing five fissures 4 with walls perceptibly parallel , the cell possessing a flat part 29 between two fissures 4 , therefore as many flat parts 29 as fissures 4 . the cell in a resting state whose section of the body 26 one sees in a transverse section ( fig1 ) of the walls with external sheath 7 perceptibly squared 16 possessing five fissures 4 with walls perceptibly parallel of which two fissures with straight walls are located at the level of the superior angles of that square , two other on the lateral sides of the squares and at the second third of the length of these sides closer to the base of the square , the bottom moving aside from the center of the cell in the direction of the bottom of the first two contiguous fissures each fissure possessing a concave wall 10 and the other one convex 11 parallel 4 and the fifth fissure with straight walls 4 at the middle of the base of the square , the cell possessing a flat part 29 between two fissures 4 , therefore at a minimum as many flat parts 29 as fissures 4 . according to the invention , the implementation of these supports can therefore apply to the realization of the mattress , pillows , padding against bedsores , but also such as a mattress involved in the comfort of an individual , pillows , back rest and as padding or protection for fragile items , the description of the advantage given by the invention is not restrictive of the process of obtaining the manufactured product with mandrels or male molds by soaking as preferred to female molds for reasons of finishing work of the surface of the molds , mold against mold by injection , mold for rotomolding , thermoforming or other processes . the fact remains , of course , that the present invention is not limited to the above - mentioned examples of realization described and represented thus but that it includes all of its variations . | 8 |
a detailed explanation of the embodiments of this invention is provided below with reference to the drawings . fig1 shows an embodiment of the present invention . inside the dotted line is located a pulse oximeter unit , any of a number of publicly known designs of which may be used in the present invention . sensor 1 is composed of an led which emits red light ( r - led ), an led which emits near - infrared light ( ir - led ), and a light receiving element , and is attached to the fingertip , etc . of the person being monitored . r - led and ir - led are driven by time - shared control signals from slave microcomputer 5 via led drive circuit 4 . light which passes through or reflects off of the patient &# 39 ; s fingertip , etc . is converted to an electrical signal via the light receiving element ( not shown in the drawings ), and is then input to analog signal processor 2 . the light is separated into signal components of the light from r - led and ir - led by r / ir diverter 13 shown in fig2 at analog signal processor 2 . each of these diverted signals is calculated in ac / dc unit 14 and ac / dc unit 15 according to a publicly - known method ( ac component of each signal )/( dc component of each signal ). the output from ac / dc unit 14 and ac / dc unit 15 undergoes a / d conversion at slave microcomputer 5 after passing through high - pass filter 16 and high - pass filter 17 , through which ac / dc signals ( pulse wave signals ) pass with each heartbeat . each signal undergoing a / d conversion at slave microcomputer 5 is input into master microcomputer 6 and shown on display unit 20 , and the patient &# 39 ; s arterial blood oxygen saturation level and pulse rate are calculated . the arterial blood oxygen saturation level and pulse rate calculated at master microcomputer 6 are output to external equipment via digital output unit 7 and analog output unit 8 , are shown on display unit 20 , and are stored along with the date and time in signal memory unit 12 . in addition , the output from high - pass filter 17 is output as an analog pulse wave signal . the above is part of a publicly - known oximeter , but it is acceptable if r - led and ir - led are not driven on a time - sharing basis , but are driven by a variable alternating frequency or variable alternating phase . a publicly - known circuit is used according to these methods in r / ir diverter 13 . the output pulse wave signal from ac / dc unit 15 is input into pulse wave base line analog signal processor 9 . pulse wave base line analog signal processor 9 comprises high - pass filter 18 and low - pass filter 19 for passing the change components of the pulse wave signal base line accompanying respiration . in these filters , the cut - off frequencies are variable and the cut - off frequencies are set by slave microcomputer 5 . the output from pulse wave base line analog signal processor 9 ( base line signal ) is output to external equipment via pulse wave base line analog output unit 10 , as well as to master microcomputer 6 after undergoing a / d conversion at slave microcomputer 5 . at microcomputer 6 , the a / d converted base line signals are shown on display unit 20 , and the signals &# 39 ; cycle ( or , breaths per minute ) and amplitude , as well as rise time and fall time , are calculated . during normal respiration , the base line signals appear as shown in fig3 ( a ), whereas when sleep obstructive apnea is present , as shown in fig3 ( b ), the amplitude is larger and the waveform is different from normal , in that the ratios t1 / t2 , t1 /( t1 + t2 ) and t2 /( t1 + t2 ) for rise time t1 and fall time t2 differ from those present during normal respiration . the method employed by microcomputer 6 to identify obstructive apnea will now be explained using the flow chart in fig4 . first , arterial blood oxygen saturation value s measured by the pulse oximeter is compared to a corresponding standard value s r ( which may be either a value set by the investigator or a fixed value ), and if s ≧ s r , respiration is deemed normal . where s & lt ; s r , arterial blood oxygen saturation has fallen , which means that apnea is occurring , and the steps below are then followed to a determine if it is central apnea or obstructive apnea . first , base line signal amplitude a is compared to corresponding standard amplitude a r ( which may be either a value set by the investigator or a fixed value ), and if a ≦ a r , it is determined that central apnea is occurring . where a & gt ; a r , the rise time / fall time ratio ( t1 / t2 ) is compared with corresponding standard value r ( which may be either a value set by the investigator or a fixed value ). if t1 / t2 ≦ r , central apnea is determined to exist , whereas if t1 / t2 & gt ; r , obstructive apnea is determined to exist . the use of both amplitude and the t1 / t2 ratio provides increased accuracy , but the two types of apnea may be distinguished using either one individually . master microcomputer 6 displays on display unit 20 either the cycle of the base line signal or the number of breaths per minute ( hereinafter ` breaths `), as well as amplitude and t1 / t2 , and , in addition to outputting this information via pulse wave base line digital information output unit 11 , stores it together with the date , time , arterial blood oxygen saturation level and pulse rate in signal memory unit 12 as described above . in addition , where it is determined that obstructive apnea exists , a signal which indicates this to be the case ( for example , the symbol ` h `) is stored in signal memory unit 12 . where it is determined that central apnea exists , a different signal which indicates this to be the case ( for example , the symbol ` c `) is stored in signal memory unit 12 . further , the system may be made to emit an alarm based on sound or light when central or obstructive apnea is determined based on the amplitude of the base line signal , t1 / t2 ratio and cycle ( or the number of breaths per minute ) and output by pulse wave base line digital output unit 11 . because the base line signal &# 39 ; s amplitude and t1 / t2 ratio increase during obstructive apnea , obstructive apnea may be detected even where the arterial blood oxygen saturation level is not known . one series of data stored in signal memory unit 12 comprises one file , and several files may be stored . stored files may be displayed on display unit 20 by pushing a file output display button ( not shown in the drawings ) and output all at once from digital output unit 7 and / or analog output unit 8 in a short period of time . the memory medium for signal memory unit 12 may consist of a removable memory card , a magnetic memory medium , a read - write optical disk , etc ., in which case the stored files may be removed from the device of this invention and read directly by a separate microcomputer . next , the setting of the cut - off frequency for the pulse wave base line analog signal processor is explained . fig5 shows one embodiment of pulse wave base line analog signal processor 9 . the cut - off frequencies of high - pass filter 18 are alternated by alternating among condensers ch1 to ch4 via switch sh . similarly , the cut - off frequencies of low - pass filter 19 are alternated by alternating among resistors rl1 to rl4 via switch sl . the cut - off frequencies among which high - pass filter 18 may be alternated are 0 . 125 hz ( position h1 ), 0 . 25 hz ( h2 ), 0 . 5 hz ( h3 ), and 1 hz ( h4 ), while those for low - path filter 19 are 0 . 5 hz ( position 11 ), 1 hz ( 12 ), 2 hz ( 13 ), and 4 hz ( 14 ). when the power switch is turned on , switch sh is in position hi and a cut - off frequency of 0 . 125 hz ( hereinafter fho ) is selected , while switch sl is in position i1 and a cutoff frequency of 4 hz ( hereinafter flo ) is selected . when the pulse rate is measured by the pulse oximeter unit , the position for switch sl corresponding to that rate is selected . in other words , the position of switch sl is selected so that flo is the smallest value satisfying the condition fp ≦ flo , where the pulse wave signal frequency calculated ( by master microcomputer 6 ) from the measured pulse rate is fp , and the signal to set this is output from master microcomputer 6 via slave microcomputer 5 . initially , where fho is selected , the cycle , etc . of the base line signal is calculated by master microcomputer 6 in the manner described above . when the cycle of the base line signal has been calculated , the frequency of the base line signal fpb is calculated by master microcomputer 6 . then the position of switch sh is selected so that the value of fho is the largest satisfying the equation fpb ≧ fho , and the signal to set this is output from master microcomputer 6 via slave microcomputer 5 . in the embodiment shown in fig5 four cut - off frequencies may be selected for high - pass filter 18 and low - pass filter 19 , but a larger number may be selected , and cut - off frequencies may be continuously set using a publicly - known method . in addition , one filter is being used in fig5 but the use of several filters is more effective in eliminating pulse wave signal components . furthermore , both a high - pass filter and a low - pass filter are used in fig5 but a single band - pass filter may also be used . moreover , fig5 uses a filter employing an analog circuit , but it may also be constructed as in fig6 using a digital filter 23 which carries out filtering via digital calculation using a publicly known method , after a / d conversion of the output from ac / dc unit 15 using a / d converter 22 . in this case , an extremely precise filter in which the setting of cut - off frequencies is simple may be obtained , and elimination of pulse wave signal components may be effectively carried out . in this embodiment , a photoelectric pulse wave signal obtained from the pulse oximeter &# 39 ; s sensor is used to measure the breaths based on the cycle of base line change component : instead , however , breaths may also be measured from the cycle of change components of the base line of a plethysmogram signal via publicly known impedance plethysmograpy , etc ., or by a publicly - known pressure pulse wave employing a pressure sensor or stress sensor , and moreover the type of apnea may be distinguished from the amplitude and waveform using a method similar to that of the above embodiment . in the respiration diagnosis appratus of this invention , by extracting changes in the base line of a pulse wave signal , central apnea and obstructive apnea may be easily distinguished . furthermore , the level of arterial blood oxygen saturation may be measured by means of a pulse wave signal . based on the measured arterial blood oxygen saturation level , apnea may be distinguished from normal respiration . the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof . the present embodiments are therefore to be considered in all respects as illustrative and not restrictive , the scope of the invention being indicated by the appended claims rather than by the foregoing description , and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein . | 0 |
fig2 shows a transistor 10 , which is a trench mosfet , with vertical current flow . in detail , the transistor 10 comprises a semiconductor body 12 made , for example , of silicon and comprises a substrate 14 , of an n ++ type and an epitaxial layer 16 of an n type extending over the substrate . further , the semiconductor body 12 comprises a region 18 of a p type , which will be referred to in what follows as the top semiconductor region 18 . the top semiconductor region 18 extends over the epitaxial layer 16 , with which it is in direct contact . present on the top semiconductor region 18 , and in direct contact with the latter , is a source region 20 , of undoped conductive material , such as for example a metal material . as previously mentioned , the transistor 10 comprises a trench 22 , which in top plan view has an annular shape . in particular , the trench 22 extends through a bottom portion of the source region 20 , as well as through the top semiconductor region 18 and a top portion of the epitaxial layer 16 . consequently , the trench 22 does not extend within the substrate 14 ; further , the trench 22 surrounds an active region 24 . present within the trench 22 is a gate region 30 , which in top plan view thus has an annular shape . the gate region 30 is made of conductive material , such as for example polysilicon . further present within the trench 22 is an insulation region 32 , which is made of dielectric material and surrounds all sides of the gate region 30 . in particular , the insulation region 32 includes a first insulation subregion 36 , which overlies the gate region 30 and is made , for example , of deposited silicon oxide ( teos ), and a second insulation subregion 38 , which surrounds at the lateral sides and underneath the gate region 30 and is made , for example , of silicon oxide . in detail , the top semiconductor region 18 forms a body region 40 , which is arranged in the active region 24 ( and is thus surrounded by the trench 22 ), and a peripheral semiconductor region 19 , which is arranged on the outside of the trench 22 . the body region 24 and the peripheral semiconductor region 19 are thus separated from one another on account of interposition of the trench 22 . further , extending underneath the body region 40 is a portion of the epitaxial layer 16 . in greater detail , the semiconductor body 12 is delimited at the top and at the bottom , respectively , by a top surface s a and a bottom surface s b , which are formed , respectively , by the top semiconductor region 18 and by the substrate 14 . yet in greater detail , fig2 shows a first top portion 39 a of the second insulation subregion 38 , which is arranged laterally with respect to the gate region 30 , contacts the body region 40 and to a first approximation is oriented perpendicular to the top surface s a . the first top portion 39 a coats the inner lateral wall of the trench 22 and is delimited laterally by a first lateral surface s c1 and a second lateral surface s c2 , which contact , respectively , i ) the body region 40 and the source region 20 , and ii ) the gate region 30 . further , fig2 also shows a second top portion 39 b of the second insulation subregion 38 , which surrounds , at a distance , the aforementioned first top portion 39 a of the second insulation subregion 38 and is delimited laterally by a third lateral surface s 3 and a fourth lateral surface s c4 , which contact , respectively , i ) the peripheral semiconductor region 19 and the source region 20 , and ii ) the gate region 30 . in practice , the second top portion 39 b coats the outer lateral wall of the trench 22 . further , the second and fourth lateral surfaces s c2 , s c4 face the gate region 30 , whereas the first and third lateral surfaces s c1 , s 3 face the body region 40 and the peripheral semiconductor region 19 , respectively . this being said , assuming a reference system oriented perpendicular to the aforementioned surfaces s a and s b and directed from the bottom surface s b towards the top surface s a , the top surface s a extends to a height lower than the height of the portion of gate region 30 arranged in contact with the second lateral surface s c2 . in other words , if we denote by h 30 the maximum height of the portion of the gate region 30 in contact with the second lateral surface s c2 , the body region 40 , and in particular the portion of the body region 40 in contact with the first lateral surface s c1 , extends up to a corresponding maximum height , which is lower than the height h 30 . equivalently , the portion of source region 20 that contacts the body region 40 and the first lateral surface s c1 extends at the bottom up to a height lower than the height h 30 . in this connection , fig2 shows , purely by way of example , an embodiment in which the gate region 30 has a non - uniform height . in particular , the height of the gate region 30 decreases starting from the peripheral portions closest to the top semiconductor region 18 towards a central portion of the gate region 30 . in other words , in cross - sectional view the gate region 30 exhibits a cusp - shaped profile , with the cusp facing downwards , this cusp being arranged , in top plan view , approximately at the middle of the gate region 30 . however possible are embodiments in which the gate region 30 has , for example , a maximum height that is substantially uniform in a direction parallel to the top surface s a . in practice , a lateral overlap is created between the gate region 30 and the source region 20 . in use , the epitaxial layer 16 forms the drain of the transistor 10 , whereas the first top portion 39 a of the second insulation subregion 38 functions as gate oxide . consequently , when the gate region 30 is biased at a voltage higher than the threshold voltage of the transistor 10 , in the portion of the body region 40 arranged in contact with the first lateral surface s c1 the ( vertical ) conduction channel of the transistor 10 is formed . the lateral overlap between the gate region 30 and the source region 20 guarantees that the source is electrically coupled to the channel . for practical purposes , since the source region 20 is made of an undoped conductive material , in the transistor 10 no parasitic transistor of an npn type is present , and consequently latch - up may not occur . the transistor 10 may be obtained with the manufacturing process described in what follows . initially , as shown in fig3 , the semiconductor body 12 is provided , which comprises the substrate 14 , the epitaxial layer 16 , and a region 18 ′ that is to form the top semiconductor region 18 , which will be referred to in what follows as the preliminary top semiconductor region 18 ′. formed on the preliminary top semiconductor region 18 ′ is a layer 44 of dielectric material ( for example , silicon oxide or teos ), which will be referred to in what follows as the temporary layer 44 . for instance , the temporary layer 44 is formed by thermal oxidation or by chemical deposition . next , as shown in fig4 , a photolithographic process and a subsequent anisotropic etch are carried out in order to remove selectively a portion of the temporary layer 44 for forming a window 46 of an annular shape in the temporary layer 44 . next , as shown in fig5 , the window 46 is used in a subsequent etch , which enables selective removal of a portion of the preliminary top semiconductor region 18 ′ and an underlying portion of the epitaxial layer 16 , to form the trench 22 . this operation entails separation , within the preliminary top semiconductor region 18 ′, of a region 40 ′, which is to form the body region 40 , and a region 19 ′, which is to form the peripheral semiconductor region 19 , which will be referred to in what follows as the preliminary body region 40 ′ and the preliminary peripheral semiconductor region 19 ′, respectively . next , as shown in fig6 , the remaining portion of the temporary layer 44 is removed . next , as shown in fig7 , formed in a per se known manner is a layer 50 of dielectric material , which will be referred to in what follows as the thin dielectric layer 50 . for instance , the thin dielectric layer 50 is made of silicon oxide and is obtained by thermal oxidation , or else is made of teos oxide , formed by deposition . further , the thin dielectric layer 50 has a thickness of , for example , to 50 nm . in greater detail , the thin dielectric layer 50 extends on the preliminary top semiconductor region 18 ′, as well as within the trench 22 , for coating the bottom and the lateral walls of the latter . next , as shown in fig8 , formed on the thin dielectric layer 50 is a further dielectric layer 52 , which will be referred to in what follows as the thick dielectric layer 52 . the thick dielectric layer 52 is made , for example , of silicon nitride ( si 3 n 4 ) and has a thickness , for example , comprised between 70 nm and 100 nm . the presence of the thin dielectric layer 50 enables reduction of the mechanical stresses induced in the semiconductor body 12 during the subsequent steps of the manufacturing process . next , as shown in fig9 , selective removal is carried out ( for example , by an anisotropic chemical etch ) of portions of the thin dielectric layer 50 and of the thick dielectric layer 52 arranged on the preliminary body region 40 ′ and the preliminary peripheral semiconductor region 19 ′, thus outside the trench 22 , as well as portions of the thin dielectric layer 50 and of the thick dielectric layer 52 that coat the bottom of the trench 22 . in this connection , in what follows referred to , respectively , as the first lateral wall p 1 and second lateral wall p 2 of the trench 22 are the inner lateral wall and the outer lateral wall of the trench 22 , as well as the bottom wall p 3 of the trench 22 . following upon the operations described previously , the bottom wall p 3 of the trench 22 is exposed , whereas the first and second lateral walls p 1 , p 2 of the trench 22 are coated by a first coating layer 56 and a second coating layer 58 , respectively , which are formed by residual portions of the thin dielectric layer 50 ; in turn , the first and second coating layers 56 , 58 are coated , respectively , by a first spacer 60 and a second spacer 62 , which are formed by residual portions of the thick dielectric layer 52 . next , as shown in fig1 , a process of thermal oxidation is carried out , which entails oxidation of the exposed portions of semiconductor material , not coated either by the first spacer 60 or by the second spacer 62 . this operation entails formation , on the preliminary body region 40 ′, of a corresponding dielectric region , which will be referred to in what follows as the central dielectric region 66 . further , this operation entails formation , on the peripheral semiconductor region 19 , of a corresponding dielectric region 68 , which will be referred to in what follows as the peripheral dielectric region 68 ; for example , the central dielectric region 66 and the peripheral dielectric region 68 have a thickness comprised between 0 . 2 μm and 0 . 3 μm . in addition , this operation of oxidation entails formation , by the central dielectric region 66 and the peripheral dielectric region 68 , of corresponding projections that extend towards the trench 22 , as well as entailing curving in the direction of the trench 22 of the top portions and bottom portions of the first and second spacers 60 , 62 . in particular , the projections of the central dielectric region 66 and of the peripheral dielectric region 68 project towards the inside of the trench 22 with respect to the preliminary body region 40 ′. further , said operation of oxidation entails formation , on the bottom of the trench 22 , of a further dielectric region 70 , which will be referred to in what follows as the bottom dielectric region 70 . once again with reference to fig1 , here the central dielectric region 66 , the peripheral dielectric region 68 , the bottom dielectric region 70 , and the first and second coating layers 56 , 58 are shown in a distinct way , for reasons of clarity , even though they may be made of a same material and may thus form a single dielectric region , made , for example , of oxide . next , as shown in fig1 , an isotropic etch is made to remove the first and second spacers 60 , 62 . then , as shown in fig1 , a further etch is made ( for example , an isotropic chemical etch in a liquid or nebulized environment ) to remove the first and second coating layers 56 , 58 , which may have previously undergone contamination . albeit not shown , this operation entails a slight reduction of the thickness of the central dielectric region 66 , of the peripheral dielectric region 68 , and of the bottom dielectric region 70 . next , as shown in fig1 , a new oxidation process is carried out . in this way , on the first and second lateral walls p 1 , p 2 of the trench 22 a first oxide layer 72 and a second oxide layer 74 are formed , respectively , which will be referred to in what follows as the first and second oxide layers 72 , 74 . the first and second oxide layers 72 , 74 contact the bottom dielectric region 70 for forming the second insulation subregion 38 . in greater detail , albeit not shown , the oxidation process described with reference to fig1 entails also a slight increase in the thickness of the central dielectric region 66 , of the peripheral dielectric region 68 , and of the bottom dielectric region 70 . further , even though in fig1 the first and second oxide layers 72 , 74 are shown as distinct with respect to the central dielectric region 66 and the peripheral dielectric region 68 , they may be made of the same material of which the latter are made . once again with reference to fig1 , this shows how , thanks to the prior use of the first and second spacers 60 , 62 , it is possible to coat the bottom wall p 3 of the trench 22 with an insulating region ( in the case in point , the bottom dielectric region 70 ) having a thickness greater than the thickness of the first and second oxide layers 72 , 74 . in this way , insulation of the gate region 30 towards the drain region is improved , without this entailing an increase of the threshold voltage of the transistor 10 . next , as shown in fig1 , a conductive region 78 , made , for example , of polysilicon is formed . for instance , the conductive region 78 may be formed by successive deposition of layers . in detail , the conductive region 78 overlies the central dielectric region 66 and the peripheral dielectric region 68 . in addition , the conductive region 78 fills the trench 22 completely . in this connection , without this implying any loss of generality , the trench 22 has a depth that is , for example , twice the respective width . next , as shown in fig1 , an anisotropic etch is made , in order to reduce the thickness of the conductive region 78 so that the residual portion of conductive region 78 forms the gate region 30 . in other words , following upon this etch , just a portion of conductive region 78 remains , which occupies the trench 22 starting from the bottom up to a height lower than the maximum height of the semiconductor body 12 . for instance , the residual portion of the conductive region 78 has a maximum height 0 . 4 μm lower than the maximum height of the semiconductor body 12 . in greater detail , and without any loss of generality , etching of the conductive region 78 may be carried out by a homogeneous “ etch back ”, in which case the gate region 30 assumes the aforementioned cusp shape . next , as shown in fig1 , dielectric material ( for example , silicon oxide ) is deposited for forming a top dielectric region 80 , which is arranged on top of the central dielectric region 66 and of the peripheral dielectric region 68 . further , the top dielectric region 80 extends within a top portion of the trench 22 until it contacts the gate region 30 . next , as shown in fig1 , a new anisotropic etch is made in order to remove a top portion of the top dielectric region 80 , the central dielectric region 66 , and the peripheral dielectric region 68 for exposing the preliminary body region 40 ′ and the preliminary peripheral semiconductor region 19 ′. in addition , this etch entails removal of a portion of the top dielectric region 80 arranged inside the trench 22 . in this way , the residual portion of top dielectric region 80 forms the first insulation subregion 36 , the maximum height of which is , for example , 0 . 2 μm lower than the maximum height of the preliminary top semiconductor region 18 ′. next , as shown in fig1 , a new etch ( for example , a chemical etch of silicon in moist , liquid , or nebulized environment ) is made in order to reduce the thickness of the preliminary body region 40 ′ and of the preliminary peripheral semiconductor region 19 ′. the residual portions of the preliminary body region 40 ′ and of the preliminary peripheral semiconductor region 19 ′ form , respectively , the body region 40 and the peripheral semiconductor region 19 . next , in a way not shown , the source region 20 is formed for example by deposition of metal material . according to a variant of the manufacturing process previously described , following upon execution of the operations described with reference to fig1 , it is possible to carry out the operations shown in fig1 . in detail , formed , for example by deposition , on the body region 4 , the peripheral semiconductor region 19 , and the first insulation subregion 36 is a further layer 84 of silicon nitride , which will be referred to in what follows as the additional layer 84 . next , as shown in fig2 , portions of the additional layer 84 that extend over the first insulation subregion 36 , as well as over a central portion of the body region 40 , are selectively removed , for example with an anisotropic etch . the residual portions of the additional layer 84 form a third spacer 86 and a fourth spacer 86 , 88 . the third spacer 86 coats a top portion of the first lateral surface s c1 of the first top portion 39 a of the second insulation subregion 38 , until it contacts a peripheral portion of the body region 40 . a central portion of the body region 40 is , instead , in contact with a portion of the source region 20 , which is surrounded by the third spacer 86 . the fourth spacer 88 coats , instead , a top portion of the third lateral surface s c3 of the second top portion 39 b of the second insulation subregion 38 , until it contacts the peripheral semiconductor region 19 . in the case where the operations represented in fig2 are carried out , the transistor 10 assumes the shape shown in fig2 . further , the presence of the third and fourth spacers 86 , 88 enables improvement of the electrical insulation between the source region 20 and the gate region 30 . optionally , following upon the operations represented in fig2 , and prior to formation of the source region 20 , it is possible to carry out an ion implantation within the exposed portion of body region 40 , i . e ., within the portion of body region 40 not covered by the third spacer 86 . in this way , as shown in fig2 , an enriched region 90 of a p + type is formed , which extends within the body region 40 , starting from the top surface s a , without contacting the underlying epitaxial layer 16 . the enriched region 90 is laterally staggered with respect to the third spacer 86 . in the case where the operations represented in fig2 are carried out , the transistor 10 assumes the shape shown in fig2 . the presence of the enriched region 90 enables improvement of the electrical behavior of the diode formed by the body region 40 and by the underlying portion of epitaxial layer 16 , without affecting the channel of the transistor 10 . further possible are embodiments that are the same as corresponding embodiments described previously , but in which the substrate is of a p + type , instead of an n + type . in this case , the transistor , designated by 100 , is of an igbt type and the epitaxial layer 16 functions as so - called “ drift layer ”. an example of such embodiments is shown in fig2 , where the substrate is designated by 99 . in this connection , the substrate 99 functions as collector of the transistor 100 . albeit not shown , further possible are embodiments in which the substrate is of a p + type and which include the third and fourth spacers 86 , 88 as well as possibly the enriched region 90 . the electronic device described presents numerous advantages . in particular , thanks to the fact that the source region 20 is made of undoped conductive material , formation of the parasitic transistor of an npn type is prevented , and thus latch - up thereof is likewise prevented . in particular , in the case of a mosfet , there is just one diode , formed by the body region 40 and by the underlying portion of the epitaxial layer 16 . instead , in the case of an igbt , just the parasitic pnp transistor is present , which in any case does not give rise to latch - up , since it has an h fe parameter lower than one . finally , it is clear that modifications and variations may be made to the electronic device and to the manufacturing process described and illustrated herein , without thereby departing from the scope of the present disclosure . for instance , the types of doping may be reversed with respect to what has been described . as regards the trench 22 , it may have , in top plan view , an arbitrary shape , such as for example a circular or elliptical shape . some steps of the manufacturing process may be carried out in a different order with respect to what has been described . in addition , one or more regions of the transistor may be formed in a way different from what has been described . the various embodiments described above can be combined to provide further embodiments . these and other changes can be made to the embodiments in light of the above - detailed description . in general , in the following claims , the terms used should not be construed to limit the claims to the specific embodiments disclosed in the specification and the claims , but should be construed to include all possible embodiments along with the full scope of equivalents to which such claims are entitled . accordingly , the claims are not limited by the disclosure . | 7 |
several embodiments of the present invention will now be described in detail with reference to the annexed drawings . in the following description , detailed descriptions of known functions and configurations incorporated herein have been omitted for conciseness and clarity . for simplicity and illustrative purposes , the principles of the present invention are described by referring mainly to exemplary embodiments thereof . in the following description , numerous specific details are set forth in order to provide a thorough understanding of the present invention . those with skill in the art will recognize that various changes and modifications can be made to the examples provided herein without departing from the scope and spirit of the invention . the exemplary embodiments of the present invention are a spin polarizer that in the general case , can contain a ferromagnetic - semiconductor ( fm - s ) junction ensuring a spin polarization of current , p j , near a boundary with a nonmagnetic semiconductor ( ns ) depending relatively weakly on the current . the spin polarizer can create spin polarization of electrons virtually to 100 %, inside some areas of the nonmagnetic semiconductor ( ns ) near the fm - s junction . this occurs when the electrons drift under the action of a strong enough electrical field from the ns into the fm even in the case when p j is relatively small ( p j can be even ˜ 5 %- 15 %). fig3 a illustrates a spin polarizer 300 according to an embodiment of the present invention . as will be discussed below , the device 300 can ensure spin polarization of electrons is equal virtually to 100 % inside some area of the nonmagnetic semiconductor ( ns ) near the fm - s junction . the spin polarizer 300 includes a nonmagnetic semiconductor ( ns ) layer 310 , a thin , highly doped degenerate semiconductor layer n +- s ′ 320 ,, above the semiconductor 310 and a ferromagnetic ( fm ) layer 330 above the semiconductor layer 320 . the spin polarizer 300 can also include electrodes 340 and 350 electrically connecting the ferromagnetic layer 330 and the ns layer 310 , respectively . the spin polarizer 300 thus formed is described as having an fm - n + - s ′ _ - n - s heterostructure with parameters adjusted to sufficiently meet the conditions discussed below . the fm layer 330 can be formed from various magnetic materials , preferably ni , fe and co , as well as various magnetic alloys , which can include one or a combination of fe , co , and ni . the ns layer 310 can be formed from various semiconductor materials including any one of si , gaas , znte , gasb , gap , ge , inas , cdse , inp , insb , cdte , cds , zns , znse , alp , alas , alsb , and also alloys of these materials . in an exemplary embodiment of the present invention , the semiconductor 310 can be formed from semiconductor materials with relatively large electron spin relaxation time , l s . these include , for example gaalas , inas , znse and zncdse among others . the ns layer 310 can be negatively doped . negative dopant metals that can be used include p , as , sb for si and ge , and ge , se , te , si , pb and sn for gaas . the high doped semiconductor , the n +- s ′ layer 320 , may be formed from various semiconductor materials having an energy bandgap narrower than that for the semiconductor 310 . for example , the n - dopant metals may be p , as , sb for si and ge , and ge , se , te , si , pb and sn for gaas . the thin degenerate semiconductor layer 320 may be used to increase tunneling transparency of the schottky barrier for electrons with energies e & gt ; f and to ensure a spin polarization of current near the fm - n +- s ′ junction weakly depending on the current . the parameters of the n +- s ′ layer 320 should be satisfied by certain conditions listed below . fig3 b illustrates an exemplary energy diagram of spin polarizer 300 along the line iii - iii of fig3 a in the case when the n - s region 310 is a degenerate nonmagnetic semiconductor . the device 300 can be used at an arbitrary temperature and can ensure spin polarization of electrons close to 100 % in an area of the nonmagnetic semiconductor near the boundary with the n ± s layer 320 . f is the fermi level ; δ and l d are the height and thickness of the schottky barrier of the fm - n +- s ′ junction , l is the thickness of the highly doped n ± s ′ layer 320 , δ 0 is a jump at the bottom of the conduction band , e c ( x ), at the boundary of the n ± s ′ layer 320 and the semiconductor 310 . fig3 c illustrates an exemplary energy diagram of spin polarizer 300 along the line iii - iii of fig3 a in the case when the n - s region 310 is a nondegenerate nonmagnetic semiconductor . the device 300 can advantageously be used at relatively high temperatures , including room temperatures , and may ensure spin polarization of electrons close to 100 % in the nonmagnetic semiconductor near the boundary with the n ± s layers 320 . f is the fermi level ; δ and l d are the height and thickness of the schottky barrier at the fm - n + s interface , 1 is the thickness of the highly doped n ± s ′ layer 320 , δ 0 is a jump at the bottom of the conduction band , e c ( x ), at the boundary of the n + - s ′ layer 320 and the semiconductor 310 . the fm - n ± s ′ junction shown in fig3 a - 3c at certain parameters presented below ensures a spin polarization of current , p jl , near the boundary between the n + - s ′ layer 320 and the semiconductor 310 , the point x = l , weakly depending on the current . these conditions ensure the 100 % spin polarization of electrons in some area of the semiconductor 310 near the boundary even for a relatively small value of p jl as will be described in further detail below . the currents of electrons with spin σ =↑, ↓ in ns are given by the following equations ( see , for example , ref &# 39 ; s [ 7 ][ 8 ][ 16 ], and [ 17 ]): where d , μ and τ s are the diffusion constant , mobility and spin - coherence lifetime of the electrons , respectively , and e the electric field . from conditions of continuity of the total current j ( x )= j { + j ↓ = const and quasineutrality n ( x )= n { + n ↓ = n s ( 4 ) δ n { ( x )= n { − n s / 2 =− δn ↓ ( x ) ( 6 ) where n s is total electron density in the semiconductor 310 . from equations ( 2 ) through ( 6 ), it follows that spin density in the semiconductor 310 , that is , for x ≧ l can be written as : δ n { ( x )= δ n { l exp [−( x − l )/ l ]= nl ( n s / 2 ) exp [−( x − l )/ l ] ( 7 ) l =( 1 / 2 ){[( l e ) 2 +( 2 l s ) 2 ] 1 / 2 −(±) l e }== l s {([( 1 +( j / 2 j s ) 2 ] 1 / 2 − j / 2 j s }, ( 8 ) l s √{ square root over ( dτ s )} and l e = μτ s | e |= l s | j |/ j s ( 9 ) are the diffusion and drift lengths of electron spin , respectively ; the index ± corresponds to the forward , j & gt ; 0 , and reverse bias voltage , j & lt ; 0 , respectively . here we introduce a typical current : and spin polarization of electrons in the semiconductor 310 ( for x ≧ l ) p n =( δ n { − δn ↓ )/ n s = p nl exp [−( x − l )/ l ], ( 11 ) p nl = p nl = p n ( l )=( δ n { l − δn ↓ l )/ n s = 2δ n { l / n s ( 12 ) is spin polarization of electrons at the boundary of the semiconductor 310 ( at the point x = l , fig1 ). from equations ( 2 ) and ( 7 ) the spin currents at the point x = l is j { l ,↓ l =( j / 2 )≅( j s / 2 ) ( l / l s ) p nl ( 13 ) from equation ( 13 ) it follows that the relationship between the spin polarization of current p ll =( j { l − j ↓ l )/( j { l + j θl )/=( j { l − j ↓ l )/ j ( 14 ) and the spin polarization of electrons , p nl , at the point x = 1 p nl =− p jl ( jl s )/( j s l ) ( 15 ) ( p jl is also called spin injection coefficient of the fm - n ± s ′ contact .) according to equation ( 8 ) l = l s at j & lt ;& lt ; j s therefore , as expected p nl l - j at p jl & gt ; 0 ( in certain cases p jl & lt ; 0 ). in the reversed - biased fm - s junctions , j & lt ; 0 , according to ( 15 ) the value of p jl = 2δn { l / n s & gt ; 0 ( δn ↓ l & gt ; 0 ), that is , the accumulation of electrons with spin σ ={ is realized in the semiconductor 310 near the boundary with the fm - s junction . at | j |& gt ; j s the spin penetration depth l ( 8 ) increases with current j and p nl → p jl at | j |& gt ;& gt ; j s . thus , the spin polarization of electrons in the semiconductor injected from fm can achieve spin polarization of current in the reversed - biased fm - s junction . another situation is realized in the forward - biased fm - s junctions , j & gt ; 0 , when electrons drift under the action of the electric field from the semiconductor into fm . here the value δn { l & lt ; 0 and δn ↓ l & gt ; 0 at p jl & gt ; 0 , that is , electrons with spin σ ={ are extracted from ns and electrons with spin σ =↓ are accumulated in the ns . the opposite situation is realized at p jl & lt ; 0 . at j & gt ; j s the spin penetration depth l ( equation ( 8 )) decreases with current j and according to equation ( 15 ) | p nl | rises to 1 ( 100 %) at : j = j t ≡ j s [| p jl /( 1 +| p jl |)] − 1 / 2 ( 16 ) l = l t ≡ l s [| p jl |/( 1 +| p jl |)] 1 / 2 ( 17 ) thus , spin polarization of electrons in the semiconductor near the forward - biased fm - s junction achieves 100 % even at relatively small spin polarization of current , p jl , in the fm - s junction . this is valid both for a degenerate semiconductor 310 , as shown in fig3 b , and for a nondegenerate semiconductor 310 , as shown in fig3 c . the value of p jl , determines the threshold current , j t , and spin penetration depth , l t , but it does not change the main result : the one requirement is a weak dependence of the spin polarization of current in the fm - s junction ( or spin injection coefficient ) p jl , on the current j . we note that when the current j & gt ; j t the value | p nl |= 2 | δn { l |/ n s =| 2n { l = n s |/ n s becomes formally more than 1 , that is , the density of electrons n { l or n ↓ l with spin σ =↓ or σ =↓ at the point x = l becomes more than the total electron density n s . this means that the condition of quasineutrality ( 4 ) is violated and a negative space charge arises near the boundary of the semiconductor with the fm - s junction , x = l in fig1 . this charge will decrease the ohmic field e = j / qμn s ( 5 ), and consequently the drift spin length l e = μτ s | e |. as a result the spin penetration depth l ( equation ( 8 )) stops decreasing with current j and the values of the spin density p nl and l are stabilized near | p nl = 1 and l = l t , respectively . thus , embodiments of the present invention provide fm - s junctions which have the spin polarization of p jl , weakly depending on the current j in the junctions . this requirement is valid , in particular , for the fm - n ± s ′ junction shown in fig3 a - 3c when the n ± s ′ layer 320 is a degenerate semiconductor and has the thickness , 1 , of the n ± s ′ layer 320 that satisfies the condition : wherein l s + =√{ square root over ( d + τ s + )}, d + and τ s + are the length of electron spin , diffusion constant , and the spin - coherence lifetime of the electrons in the n ± s ′ layer 320 , respectively ; l d is the width of the schottky depletion layer in the n - semiconductor 320 near the fm - n ± s ′ interface which is represented by the following equation : l d =( 2εε 0 δ / q 2 n d + ) 1 / 2 ( 20 ) wherein ε 0 is the permittivity of free space , ε is the relative permittivity of the n + - semiconductor 320 , q & gt ; 0 is the elementary charge , and n d + is the concentration of shallow donors in the highly doped n ± s ′ layer 320 . the part of the n ± s ′ layer 320 , corresponding to x such that l d & lt ; x & lt ; l , shown in fig3 b , should be a degenerate semiconductor which has the electron density n + = n d + . this means that n + = n d + should correspond to a case when the fermi level f & gt ; e co + in this part , as shown in fig3 b and 3c . this is realized when l & gt ; 3l d and the donor concentration n d + satisfies the condition 4πn d + a b 3 / 3 & gt ; 1 , where a b is the borh radius of the shallow donor . the donor concentration n d + in the n +- s ′ layer 320 has to be much more than a donor concentration n d in the n - semiconductor 310 which can be either a degenerate semiconductor , as shown in fig3 b , or a nondegenerate semiconductor , as shown in fig3 c . moreover , the following condition should be satisfied : where l 0i s given by eq . ( 1 ). more precise requirements for the parameters l d , l and n d + are presented below . because of the very high density of electrons in the fm metal 330 and the degenerate semiconductor layer 320 the tunneling current through the fm - n ± s ′ layer is determined by the well - known formula ( see , for example , ref .&# 39 ; s [ 18 ] and [ 19 ]): j σ0 = q h ∫ ⅆ e [ f ( e - f - ev ) - f ( e - f ) ] ∫ ⅆ 2 k 𝕀 ( 2 π ) 2 t σ ( 22 ) where k ii is the component of the wave vector k parallel to the fm - s interface , f ( e - f ) the fermi function , v is a bias voltage and t σ is the tunneling transmission probability of the fm - n +- s ′ junction . the value of t σ may be estimated in a semiclassical approximation ( wkb ) ( see , for example , ref .&# 39 ; s [ 14 ] and [ 15 ]) as follows : t σ = 16 α v α x v x v α x 2 + v tx 2 exp ( - ηκ l d ) ( 23 ) where ν σx is the x - component of velocity ν σ of electrons with the wave vector k and spin σ in a direction of current ; κ =( δ + f − e + e ii ) 3 / 2 [ δ ( δ − qv ) l 0 ] − 1 , ν xt = hκ / 2πm * is the “ tunneling ” velocity ; e ii = h 2 k ii 2 / 8π 2 m *; m * and ν x =[ 2 ( e − e c0 − qv − e ii )/ m *] 1 / 2 are an effective mass and x - component of the velocity of electrons in n + - semiconductor layer 320 ; α = 1 . 2 ( κl d ) 1 / 3 and η = 4 / 3 or α = 1 and η = 2 for the schottky barrier of triangular or rectangular shape , respectively . the real shape of the barrier is not significant . for definiteness we consider the case when the temperature k b t & lt ;& lt ; μ + s =( f − e c0 ). taking into account that the velocity ν x is real only at e & gt ; e c0 + qv + e ii and also a property of the fermi function at k b t & lt ;& lt ; μ + s one can find from equations ( 22 ) and ( 23 ) that the spin current at the fm - n +- s ′ interface , at the point x = 0 in fig1 , can be written at qv ≦ μ + s as : j σ0 = qn s + v μ α 0 t t ( v ) d σ [ 1 - ( 1 - qv / μ s + ) 5 / 2 ] , ( 24 ) t t ( v ) = exp [ - η l d ( δ - qv ) 1 / 2 l 0 δ 1 / 2 ] , ( 25 ) d σ = v μ v σ0 v t 0 2 + v σ0 2 , ( 26 ) wherein ν σ0 = ν σ ( f + qv ) and ν μ =( 3μ s + / m *) 1 / 2 are velocities of electrons with spin σ and the energies e = f + qv and μs + in fm and n +- s ′ layers 330 and 320 , respectively ; ν t0 =( 2 ( δ − qv )/ m *. from equations ( 24 )-( 26 ) it follows that the total current j = j { 0 + j ↓ 0 is equal to : j = j 0 d σ [ 1 −( 1 − qv / μ s + ) 5 / 2 ], ( 27 ) j 0 = dqn s + ν μ α 0 t t ( v ) ( 28 ) and the spin polarization of current , p j0 , at the fm - n +- s ′ interface is equal to : p j 0 = j ↑ 0 - j ↓ 0 j ↑ 0 + j ↓ 0 = ( v ↑ 0 - v ↓ 0 ) ( v t 0 2 - v ↑ 0 v ↓ 0 ) ( v ↑ 0 + v ↓ 0 ) ( v t 0 2 + v ↑ 0 v ↓ 0 ) ≡ p f ( 29 ) the expression for p j0 = p f coincides with that for spin polarization of current in usual tunneling fm - i - fm structures [ 18 , 19 ]. one can see that p j0 — = p f does not depend on the current . when the thickness of the n +- s ′ layer l & lt ;& lt ; l s + , where l s + =( d + τ s + ) 1 / 2 and τ s + are the length and relaxation time of electron spin in the n +- s ′ layer , but l & gt ; l d , spin currents in the n +- s ′ layer do not change practically , therefore we can put j σ0 = j σl and p j0 = p jl where p jl is the spin polarization of the current at the boundary between the n +- s ′ layer 320 and the n - s region 310 . by analogy with equation ( 13 ) the spin current in the n +- s ′ layer is equal to j { l ,↓ l =( j / 2 )≅( j s + / 2 ) p + nl , ( 30 ) wherein p + nl = 2δn + { l / n + s is the spin polarization of electrons in the n ± s ′ layer changing with the typical length l s + and the typical current is : where n + s is the electron density in the degenerated region of the n ± s ′ layer . therefore for arbitrary l the value of p jl = p f / cos h ( l / l s + ). thus , p ji ≅ p f when l & lt ;& lt ; l s + in the considered fm - n + - n - s heterostructure shown in fig3 a - 3c . p jl very weakly depends on the current , therefore according to equations ( 15 ) and ( 18 ) the spin polarization electrons in the forward - biased fm - n + - n - s heterostructure near in the n - s region p n0 = 1 ( 100 %) at the threshold current and spin penetration depth in the n - s region is determined by eqs . ( 16 ) and ( 17 ). eqs . ( 16 ) and ( 17 ) are valid when the thickness of the n ± s ′ layer l l s ( β + s / β s )[( 1 + p f )/ p f ), but l & gt ; 3l d . ( 32 ) the larger l is , the less p jl is , and the greater the threshold current j t ( equation ( 15 )) is . the conditions of the 100 % spin polarization electrons are j s + & gt ;& gt ; j 0 & gt ;& gt ; j s . taking into account equations ( 10 ), ( 28 ) and ( 31 ) these conditions can be written as : n s n s + ( d l s v μ ) & lt ; t t ( μ s + ) & lt ;& lt ; ( d + l s + v μ ) ( 33 ) n s + n s & gt ;& gt ; ( d l s + d + l s ) = ( d τ s + d + τ s ) 1 / 2 , ( 34 ) wherein the parameter t t ( μ s + ) is equal to t t ( μ s + ) = d 0 exp [ - η l d ( δ - μ s + ) 1 / 2 l 0 δ 1 / 2 ] . ( 35 ) the conditions of equations ( 19 ) and ( 33 )-( 35 ) can be rewritten as : 2 l 0 η ln ( l s + v μ d d + ) & lt ; l d & lt ; l 0 η ln ( n s + l s v μ d n s d ) ( 36 ) 3 l d & lt ; l ℵl s + ( 37 ) where l d is given by equation ( 20 ), that is , l d is determined by n s + = n d + . the condition of equations ( 33 )-( 36 ) determine the requirements of the electron densities n s = n d and n s + = n d + in the n +- s ′ layer 320 and the n - semiconductor 310 , the thickness id of the schottky depletion layer of fm - n +- s ′ junction , the thickness l of the n + - s ′ layer and also the value of a jump δ 0 of the bottom of the conduction band , e c ( x ), at the boundary of the n ± s ′ layer 320 and the semiconductor 310 , δ 0 =( e c0 − e c0 + ) both for the case of a degenerate semiconductor 310 as shown in fig3 b and for the case of a nondegenerate semiconductor 310 as shown in fig3 c . here eco and e c0 + are the bottom of the conduction band in the semiconductor 310 and the thin degenerate semiconductor n + - layer 320 near the semiconductor 310 . typical parameters for ni — gaas — gaalas heterosructure are n d + ≈ 10 18 - cm − 3 - 10 19 - cm − 3 , n d + ≈ 10 16 - cm − 3 - 10 17 - cm − 3 , δ ≈ 500 me v , μ s + ≈ 30 mev - 50 mev , l d ≈ 5 nm , l d ≈ 5 nm , l ≈ 1 nm , l x ≈ 300 nm , and δ 0 ≈ μ s + ). fig4 a illustrates a spin polarizer 400 according to another embodiment of the present invention . as shown , the spin polarizer 400 may include a nonmagnetic semiconductor 410 , a ferromagnetic 430 and two thin negative and positive highly doped degenerate nonmagnetic semiconductor layers , n + - s layer 420 and p + - s layer 415 . the layers 420 and 415 are situated between the ferromagnet 430 and negative doped semiconductor , n - s region 410 , and have the same energy bandgap as that of the n - s region 410 . these layers can be formed by heavily negative and positive doping of a portion of the semiconductor 410 . the spin polarizer 400 may also include electrodes 440 and 450 electrically connecting the ferromagnetic layer 430 and the semiconductor 410 , respectively . the spin polarizer 400 thus formed may be described as having a fm - n + - p + - n - s heterostructure with parameters adjusted to sufficiently meet the conditions described below . the ferromagnetic layer 430 may be formed from various magnetic materials , preferably ni , fe and co , as well as various magnetic alloys , which may include one or a combination of fe , co , ni . the semiconductor 410 may be formed from various nonmagnetic semiconductor materials including si , gaas , znte , gasb , gap , ge , inas , cdse , inp , insb , cdte , cds , zns , znse , alp , alas , alsb and also alloys of these materials . in general , it is preferred that the semiconductor 410 be formed from semiconductor materials with relatively large electron spin relaxation time , l s , for example gaalas , inas , znse and zncdse . the semiconductor 410 can be negatively doped . fig4 b illustrates an exemplary energy diagram of the spin polarizer shown in fig4 a along the line iv - iv in the case when the n - s region is a degenerate nonmagnetic semiconductor . the device 400 may be used at arbitrary temperature and may ensure spin polarization of electrons close to 100 % in an area of the nonmagnetic semiconductor near the boundary with the p + - s layer 415 . f is the fermi level ; δ and l d are the height and thickness of the schottky barrier of the fm - n + - s junction , l p is the total thickness of the highly doped p + - s layer 415 , 1 is the total thickness of the high doped n + - s layer 420 and the p + - s layer 415 , e c ( x ) is the bottom of the conduction band and e v ( x ) is the top of the valence band of the semiconductor 420 , 415 and 410 , e c0 and e c0 + are the bottoms of the conduction band in the n - s region 410 and the part of the n + - s layer 420 corresponding to a region of the degenerate semiconductor , where l d & lt ; x & lt ;( l − l p )). fig4 c illustrates an exemplary energy diagram of the spin polarizer shown in fig4 a along the line iv - iv in the case when the n - s region is a nondegenerate nonmagnetic semiconductor . the device 300 can be used at relatively high temperatures , including room temperatures , and can ensure spin polarization of electrons close to 100 % in an area of the nonmagnetic semiconductor near the boundary with the p + - s layer 415 . f is the fermi level ; δ and l d are the height and thickness of the schottky barrier of the fm - n + - s junction , l p is the total thickness of the highly doped p + x - s layer 415 , l is the total thickness of the highly doped n + - s layer 420 and the p + - s layer 415 , e c ( x ) is a bottom of the conduction band and e v ( x ) is a top of the valence band of the semiconductors 420 , 415 and 410 , e c0 and e c0 + , are the bottoms of the conduction band in the n - s region 410 and the part of the n + - s layer 420 corresponding to the degenerate semiconductor corresponding to l d & lt ; x & lt ;( l − l p ). a spin polarization close to 100 % in the fm - n + - p + - n - s heterostructure shown in fig4 can be achieved if the following condition is satisfied : n a l p 2 ≈ 2εε 0 ( e c0 − e c0 + )/ q 2 ( 39 ) wherein e c0 and e c0 + are the bottoms of the conduction band in the n - s region 410 and the part of the n + - s layer 420 corresponding to the degenerate semiconductor , where l d & lt ; x & lt ;( l − l p ), in fig4 b and 4c , respectively . for example , equations ( 38 ) and ( 39 ) may be satisfied if n d ranges between 10 18 cm − 3 and 10 19 cm − 3 , l p ≦ 30 nm , and e c0 and ( e c0 − e c0 + )≈ 50 mev . when the conditions of equations ( 38 ) and ( 39 ) are satisfied the region of the n + - s layer 420 and the p + - s layer 415 corresponding to l d & lt ; x & lt ; l is a degenerate semiconductor and the energy diagram of the fm - n + - p + - n - s heterostructure , spin polarizer , has the form shown in fig4 b or 4 c for the case when the n - s region 410 is a degenerate semiconductor or nondegenerate semiconductor , respectively . one can see that these energy diagrams coincide qualitatively with those shown in fig3 b and 3c . therefore , all results presented above for the fm - n + - s heterostructure shown in fig4 a - 4c are valid for the fm - n + - p + - n - s heterostructure , spin polarizer , shown in fig4 a - 4c . all of the above described structures and conditions are also valid for a negatively doped semiconductor . in this case the words electrons , donor and acceptor should be substituted for the words holes , acceptor and donor , respectively , and the n -, n + - and p - semiconductor regions should be substituted for p -, p + - and n - semiconductor regions . different spintronic devices based on ferromagnetic - semiconductor - ferromagnetic ( fm - s - fm ) structures have been suggested , including those using an electric field [ 5 , 6 ], external magnetic field [ 7 ], and a nanowire current [ 8 ] to control an electron spin . all of these devices are spin valves where one of fm - s junctions works as a spin injector and another one as a spin filter . the spin filter efficiently admits electrons with a certain spin projection and efficiently reflects electrons with the opposite spin . the spin polarizer and the fm - n + - n - s heterostructures shown in the fig3 and 4 according to an embodiment of the present invention can be used as the spin filter and spin injector in all of these devices and also in semiconductor systems for quantum computing . one of possible variant of use of the spin polarizer and the fm - n + - n - s heterostructures is shown in fig5 . fig5 a illustrates an exemplary variant of a spin device according to an embodiment of the present invention based on a ferromagnetic - semiconductor fm - n + - n - n + - fm heterostructure containing a donor doped nonmagnetic semiconductor ( n - s ) layer localized between two ferromagnetic metal ( fm ) layers and also two thin layers of a heavily doped degenerate semiconductor ( n + - s layers ) between the n - s and fm layers . fig5 b illustrates an exemplary energy diagram of the spin devise shown in fig5 a in equilibrium ( broken curves ) and at a bias voltage v ( solid curves ) in the case when the n + - s layers have a narrower energy bandgap than that of the n - s region and the n - s region is a degenerate semiconductor ( for the nondegenerate n - s region e c0 & gt ; f ). here f is the fermi level in equilibrium , e c ( x ) is bottom of semiconductor conduction band , e c0 and e c0 + _ are the values of e c ( x ) in the n - s and n + - s layers , respectively ; w and l thickness of the n - s and n + - s layers , respectively ; δ and l d — are the height and thickness of the schottky barrier of the fm - n + - s junctions . one of the two fm - n + - s contacts is used as a spin injector and another as a spin filter . such fm - n + - n - n + - s heterostructures ensure spin polarization of electrons is equal substantially to 100 % inside the nonmagnetic semiconductor layer when its thickness , w , is less than l s and magnetizations , m 1 and m 2 have opposite direction , as it is shown in the fig5 a . this occurs even in these cases when spin polarization of the current in fm - n + - s contacts , p j , are relatively small ( p j can be even ˜ 5 %- 15 %). the present invention has been described with reference to an exemplary embodiment . however , it will be readily apparent to those skilled in the art that it is possible to embody the invention in specific forms other than that of the exemplary embodiment described above . this may be done without departing from the spirit and scope of the invention . the exemplary embodiment is merely illustrative and should not be considered restrictive in any way . the scope of the invention is given by the appended claims , rather than the preceding description , and all variations and equivalents that fall within the range of the claims are intended to be embraced therein . | 7 |
hereinafter , embodiments will be described with reference to drawings . however , the embodiments can be implemented with various modes . it will be readily appreciated by those skilled in the art that modes and details can be changed in various ways without departing from the spirit and scope of the present invention . thus , the present invention should not be interpreted as being limited to the following description of the embodiments . in this embodiment , a semiconductor memory device in fig1 a will be described . the semiconductor memory device in fig1 a includes a row driver 101 , a column driver 102 , a plurality of word lines 103 connected to the row driver 101 , a plurality of bit lines 104 ( indirectly ) connected to the column driver 102 , and memory cells 105 each provided at the intersection of the word line 103 and the bit line 104 . this structure is the same as that of the conventional dram in fig2 a and 2b . the semiconductor memory device in fig1 a further includes back gate transistors 108 each inserted between the column driver 102 and the bit line 104 . it can also be said that the back gate transistor 108 is inserted in the bit line 104 . it can also be said that a source of the back gate transistor 108 is connected to the column driver 102 , and a drain of the back gate transistor 108 is connected to the bit line 104 . it can also be said that the back gate transistor 108 is inserted between the column driver 102 and the memory cell 105 that is the closest to the column driver 102 . a gate of the back gate transistor 108 is connected to a bit line controlling line 112 , and a back gate of the back gate transistor 108 is connected to a back gate line 111 . the potential of the bit line controlling line 112 is set by a bit line controlling circuit 110 . the back gate line 111 is connected to one electrode of a capacitor 109 , and the potential thereof is held at an appropriate negative value regardless of whether or not an external power supply is provided . for that purpose , charge may be injected so that the potential of the capacitor 109 ( the back gate line 111 ) becomes appropriate , and then the back gate line 111 may be brought into a floating state . alternatively , with the back gate line 111 placed in a floating state , an electron beam with an energy of several tens of kilo electron volts or higher may be injected into part thereof . note that as illustrated in fig1 b , the back gate line 111 may be connected to a negative electrode of a battery 113 provided over a substrate where the semiconductor memory device is formed or in a package including the substrate . since the amount of current flowing through the back gate line 111 is significantly small , the capacity of the battery 113 can be extremely low . when the semiconductor memory device is powered by an external power supply and is determined to be usable , the bit line controlling circuit 110 supplies the bit line controlling line 112 with an appropriate potential to turn on the back gate transistor 108 . when interruption of power from the external power supply is detected , or termination of the use of the semiconductor memory device is detected even while the semiconductor memory device is powered by the external power supply , the bit line controlling circuit 110 sets the potential of the bit line controlling line 112 to 0 v or less to rapidly turn off the back gate transistor 108 . a semiconductor memory device according to this embodiment will be described with reference to fig3 . the semiconductor memory device in fig3 has sense amplifiers 114 inserted in bit lines 104 . the sense amplifier 114 is used to divide the bit line 104 into appropriate lengths to lower the bit line capacitance during read operation so that read accuracy can be increased . with the sense amplifier 114 inserted in the bit line 104 in this manner , when power from an external power supply is interrupted , for example , the charge in the bit line 104 flows out also through the sense amplifier 114 . as a result , when power from the external power supply is interrupted , the potential of the bit line 104 connected to the sense amplifier decreases to 0 v . therefore , it is necessary to prevent charge in the bit lines 104 from flowing out when power from the external power supply is interrupted , by providing the back gate transistors such that the sense amplifier 114 is sandwiched therebetween . the semiconductor memory device in fig3 includes a column driver 102 , a plurality of word lines 103 , a plurality of bit lines 104 , and memory cells 105 each provided at the intersection of the word line 103 and the bit line 104 . in addition , the sense amplifier 114 is inserted in the bit line 104 . like the semiconductor memory device described in embodiment 1 , the semiconductor memory device in fig3 further includes back gate transistors 108 _ 1 each inserted between the column driver 102 and the bit line 104 . a gate of the back gate transistor 108 _ 1 is connected to a bit line controlling line 112 _ 1 , and a back gate of the back gate transistor 108 _ 1 is connected to a back gate line 111 _ 1 . the potential of the back gate line 111 _ 1 is held at an appropriate negative value regardless of whether or not the external power supply power is provided . the semiconductor memory device in fig3 further includes back gate transistors 108 _ 2 and back gate transistors 108 _ 3 each provided between the sense amplifier 114 connected to the bit line 104 and the memory cell 105 that is the closest to the sense amplifier 114 . a gate of the back gate transistor 108 _ 2 is connected to a bit line controlling line 112 _ 2 , and a gate of the back gate transistor 108 _ 3 is connected to a bit line controlling line 112 _ 3 . a back gate of the back gate transistor 108 _ 2 is connected to a back gate line 111 _ 2 , and a back gate of the back gate transistor 108 _ 3 is connected to a back gate line 111 _ 3 . the potentials of the back gate line 111 _ 2 and the back gate line 111 _ 3 are each held at an appropriate negative value regardless of whether or not the external power supply power is provided . in such a semiconductor memory device , the potentials of the bit line controlling lines 112 _ 1 to 112 _ 3 change according to conditions in a manner similar to that in embodiment 1 . in other words , when the semiconductor memory device is powered by an external power supply and is usable , the bit line controlling lines 112 _ 1 to 112 _ 3 are supplied with such a potential that the back gate transistors 108 _ 1 to 108 _ 3 are turned on . in contrast , when power from the external power supply is interrupted or when the use of the semiconductor memory device is terminated even while the semiconductor memory device is powered by the external power supply , the bit line controlling lines 112 _ 1 to 112 _ 3 are supplied with such a potential that the back gate transistors 108 _ 1 to 108 _ 3 are turned off . for example , when power from the external power supply is interrupted , the potential of the bit line controlling lines 112 _ 1 to 112 _ 3 rapidly becomes 0 v or less to turn off the back gate transistors 108 _ 1 to 108 _ 3 . consequently , the bit line 104 is divided by the back gate transistors 108 _ 1 to 108 _ 3 . thus , even if the potential of portions of the bit line 104 connected to the column driver 102 and the sense amplifier 114 becomes 0 v , the potential of the other portions ( portions connected to the memory cells 105 ) can remain at an appropriate value (& gt ; 0 v ). on the other hand , because the potential of the word line 103 is 0 v , the cell transistor in the memory cell has sufficiently high resistance , and thus enables charge accumulated in the capacitor to be retained for a long period of time . a semiconductor memory device in fig4 a and 4b will be described . memory cells 117 in the semiconductor memory device in fig4 a and 4b have the same configuration as those described in patent document 4 . refer to patent document 4 for the operation and the like of the memory cells 117 . as illustrated in fig4 b , the memory cell 117 according to this embodiment includes a write transistor 118 , a read transistor 119 , and a capacitor 120 . a source of the write transistor 118 and a source of the read transistor 119 are connected to a bit line 104 . a gate of the write transistor 118 is connected to a write word line 115 . a drain of the write transistor 118 and a gate of the read transistor 119 are connected to one electrode of the capacitor 120 . the other electrode of the capacitor 120 is connected to a read word line 116 . the potentials of the write word lines 115 and the read word lines 116 are controlled by a row driver 101 . the potential of the bit line 104 is controlled by a column driver 102 . while there are such many differences between the memory cell 105 according to embodiment 1 or 2 and the memory cell 117 according to this embodiment , these memory cells are the same in that the source of the write transistor 118 ( which corresponds to the cell transistor 106 in the memory cell 105 in fig1 a ) is connected to the bit line 104 and the drain of the write transistor 118 is connected to one electrode of the capacitor 120 . in other words , for data retention , the write transistor 118 needs to exhibit high resistance in the off state . thus , in a manner similar to that in embodiments 1 and 2 , back gate transistors 108 each inserted between the column driver 102 and the bit line 104 are provided , which can achieve sufficiently high resistance even when power from an external power supply is interrupted ( see fig4 a ). a gate of the back gate transistor 108 is connected to a bit line controlling line 112 , and a back gate of the back gate transistor 108 is connected to a back gate line 111 . the potential of the back gate line 111 is held at an appropriate negative value regardless of whether or not the external power supply is provided . in such a semiconductor memory device , the potential of the bit line controlling line 112 changes according to conditions in a manner similar to that in embodiment 1 . in other words , when the semiconductor memory device is powered by the external power supply and is usable , the bit line controlling line 112 is supplied with such a potential that the back gate transistor 108 is turned on . in contrast , when power from the external power supply is interrupted or when the use of the semiconductor memory device is terminated even while the semiconductor memory device is powered by the external power supply , the bit line controlling line 112 is supplied with such a potential that the back gate transistor 108 is turned off . for example , when power from the external power supply is interrupted , the potential of the bit line controlling line 112 rapidly becomes 0 v or less to turn off the back gate transistor 108 . consequently , the potential of the bit line 104 can remain at an appropriate value (& gt ; 0 v ). on the other hand , because the potential of the write word line 115 is 0 v , the write transistor 118 in the memory cell 117 has sufficiently high resistance , and thus enables charge in the capacitor 120 to be retained for a long period of time . the memory cell 117 is characterized by being capable of amplifying a signal with the read transistor 119 and output the amplified signal to the bit line even if the capacitance of the capacitor 120 is low . however , the fact that the capacitance of the capacitor 120 is low means that it is difficult to retain data for a required time if the resistance of the write transistor 118 in the off state is not sufficiently high . therefore , keeping , during power interruption , the potential of the bit line 104 at an appropriate positive value with the back gate transistor 108 to increase the resistance of the write transistor 118 in the off state is particularly effective in this embodiment . a brief description is given of a process for manufacturing the semiconductor memory device illustrated in , for example , fig1 a and 1b or fig3 with reference to fig6 a to 6c , fig7 a and 7b , and fig8 . refer to known semiconductor integrated circuit manufacturing techniques for the details . note that fig6 a to 6c , fig7 a and 7b , and fig8 illustrate the concepts of the manufacturing process and do not show specific cross sections . first , device isolation insulators 202 , n - type impurity regions 203 n , p - type impurity regions 203 p , an n - channel transistor gate 204 n , a p - channel transistor gate 204 p , a first interlayer insulator 205 , first contact plugs 206 a to 206 d , and the like are formed over a surface of a substrate 201 of a semiconductor or the like by known semiconductor integrated circuit manufacturing techniques . the n - channel transistor or the p - channel transistor here may be used in a row driver , a column driver , a sense amplifier , or the like in a semiconductor memory device . next , first layer wirings 208 a to 208 d are formed so as to be embedded in a first embedment insulator 207 . these wirings are used in , for example , the row driver 101 or the column driver 102 in fig1 a and 1b , or the sense amplifier 114 . further , a second interlayer insulator 209 , a second contact plug 210 , a second embedment insulator 211 , second layer wirings 212 a to 212 c are formed . here , the second layer wiring 212 b corresponds to the back gate of the back gate transistor 108 or the back gate line 111 in fig1 a and 1b . note that one or more layers including another wiring may be additionally provided between a layer including the second layer wirings 212 a to 212 c and a layer including the first layer wirings 208 a to 208 d . further , a third interlayer insulator 213 , third contact plugs 214 a to 214 c , a third embedment insulator 215 , and third layer wirings 216 a to 216 e are formed . note that the first contact plug 206 a , the first layer wiring 208 a , the second contact plug 210 , the second layer wiring 212 a , the second layer wiring 212 c , the third contact plug 214 a , the third contact plug 214 b , the third layer wiring 216 a , and the third layer wiring 216 b serve as part of the bit line 104 in fig1 a and 1b . subsequently , an oxide semiconductor layer 217 a and an oxide semiconductor layer 217 b are formed , and a gate insulator 218 is formed so as to cover them . at this time , it is preferable that the physical thickness of the gate insulator 218 be two or more times that of the oxide semiconductor layer 217 a and the oxide semiconductor layer 217 b , because this enables the oxide semiconductor layer 217 a and the oxide semiconductor layer 217 b to be covered with the gate insulator 218 reliably , thereby preventing shorts between wirings . on the other hand , it is preferable that the effective thickness of the gate insulator ( e . g ., the equivalent oxide thickness ) be less than or equal to that of the oxide semiconductor layer 217 a and the oxide semiconductor layer 217 b . therefore , it is preferable that the gate insulator 218 be formed using a material whose dielectric constant is twice that of the oxide semiconductor layer 217 a and the oxide semiconductor layer 217 b . for example , the gate insulator 218 may be formed using a high dielectric constant material such as hafnium oxide , tantalum oxide , or zirconium oxide . materials such as barium oxide , strontium oxide , calcium oxide , and lithium oxide which form silicides on silicon semiconductor have been prevented from being used with silicon semiconductor , but may be used with an oxide semiconductor without problems . therefore , any of these materials can be used for the gate insulator 218 as long as it has high dielectric constant . then , fourth layer wirings 219 a to 219 d are formed . the fourth layer wiring 219 a here corresponds to the gate of the back gate transistor 108 or the bit line controlling line 112 in fig1 a . the fourth layer wirings 219 b to 219 d correspond to the word lines 103 in fig1 a . stacked capacitors are formed by known dram manufacturing techniques . specifically , a fourth interlayer insulator 220 , a fourth contact plug 221 a , and a fourth contact plug 22 lb are formed , and then a fifth interlayer insulator 222 , a capacitor electrode 223 a and a capacitor electrode 223 b are formed thereover . subsequently , a capacitor insulator 224 and a cell plate 225 are formed . thus , the semiconductor memory device can be manufactured . a brief description is given of a process for manufacturing the semiconductor memory device illustrated in fig4 a and 4b with reference to fig9 a to 9d and fig1 a to 10c . refer to known semiconductor integrated circuit manufacturing techniques or patent document 2 for the details . note that fig9 a to 9d and fig1 a to 10c illustrate the concepts of the manufacturing process and do not show specific cross sections . first , a box layer 302 , an soi layer 303 a , and an soi layer 303 b are formed over a surface of a substrate 301 of a semiconductor or the like by known semiconductor integrated circuit manufacturing techniques . next , read gates 304 a and 304 b are formed , and an impurity is added to the soi layer 303 a and the soi layer 303 b by using these gates as a mask to form impurity regions 305 a to 305 d . here , the impurity region 305 a corresponds to the back gate of the back gate transistor 108 or the back gate line 111 in fig4 a . the read gates 304 a and 304 b correspond to the gates of the read transistors 119 in fig4 a and 4b . then , a first interlayer insulator 306 is formed and then is planarized to expose top surfaces of the read gates 304 a and 304 b . first layer wirings 307 a to 307 e and a first embedment insulator 308 are formed . subsequently , an oxide semiconductor layer 309 a and an oxide semiconductor layer 309 b are formed , and a gate insulator 310 is formed so as to cover them . then , second layer wirings 311 a to 311 e are formed . the second layer wiring 311 a here corresponds to the gate of the back gate transistor 108 or the bit line controlling line 112 in fig4 a . the second layer wirings 311 c and 311 d correspond to the write word lines 115 in fig4 a and 4b . the second layer wirings 311 b and 311 e correspond to the read word lines 116 in fig4 a and 4b . a second interlayer insulator 312 with a plane surface is formed . then , contact plugs 313 a , 313 b , and 313 c connected to the first layer wirings 307 a , 307 b , and 307 d are formed . third layer wirings 314 a and 314 b are formed . the third layer wirings 314 a and 314 b correspond to the bit line 104 in fig4 a . a third interlayer insulator 315 is formed . any other wirings , interlayer insulators , and the like may additionally be formed . through the aforementioned process , a semiconductor memory device including a back gate transistor 316 , a read transistor 317 , a write transistor 318 , and a capacitor 319 is formed . the back gate transistor 316 corresponds to the back gate transistor 108 in fig4 a . the read transistor 317 , the write transistor 318 , and the capacitor 319 form one memory cell . the read transistor 317 , the write transistor 318 , and the capacitor 319 correspond to the read transistor 119 , the write transistor 118 , and the capacitor 120 in fig4 b , respectively . note that fig1 c illustrates two memory cells ( a memory cell 320 a and a memory cell 320 b ). these memory cells are connected to the same bit line . this application is based on japanese patent application serial no . 2011 - 129685 filed with japan patent office on jun . 10 , 2011 , the entire contents of which are hereby incorporated by reference . | 6 |
turning now to the drawings and , more particularly to fig1 and 2 , the basic structure of a preferred embodiment of the invention is illustrated . here , an under - pavement light armature is shown , for example , as it can be used on the runway 1 of an airport . the runway and associated ground support comprise the support base for the signal lamp of the present invention . the light armature has a housing 2 , which is cemented in a known manner into runway 1 . a round cover 3 is attached to the housing 2 . vehicles can run over this cover . as seen in fig2 the cover 3 includes two generally flat recessed segments 4 , which lie between two segments 5 that are raised by a few millimeters . also , more than two flat segments 4 or only one may be provided . a light processing assembly 6 , also discussed herein as optics , is arranged in approximately the middle of each recessed segment 4 . the structure will be discussed in greater detail below . a lamp 8 is disposed in approximately the center of the housing 2 , below cover 3 . the lamp 8 is arranged in a parabolic reflector 9 , so that its light will impinge on the light processing assembly 6 upward as an essentially “ parallel ”, i . e ., neither convergent nor divergent , light beam 10 . the light source consists of a lamp 8 and a reflector 9 . the reflector 9 , optionally , as well as the light source with lamp 8 , is appropriately removably attached onto a mounting plate 12 , which in turn supports each of the light processing assemblies 6 on the respective base 13 . the light source is arranged in a holder 14 and is connected to the power source through a plug connection 15 . the light source can also be mounted separately in the lower part . the signal light of the present invention is generally suitable for an essentially flush incorporation into traffic surfaces . the term “ essentially flush ” indicates that the projection above the traffic surface is on the order of a few millimeters . the present inventive signal light protrudes above the traffic surface by a maximum of 6 mm , has no recesses in which water could collect and is constructed so robustly that vehicles can drive over it . a first preferred embodiment of the light processing assembly 6 can be seen in fig3 . in general , light processing assembly 6 collects incoming parallel light beam 10 impinging on it from underneath , deflects it to the horizontal direction and emits it again as a substantially parallel , i . e . neither divergent or convergent , light beam . as seen in fig3 light processing assembly 6 consists of a prismatic transparent body , preferably made of borosilicate glass and is constructed so as to be essentially translational - symmetrical in the direction generally perpendicular to incoming light . borosilicate glass is preferred because of its resistance to temperature shock or temperature changes . as previously addressed , the light processing assembly 6 rests with its base 13 on a mounting plate 12 . toward the top , it is protected by a cover plate 20 , which is screwed into the cover 3 . the light processing assembly 6 is sealed with a hardenable putty 19 against cover 3 , so that the inside of the device is effectively sealed and at the same time can withstand thermal dilatations of the component parts , in addition to shock and vibrations . the housing includes a light emitting aperture 30 , at which the light outlet , or exit surface , 25 of the light processing assembly 6 is disposed . the light processing assembly 6 includes first and second arrangements for receiving and directing light either formed therein or operatively associated therewith , depending on the embodiment , with the first arrangement for receiving and directing light being disposed at a light inlet portion of the housing . the second arrangement for receiving and directing light is disposed a predetermined distance from the first arrangement for receiving and directing light within the light processing assembly 6 . with reference to the first preferred embodiment illustrated in fig3 the first arrangement for receiving and directing light is disposed at the entry region of the light processing assembly 6 and is formed by a approximately cylindrical lens surface 21 arched , or curved toward the outside , which deviates the entering light radiation 10 into a convergent light beam 22 , that is , converging toward the second arrangement for receiving and directing light . the convergent light beam 22 impinges on the second arrangement for receiving and directing light , namely , a mirror surface 23 of the light processing assembly 6 , which is formed by a mirrored surface area curved cylindrically toward the inside . the curvature of the mirror surface 23 is designed so that the convergent light beam 22 is deflected into a linearly extending light beam 24 , which has an elevation angle of approximately 5 °. the light beam 24 impinges essentially perpendicularly onto the exit surface 25 of light processing assembly 6 and leaves the signal light through the light emitting aperture 30 as light beam 18 . the light from the light source is intensified during its passage through the light processing assembly of the present invention . as a result of the focusing action of the curved lens surface 21 , the cross - sectional area of the light field is reduced upon passage through the light processing assembly so that its intensity , i . e . the radiation output per transparent cross - sectional unit area ( cm 2 ) is greater at the exit than at the entry and the entry area has a larger cross - sectional area than the exit area . this permits the light outlet 25 to be designed very small , so that the projection of the device above the pavement can remain small . the small size of the light outlet 25 also reduces the danger of damage , for example , during snow removal or cleaning work . in this connection , it is also advantageous that the light outlet 25 is flat and thus it is more difficult to damage functionally . preferably , the entry lens surface 21 and the light outlet 25 of light processing assembly 6 are provided with suitable coatings . a dichroic filter can be applied to the entry lens surface 21 , which reflects heat radiation in the infrared region or which allows only light of a certain wavelength region to be transmitted . for example , on the light outlet 25 , one can apply a dirt - repellant and / or scratch - resistant coating . alternatively , or in addition to this , a transparent protective plate can be arranged on the exit side of the light outlet 25 , which can also be designed so that it is optically effective . for example , it may have a fresnel structure . the design of the optics according to fig3 is preferred , because only one glass optical body is necessary . as a result of this , the manufacture and adjustment are simpler and reflection losses are smaller . however , several embodiments of the invention are possible . while six embodiments of the present invention are herein described and illustrated , it will be appreciated by those skilled in the art that other versions of the present signal light are attainable without departing from the spirit and scope of the present invention . thus , for example , fig4 illustrates a second preferred embodiment in which the light processing assembly 6 is made of a prism portion 6 a and a plane convex cylindrical lens 6 b . the plane - convex cylindrical lens 6 b focuses the entering beam 10 in the same way as the curved entry surface 21 of the first embodiment . the deflection of the beam is done again with the aid of a cylindrical mirror 23 . fig5 illustrates a third preferred embodiment of the light processing assembly with a prismatic body 6 c and a convex - concave collecting light processing assembly 6 d . here , the entering light beam 10 is collected by the cylindrical outward - arching entry surface 26 and again converted by the cylindrical inwardly arched surface 27 into a parallel light beam again . the “ arching ” curvature is taken with respect to the central portion of the light processing assembly 6 d . the prismatic body 6 c acts as a mirror prism to deflect the light beam without its divergence being changed . the fourth preferred embodiment according to fig6 is constructed essentially the same way . however , it shows that the surfaces 26 and 27 can be designed as fresnel lenses or cylindrical lens segments , respectively . in the same way , it is possible to use holographic lenses , especially when , instead of an incandescent lamp 8 , an essentially monochromatic semiconductor light source is used . fig7 shows the a fifth variant of the light processing assembly 6 in which it is assumed that the parallel light beam 10 runs essentially flat already from the light source so that , at most , a slight deflection is necessary and the mirror can be omitted . in this case , a convex - concave glass optical body can be used as the light processing assembly 6 , the cylindrical , outward curved entry surface 26 of which collects the light and the cylindrical inwardly curved exit surface of which again produces an essentially parallel light beam 18 with the desired inclination . in the practical examples discussed so far , it was assumed that the exiting light beam 18 is essentially linearly directed or parallel , that is , that its divergence is small , for example , ± 5 °. however , depending on the requirements , only the divergence in the vertical direction should be so small , while the horizontal divergence should be higher e . g ., in curves on a taxiway . a corresponding radiation field 18 is illustrated in fig8 . this radiation field is “ parallel ” that is , nondivergent , only in the vertical direction , while it has a large divergence in the horizontal direction . there are various possibilities for producing a radiation field 18 according to fig8 . thus , in the embodiment according to fig3 for example , the entry lens surface 21 can be designed to be convex or concave in the direction perpendicular to the plane of the drawing or it can be provided with scattering ribs which run parallel to the plane of the drawing . however , the mirror surface 23 or the light outlet 25 may be designed for producing a divergent radiation field in the horizontal direction , again by using suitable curvature or scattering bodies . finally , the light source may be designed in such a way that already the entering light beam is divergent in one direction , i . e ., in the direction perpendicular to the plane of fig3 . by designing the entry lens surface 21 , 26 , so that it is concave , it can be achieved , in the direction perpendicular to the plane of the drawing of fig3 that the light beam 22 is convergent in both directions . as a result of this , a smaller mirror surface 23 and light outlet 25 is necessary . if the exiting light beam 18 should be linearly extending in both directions simultaneously , that is , should have small divergence in the horizontal and vertical direction , then , for example , the mirror surface 23 or the light outlet 25 can be provided with a corresponding curvature which compensates again the divergence of the light beam 24 in the horizontal direction . fig9 illustrates a sixth preferred embodiment of the present invention using light diodes ( leds ) 31 as light source 8 . the leds are mounted to a common support 32 , e . g . a curved printed circuit board , and they are arranged in a cylindrically curved matrix . fig9 shows a cross section of this matrix , which matrix is extending perpendicular to the plane of the drawing . the axes of the leds all meet in a common line , i . e . the leds generate a cylindrically converging input light field 10 . light processing assembly 6 is a single prism having a flat input surface section 33 for receiving the light 10 from the leds . this light impinges on curved mirror 23 formed by a mirror surface section of light processing assembly 6 . the curvature of mirror 23 is such that the reflected light is substantially parallel in vertical direction , i . e . the light &# 39 ; s aperture in vertical direction is small . the reflected light exits through the flat exit surface section 25 and exit aperture 30 . preferably , leds of different colors are used . they can either be operated together to generate substantially white light , or they can be operated in blocks of differing colors to generate colored light , e . g . for signaling purposes . in the embodiments shown so far , the optics was embedded in a putty 21 . however , one can also consider equipping the optics with a suitable tight sleeve and replacement system so that , if necessary , it can be replaced simply . it will therefore be readily understood by those persons skilled in the art that the present invention is susceptible of a broad utility and application . many embodiments and adaptations of the present invention other than those herein described , as well as many variations , modifications and equivalent arrangements , will be apparent from or reasonably suggested by the present invention and the foregoing description thereof , without departing from the substance or scope of the present invention . accordingly , while the present invention has been described herein in detail in relation to its preferred embodiment , it is to be understood that this disclosure is only illustrative and exemplary of the present invention and is made merely for purposes of providing a full and enabling disclosure of the invention . the foregoing disclosure is not intended or to be construed to limit the present invention or otherwise to exclude any such other embodiments , adaptations , variations , modifications and equivalent arrangements , the present invention being limited only by the claims appended hereto and the equivalents thereof . | 5 |
whilst for connivance of explanation , the description focuses mainly in umd that is utilized by rescue forces in disaster areas , those versed in the art will readily appreciate that the umd of the invention is by no means bound by this application . accordingly , the umd of the invention may be utilized by an operator or operators in any area of interest . the und : a umd in accordance with the invention is adapted to function as a robot scout to reconnoiter a disaster area . as shown in fig1 ( a ) and 1 ( b ) , the basic structure of umd 10 is constituted by a toroidal duct 11 surrounding a rotor and propeller assembly 12 and a main center body 13 . centerbody 13 is supported within duct 11 by structured elements such as an array of struts 14 . this basic structure creates a ducted aerodynamic fan blowing an air stream through the duct which acts to propel the umd . the embodiment of the umd illustrated herein is highly compact and light weight . duct 11 has a diameter 0 . 4 meters . the gross take - off weight of the umd is 2 kg ( 2000 grams ). the primary structural material for the umd is kelvar which has a high strength - to - weight ratio . the invention can , of course , be embodied in other robot scout structures having different weights and dimensions . centerbody 13 houses the main engine , the energy source and the electronics compartment containing a computer unit . in the present embodiment , the main rotor engine is an electrical brushless dc motor having 200 watts output power . the energy source is constituted by a bank of lithium batteries . structure elements 14 fix the centerbody 13 to the duct 11 . the air mobility capability of the umd is based essentially on the concept of a ducted fan vtol air vehicle as described in the ebbert et . al . u . s . pat . no . 5 , 295 , 643 . a circular array of control vanes 15 mounted within toroidal duct 11 affords the aerodynamic means required to control the flight and attitude of the umd . in operation , when the driven propellers in the ducted fan rotate to blow an air stream in the downward vertical direction , this provides the umd with the necessary lift forces . to cause the umd to descend vertically toward the ground , the rotor speed is reduced . the legs of the umd are then outstretched to function as landing gear . upon landing at a disaster site or elsewhere , the legs function to maintain the robot erect and as a walking mechanism . when the umd is aloft , its flight direction is controlled by the four vanes 15 which intercept the air stream being blown out of the duct to produce a lateral force causing the umd to fly in the north , south , east or west direction depending on the angular position of the four vanes in the circular array shown in fig1 ( a ). to support the geo - navigation and flight control functions of the umd , several sensors are required for this purpose . these include ( see fig6 which shows the units in the electronics compartment ) the following : ( a ) three piezoelectric gyros 62 ( such as piezo gyro model hxm1010 , commercially available from heli - max which weighs only 13 grams ) actuation means for flight control include rotor - control 76 and control vane servo actuators 77 for the four vanes . the required set of sensors 17 as shown in fig1 ( a ) are assembled in a housing 16 mounted on the exterior of the toroidal duct . a communication unit 18 provided with an antenna 19 is mounted on the outer surface of the ducted fan 11 . low weight components are preferred for implementing communication unit 18 . for example fm receiver model tetra 301fm , commercially available from fma direct inc ., weighs only 14 grams and provides the onboard end of the uplink 68 ( see fig6 ). a video transmitter model tsg tx , commercially available from the security group which also weighs only 14 grams , provides the onboard end of the downlink 69 . communication unit 18 establishes a two - way wireless data link between umd 10 and remotely - located operating personnel . it also establishes a two - way wireless data link between umd 10 and other umds in order to coordinate a mission assigned to a group of umds . those versed in the art will readily appreciate that the invention is by no mean bound by the specific structure of the umd in accordance with fig1 ( a ) and 1 ( b ), and by the same token it is not bound by the system architecture , described with reference to fig6 . various approaches have heretofore been proposed to solve the problem of command and control of multiple unmanned mobile systems . in accordance with a preferred embodiment , a distributed - decentralized architecture is utilized , the details of which are disclosed in yavnai a ., “ distributed decentralized architecture for autonomous cooperative operation of multiple agent system ”, in proceedings of ieee symposium on autonomous underwater vehicle technology , jul . 19 - 20 , 1994 , cambridge , pp . 61 - 67 and guelman , m ., and yavnai , a ., u . s . pat . no . 5 , 340 , 056 , 1994 . the all - terrain ground mobility of the scouting device is achieved by using active multiple mechanical legs to support the umd and cause it to walk on the terrain of the disaster site . fig1 ( a ) illustrates a situation in which the legs are in a retracted state . fig1 ( b ) illustrates a situation where the legs are in an extended outstretched position . in the present embodiment four legs are provided which are similar to those shown in fig1 of u . s . pat . no . 5 , 842 , 533 to takeuchi . in the present embodiment , each leg has two links , namely , an upper link 21 and a lower link 20 . the kinematic arrangement of the leg &# 39 ; s joints and links of the present invention is similar to that shown in fig9 of the paynter , u . s . pat . no . 5 , 040 , 626 . upper link 21 is actuated by a double - actuator 22 mounted on the external surface of the duct 11 . an active joint 23 provides a relative one - degree - of - freedom controlled motion between upper link 21 and lower link 20 , each lower link 20 having a foot 24 . the legs also function as landing gear struts , preferably with energy absorbing capability . the legs are capable of compensating for ground irregularities , so that the main body of umd 10 is kept in a level state . a payload housing 25 is mounted on top of centerbody 13 above the rotor assembly . housing 25 has an optical window 26 to protect the internal electro - optical sensors and associated electronics . the main sensor housed in payload housing 25 is a video camera 70 such as a ccd video camera with resolution of 256 × 256 pixels , such as model sg - 2000 - cmos , commercially available from the security group , ( weighing 5 grams ). a light emitting unit is aligned with the video camera 70 line - of - sight to facilitate camera operation under low light conditions . an infra - red uncooled camera 71 ( see fig6 ) is also included as an option . payload housing 25 is capable of rotating 360 degrees around an axis which is aligned with the central axis of the centerbody 13 and with the axis of rotation of the rotor . this rotation is effected by a light weight dc servo motor 79 . a suitable motor for this purpose is dc servo model ls - 3 . 0 commercially available from wes - technik , germany ( weight 3 grams ). whilst in the example above the payload includes housing 25 equipped with window 26 for accommodating video camera 70 and possibly also ir camera 71 , by another embodiment other payload equipment may be employed in addition or in lieu of the specified video camera and ir camera , depending upon the designated mission ( s ) of the unm . turning now to fig2 umd 10 is capable of operating in several alternative modes . in a standing mode 30 , umd 10 is supported by the legs extended therefrom which support the weight of the umd and also compensate for ground irregularities in order to maintain umd &# 39 ; s main body in a level state . in a hovering mode 31 , umd 10 is capable of moving in one of three alternate directions : ( 1 ) vertical take - off 35 ; ( 2 ) vertical landing 34 ; and ( 3 ) hovering flight 36 . it is also capable of hovering above the same ground location in a keep - on - station mode . in cruise dash flying mode 32 , umd 10 then flies in direction 37 . in a walking mode 33 , umd 10 then walks on the ground or climbs stairs in the general direction 38 . in a ground mobility mode umd 10 can creep or otherwise move along the ground using the legs as supporting mechanisms . fig3 ( a ) and 3 ( b ) show umd 10 in an exemplary walking mode . fig3 ( a ) being a top view and fig3 ( b ) a side view . umd 10 is shown moving on an uneven terrain 27 in the general direction 28 . in the present embodiment , umd 10 has four legs , each leg being constituted by two interconnected links — the upper link 21 and the lower link 20 . the upper link 21 is actuated by a double - actuator 22 which is mounted on the external surface of the duct 11 . the double - actuator 22 provides two one - degrees - of - freedom controlled rotary motions around axes perpendicular to upper link 21 . in the present embodiment , each degree - of - freedom of the double - actuator 22 is provided by a light - weight ( several grams ) rotary dc servo brushless motor such as dc servo model ls - 3 . 0 , commercially available from wes - technik , germany ( weight 3 grams ). an active joint 23 provides a relative one - degree - of - freedom controlled rotary motion between upper link 21 and lower link 20 . the one - degree - of - freedom motion of the active joint 23 of the present embodiment is also provided by a light weight ( several grams ) rotary dc servo brushless motor such as the above noted dc servo model ls - 3 . 0 . all three degrees - of - freedom of each leg are rotary , and each one thereof is provided by a one - degree - of - freedom rotary actuator . the kinematic arrangement of the leg &# 39 ; s joints and links of the present invention is by one embodiment similar to that shown in fig9 u . s . pat . no . 5 , 040 , 626 to paynter . the double - actuator 22 provides the two rotary motions around axes which are analogous to axis 1 and axis 2 in fig9 of the paynter patent . actuator 23 provides the rotary motions around an axis which is analogous to axis 3 in the above - noted fig9 . the total number of active controlled degrees - of - freedom of the walking mechanism in the present embodiment is therefore twelve . each lower link 20 has a foot 24 . the foot can be either fixed to the lower link 20 , or can be linked to the lower link 20 via a pivot or via a passive elastic energy absorbing element such as a spring , or a combination thereof . the legs also function as landing gear struts , preferably with energy absorbing capability . the legs are capable of compensating for ground irregularities to keep the main body level . automatic control of legged locomotion is necessary in order to exploit the all - terrain mobility of the umd . it is particularly required in a disrupted terrain or environment , such as when ruined buildings are encountered by the umd . this capability raises relatively complex control problems . for example , in the present embodiment up to as many as twelve degrees - of - freedom must be controlled simultaneously . thus , the control system is called upon to issue as many as twelve coordinated commands to the actuators , ( e . g ., to dc servo motors ) simultaneously , in real time . some of the principles of controlling the multi - legged walking mechanisms in the present embodiment are based on techniques described in the following publications : a ) todd , d . j ., “ walking machines — an introduction to legged robots ”, kogan page ltd ., london u . k ., 1985 , pp . 91 - 150 ; b ) song , shin - min , et . al ., “ machines that walk ”, the mit press , cambridge , mass ., 1989 , pp . 23 - 164 ; c ) chen , chun - hung et . al ., “ motion planning of walking robots in environments with uncertainty ”, journal of robotic systems , john wiley & amp ; sons , inc ., volume 16 , no . 10 , pp . 527 - 545 , 1999 . the invention is , of course , not bound by these techniques . when umd 10 is walking in general direction 28 , a plurality of sensors are activated in order to determine its geographical location ; the geometrical features of the surrounding environment ; its position relative to other objects ; and any obstacles in its way . the plurality of sensors 17 which encompass a 360 degrees field of view satisfies these needs . also supporting these needs are the electro - optical sensors housed in payload housing 25 , these being directed forward through optical window 26 which is capable of rotating 360 degrees around its main axis . some of the sensing devices and techniques used in the present embodiment are disclosed in : a ) borenstein , j ., et . al ., “ mobile robot positioning — sensors and techniques ”, the journal of robotic systems , vol . 14 , no . 4 , 1997 , pp . 231 - 249 ; b ) borenstein , j ., et . al ., “ navigating mobile robots : sensors and techniques ”, a . k . peters ltd ., wellesley , mass ., 1995 ; c ) adams , martin david , “ sensor modeling , design and data processing for autonomous navigation ”, world scientific publishers , singapore , 1999 , pp . 153 - 208 . the invention is , of course , not bound by these techniques . it is known to use computer - controlled visual techniques for navigation and for obstacle detection and avoidance . some of the visual devices and techniques for this purpose include the present embodiment , and are described in : a ) movarec , hans p ., “ robot rover visual navigation ”, umi research press , ann arbor , mich ., 1981 , pp . 49 - 147 ; b ) robert , luc , et . al ., “ applications of non - metric vision to some visually guided robotic tasks ”, in aloimonos , yiannis , ed ., “ visual navigation — from biological systems to unmanned ground vehicles ”, lawrence erlbaum associates publishers , mahwah , n . j ., 1997 , pp . 89 - 134 ; c ) weng , j . j ., et . al .,“ visual navigation using fast content - based retrieval ”, in aloimonos , yiannis , ed ., “ visual navigation — from biological systems to unmanned ground vehicles ”, lawrence erlbaum associates publishers , mahwah , n . j ., 1997 , pp . 178 - 217 ; d ) dean , thomas , et . al ., “ planning and navigation in stochastic environments ”, in aloimonos , yiannis , ed ., “ visual navigation - from biological systems to unmanned ground vehicles ”, lawrence erlbaum associates publishers , mahwah , n . j ., 1997 , pp ., 251 - 274 . the invention is , of course , not bound by these techniques . path planning techniques employed in the present embodiment are based , e . g . on techniques described in the following references : a ) a system for obstacle avoidance and path planning disclosed in u . s . pat . no . 5 , 502 , 638 to takenaka b ) “ motion planning of walking robots in environments with uncertainty ”, chen et . al ., journal of robotic systems , john wiley & amp ; sons , inc ., volume 16 , no . 10 , pp . 527 - 545 , 1999 . the problem of indoor navigation falls into two categories ; namely navigating with an a - priori map or database ; and navigating without this map or database . where an a - priori map is available , the navigation function uses a - prior data about the building layout , by employing appropriate lfms — local feature maps ( see fig8 ( a ) and 8 ( b )). if an a - priori map is not available or if the object 54 to be visited has been damaged so that the a - priori map is no longer a true representation of the actual object , then a different navigation procedure is executed , the so - called “ navigating in a maze ”. a process called “ map building ” is then a part of the navigation process . in order to meet the requirements for a highly compact and light weight umd , use is made in the present embodiment of miniature light weight sensors . for example , a ccd camera with a resolution of 256 × 256 pixles is only 5 grams in weight . ( model sg - 2000 - cmos , commercially available from the security group ) also usable are acoustic sensors which weigh only 5 grams each , or infra - red led - based range finders which weigh only 5 grams each . scenario : referring now to fig4 illustrated therein is a typical , yet not exclusive , scenario of a umd executing a data gathering and situation - monitoring mission within a disaster site . an operator 40 is put in charge of operating umd 10 and of supervising its operation from a safe location , preferably in the vicinity of the disaster area . when arriving at the station from which to launch umd 10 on its scouting mission and to thereafter manage its operation , operator 40 then has the following series of pre - mission activities to undertake : a ) unpack umd 10 from its protective packaging ; b ) place umd 10 on an uncluttered surface for safe take - off and landing ; c ) press a key on the command and control portable unit keyboard in order to transmit an on command ( see oncmd 99 in fig7 ) so as to “ wake - up ” umd 10 and change its state from system non - active state 89 to system preparing state 90 . upon entering the state of system preparing 90 , a built - in - testing (“ bit ”) is automatically initiated ; d ) using the command and control portable unit 41 to edit a mission ; e ) press a key on the command and control portable unit keyboard in order to download the mission plan file to umd 10 via wireless data link 42 . when this pre - mission series of activities is completed , umd 10 is now ready for its mission . it is important that the pre - mission procedure be accelerated to enable a fast reaction to a disaster situation . thus , the mission edition activity , the most time consuming activity of all pre - mission activities , is designed to be as rapid and as simple as possible . the mission editing display is shown in fig5 . as previously mentioned , operator 40 uses a command and control portable unit 41 to edit a mission plan and to control operation of umd 10 while on its mission . a wireless communication unit 49 is connected to the command and control portable unit 42 , thereby establishing a two - way data link with umd 10 and with self - contained unattended sensor means 46 , if these are deployed by umd 10 . after a mission plan is edited and generated , it is transmitted and downloaded to umd 10 via wireless data link 42 . while in operation , operator 40 may transmit orders to umd 10 and receive data from it via data link 42 . as shown in fig4 umd 10 is travelling along the planned path 43 in the general direction 44 . and in a manner appropriate to the situation , umd 10 is moving in various alternate modes , as described in connection with fig2 . in the actual scenario illustrated in fig4 umd 10 is moving either outside or inside a burning building 45 . when umd 10 is walking or otherwise moving within this building , it then navigates its way either with or without an a - priori map . where an a - priori map is available and is applicable to the situation , the navigation function uses a - priori data about the building layout , by employing the appropriate lfms — local feature maps ( see fig8 ( a ) and 8 ( b )). when an a - priori map is not available or where the building 45 to be explored has been so damaged that an a - priori map is no longer applicable , a different navigation procedure is executed and a process called “ map building ” becomes a part of the navigation process . as may be appropriate to the circumstances , umd 10 can land vertically , stand for a while on a supporting surface , take - off vertically , and then hover over the site . this sequence of movements can be repeated when necessary . when umd 10 is gathering data and monitoring the situation , its sensors are then operative . the electro - optical sensor housed in payload housing 25 has a field - of - view 48 which is directed forward in the direction of movement or toward an area of interest . other sensors which constitute payload whose activation depends on the specific situation may include a microphone 72 , a smoke detector 73 and a gas detector 74 . it may also be desirable to include a seismograph to sense earth tremors . umd 10 , when landing vertically , can then deploy by using a device release actuator 80 , self - contained unattended sensor means 46 for further data gathering in the disaster area . sensor means 46 which may be situated on various supporting surfaces such as on the ground transmits data it gathers to communication unit 49 attached to the command and control portable unit 41 via a wireless data link 47 . shown in fig5 is an overhead view of display 50 of the command and control portable unit 41 in accordance with one embodiment of the invention . display 50 comprises a video display window 51 , as well as an alphanumeric display window 53 . when umd 10 is on the disaster site , a scene 52 sensed by the electro - optical video sensor , ( see video camera 70 in fig6 ) and transmitted from umd 10 via wireless rf data link 42 to the communication unit 49 , is displayed on video display window 51 . the largest area of the display is then used for the graphical symbolic representation of the main elements of the mission plan . by way of example , two objects 54 in the disaster site have to be monitored . operator 40 edits a mission plan consists by this embodiment of the following elements : a ) a mission starting and terminating location st 55 ; b ) a travelling route represented by an ordered series of way - points , wp 56 , connected by route segments 58 . in the example shown in fig5 there are seven way - points wp 56 designated wp 1 to wp 7 by the order they are planned to travel . each wp 56 represents a specific location ; c ) a series of ordered device deployment locations dd 57 . in fig5 there are two dd 57 points , dd 1 and dd 2 ; d ) a return segment 59 which connects the last way - point wp 7 to the terminal point 55 ; e ) an indoor travelling segment inside an object to be monitored , this segment being between wp 5 and wp 6 . in a situation where local feature maps - lfms , ( see fig8 b ), of the object 54 to be monitored , are available a - priori , these are linked to the mission plan and downloaded from the memory storage of the command and control portable unit 41 to umd 10 , along with the mission plan . for such situations , the command and control portable unit 41 has a data base of the lfms , ( see fig8 ( a ) and 8 ( b )) of objects in the disaster area . this data base is downloaded and stored in the command and control portable unit 41 before going to the disaster area . as shown in fig6 the functional architecture of the electronics unit is of the “ bus network topology ” type . computer unit 60 is connected to all of the associated elements via a local area network — lan 61 . computer unit 60 is provided with processing elements , memory elements , and i / o elements and whatever other elements are desirable to execute all of the required computations , such as : a ) flight control ; b ) navigation ; c ) sensor data processing ; d ) multi - legged control ; e ) path planning and obstacle avoidance . in umd 10 , a set of three piezoelectric gyros 62 are used to measure the angular rate about three perpendicular axes which together establish a right - handed orthonormal coordinate system . gps receiver 63 provides location and velocity navigational information , while a magnetometer 64 provides directional data with respect to the geomagnetic field which is in turn related to the geographic coordinate system and thus provides approximated azimuth information . a set of piezoelectric tilt sensors 65 serve to determine the attitude of the umd 10 with respect to the gravity vector . also provided are infra - red (“ ir ”) light emitting diodes (“ led ”)- based rangefinders 66 to effect short range distance measurements ( effective up to about 10 meters ) to surrounding objects . these measurements provide crucial data for positioning , navigating and obstacle avoidance when umd 10 is moving in its ground mobility mode . in the present embodiment , each rangefinder 66 weighs only 5 grams . a plurality of acoustic rangefinders 67 are also used for measuring distance to the surrounding objects . the addition of acoustic rangefinders 67 affords more comprehensive coverage than when using only ir - led rangefinders 66 . the two - way wireless data link of the robot scout is preferably a radio - frequency rf data link . it comprises a rf uplink 68 for communicating data to umd 10 , and an rf downlink 69 for communicating data , including video data , from the umd . a commercially - available receiver for this purpose may weigh as little as 12 grams for a range of over 2 kilometers . a commercially - available video transmitter may weigh as little as 14 grams for a range of over 4 kilometers , providing that a line - of - sight exists between the transmitter and receiver . a video camera 70 , preferably a ccd type , serves to provide : a ) a close - up viewing of the disaster site which can be displayed to remote operator 40 ; b ) a visual sensor for visual positioning , navigation and obstacle avoidance . similar arrangements are described in : a ) movarec , hans p ., “ robot rover visual navigation ”, umi research press , ann arbor , mich ., 1981 , pp . 49 - 147 ; b ) robert , luc , et . al ., “ applications of non - metric vision to some visually guided robotic tasks ”, in aloimonos , yiannis , ed ., “ visual navigation — from biological systems to unmanned ground vehicles ”, lawrence erlbaum associates publishers , mahwah , n . j ., 1997 , pp . 89 - 134 ; c ) weng , j . j ., et . al .,“ visual navigation using fast content - based retrieval ”, in aloimonos , yiannis , ed ., “ visual navigation - from biological systems to unmanned ground vehicles ”, lawrence erlbaum associates publishers , mahwah , n . j ., 1997 , pp . 178 - 217 ; d ) dean , thomas , et . al ., “ planning and navigation in stochastic environments ”, in aloimonos , yiannis , ed ., “ visual navigation — from biological systems to unmanned ground vehicles ”, lawrence erlbaum associates publishers , mahwah , n . j ., 1997 , pp ., 251 - 274 . the invention is , of course , not bound by these arrangements . in practice , flood lights may be added to the umd in order to provide acceptable light conditions for the camera , especially in indoor situations . an uncooled infra - red camera 71 may be used for poor light situations , as well as a hot spot detector . for situation monitoring missions , such as for finding missing people in ruined buildings use may be made of microphones 72 . acoustic signals received by the microphones 72 are conveyed to operator 40 at the remote station via the rf downlink 69 . a smoke detector 73 provides means to detect sources of smoke and smoke - generating situations . a gas detector 74 serves to detect gas contamination , especially in areas of high and dangerous gas concentration . the legs of umd 10 may be equipped with leg load sensors 75 for controlling the multi - legged walking . as an alternative , measuring the current at the leg servo motors may provide the necessary control information . a rotor control function 76 provides the command signals necessary to control rotor motion . a vane servo actuators function 77 provides the command signals to control vanes 15 . a leg servo actuators function 78 provides the command signals for the plurality of leg actuators . a sensor payload servo actuator 79 provides the command signals to control the payload servo . a device release actuator 80 is used to produce the command signal to the device release actuator when unattended sensor means 46 has to be deployed . power supply 81 supplies all of the electrical power consumed by all onboard units . for this purpose use may be made of a bank of lithium batteries . [ 0107 ] fig7 is a diagram state graph notation of the main operational and mobility modes of umd 10 and of the transitions between these modes , in accordance with one embodiment of the invention . a notation of state is assigned to each mobility mode , as well as to start and standing situations . the following states constitute , by this embodiment , the state graph : a ) system non - active 89 ; b ) system preparing 90 ; c ) standing 91 ; d ) vtol — vertical take - off / landing 92 ; e ) hovering 93 ; f ) transitioning 94 ; g ) dash flying 95 ; h ) walking 96 . in fig7 states 92 through 95 are air mobility states and state 96 is a ground mobility state . prior to the mission , and after completing the mission , the power is preferably off , and umd 10 is then in its system non - active state . upon receiving an on command oncmd 99 from operator 40 via the data link , the state of umd 10 is transitioned to system preparing state 90 . on entering the system preparing state 90 , a built - in - testing (“ bit ”) procedure is automatically initiated . if the bit result is ok , and the mission plan has been downloaded correctly , the condition systemready 100 is logically true , and the state of umd 10 is transitioned to standing state 91 . but if the bit procedure failed , bitfailed condition 112 is true . or in case operator 40 sends a mission abort command abortcmd 112 , the state of umd 10 is transitioned to system non - active state 89 and the umd 10 power is off . depending on the specific phase of the mission , when in standing state 91 , various unm functions may be active , as required . for example , umd 10 when in the standing state 91 may be in a waiting situation , in a data gathering situation , or in a sensor means 46 deploying situation , or in a combination of these situations . upon receiving a takeoffcmd 101 , und 10 is transitioned from standing state 91 to vtol state 92 , starting to take - off . if flying conditions do not exist , the umd is either in a staying or standing state 91 or is transitioned to walking state 96 . while in vtol state 92 , unm 10 is transitioned to hovering state 93 when its altitude approach the desired hovering altitude , the condition hoveringaltitude 102 is then logically true . umd 10 keeps hovering until one of the two following conditions is met : a ) conditions for dash flight exists , condition dashconditionsok 103 is true and umd 10 is then transitioned to intermediate transition state 94 ; b ) a landing command landindcmd 107 was issued , either by remote operator 40 , or internally by its mission controller , and umd 10 is transitioned to vtol state 92 , starting to land . when the umd 10 is touching down a supporting surface , condition touchdown 108 is true , and the unm 10 is transitioned to standing state 91 . upon transitioning from hovering state 93 , to transitioning state 94 , unm 10 is then performing a transitioning maneuver , in which the condition transtodashcompleted 104 is true , and unm 10 then enters the dash flying state 95 . as long as the conditions for flying in a dash flying mode exists , unm 10 remains in this state . if these conditions cease to exist , condition dashconditionsout 105 is true , and umd 10 is transitioned to the temporary transitioning state 94 . upon completing the transitioning maneuver , condition transtohovercompleted 106 is true , and umd 10 is transitioned to hovering state 93 . the transition from an air mobility mode to a ground mobility mode and vice versa , is always carried out by first going to standing state 91 , and thereafter to the desired mobility mode , either ground or air . while in standing state 91 , upon receiving a walkingcmd 109 , umd 10 is transitioned to walking state 96 . the walkingcmd 109 is issued either by remote operator 40 , or internally by the umd mission controller . when in the walking state 96 , und 10 is keep walking unless it comes to the desired destination , atlocation condition 110 is true or stop command stopcmd 110 is issued either by remote operator 40 or internally by the umd mission controller . a situation which is typical for the internal issuance of a stopcmd 110 is when umd 10 encounters a large obstacle while walking . when umd 10 is in standing state 91 , an off command offcmd 111 will transit the umd 10 state from standing state 91 to system non - active state 89 , and umd 10 power will shut - off . offcmd 111 is issued either internally by the umd 10 mission controller or by the remote operator 40 . upon completing the mission , offcmd 111 is usually issued internally . [ 0114 ] fig8 ( a ) shows the layout of a building interior section , while fig8 ( b ) is its associated graph - based data structure representation ( according to one possible variant ), termed local feature map — lfm . by this example , fig8 ( a ) is a layout of a building section consisting of : a ) two corridors c 1 - 121 and c 2 - 122 ; b ) a corner cr 12 120 which connects the two corridors ; c ) four rooms r 1 123 , r 2 124 , r 3 125 , and r 4 126 which are accessed from the corridors through openings ; d ) the following openings : o 1 127 between corridor c 1 121 and room r 1 123 ; o 2 128 between corridor c 1 121 and room r 2 124 ; o 31 and o 32 both between corridor c 2 122 and room r 3 125 ; o 4 131 between corridor c 2 122 and room r 4 126 . [ 0115 ] fig8 ( b ) is an example of the associated local feature map — lfm which is used in the present embodiment to represent the essential features of the building section layout . the data structure which is used to represent the lfm is a non - directional graph ( see even , s ., “ graph algorithms ”, computer science press , maryland , usa , 1979 , for more details on non - directional graphs ). referring now to fig8 ( b ), the root node of the graph is the comer cr 12 140 . it has two associated daughter nodes , corridor c 1 node 141 and corridor c 2 node 142 . the connecting arcs 147 and 148 symbolizes the connection between the comer cr 12 and its connected corridors c 1 and c 2 . corridor c 1 node 141 has two associated daughter nodes namely , room r 1 node 143 and room r 2 node 144 . the connecting arcs 149 and 150 symbolize the associated openings o 1 149 and o 2 150 respectively . similarly , corridor c 2 node 142 has two associated daughter nodes namely , room r 3 node 145 and room r 4 node 146 . the connecting arcs 151 , 152 and 153 symbolizes the associated openings o 31 151 and o 32 152 and o 4 153 , respectively . whenever the layout of the buildings to be monitored by the umd 10 is known a - priori , the associated lfms can be prepared in advance . it should be noted however , that although an lfm is possibly prepared a - priori , during a major disaster , such as an earthquake , so many changes may occur that the original lfm may no longer represent the actual layout . while there has been disclosed a preferred embodiment of a umd functioning as a robot scout , it is to be understood that many changes may be made therein without departing from the scope of the following claims : | 1 |
fig1 shows a front end loader 1 having a bucket 2 which can be raised and lowered by conventional mechanism 3 operated by cylinders 4 . attached to the bucket 2 is a snow plough accessory 5 , the details of which are shown in fig2 and 3 . as best seen in fig3 a snow plough blade 6 has rigidly attached to its rear face a semicircular beam 7 . radiating from the centre of the semicircle defined by the beam are angular portions 8 of a blade - supporting frame 9 . the frame 9 and blade 6 are pivotally connected by means of a bolt or pin 10 which passes vertically through the frame and through brackets 11 fixed to the blade midway along its length , whereby the blade can swing horizontally relative to the frame . the beam 7 is slidably supported on the radial portions 8 of frame 9 , the beam passing through guides 12 fixed to the radial portions 8 . the radial portions 8 constitute the forward portions of a pair of beams 13 which have parallel rearward portions 14 . pivoted on these rearward portions are brackets 16 which carry hydraulic cylinders 17 . piston rods 18 of the cylinders are pivotally connected at 19 to the semicircular beam 7 . the action of cylinders 17 can be remotely controlled through hoses 21 that can quickly be coupled to lines ( not shown ) running to the operator &# 39 ; s cab 22 , whereby the blade 6 and beam 7 can be swung horizontally about the pivot pin 10 . secured to the undersides of the parallel portions 14 of beams 13 are rearwardly facing angle irons 23 . with the beams 13 these angle irons define rearwardly facing channel structures which receive the lower lip 24 of the bucket 2 . the beams 13 have , at their rearward ends , abutments 25 with forwardly facing surfaces 26 which engage rearwardly facing surfaces 27 of corresponding abutments 28 fixed to the bottom of the bucket 2 . final securement of the frame 9 to the bucket is achieved by a connector arm 29 , which is pivotally connected to the frame 9 about a horizontal pin 30 near the vertical pin 10 , the arm 29 being connected at 31 to an upper part of the bucket 2 by a simple hook or pin connection . the arm 29 may be of adjustable length . angle iron brackets 32 are attached to the rear face of blade 6 to engage bottom corners 33 of the bucket 2 when blade 6 is fully angled about pivot pin 10 . brackets 32 , when thus engaged , serve as bumpers which assist in absorbing any sudden shock which might occur during a ploughing operation , thereby alleviating to some extent stress on cylinders 17 and frame 9 . the snow plough accessory 5 can quickly be attached to the bucket 2 by the operator of the front end loader , working alone . the operator drives the loader to maneuver the lip 24 of the bucket under the frame 9 of the accessory . as he slides the lip 24 forwardly under the frame he lifts the bucket slightly to tilt the frame so that the abutments 25 can pass over the abutments 28 on the bucket , and when the bucket lip 24 enters the channel structure 23 he allows the abutments 25 to drop or hook behind the abutments 28 so that the beams 13 rest on the bottom of the bucket . then he engages the connector arm 29 with the upper portion of the bucket at 31 , and connects the hoses 21 to the abovementioned lines running to his cab . with the accessory connected to the bucket , the lower lip 24 pushes against the channel structure at 23 during a ploughing operation . when the loader is backing up , the connector arm 29 prevents the rear of the frame 9 from lifting and therefore engagement of the abutments 28 , 25 draws the accessory rearwardly . the blade can be swung horizontally by actuating the cylinders 17 from the driver &# 39 ; s cab 22 . the accessory can be lifted upwardly by raising the bucket , if it is desired to push the top of a pile of snow , or the bottom of the blade 6 can be raised over the top of a pile and then lowered so that the top of the pile can be pushed either forwardly ahead of the blade or rearwardly behind it . thus , the blade is highly maneuverable , and the operator has good visibility . snow may also collect in the bucket and be lifted and dumped because there is ample clearance between the blade 6 and bucket 2 . when the bucket is lifted , the forward lip 24 of the bucket is held in the channel structure by the beams 13 which form upper horizontal legs of the channel structure , and similarly the bottom portions of the angle irons 23 form lower legs of the channel structure , preventing separation of the bucket from the accessory . relative forward and rearward movement of the bucket and the accessory is prevented by the engagement of the bucket in the channel structure and by the abutments 25 , 28 . however , it is a simple matter to disconnect the accessory from the bucket by disconnecting the hoses 21 , undoing the connection 31 , and then tilting the bucket so that the abutments 25 , 28 are disengaged and the bucket can be withdrawn from the channel structure . referring to fig4 and 5 , a variant of the snow plough accessory may be used for attachment to a log grapple 40 of a front end loader . the blade 6 and frame 9 may be identical to those already described . the parallel rearward beam portions 14 are open ended thereby providing channel structure into which are inserted lower arms 41 of a conventional log grapple 40 . the frame 9 is secured to the grapple 40 by an adjustable connector arm 29 , pivotally connected at 30 to the frame 9 , the arm 29 being connected at 42 to an upper part of the grapple by a simple hook or pin connection . the grapple has a conventional upper arm 43 that can be remotely controlled by a cylinder 44 , the lower arms being connectable by eyes 45 to the manipulation mechanism 3 of the front end loader . the snow plough accessory can be quickly attached to the log grapple simply by maneuvering the lower arms 41 into the channel structures defined by beam portions 14 , and then engaging arm 29 with the upper portion of the grapple at 42 . hoses 21 of cylinders 17 are connected to lines running to operator &# 39 ; s cab 22 by means of quick coupling devices . said hose lines may be disconnected from cylinder 44 , thus freeing them for use in operating cylinders 17 . with the accessory connected , the lower arms 41 push against the channel structure at 48 during a ploughing operation . the length of the channel structure and the attachment of arm 29 prevents disengagement of the accessory when the loader is backing up . the blade 6 is fully functional as described when attached to a bucket . the accessory may be easily disconnected simply by reversing the connection steps outlined above . modifications to the preferred embodiments will readily occur to those skilled in the art . | 4 |
the light and proprietary ( lp ) embodiment of the present invention exploits smart messages that may be implemented as bearer - independent objects ( bio ), or exploits unconfirmed wireless access protocol ( wap ) push messaging . according to the alternative heavy and open ( ho ) embodiment , implementation is accomplished according to syncml device management . syncml dm is very memory - intensive , and many terminals will not be able to support this feature . if a mobile terminal already supports syncml dm then this may be the most efficient of the two alternative preferred embodiments . referring now to fig1 , this flow chart illustrates a method according to an embodiment of the present invention . the user input 102 a mobile terminal identifier ( which may be as simple as a telephone number ), plus a personal identification code that is different from a pin used to operate the mobile terminal , and the user enters these inputs at a location separate from the mobile terminal , which has presumably been lost , misplaced , stolen , or the like . an attendant then receives 104 these user inputs entered in step 102 . the attendant may be automated or human or both , and typically would be linked to the user by a telephone connection . the attendant will determine 106 whether the mobile terminal employs synchronization markup language device management . if so , then the attendant will send 108 a guard message using synchronization markup language dm , and will do so repeatedly until the guard message is acknowledged ( this is the ho embodiment ). however , if the mobile terminal does not employ synchronization markup language dm then the attendant will send 110 the guard message , repeatedly if necessary , using either wap push messaging or smart message bio ( this is the lp embodiment ). the mobile terminal will then authenticate 112 the guard message , which of course could entail verifying the non - operational pin entered in step 102 . if the guard message is authenticated , then the mobile terminal will lock communication and secure data 114 . this will not necessarily completely prevent communication from the mobile terminal , but it will at least greatly restrict it , while also making stored data less accessible . especially sensitive data ( or all data ) may be deleted , although the user may request that the sensitive data first be uploaded with encryption to the attendant ( for safekeeping or transfer to the user ), prior to its deletion from the mobile terminal . a thief might try to remove a battery , or otherwise deprive the mobile terminal of power , in order to ensure that the mobile terminal cannot respond to any guard message , and cannot reveal its location . therefore , a user may purchase a mobile terminal that is equipped with a small emergency power unit that cannot be easily removed ; that small emergency power unit can provide sufficient power for the mobile terminal to respond to the guard message by at least locking communication and securing data , if not by uploading data that is subsequently secured ( e . g . deleted ). regarding message construction , in the lp embodiment , the message content required for terminal format or lock includes push message identifiers : generic push port and meta data ( e . g . secfl ). the message content also includes a function : & lt ; format & gt ; and / or & lt ; lock & gt ;. and , the message content includes the international mobile station equipment identity : & lt ; imei code & gt ;. additionally , the message content includes the user personal pin : & lt ; 4 - digits , not same as sim pin & gt ;. the message format could be , for example , extensible markup language ( xml ) or wireless binary extensible markup language ( wbxml ) depending upon the selected solution configuration . referring now to fig2 , this is a block diagram of a mobile terminal 200 according to an embodiment of the present invention . the transceiver 202 receives a guard message 204 which it passes along to an authentication unit 206 . upon authenticating the guard signal 204 , the authentication unit provides an authentication signal 208 to a data securing mechanism 210 as well as to a communication locking mechanism 212 . in response to the authentication signal 208 , the data securing . mechanism 210 secures at least some of the data in a data storage unit 216 , for example by deleting that data after encrypting and uploading the data via the transceiver 202 . the communication locking mechanism 212 will respond to the authentication signal 208 by sending a disabling signal 214 to the transceiver , so as to completely or partially disable the transceiver ( e . g . by barring the transceiver from communicating with any phone number except an emergency number ). turning now to fig3 , this is a high - level architecture of the light and proprietary ( lp ) embodiment of the present invention . regarding requirements for the client and server software in the lp embodiment , the client software 310 allows the user to enable a remote format and lock service from the user interface of his terminal , including entry of the user personal pin . the terminal software is subsequently executed when a new message is received with appropriate meta information ( e . g . secfl to push port ). no user interface should be displayed when the new message is received , because an unauthorized person may be observing the user interface . when the new message is received , then the software verifies the imei and user personal pin . if those are correct , then the terminal software executes functions requested by the content of the new message . regarding the server software 302 in the lp embodiment of the present invention , the server has a database that includes imei information of users &# 39 ; terminals . the server software has an application programming interface ( api ) with a short message service center ( i . e . an smsc 306 such as a cimd - type of smsc ). an attendant , such as an information technology ( it ) staff person in the user &# 39 ; s company or a telephone operator of a wireless service provider , is able to construct the message that will be sent to the lost or stolen mobile terminal , using the imei and pin that are told by the user to the attendant . then the message will be sent to a number that is in the database ( db ) with the imei , via the gsm network 308 . this functionality could be easily built inside a manufacturer management system , integrated with other it management systems , or implemented separately . regarding the heavy and open ( ho ) embodiment of the present invention , the same functionality as the lp embodiment can be achieved by exploiting synchronization markup language ( syncml ) device management ( dm ). it is to be understood that all of the present figures , and the accompanying narrative discussions of best mode embodiments , do not purport to be completely rigorous treatments of the method , terminal , and system under consideration . a person skilled in the art will understand that the steps and signals of the present application represent general cause - and - effect relationships that do not exclude intermediate interactions of various types , and will further understand that the various steps and structures described in this application can be implemented by a variety of different sequences and configurations , using various different combinations of hardware and software which need not be further detailed herein . | 6 |
hereafter , description of the invention will be made with reference to the articulation of the hip . however , the invention is not limited to this illustrative example and the person skilled in the art will easily transpose this description to any other articulation partially formed by a bone head , such as the shoulder . some critical anatomical elements are necessary to measure some specific anatomical characteristics of the proximal femur , such as the femoral neck version angle , and the amplitude of the head - neck junction bump deformation measured by the alpha angle , which participates in the characterization of the proximal femur deformity in femoro acetabular impingement ( fai ) pathology . the method is described by specifically addressing the femur but it can be extended to other bones of the human or animal body such as the humerus or other bones having a rotoid articulation . the general purpose of the invention is to determine from the 3d image of the bone , major parameters for characterizing a bump deformation on the head - neck junction of the bone , in a fast , precise and reproducible manner . the method detailed hereafter has to be understood as an algorithm implemented in the form of a software program on a processing unit . the head of the bone is assumed to have a spherical portion and the neck is assumed to have roughly a diabolo shape . the deformation of the bone consists in the formation of a bump at the head neck junction , generally in a location where there are repetitive collisions between the femur and the acetabulum during hip motion . as described earlier , the characterization of the anatomy is based on the measurement of the neck version angle , and the characterization of the deformation is based on the measurement of the alpha angle , in one or several 2d slices in the 3d image volume . in standard practice , the determination of those characteristic elements of a bone are performed manually by the radiologist in the 3d image , using interactive software tools that rely mostly on reformatted 2d images in the 3d image volume . working on 2d images for determination of 3d geometric elements leads to errors . interactive software using a mouse is also prone to human errors . and in all cases , such determination is time consuming . in order to compute accurate characteristic anatomical values for the femoral bone features such as the neck version angle , and the alpha angle in three dimensions , the computations need to be based on the precise determination of the following reference anatomical elements : the femoral head sphere center and radius , the femoral neck axis , the clock face on the femoral head , and the knee rotation axis . the purpose of the invention is to describe a method of automatic and accurate determination of the characterization values of the femoral anatomy deformity very quickly , based on of those critical geometric elements from the 3d image . as illustrated in fig1 , a 3d medical image examination of the patient is performed in order to provide a 3d image of the hip bones using a specific predefined protocol as initial input to the method . as an example of medical image examination , a computer tomography ( ct ) examination can be performed . in addition to the conventional 3d image acquisition protocol for the hip , our method requires the acquisition of a few extra images at the level of the knee . the 3d image is represented by a stack of parallel 2d images , with known relative positions . the acquisition of the 3d image is a preliminary step that can be directly included in the method of the invention or carried out previously . the method is implemented as image processing software running on a standard computer . the user can interact with the software by a standard user interface medium like a mouse , touch screen or the like . images are displayed on the monitor of the computer . at the beginning , the software is used to select and load the 3d image of the specific patient . as shown in fig1 , the method contains successive steps , using as input the 3d image of the bone , and producing as output the indices characterizing the bump deformation of the head - neck junction of the bone . the first two steps ps 1 and ps 2 are preliminary steps necessary for the method of the invention but they are not in the scope of the invention itself . therefore the first two steps are not described in full details , but only examples of their implementation and the resulting elements from these steps are described . the first preliminary step ps 1 of the method consists in creating from the 3d medical image of the bone , a 3d surface model of the bone surface s as illustrated in fig2 . in the case of ct image , a thresholding process is used to determine an initial surface model by comparing each value of the 3d image point to a predefined threshold value in hounsfield units representing cortical bone , and retaining points that have a value close to the threshold value , “ close ” generally meaning within a range of + 10 % and − 10 % from the threshold value . it generates multiples binary objects defining connected components in the space of the 3d image . additional processing using well known mathematical morphology operators is applied to those binary objects to eliminate small connected components and to fill the inside of closed surfaces so that only the external surface of the bone remains . however , the generated surface model s is usually not perfect since the thresholding tends to merge the bone surface with adjacent bones and to create some defects in the surface . those imperfections are due to many phenomena including the quality of image acquisition and reconstruction , but also to the poor quality of bone density in some pathological areas . similar conventional methods such as the marching cube or the dividing cube can be applied to build a surface model of the bone . in the following , the surface of the bone reconstructed from the 3d image is referred to as the 3d surface model . the 3d surface model comprises different portions of anatomical surfaces , including the head surface and the neck surface . the next preliminary step ps 2 starts by the identification in the 3d surface model a sphere s f fitting the spherical portion of the head of the bone as illustrated in fig2 . several methods exists for computing that sphere sf , from fully manual identification of circles in at least two orthogonal 2d reformatted slices selected so as to pass through the head to fully automatic iterative methods , converging to the best fitting sphere , thus providing a 3d head center point h and a radius r . one example of a method for the determination of the sphere s f is to apply an iterative method based on the identification of an approximate head center point and an approximate radius , and then applying robust least - square fitting of a sphere to the 3d surface model points , starting from the approximate head center point and the approximate radius . the result is the determination of the head center point h and the radius r of the sphere s f . secondly , from the detected head center h , it is necessary to identify the 3d neck axis ax , characterizing the orientation of the neck of the bone . again , several methods can be applied , from manual identification of lines in at least two orthogonal 2d reformatted slices selected so as to pass through the neck , to fully automatic iterative methods . one example of an option for the detection the neck axis ax is illustrated in fig3 a and 3b . it consists in applying an iterative method based on the identification of an approximate axis ax 0 passing through the head center h and then applying a minimization process in two orthogonal cross - sections of the 3d surface model passing through ax 0 . in each section , the process is to adjust the position of ax 0 in order to minimize the distances from ax 0 to the contours of the neck portion in the cross - section of the 3d surface model . as illustrating in fig3 a and 3b , the closest points a i and a ′ i of the contours of the neck portion on each side of the axis ax 0 are computed in both cross - sections . the minimization process consists in adjusting the position of ax 0 in both cross - sections in order to minimize the distance of the points a i and a ′ i to their respective orthogonal projection on ax 0 . the resulting axis is the neck axis ax . finally , once the femoral head sphere s f with its center h and the femoral neck axis ax have been determined , a 3d mechanical femur coordinate system is constructed from the femur head center h , the knee center k and the knee transverse axis ml that joins the points m and l which are the medial and lateral epicondyles of the knee or that joins the most posterior points of the knee condyles . these last two anatomical elements are determined from 3d images acquired at the level of the knee joint as shown in fig4 a . from these images , the knee center point k is determined . it is easy to find the centroid of these images after appropriate thresholding and compute an initial knee center k 0 . from that point , a rectangular box is computed around k 0 in the axial image plane containing k 0 , such box being adjusted to be the smallest in contact with surface points detected on the bone . the center of the rectangular box becomes the estimation of the knee center k 1 . to refine even more the location of the knee center , it is further possible to extract the femur medio - lateral axis mle as being the epicondylar axis in the knee 3d image . the epicondyles points e 1 and e 2 can be automatically detected by searching for example the two most distant bone points in the rectangular box computed above , passing within a given range of the knee center point k 1 . other algorithms can be used to detect the epicondylar axis . once this mle axis has been determined , the knee center point k can be defined as the middle of the mle segment . in another embodiment , a medio - lateral axis that we can extract is the postero - condylar axis mlp . it can be extracted using iterative methods to search for the most posterior points in the axial images of the knee . from all these anatomical elements , the femur coordinate system is constructed as follows : its origin is centered on the femoral head center h , the xf axis is defined by the vector hk , the zf axis is defined as the vector product of xf by ml , and the y f axis is defined as the vector product of z f by x f . it is then possible to measure the neck version angle , which is the neck axis orientation relatively to the ml axis in the axial plane of the femur coordinate system , which is an important element to be taken into account in the analysis of the whole case for decision of the surgical treatment . it is possible to use directly the 3d image referential to orientate the 3d mechanical referential , though assuming the position of the patient during the exam can be controlled to meet expected mechanical orientation . in further description , the anatomical directions are defined from the axes of the 3d mechanical referential and of the neck as follows : [ a ] superior - inferior direction is orientated along x f , [ b ] medial - lateral direction is orientated along y f , [ c ] posterior - anterior direction is orientated along z f , [ d ] and proximal - distal direction is orientated along the neck axis , in the direction from the head center h down to the neck . the next step s 3 of the method consists in mapping automatically on the 3d surface model of the head of the bone , a clock face referential system , which has clinical significance when addressing bones with a head portion . as shown in fig5 a and 5b , the clock face is a radial referential system representing 12 hours angular segments commonly used by surgeons to identify location of points on the femoral head surface . the clock face can be fully determined by determining the location of the 12 o &# 39 ; clock plane p 12 h . successive rotations of this plane around the neck axis ax will then define the 1 o &# 39 ; clock , 2 o &# 39 ; clock , and followings , until 11 o &# 39 ; clock location . as shown in fig5 a , our method consists in determining the position of the 12 o &# 39 ; clock plane p 12 h , as the location of the most superior portion of the intersection line of the 3d surface model and the plane passing through the neck axis ax and the knee center point k determined by the method defined previously . it provides a fully automated determination of the clock face from the 3d image . once the clock face has been determined on the femur , the goal is to characterize the femur bump deformation by superimposing the 3d femoral head sphere sf and the femur 3d bone surface model in order to locate and quantify the 3d curve where the two surfaces intersect . the next step s 4 of the method consists in determining automatically the 3d curve characterizing the head - neck junction of the bone . to determine the 3d head - neck junction curve , series of hemi - planes pi passing through the head center h and around the neck axis ax are computed in the 3d image volume , as shown in fig5 b . those hemi - planes pi are identified by a clock index i , starting at 12 o &# 39 ; clock . in a preferred embodiment , hemi - planes pi are computed every hour around the clock . but it could be also every half hour or even more precisely . one of the difficulty of this step is that the 3d surface model of the head neck junction represents an imperfect surface , and local small deviations generated by artifacts during the surface reconstruction can lead to an erroneous determination of the 3d curve . as shown on fig6 , for each plane hemi - plane pi around the neck axis ax , for all indexes i in the clock face ( i = 12 , 1 , 2 , . . . 11 ), the intersection of the femoral head sphere sf with the hemi - plane pi is computed producing a circle ci overlaying the intersection of the 3d surface model with the hemi - plane pi producing a contour of the femoral head fci . now for each hemi - plane pi , a point mi on the contour fci corresponding to the location where the contour fci deviates outside of the circle ci is computed according to the following description : a femoral head apex point ap is defined as the intersection point between the femoral neck axis ax and the circle ci opposite to the neck . the point mi is determined in the following manne : the closest point from the femoral head apex ap which is lying on the contour fci and which is lying outside the circle ci , over a given threshold distance td , and which neighbour m ′ i further down along the contour fci in the direction of the neck is also lying outside the circle ci . such a threshold distance td is generally set between 0 . 5 mm and 1 mm and it must be below 2 mm to provide accurate results . the neighbour m ′ i along the contour fci is generally considered up to a maximum distance of 2 mm for mi . this point mi is considered as the head - neck junction point of the bone in the hemi - plane pi . in one embodiment of the method , the process for detecting the point mi complying with the above conditions is illustrated in fig7 and is carried out automatically in the following manner : starting from the apex point ap , a point mij ( wherein j is an integer greater than 1 of an index position of an angle between 0 ° and 180 °) is following the contour of the femoral head in the direction of the neck . if a first point mi 1 lying outside the circle ci is detected . however , if its distance from the border of the circle ci is smaller than the threshold distance td , mi 1 is discarded and the point mij continues its path on the femoral head contour in the direction of the neck . if a next point mi 2 lying outside the circle ci is detected , which distance from the border of the circle ci is equal to or greater than the threshold distance td , then its neighbour m ′ i 2 on the contour of the femoral head in the direction of the neck is also tested . if m ′ i 2 is lying outside the circle ci but its distance from the border of the circle ci is smaller than the threshold distance , then mi 2 is also discarded and the point mij continues its path on the femoral head contour in the direction of the neck . if a next point mi 3 lying outside the circle ci is detected , which distance from the border of the circle ci is equal or greater than the threshold distance td , then its neighbour m ′ i 3 on the contour of the femoral head in the direction of the neck is also tested . if m ′ i 3 is lying outside the circle ci at a distance from the border of the circle ci greater than the threshold distance td , then the point mi 3 is selected to be the point mi searched for . this process avoids detecting small local bumps which might come from the imperfection of the reconstructed 3d surface model , and insures to take into account only the actual bump of the head - neck deformation when determining the 3d curve of the head - neck junction . in another embodiment of the method , the neighbour test described previously can also be performed in the orthogonal direction to the hemi - plane pi , the neighbours being then located on the 3d surface model , on both sides of the contour fci , thus reinforcing criteria for the detection of an actual bump in 3d and not only in 2d . in another embodiment of the method , the position of the detected point mi in the hemi - plane pi on the contour fci can be further adjusted in order to comply with a continuity constraint with point mi + 1 and point mi − 1 respectively detected on the contours fci + 1 and fci − 1 in the hemi - planes pi + 1 and pi − 1 . in order to anticipate on the smoothness of the final 3d curve created from all mi points , it is possible to adjust the position of the central point mi in a triplet of contiguous points ( mi − 1 , mi , mi + 1 ) for all points mi , by minimizing the sum smi of the distances from mi − 1 to mi , and mi to mi + 1 . the point mi is therefore adjusted into the point ni , where ni is lying on the contour fci , outside the circle ci , within a distance less or equal to the threshold td and such that the sum sni of the distances from mi − 1 to ni , and ni to mi + 1 is smaller than smi . as shown in fig8 , when all the points mi have been determined in the successive pi hemi - planes around the clock , linking all points mi around the femoral head surface determines a 3d curve 1 . in one embodiment of the method , the linking of the points mi can be performed using straight linking segments between contiguous points mi , thus creating a 3d pecked line . in another embodiment , a minimal 3d curve can be determined by fitting a 3d spline curve of minimal length , interpolating contiguous mi points . now in each hemi - plane pi , the 2d alpha angle ai which is a common index used for characterizing the femoral head - neck junction is automatically computed as the angle between the hemi - line from the femoral sphere center h and in the direction of the neck axis ax and the hemi - line from femoral sphere center h and the point mi as shown in fig6 . the 3d curve passing through the mi points is then referred to as the 3d alpha curve . as illustrated in fig9 , and as a synthesis from the steps described above , from all the 2d alpha angles αi , a 3d alpha angle α3d is determined as the maximum value amongst the 2d alpha angles αi . the corresponding point mi determines the summit of the head - neck junction curve characterizing the bump deformation and is referred to as the maximum point mmax and the corresponding clock index as the maximum index imax . the maximum α3d angle is a first parameter that characterizes the 3d bump by quantifying the “ amount ” of the bone deformity . the maximum clock index imax is a second parameter that characterizes the 3d bump by giving its location on the clock face . the 3d alpha curve and the pair of indices ( α3d , imax ) then fully characterize the femoral head - neck junction bump deformation . together with the neck version measurement described previously , the parameters characterizing the bump will enable the surgeon to decide of the most appropriate surgical treatment . the advantage of the invention is the precise , and automatic determination of characteristic elements quantifying and locating the deformation of the head - neck junction of a bone in a 3d image requiring the least possible input from user interaction . from the determination of these elements , it is then possible for surgeons to decide on the most appropriate surgical treatment . usually those characterization measurements are performed manually by a radiologist , which takes time and efforts and is prone to human errors or inaccurate measurements , and potentially misleading the choice of surgical treatment . our method provides then a fast and more reliable process to perform these measurements during the analysis of the pathology . | 6 |
the inventors have found that lysocellins , ( including its salts or esters ) are effective for controlling various plant parasitic mites and the mechanism for controlling the plant parasitic mites has a special characteristic . it has been found that lysocellins are effective for controlling imagines , larvae and ova of mites as the conventional miticides and for preventing ecdysis of larvae to cause mortality and for sterility by a treatment with a dilute concentration remarkably lower than the usual concentration for mortality . the present invention has been attained by said finding to provide a miticidal composition comprising lysocellin , its salt or ester as an active ingredient . lysocellin is an antibiotic having excellent antibial activity which is isolated from a fungus body and medium which is cultured from streptomyces and has the formula ## str3 ## the active ingredient of the miticidal composition of the present invention can be lysocellin in free form , or its carboxylic salts such as sodium , potassium , calcium , magnesium or ammonium salt or its esters for hydroxyl group at 21 - position , preferably acetyl ester . two or more active ingredients can be also used . the parasitic mites which are controlled by the miticidal composition of the present invention include plant parasitic mites , spider mites such as citrus red mite , european red mite , kanzawa spider mite , two - spotted spider mite , carmine mite , sweet cherry spider mite , clover mite , sugi spider mite , sourthern red mite , smith spider mite and rust mite , red mite , root mite , and animal parasitic mites such as house mite , rickettsia orientalis , hair mite , powder mite and dust mite , etc . the miticidal compositions of the present invention can be in the form of an emulsifiable concentrate , a suspension , an aqueous solution , a wettable powder , a dust , an oily solution , an aerosol smoking composition . these miticidal compositions can be prepared by desired methods . the carriers can be natural or synthetic organic or inorganic compounds . suitable solid carriers include inorganic carriers such as clay , talc , mica , agalmatolite , vermiculite , gypsum , calcium carbonate , diatomaceous earth , zeolite , bentonite , fine silica and anhydrous silica ; organic carriers such as saw dust , wheat powder , soybean powder , starch , alkyd resin , polyvinyl chloride , ester rubber and urea . suitable liquid carriers include water , ketones , alcohols , esters , ethers , aromatic and aliphatic hydrocarbons , chlorinated hydrocarbons , and polar solvents such as dimethylformamide and dimethylsulfoxide . it is possible to incorporate a nonionic , anionic , cationic or ampholytic surfactants with said carrier depending upon the form , for a purpose of an emulsification , a dispersion or a wetting . the miticidal composition of the present invention can be used together with the other ingredient such as fungicides , insecticides , herbicides , plant growth regulator , other miticides , fertilizers , external preparations for animals repellents , etc . the miticidal compositions of the present invention are applied by a soil treatment , a foliage application , a spray application in animal cages and fowls cages , and coating on external part of an animal etc . at suitable ages of larvae , ova and imagines of mites depending upon the purpose of the application . suitable dose of the active ingredient of lysocellin ( including its salt or ester ) is depending upon the object mites and applications and is usually in a range of 1 to 1000 g . preferably 10 to 100 g . of lysocellin per 10 ares in the foliage treatment . the purpose can be attained with the similar does in the spray application in animal cages and fowls cages . lysocellin ( including its salt or ester ) can exhibit remarkable miticidal effect as shown in the following experiments and is usually applied as the miticidal compositions . typical examples of miticidal compositions are illustrated . a dust was prepared by mixing 0 . 1 wt . part of lysocellin , 5 wt . parts of fine silica , 30 wt . parts of clay and 64 . 9 wt . parts of talc and pulverizing the mixture . a wettable powder was prepared by mixing 2 wt . parts of lysocellin , 10 wt . parts of fine silica , 50 wt . parts of clay , 35 wt . parts of diatomaceous earth and 3 wt . parts of an emulsifier ( sorpol 4048 : toho chem . ), and pulverizing the mixture . in the application , the wettable powder is diluted with water for the spray . an emulsifiable concentrate was prepared by uniformly mixing 20 wt . parts of lysocellin , 20 wt . parts of isopropanol , 55 wt . parts of xylol and 5 wt . parts of an emulsifier ( sorpol 2680 : toho chem .) to dissolve lysocellin . in the application , the emulsifiable concentrate is diluted with water for the spray . kidney bean seedlings were cultured in a pot having a diameter of about 6 cm . about 30 female imagines of carmine mites ( tetranychus tetrarus ) were positioned on primary leaves at two leaf stage ( two days after germination ). one day later , the damaged mites were removed and the primary leaves were dipped into each solution obtained by diluting the emulsifiable concentrate of composition 3 with water at a concentration of the active ingredient shown in table 1 , for 10 seconds . two days after the treatment with the composition , each mortality of the imagines of the mite was measured . the results are shown in table 1 . table 1______________________________________concentration of mortality oflysocellin imagines ( ppm ) (%) ______________________________________ 10 59100 73500 100______________________________________ about 30 to 40 ova were ovipositioned by imagines of carmine mites , on primary leaves of kidney bean at two leaf stage ( two days after germination ). the imagines were removed . the primary leaves were dipped into each solution obtained by diluting the emulsifiable concentrate of cmposition 3 , with water at a concentration of the active ingredient shown in table 2 , for 10 seconds . eight days after the treatment with the composition , each mortality of the ova and larvae were measured . the results are shown in table 2 . the mortality of the larvae is considered to be caused by the ecdysis inhibition of lysocellin . table 2______________________________________concentration oflysocellin mortality (%)( ppm ) ova larvae______________________________________ 0 0 050 90 . 9 100100 98 . 1 100200 100 100______________________________________ in accordance with the test of experiment 3 , the oviposition was resulted after six days from the position , the primary leaves with the larvae were dipped into a solution containing lysocellin at the specific content of 10 seconds . ten days after the treatment , with the composition , each mortality of larvae was measured . the results are shown in table 3 . table 3 : ______________________________________concentration oflysocellin mortality of larvae ( ppm ) (%) ______________________________________ 5 10010 10020 100______________________________________ in accordance with the process of experiment 1 , 10 female imagines of carmine mites were positioned on primary leaves of kidney bean and the primary leaves were dipped into each solution having each desired concentration of the active ingredient for 10 seconds . ten days after the treatment with the composition , the mortality was measured . the results are shown in table 4 . table 4______________________________________concentration oflysocellin mortality ( ppm ) (%) ______________________________________0 02 . 5 52 . 63 . 75 76 . 95 . 0 66 . 77 . 5 94 . 110 100______________________________________ the primary leaf of kidney bean of experiment 1 was dipped into each solution containing lysocellin at the specific content , for 10 seconds and dried at the ambient temperature . after the treatment , 10 female imagines of carmine mites were positioned on each treated cotyledon to result the oviposition for 3 days , and the mortality was measured five days after the oviposition . the results are shown in table 5 . ______________________________________ concent - ration of lysocellin mortality (%) oviposition ( ppm ) ova imagines______________________________________dipped day 10 65 . 5 100dipped day 100 86 . 7 1003 days after dip . 10 27 . 9 1003 days after dip . 100 93 . 0 1007 days after dip . 10 68 . 1 82 . 57 days after dip . 100 78 . 3 95 . 5______________________________________ | 0 |
the present invention now will be described more fully with reference to the accompanying drawings , in which preferred embodiments of the invention are shown . the present invention may , however , be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein ; rather these embodiments are provided so that this disclosure will be thorough and complete and will fully convey the invention to those skilled in the art . indeed , the invention is intended to cover alternatives , modifications and equivalents of these embodiments , which will be included within the scope and spirit of the invention as defined by the appended claims . furthermore , in the following detailed description of the present invention , numerous specific details are set forth in order to provide a thorough understanding of the present invention . however , it will be clear to those of ordinary skill in the art that the present invention may be practiced without such specific details . in other instances , well known methods , procedures , components , and circuits have not been described in detail as not to unnecessarily obscure aspects of the present invention . fig1 a is a block diagram illustrating functional blocks of one embodiment of the portable device of the present invention and an illustrative operational configuration thereof fig1 a shows a portable device 70 coupled to a host platform 90 . in this embodiment , host platform 90 is coupled to a power supply circuit 80 located in portable device 70 . power supply circuit 80 draws power from host platform 90 and serves as a power source for various components of portable device 70 . referring still to fig1 a , portable device 70 further includes an integrated circuit 10 , a flash memory 20 , a volatile memory 30 and a fingerprint module 50 . integrated circuit 10 can be conveniently implemented as an application - specific integrated circuit ( asic ). in a currently preferred embodiment , flash memory 20 can have a storage capacity between 8 mb and 512 mb , a portion of which can be used to store one or more templates generated in accordance with the present invention as described below . moreover , in a preferred embodiment , the template ( s ) are stored in a reserved area of flash memory 20 which is specifically designated for this purpose and which is not otherwise accessible to the user . additionally , as described in detail further below , a template is encrypted before it is stored in flash memory 20 in a currently preferred embodiment , thereby providing added security against hacking . in one embodiment , volatile memory 30 is external to integrated circuit 10 and can comprise either a dynamic random access memory ( dram ) or a static random access memory ( sram ). among other uses , volatile memory 30 can serve as an initial storage and staging area for a fingerprint image captured in accordance with the present invention . integrated circuit 10 comprises a microprocessor 11 which , in one embodiment , is a risc processor . in a currently preferred embodiment , an authentication engine 12 is included in integrated circuit 10 . authentication engine 12 in turns comprises a template generator 12 a and a verification module 12 b . template generator 12 a is used to generate an encoded version of an image of a fingerprint . within the scope of the present invention , such an encoded fingerprint image is referred to as a template . it should be appreciated that according to current biometrics technology , a fingerprint can be uniquely identified using between 8 and 13 distinct points in the raw image of the fingerprint . fingerprint information can thus be conveniently stored in a condensed fashion as data pertaining to the 8 to 13 relevant data points . a preferred embodiment of the present invention advantageously stores a fingerprint in a compact format as a template referred to above . in this embodiment , a template has a size of 512 bytes . other embodiments can use templates of different sizes . the other component of authentication engine 12 , verification module 12 b , is used to compare a newly generated template against a stored template to validate the authenticity of a fingerprint provided by someone purporting to be an authorized user . thus , authentication engine 12 works in conjunction with fingerprint module 50 , described in greater detail below , to implement user authentication in accordance with the present invention . it should be appreciated that authentication engine 12 is well - adapted to numerous implementations within the scope of the present invention . in one embodiment , authentication engine 12 is implemented as firmware stored in a non - volatile memory within portable device 70 . in another embodiment , authentication engine 12 is implemented as part of microprocessor 11 . in still another embodiment , authentication engine 12 is implemented as a processor separate from microprocessor 11 . in yet another embodiment , authentication engine 12 includes the same components and serves the same functions as described herein , but is located in host platform 90 rather than in portable device 70 . in other words , within the scope of the present invention , authentication engine 12 is not required to reside in portable device 70 . instead , where authentication engine 12 is to be placed is a design choice , thus affording design flexibility to suit different applications in which the present invention can be utilized . referring still to fig1 a , in a preferred embodiment , integrated circuit 10 also comprises a bus interface 13 which facilitates communication between integrated circuit 10 and other components , such as volatile memory 30 . integrated circuit 10 further includes a flash controller 14 for controlling access to flash memory 20 . in one embodiment , upon the successful generation of a template during user registration , flash controller 14 communicates with template generator 12 a to store the newly generated template into flash memory 20 for use in subsequent user authentication . moreover , in a currently preferred embodiment , portable device 70 is compatible with the universal serial bus ( usb ) standard and includes a usb connector ( not shown ). in this embodiment , integrated circuit 10 also includes a usb device controller 15 , which serves to control the communication between portable device 70 and host platform 90 , such as a usb - compatible personal computer ( pc ) having a usb host controller 93 therein . with reference still to fig1 a , integrated circuit 10 also includes a volatile memory 16 and a non - volatile memory 17 . in a preferred embodiment , volatile memory 16 is a random access memory ( ram ) that serves as a working memory for microprocessor 11 during its operation . non - volatile memory 17 is a read - only memory ( rom ) in this embodiment and can be used to store firmware that perform various functions of portable device 70 . additionally , integrated circuit 10 includes an optional error checking ( ecc ) engine 19 for performing various error checking tasks during the operation of portable device 70 . it should be appreciated that ecc engine 19 , like authentication engine 12 , is well - suited to numerous implementations within the scope of the present invention . for example , ecc engine 19 can be implemented by software ( e . g ., firmware stored in a non - volatile memory ), as part of microprocessor 11 , or as a processor unit separate from microprocessor 11 . referring again to fig1 a , fingerprint module 50 comprises a sensor 52 which is used to capture the fingerprint image of a finger being placed thereon . fingerprint module 50 also comprises a converter 54 , which serves to convert a captured fingerprint image into electrical signals representing the image . in a currently preferred embodiment , a fingerprint print image is converted into 64 kb of data by converter 54 and sent to volatile memory 30 of portable device 70 for temporary storage . in other embodiments , converter 54 can produce image data of different sizes . fingerprint module 50 further includes an optional control unit 56 which , in a currently preferred embodiment , is controlled via microprocessor 11 in portable device 70 and is used for checking the quality of fingerprint images captured by sensor 52 to determine whether a given image is acceptable or not . as described in more detail below , if it is determined that the quality of a captured image is unacceptable , the user will be prompted to place his / her finger on sensor 52 again so that a new image can be captured . reference is now made to fig1 b , which is a block diagram illustrating functional blocks of another embodiment of the portable device of the present invention . in this embodiment , portable device 170 is compatible with the usb standard and includes a usb plug 118 which , as fig1 b shows , is coupled to a usb host controller 193 of a host platform . optionally , portable device 170 further includes an additional usb port 162 that is coupled to usb plug 118 . usb port 162 is provided as a convenient feature that can be used to couple other usb - compatible device ( s ) to the usb via portable device 170 . in this embodiment , portable device 170 also includes a usb device controller 115 for controlling the communication between portable device 170 and the host platform via usb host controller 193 . in one embodiment , a driver software 177 and an application programming interface ( api ) 197 , which in turn includes monitoring software 199 , reside in the host platform and communicate with usb host controller 193 to facilitate the operation of portable device 170 . portable device 170 further comprises an integrated circuit 110 , a flash memory 120 and a volatile memory 130 . integrated circuit 110 can be conveniently implemented as an asic . in a preferred embodiment , a reserved area 122 of flash memory 120 is used to store one or more templates generated in accordance with the present invention . furthermore , in this embodiment , reserved flash memory area 122 includes a status flag 121 which indicates whether or not portable device 170 has been previously registered in accordance with the present invention . status flag 121 thus enables portable device 170 to automatically invoke a registration process upon its initial use , as described in detail further below . in one embodiment , volatile memory 130 comprises either a dram or a sram , which serves as an initial storage area for a fingerprint image captured in accordance with the present invention . referring still to fig1 b , integrated circuit 110 comprises a microprocessor 111 which preferably is a risc processor . integrated circuit 110 further includes a flash controller 114 for controlling access to flash memory 120 and a memory controller 133 for controlling access to volatile memory 130 . integrated circuit 110 also includes a volatile memory 116 and a non - volatile memory 117 . preferably , volatile memory 116 comprises a ram for use as a working memory for microprocessor 111 during its operation , while non - volatile memory 117 comprises a rom for storing firmware that perform various functions of portable device 170 . specifically , in one embodiment , rom 117 stores the following firmware code : firmware 117 a for reading fingerprint sensor 152 , firmware 117 b for processing fingerprint images , firmware 117 c for generating templates , firmware 117 d for encrypting fingerprint images and / or templates , and firmware 117 e for verifying fingerprint authenticity . nevertheless , it should be appreciated that in an alternative embodiment of the present invention , such firmware can be stored in a non - volatile memory within the host platform rather than in portable device 170 . additionally , integrated circuit 110 includes an optional error checking ( ecc ) engine 119 for performing various error checking tasks during the operation of portable device 170 . it should be appreciated that ecc engine 119 can be implemented as software ( e . g ., firmware ) or hardware ( e . g ., processor / processor module ) within the scope of the present invention . referring still to fig1 b , fingerprint module 150 comprises a sensor 152 , a converter 154 and an optional controller 156 . in this embodiment , sensor 152 is used to capture the fingerprint image of a finger being placed thereon , converter 154 serves to convert a captured fingerprint image into electrical signals representing the image , and optional controller 156 is used to check the quality of fingerprint images captured by sensor 152 to determine whether a given image is acceptable or not . it should be appreciated that such image processing capabilities can be implemented using software ( e . g ., firmware ) or hardware ( e . g ., processor / processor module ) within the scope of the present invention . in a currently preferred embodiment as illustrated in fig1 b , microprocessor 111 controls various components of portable device 170 , including flash controller 114 , usb device controller 115 , ram 116 , rom 117 ( and execution of firmware code stored therein ), ecc engine 119 , memory controller 133 , and controller 156 of fingerprint module 150 . in this embodiment , portable device 170 also includes a write - protection switch 140 which , when activated , triggers microprocessor 111 to disable write - access to flash memory 120 . with reference next to fig2 , a front perspective view of a portable device with an integrated fingerprint module in accordance with one embodiment of the present invention is shown . in fig2 , portable device 70 is shown with usb connector 18 protruding from its front end . fingerprint module 50 is shown as being structurally integrated with portable device 70 in a unitary construction , with sensor 52 disposed on the top side of portable device 70 . a light emitting diode ( led ) 73 is also shown disposed near the edge of the top side of portable device 70 . in one embodiment , led 73 flashes when data in portable device is being accessed , thus serving as an activity indicator . in another embodiment , led 73 lights up to indicate that an authentication process is underway . referring next to fig3 , a rear perspective view of the portable device with an integrated fingerprint module as depicted in fig2 is shown . again , portable device 70 is shown with usb connector 18 protruding from its front end , and fingerprint module 50 is shown as being structurally integrated with portable device 70 in a unitary construction , with sensor 52 disposed on the top side thereof led 73 is again shown disposed near the edge of the top side of portable device 70 . optional write protection switch 40 is also shown as being located at the rear end of portable device 70 . reference is now made to fig4 , which shows a bottom plan view of the portable device with an integrated fingerprint module as illustrated in fig2 . a substantially semicircular indentation 77 , an optional feature which allows a user to hold portable device 70 firmly while coupling or decoupling portable device 70 to / from host platform 90 ( fig1 a ), is shown on the bottom side of portable device 70 in fig4 . usb connector 18 is also shown . referring next to fig5 , a top plan view of the portable device with an integrated fingerprint module as shown in fig2 is depicted . portable device 70 is shown with usb connector 18 protruding from its front end , and fingerprint module 50 is shown as being structurally integrated with portable device 70 in a unitary construction , with sensor 52 disposed on the top side thereof led 73 is again shown disposed near the edge of the top side of portable device 70 . reference is now made to fig6 , which is a left side elevation view of the portable device with an integrated fingerprint module as shown in fig2 . usb connector 18 is shown protruding from the front of portable device 70 , and the periphery of sensor 52 is shown slightly raised from the top side of portable device 70 . next , fig7 is a right side elevation view of the portable device with an integrated fingerprint module as shown in fig2 . once again , usb connector 18 is shown protruding from the front of portable device 70 , and the periphery of sensor 52 is shown slightly raised from the top side of portable device 70 . referring next to fig8 , a front elevation view of the portable device with an integrated fingerprint module as shown in fig2 is depicted . the insertion end of usb connector 18 is centrally depicted , and the periphery of sensor 52 is shown slightly raised from the top side of portable device 70 . reference is now made to fig9 , which is a rear elevation view of the portable device with an integrated fingerprint module as shown in fig2 . the periphery of sensor 52 is shown slightly raised from the top side of portable device 70 , and optional indentation 77 on the bottom side of portable device 70 is also visible . optional write protection switch 40 is also shown as being located at the rear end of portable device 70 . referring next to fig1 , a flow diagram 200 illustrating steps of a user registration / authentication process using the portable device with an integrated fingerprint module in accordance with one embodiment of the present invention is shown . in the following description , various modules and components referred to have been described above with reference to fig1 a using the same reference numerals . in step 210 , upon being coupled to a host platform , portable device 70 undergoes an initialization procedure . in a currently preferred embodiment , the initialization procedure involves establishing communication with the host platform and ensuring the host platform is aware that portable device 70 has been coupled thereto . in step 220 , portable device 70 determines whether a user registration is necessary . for example , if portable device 70 is being used for the first time and no template has yet been stored in flash memory 20 , portable device 70 will guide the user to complete a registration process ( steps 225 , 235 , 245 and 255 as described below ) via a user interface ( e . g ., pop - up message windows ) through the host platform . thus , upon the first use of portable device 70 ( e . g ., immediately after purchase ), a preferred embodiment automatically initiate the registration process to generate the first (“ master ”) template . this is preferably accomplished by checking a status flag ( e . g ., flag 121 in flash memory 120 of fig1 b ). subsequent registration ( s ), as described below , can be activated by individual users via software on the host platform . in one embodiment , portable device 70 supports more than one user . in another embodiment , the same user may register multiple fingerprints as separate templates . in yet another embodiment , the same user fingerprint may be registered multiple times as different templates . thus , portable device 70 can facilitate the registration of additional user ( s ) and / or additional template ( s ) either by periodically ( e . g ., upon startup ) inquiring whether a new user / template needs to be added or upon the user &# 39 ; s request in step 220 . if an additional user / template is to be registered , the registration process will be invoked . if it is determined that no new registration is necessary , process 200 proceeds with an authentication process ( steps 230 , 240 and 260 as described below ). it should be appreciated that within the scope of the present invention , software ( e . g ., a software driver ) may need to be installed on the host platform prior to the first use of portable device 70 to enable its utilization of the host platform &# 39 ; s user interface to communicate with the user . it should also be appreciated that if the operating system of the host platform has built - in support for such functionality , no additional software needs to be installed thereon . referring still to fig1 , the registration process is now described . in step 225 , the registration process is initiated . in one embodiment , this involves informing the user that a registration process will commence and prompting the user to place his / her finger on sensor 52 . in step 235 , sensor 52 is read to capture an image of the fingerprint of the user &# 39 ; s finger that has been placed thereon . in a currently preferred embodiment , step 235 also includes verifying that the captured image is of sufficient quality for further processing ( e . g ., template generation ). this is preferably performed by control unit 56 as directed by microprocessor 11 . in one embodiment , step 235 will be repeated if the quality of the captured fingerprint image is unacceptable . under such circumstances , the user will be prompted to place his / her finger on sensor 52 again so that a new image can be captured . preferably , the number of retry is user - configurable . once an acceptable fingerprint image has been captured in step 235 , process 200 proceeds to step 245 , wherein a template is generated based on the captured fingerprint image . as described above , in a preferred embodiment , the captured image is converted into 64 kb of data , which is then used as input to template generator 12 a for generating a 512 - byte template . in step 248 , the template generated in step 245 is encrypted . in one embodiment , the encryption is performed by firmware ( e . g ., encryption firmware 117 d of fig1 b ), thereby providing an added level of security against hacking . in step 255 , the encrypted template is stored into flash memory 20 . in one embodiment , upon successful generation and encryption of a template , flash controller 14 is prompted by template generator 12 a to store the newly generated and encrypted template into flash memory 20 for use in subsequent user authentication . moreover , as described above , in a preferred embodiment , the template is stored in a reserved area of flash memory 20 which is specifically designated for storing template ( s ) and which is not otherwise accessible to the user . in step 280 , a signal or message indicating the successful completion of the registration process is generated . in an embodiment where portable device 70 is used as a secure storage device , step 280 can also entail enabling portable device , i . e ., granting the newly registered user access ( e . g ., read data therefrom and write data thereto ) to portable device 70 and mapping portable device 70 to a valid drive letter on host platform 90 . with reference still to fig1 , the authentication process is now described . in step 230 , sensor 52 is read to capture an image of the fingerprint of the user &# 39 ; s finger that has been placed thereon . in a currently preferred embodiment , step 230 also includes a quality check of the captured image by control unit 56 , so that the image capture will be repeated if the quality of the captured fingerprint image is unacceptable for template generation . if a repeat capture is needed , the user will be so prompted . preferably , the number of retry is user - configurable . in a currently preferred embodiment , step 230 also includes generating a template based on the captured fingerprint image and storing the resulting template into volatile memory 16 . in step 240 , the stored template ( s ) are read from flash memory 20 for use as the basis of authenticating the identity of the user whose fingerprint image has been captured in step 230 . in a currently preferred embodiment , microprocessor 11 directs flash controller 14 to retrieve the registered template ( s ) from flash memory 20 . in step 250 , the registered template ( s ) read from flash memory 20 , which are stored in encrypted form in a preferred embodiment , are decrypted . the decrypted template ( s ) are loaded into volatile memory 16 in one embodiment . in step 260 , it is determined whether the user &# 39 ; s fingerprint can be authenticated against the registered fingerprint template on record . in a currently preferred embodiment , verification module 12 b compares the template pending verification against the registered template ( s ). if a match is detected , the user is authenticated ; otherwise , authentication fails . in one embodiment , the user is allowed to reattempt the authentication process if an initial attempt fails ( e . g ., steps 230 , 240 and 250 are repeated ). preferably , the number of repeated attempts is user - configurable and can be set once an authorized user has been authenticated and granted access . in one embodiment , when a user has failed to authenticated his / her identity as an authorized user , access to flash memory 20 will be blocked ( e . g ., in an embodiment where a software driver resides in host platform 90 , the software driver can forbid such access ). in another embodiment , microprocessor 11 in portable device 70 will shut down or otherwise disable flash controller 14 upon such authentication failure . these actions serve as added security measures against potential hacking and other forms of unauthorized access to the data stored in flash memory 20 and are triggered by repeated failed authentication attempts . in one embodiment , optional step 270 is provided . in this embodiment , should verification module 12 b malfunction and refuse to authenticate an authorized user whose fingerprint has been previously registered , the user is provided with an option to bypass the fingerprint authentication and provide a password to gain access instead . this embodiment affords the user the ability to avoid a helpless situation where access to contents of flash memory 20 cannot be had unless and until verification module 12 b is fixed . if the bypass password is correctly entered , user authentication is deemed to be successful ; otherwise , user authentication remains a failure . it should also be appreciated that if added security is desired , a password requirement can be implemented in addition to the fingerprint authentication even for normal routine authentication within the scope of the present invention . in step 280 , a signal or message indicating the successful authentication is generated . in an embodiment where portable device 70 is used as a secure storage device , step 280 can also entail enabling portable device , i . e ., granting the newly registered user access ( e . g ., read data therefrom and write data thereto ) to portable device 70 and mapping portable device 70 to a valid drive letter on host platform 90 . it should be appreciated that in an embodiment where authentication engine 12 is located in host platform 90 , appropriate modifications to the authentication process described above are needed . in particular , once a satisfactory fingerprint image has been obtained in step 230 , the image data is first encrypted and then transmitted to host platform 90 , wherein the steps to be performed by authentication engine 12 will be carried out . thus , depending on the particular implementation or application , the information being transmitted from portable device 70 to host platform 90 can either be a simple notification of success upon successful authentication , or image data representing a user fingerprint that is pending authentication . in a currently preferred embodiment , performance of various steps of process 200 are controlled by microprocessor 11 executing firmware code , which is preferably stored in non - volatile memory 17 of portable device 70 . significantly , it should be appreciated that the present invention not only contemplates using portable device 70 as a secure data storage device but also as an access control device . in particular , within the scope of the present invention , portable device 70 can act as an “ access key ” to host platform 90 to which portable device 70 is coupled . more specifically , in one embodiment , in order to access any resource on host platform 90 ( e . g ., data , files , application programs , peripherals ) and / or any resource attached thereto ( e . g ., network access , network printers and storage devices , electronic mail ) a user is required to first successfully authenticate his / her identity as an authorized user using portable device 70 with integrated fingerprint module 50 . in accordance with this embodiment , such fingerprint authentication is used preferably in lieu of ( or alternatively in addition to ) conventional password - based authentication . thus , the user inconvenience and less stringent security that is inherent in the prior art password - based authentication approach is advantageously eliminated in accordance with the present invention . beyond access control to various computer resources , the present invention can also be advantageously utilized in numerous other applications that require security clearance , such as entry into private homes , offices , hotel rooms , bank vaults and security deposit boxes , and so on . the present invention can also be beneficially applied to restrict the operation of machinery , such as factory machines and vehicles , to those who have been properly trained . in one embodiment , access control device 70 can be used as a house key to a private home or room key to a hotel room in place of conventional keys . in the first example , the home owner first registers his / her fingerprint when the biometrics - based lock is installed at the house . in the latter example , a hotel guest first registers his / her fingerprint upon check - in at a hotel . thereafter , access to the house or hotel room is securely restricted to the respective key holder ( home owner or hotel guest ). these and other wide - ranging applications of the biometrics - based access device technology disclosed herein are all intended to be within the scope and spirit of the present invention . although embodiments of the present invention have been described herein as using fingerprint authentication technology to implement access control , it should be appreciated that the present invention is not limited thereto but rather encompasses the use of other biometrics - based authentication techniques . one such technique is iris scan technology . while such other biometrics - based techniques are not expressly described herein , their applicability to access control implementations using a portable device is within the scope and spirit of the present invention disclosed . moreover , while preferred embodiments of the present invention have been described herein as using flash memory as a storage media , it should be appreciated that other types of non - volatile memory , such as ferroelectric random access memory ( fram ) or magnetic random access memory ( mram ), can also be used within the scope of the present invention . in addition , while such preferred embodiments have been described herein as being compatible with the usb standard , the portable device of the present invention is not intended to be restricted thereto . rather , the present invention is intended to encompass portable devices that support other communication protocols and / or bus standards , such as the ieee 1394 (“ firewire ”) standard . while preferred embodiments of the present invention , a method and system for implementing access control using biometrics - based technology , have been described , it is understood that those skilled in the art , both now and in the future , may make various improvements and enhancements which fall within the scope of the claims that follow . these claims should be construed to maintain the proper protection for the invention first disclosed herein . | 6 |
fig1 schematically shows first and second transceivers 21 and 31 , hereinafter referred to as dwm transceivers 21 and 31 , communicating using dynamic waveform modulation ( dwm ) to package data in u - pacs , in accordance with an embodiment of the invention . by way of example , dwm transceiver 21 is coupled to the ethernet and at least one source 51 of high definition uncompressed audiovisual ( av ) multimedia data from which dwm transceiver receives data to transmit to a sink 52 via dwm transceiver 31 . optionally , the dwm transceivers 21 and 31 transmit data to each other over an unshielded twisted pair ( utp ) cable 40 . optionally , utp cable 40 is a cat5e or cat6 cable comprising four twisted pairs , tp 41 , tp 42 , tp 43 and tp 44 . the multimedia data is assumed to be transition minimized differential signaling audio visual ( tmds - av ) data . dwm transceiver 21 optionally comprises signal processing and control circuitry 24 for encoding / decoding and modulating / demodulating data it receives and for each twisted pair tp 41 , tp 42 , tp 43 and tp 44 of utp cable 40 , a transmitter , receiver and hybrid circuit . the various transmitters , receivers and hybrid circuits are schematically represented by a transmitter 25 , a receiver 26 and a hybrid circuit 27 respectively . optionally , an rj45 patch 46 mounted to a wall plate 47 couples hybrid circuit 27 to each twisted pair tp 41 , tp 42 , tp 43 and tp 44 . dwm transceiver 31 comprises signal processing and control circuitry 34 for encoding / decoding and modulating / demodulating data it receives and for each twisted pair tp 41 , tp 42 , tp 43 and tp 44 of utp cable 40 , a transmitter , receiver and hybrid circuit . the various transmitters , receivers and hybrid circuits are schematically represented by a transmitter 35 , a receiver 36 and a hybrid circuit 37 respectively . optionally , an rj45 patch 46 mounted to a wall plate 47 couples hybrid circuit 37 to each twisted pair tp 41 , tp 42 , tp 43 and tp 44 . dwm transceiver 21 receives ethernet data from the ethernet and tmds - av data and control data from source 51 and its processing and control circuitry 24 encodes and modulates the data optionally onto symbol ( i . e . waveform ) sets s4d - s ( m , i ) of different size responsive to a degree of resistance to noise that is desired for the data . circuitry 24 then controls transmitter 25 to transmit the symbols in packets , u - pacs , having a same format . in accordance with an embodiment of the invention , the index i is smaller for data warranting higher noise resistance than for data warranting lower noise protection . dwm transceiver 31 receives the u - pacs and its processing and control circuitry 34 demodulates and decodes the symbols they comprise to un - packetize the data they contain and transmits the data to sink 52 . whereas tmds - av data is transmitted in simplex mode from source 51 to sink 52 , ethernet and / or control data transmitted from the sink to the source in general requires that the sink provide a response to the source and ethernet and control data is transmitted in full duplex between the source and sink , in accordance with an embodiment of the invention . large block arrows 61 schematically represent simplex multimedia tmds - av data and double arrowhead block arrows 62 represent full duplex ethernet and / or control data . in responding to ethernet and control data received from source 51 , sink 52 optionally packetizes its response in u - pacs using symbol sets s4d - s ( m , i ) for transmission similarly to the way in which source 51 packetizes its data for transmission . however , the inventors have noted that transmission of tmds data and full duplex ethernet data over a same channel , such as the twisted pair ( tp ), hybrid terminated channel shown in fig1 a , at high transmission rates required by tmds data can generate substantial amounts of noise in the channel . in particular , echo and near end cross talk ( next ) generated by near end transmitters make substantial contributions to the noise . both the near end transmitter echo and next can exhibit exponential growth with frequency of signal transmission over a tp channel similar to that shown in fig1 a . for example , for a 50 m cat6 cable , noise can increase by as much as about 30 db for an increase in frequency of transmission from about 10 mhz to about 300 mhz . the inventors have further noted that full duplex transmission of ethernet does not in general require a same data transmission rate as transmission of simplex tmds data . therefore , in some embodiments of the invention , whereas transceiver 21 is configured to transmit both tmds data and full duplex ethernet and / or control data , at a relatively high transmission rate required by tmds data , transceiver 31 is configured to transmit ethernet and / or control data to transceiver 21 at a substantially lower transmission rate . the lower transmission rate at which transceiver 31 transmits data can substantially reduce echo and next at transceiver 31 . in some embodiments of the invention , dwm transceiver 21 transmits tmds and ethernet and / or control data to transceiver 31 at a transmission rate greater than about 10 times the transmission rate at which dwm transceiver 31 transmits ethernet and / or control data to transceiver 21 . optionally , dwm transceiver 21 transmits at a transmission rate 20 times greater than dwm transceiver 31 . optionally , dwm transceiver 21 transmits at a transmission rate 30 times greater than dwm transceiver 31 . optionally , dwm transceiver 21 transmits at a transmission rate 40 times greater than dwm transceiver 31 . for example , in some embodiments of the invention , dwm transceiver 21 transmits tmds and ethernet and / or control data to dwm transceiver 31 at 250 msym / sec or 500 msym / sec and dwm transceiver 31 transmits ethernet and / or control data to transceiver 21 at 12 . 5 msym / sec . it is noted that the relatively low transmission rates at which dwm transceiver 31 transmits data to dwm transceiver 21 can generate significant base line wander ( blw ) due to transformers that optionally couple each transceiver to tp cable 40 . to reduce possible blw , dwm transceiver 31 optionally transmits data using “ dc - balanced ” waveform sets , i . e . dc - balanced symbol sets . whereas , any suitable dc - balanced waveform set and methods of transmitting such waveform sets known in the art may be used by dwm transceiver 31 to transmit data , optionally dwm transceiver 31 is configured to transmit data using s4d - p ( m , i ) symbols . let a dc - balanced symbol set in accordance with an embodiment of the invention be represented by “± s4d - p ( m , i )”. in accordance with an embodiment of the invention , the set comprises positive and negative voltage level symbols s4d - p ( m , i ) and for each positive voltage level symbol , the set comprises a “ mirror image ” negative voltage level symbol having a same magnitude as the positive level symbol . mirror image symbols represent identical data and are selectively transmitted by dwm transceiver 31 so that blw generated by positive symbols is substantially neutralized by transmission of negative mirror image symbols . in accordance with an embodiment of the invention , dwm transceiver 31 uses symbols from a data set ± s4d - p ( m , i ) having a smaller value of i for data warranting higher noise resistance . optionally , the s4d - s ( m , i ) symbol sets are four dimensional pam symbols sets s4d - p ( m , i ) and with each component one - dimension pam ( m , i ) symbol of the four dimensional s4d - p ( m , i ) symbol transmitted substantially simultaneously over a different one of tp 41 , tp 42 , tp 43 and tp 44 . for convenience of presentation , it is assumed that the one dimensional pam symbols are pam ( 16 , i ) symbols and that i = 2 k where k is equal to a number of bits of information represented by a pam ( 16 , i ) and satisfies a condition 1 ≦ k ≦ 4 . the index i has a value equal to 16 for the largest pam set and assumes values 8 , 4 or 2 for subsets of the largest set with symbols in subsets having smaller i and therefore smaller numbers of symbols being easier to distinguish one from the other and having improved symbol error rate ( ser ). for values of i equal to 16 , 8 , 4 and 2 each pam symbol respectively contains 4 , 3 , 2 and 1 bit of information . each symbol of the corresponding four - dimensional s4d - p ( m , i ) symbol sets contains 16 , 12 , 8 and 4 bits of information . it is noted that for each decrease in k by 1 , an amplitude difference between symbols in a symbol set s4d - p ( m , i ) is doubled , making it is easier to differentiate between symbols transmitted between transceiver 21 and 31 and improving the signal to mean squared error ( mse ) ratio of slicers in the transceivers used in determining which symbols is received by the transceivers . signal to mse ratio ( mser ) is defined by an expression mser =( 10 * log 10 (( d / 2 ) 2 / e ( e 2 )) where d is a minimal distance between slicer decision levels and e ( e 2 ) is a mean of the squared slicer error signal at the decision levels . as a result , for each decrease in k by 1 , d doubles and the mser improves by 6 db . assuming additive white gaussian noise ( awgn ), in the channel coupling transceivers 21 and 31 , for a given level of noise in the channel , improvement in mser by 6 db , substantially improves a symbol error rate ( ser ) in symbols transmitted between the transceivers . for example assuming a ser of 10 − 5 a 6 db improvement in mse improves the ser to 10 − 17 and sers of 10 − 7 and 10 − 9 are improved to 10 − 25 , and 10 − 32 respectively . the inventors have determined that the improvement in ser provided by reducing i by 1 provides about a same improvement in ser for a awgn channel as is provided by encoding data in accordance with a reed - solomon ( rs ) code having an error correction capability of up to 3 data symbols . fig1 b schematically shows a u - pac 100 comprising s4d - p ( 16 , i ) symbols in accordance with an embodiment of the invention . u - pac 100 comprises a header section 101 , a payload section 102 and a tail section 103 . payload section 102 comprises a plurality of symbols 110 that encode “ payload ” data to be delivered from one to the other of source 51 and sink 52 ( fig1 a ). the data in the payload section of u - pac 100 is encoded and modulated onto s4d - p ( 16 , i ) symbols having index i which depends upon a level of protection against noise with which it is desired to protect the data . in accordance with an embodiment of the invention , different parts of payload 102 may have different values of i and thereby different levels of ser and anti - noise protection . header 101 and tail 103 comprise management data used for processing information comprised in the packet and data in the header and tail is encoded and modulated onto s4d - p ( 16 , 4 ) symbols each representing 8 bits to provide the data with relatively low ser . optionally , the header comprises two symbols , a type symbol 112 and a stream id symbol 113 . type symbol 112 is optionally configured to characterize up to 64 different types , examples of which are discussed below , of u - pacs . stream id comprises data that identifies source 51 and sink 52 . tail 103 optionally comprises a crc - 8 symbol 114 and an idle symbol 115 that marks the end of u - pac 100 . by way of example , fig2 shows a flow chart 200 schematically illustrating encapsulating ethernet data into a u - pac 100 , in accordance with an embodiment of the invention . in a process step 201 a stream of ethernet data to be transmitted to sink 52 is received by first transceiver 21 . a block 202 of eight ( 8 ) ethernet octets in the stream of ethernet data is schematically shown to the right of process step 201 . in a process step 203 a data / control bit shown shaded is added to the eight ( 8 ) ethernet octets shown in block 202 to a form a “ 64 b / 65 b ” code block 204 of sixty - five ( 65 ) bits . in a step 205 twelve sixty - five ( 65 ) bit code blocks 204 are aggregated to form a payload data section 207 that will become with further processing a payload section of u - pac 100 . a header data section 206 and tail data section 208 are added to the payload section to form an aggregate code block 210 . header data section 206 optionally comprises a “ type ” octet that defines the type of data in the aggregate and u - pac 100 as ethernet data and a stream id octet . tail 208 optionally comprises a crc - 8 octet . aggregate code block 210 comprises 768 ethernet payload bits and 36 control bits ( header and tale bits plus the control bit added in step 203 ) for a total of 804 bits . optionally , the data in aggregate block 210 is scrambled in a step 212 to provide a scrambled aggregate data block s 210 having header , payload and tail sections s 206 , s 207 and s 208 respectively . in a step 214 , the data in scrambled , aggregate code block s 210 is mapped onto a set of s4d - p ( 16 , i ) symbols and a symbol is added to tail s 208 to generate header 101 , payload 102 and tail 103 of a u - pac 100 . in accordance with an embodiment of the invention , data in header section s 206 and tail section s 208 of scrambled aggregate s 210 is mapped to s4d - p ( 16 , 4 ) symbols , each of which represents 8 bits of data , to provide the control data with a relatively low ser . header 101 and tail 103 have two ( 2 ) s4d - p ( 16 , 4 ) symbols each . the ethernet data in payload section s 207 is optionally mapped to s4d - p ( 16 , 8 ) symbols in payload 102 , each of which symbols represents 12 bits of data , so that payload 102 has sixty - five ( 65 ) s4d - p ( 16 , 8 ) symbols . u - pac 100 therefore comprises a total of sixty - nine ( 69 ) s4d - p ( 16 , i ) symbols and comprises 768 bits of ethernet payload data . assuming the ethernet data received by dwm transceiver 21 is 100 mbps ethernet , to support the data transmission rate the transceiver transmits an ethernet u - pac 100 of 69 s4d - p ( 16 , i ) symbols to sink 52 via dwm transceiver 31 , in accordance with an embodiment of the invention , every 7 . 68 μs for a transmission rate of about 9 mega - symbols of ethernet data per second ( msym / sec ). optionally , sink 52 ( fig1 a ) responds to the ethernet information it receives at a same rate , and transmits back to transceiver 21 via transceiver 31 about 9 mega - symbols of ethernet data per second ( msym / sec ). symbol transmission between dwm transceivers 21 and 31 in accordance with an embodiment of the invention , therefore operates in a full duplex mode that supports 100 mbps full duplex ethernet transmission . fig3 shows a flow chart 300 that schematically illustrates encapsulating tmds - av data from a tmds - av data stream used for generating an audiovisual display into u - pacs , in accordance with an embodiment of the invention . a stream of tmds - av data comprises three different types of data transmitted during periods , hereinafter referred to as “ tmds periods ” or “ t - periods ”, having fixed duration “ t ”. during each tmds period one of the three different types of data is transmitted for each of three tmds channels . the types of data are video data (“ v ” data ), control data (“ c ” data ) and data - island packet data (“ i ” data ). during video data periods , also referred to as a “ v periods ”, each tmds channel carries pixel color data encoded in 8 bits , for a total of 24 bits of video data per period . during data island tmds periods , also referred to as “ i periods ”, the tmds channels carry audio data , which may comprise for example audio samples acquired at 192 khz for each of 8 audio channels and information frames , “ infoframes ”, comprising data that characterizes audio and video data in the tmds - av stream . during an i period each tmds channel carries 4 bits of data so that the three tdms channels carry a total of 12 bits of data during the i period . during control data tmds periods , also referred to as “ c periods ”, the tmds channels carry inter alia horizontal and vertical synchronization data . each tdms channel typically carries 2 bits of control data during a c period for a total of 6 bits of control data during the period . sequences of different types of tmds periods in the tdms - av stream are generally separated from each other by “ guard bands ” that are 2 tdms periods , “ g periods ”, long . in a process step 302 in fig3 dwm transceiver 21 receives a tmds - av data stream to be transmitted to sink 52 via dwm transceiver 31 . a data block 304 of data in the tmds - av stream encoding a single horizontal line of video data and accompanying audio data is schematically shown being received by the transceiver . the data is assumed , by way of example , to be used to generate a progressive video display that is refreshed at 60 hz and comprises 1080 active and 45 blank horizontal lines , each having 1920 24 bit pixels and 280 blank pixels . the video display is assumed accompanied by eight 8 audio channels sampled at 192 khz to provide 8 level samples . data block 304 therefore is 2200 tmds periods long , of which 1920 periods are video data periods , i . e . v periods , during each of which 24 bits of pixel data are transmitted and 280 tmds periods are “ blank ” tmds periods . in fig3 a tmds t - period is generically denoted by its duration “ t ”. of the 280 blank t - periods a first 96 t - periods comprise control , c periods , or guard band , g periods each carrying 6 bits of data , a middle 96 periods comprise data island , i periods each carrying 12 bits encoding audio data and a last 88 periods comprise control c or g periods . in accordance with an embodiment of the invention , in a process block 306 each 16 t - periods of tmds data in data block 304 are encoded into s4d - p ( 16 , i ) symbols , and a header , hereinafter a “ sub - packet header ”, added to the symbols to form a sub - packet . the sub - packet header optionally comprises a s4d - p ( 16 , 4 ) symbol that characterizes the data in the sub - packet . for example , the sub - packet header optionally distinguishes between a sub - packet comprising only control data from a sub - packet comprising control and guard data or a sub - packet comprising only data island data . sub - packets 310 generated in process step 306 from data in data block 304 are schematically shown in a data block 308 and are labeled with a letter or letters indicating the type of data they contain . sub - packets 310 labeled “ c ”, “ i ”, or “ v ” comprise only control , data island or video pixel data respectively . “ mixed ” sub - packets comprising more than one type of data are labeled by the letters of each of the data types they contain . for example , sub - packets 310 in block 308 that contain both control ( c ) data and guard ( g ) data are labeled by both g and c . in accordance with an embodiment of the invention , v data , is encoded into s4d - p ( 16 , 16 ) symbols , and i data , c data and g data are encoded into s4d - p ( 16 , 8 ) symbols . since each t - period of v data comprises 24 bits of data , each v period is encoded to 1 . 5 s4d - p ( 16 , 16 ) symbols . similarly , each i data period comprises 12 bits of data and is encoded to 1 s4d - p ( 16 , 8 ) symbol and each c data or g period comprises 6 bits of data and is encoded to 0 . 5 s4d - p ( 16 , 8 ) symbols . with the addition of the sub - packet header comprising one s4d - p ( 16 , 4 ) symbol , each type of v data sub - packet 310 comprises 25 s4d - p ( 16 , 16 ) symbols , each i data sub - packet comprises 17 s4d - p ( 16 , 8 ) symbols and each c or cg sub - packet 310 comprises 9 s4d - p ( 16 , 8 ) symbols . the number of s4d - p ( 16 , i ) symbols in each type of sub - packet 310 in fig3 is shown in parentheses for at least one of the type of sub - packet below the sub - packet . in accordance with an embodiment of the invention , v data is always encapsulated in sub - packets 310 comprising only v data in addition to the sub - packet header . therefore , if data in a sequence of 16 t - periods that is to be encapsulated in a sub - packet includes t - periods having data other than v data followed by t - periods having v data , the sub - packet is a “ shortened sub - packet ” generated only from data in the non - v data t - periods and includes data in less than 16 t - periods . v data in the remaining t - periods are encapsulated in a next sub - packet . a shortened sub - packet 310 comprising data from only 8 t - periods is distinguished by a reference numeral 312 . in a process step 314 , sub - packets 310 are encapsulated in u - pacs 320 having a configuration shown for u - pac 100 ( fig1 b ). u - pacs 320 encapsulating sub - packets 310 generated in process step 314 are shown in a u - pac data block 330 . in accordance with an embodiment of the invention , each u - pac 320 typically comprises , 4 sub - packets 310 ( data from 64 t - periods of data block 304 ), a u - pac header 321 comprising two s4d - p ( 16 , 4 ) symbols and a u - pac tail 322 comprising two s4d - p ( 16 , 4 ) symbols . similar to the case of sub - packets 310 , optionally , a u - pac 320 does not “ mix ” sub - packets 310 having v data with sub - packets 310 comprising other than v data . in accordance with an embodiment of the invention , a sub - packet 310 comprising v data is encapsulated in a same u - pac 320 only with other sub - packets 310 comprising v data . as a result , to satisfy the non - mixing constraint , a u - pac 310 such as for example a u - pac 320 distinguished in fig3 by a reference numeral 324 , may comprise less than 4 sub - packets 310 . a total of 35 u - pacs 320 , labeled u - pac 1 - u - pac 35 , generated as described above are required to encapsulate all the tmds data comprised in data block 304 that defines a single 1080p 24 bpp + 8 l - pcm audio sampled at 192 khz . of the 35 u - pacs 320 , 30 u - pacs comprise pixel defining d data and 5 u - pacs comprise control and / or audio data . since different sub - packets 310 may comprise different numbers of s4d - p ( 16 , i ) symbols and as noted above , different u - pacs 320 may comprise different numbers of sub - packets , different u - pacs 320 may comprise different numbers of s4d - p ( 16 , i ) symbols . a number of s4d - p ( 16 , i ) symbols in each u - pac 320 in u - pac data block 330 is shown for each u - pac 320 . a total of 3346 s4d - p ( 16 , i ) symbols are used to encapsulate the tmds data for data block 304 . in order to support the refresh rate of 60 hz , dwm transceiver 21 must transmit 60 × 1125 lines of 3346 s4d - p ( 16 , i ) symbols to dwm transceiver 31 every second for a transmission rate of about 226 msym / sec . in an embodiment of the invention , dwm transceivers 21 and 31 operate at transmission rates of 250 msym / sec , which readily supports the bandwidth required for 226 msym / sec simplex transmission of tmds data plus 9 msym / sec full duplex ethernet transmission noted above between the transceivers . in an embodiment of the invention , the transceivers operate at transmission rates of 500 msym / sec which supports simultaneous transmission of two tmds streams plus full duplex ethernet . in the description and claims of the application , each of the words “ comprise ” “ include ” and “ have ”, and forms thereof , are not necessarily limited to members in a list with which the words may be associated . the invention has been described using various detailed descriptions of embodiments thereof that are provided by way of example and are not intended to limit the scope of the invention . the described embodiments may comprise different features , not all of which are required in all embodiments of the invention . some embodiments of the invention utilize only some of the features or possible combinations of the features . variations of embodiments of the invention that are described and embodiments of the invention comprising different combinations of features noted in the described embodiments will occur to persons with skill in the art . it is intended that the scope of the invention be limited only by the claims and that the claims be interpreted to include all such variations and combinations . | 7 |
the container end of the present invention is comprised of two major parts , a dome structure 10 and a cap or hat member 12 which is in the general form of an inverted cup , including an outwardly curled rim 13 depending from the top panel 14 of hat member 12 . in fig1 a pair of containers including can type bodies 15 each provided with this end , such bodies having a concave central portion 16 in their bottoms are shown stacked one upon the other to demonstrate the ability of the container to be so stacked while including the novel resealable end . such bottom configuration of can bodies is per se known . referring to fig2 the dome includes a neck structure 11 with a wing - like lower rim 20 capable of being seamed to the upper end or rim of a can body ( see the left edge of fig2 ), and optionally including a sealing compound 21 on the underside of rim 20 . rim 20 extends outward from the lower edge of a generally frusto - conical central neck section 22 which has formed on its upper edge a generally cylindrical upper neck section 25 which terminates at its upper edge in a outward curled seal rim 30 formed upon a ledge 31 . about seal rim 30 there is shown an elastomeric preferably circular seal 32 , which may take different forms as later explained , but in general is fitted within cap 12 . extending outward from upper neck section 25 are a first set of elongated lugs 35 , generally triangular in shape ( see fig2 a ), with angled lower cam surfaces 35c extending at a predetermined angle to the generally vertical outer surface of neck section 25 . these lugs 35 cooperate with a second set of inwardly extending lug members 36 formed in the curled rim 13 of hat member 12 to hold the cap firmly on the dome structure , as later explained . when the hat member is attached to the upper neck portion , the cooperating first and second lug members 35 , 36 draw top panel 14 against the curled seal rim 30 , and compress seal 32 against the curled rim 30 and ledge 31 , as shown in fig2 . seal 32 can take different forms . in a first form the annular o - ring type seal is molded as a peripheral part of a thin flexible and compliant disk 33 which is attached to the underside of top panel 14 . in another form , the o - ring type seal is made as a rim of a circular thin member which is applied to the outer portion of the underside of top panel 14 . in any event , the compressible elastomeric seal member is positioned within the hat member 12 , as shown in fig2 . this arrangement will retain initial pressurization of product ( if necessary ), and hold residual pressure after reclosing . the tooling which is disclosed herein is intended for use in reciprocating high speed presses , although other forms of tooling and actuation are within the scope of the invention . in general , with regard to fig3 a - b and fig5 a - b , a typical press includes an upper die plate up , a lower die plate lp , and guide posts gp which maintain the alignment of a punch or punches on upper plate up and a corresponding die or dies on lower plate lp . the various ones of these figures represent , in somewhat schematic fashion , the tooling at different stations within a press . fig3 a - b and 4a - b show the hat or cap and the two steps of forming the completed lugged hat 12 . both steps may be contained in the same press , as this is convenient in a high production environment , however the second operation can be performed in an auxiliary piece of equipment . in the first operation ( at a first station i - h ), a blank is cut from either sheet or coiled material on the down stroke of the press by blank punch 45 . on the continuation of the down stroke , the blank is drawn into a cup shaped hat part 40 - 1 . at the bottom of the stroke the panel shape 42 is formed into the top of the hat part 40 - 1 by the punch 45 and cooperating die 46 ( fig3 a ). on the up stroke , the lower curl ring 48 , which is under spring pressure , raises - with the blank punch . the edge 50 of the hat part 40 - 1 is curled outward into the cavity formed by curl ring 48 and blank punch 45 , thus completing a formed hat or cap part 40 - 1 with an outside curl 55 , as shown in fig4 a . in the second operation ( which as mentioned can be another station in the press or in an auxiliary piece of equipment ), at a second station ii - h there are a punch 60 and die 62 having a cavity which receives the hat part 40 - 1 in an inverted - orientation with the outside curl 55 resting in a cavity 63 in die 62 . a punch probe , comprising a plurality ( e . g . three or four ) of radially movable fingers 64 cooperating with a central tapered actuating cam 65 , is inserted first into the product side ( interior ) of the formed hat part 40 - 1 before the punch closes against the hat part 40 - 1 . the fingers 64 are extended by cam 65 ( to the position shown in fig4 b ) and the finger ends 66 extend into the hat part 40 - 1 against the interior of curl 55 to establish the height of the lugs 36 to be formed from material of curl 55 . a curling ring 67 on the punch has a set of cavities in its radially inward section , these corresponding to the location and size of the lugs 36 . the radially outward region of ring 67 has corresponding inward extending surfaces 68 which move material from the outside curl 55 toward the inside of the hat part 40 - 1 , as the curling ring 67 bottoms out over finger ends 66 . this will establish the final form of hat part 40 - 2 , including inwardly directed lugs 36 ( preferably three or four ) above the outward curled edge 50 . the neck / dome structure 11 is formed in seven operations as described hereafter . however the first station blank & amp ; draw operation and the second station redraw operation can if desired , be combined into a single station , reducing the total number of stations to six . the following description will assume that the first and second stations are separate . at the first station i - n , a blank is cut from either sheet or coiled material , and is drawn into a cup shaped part 70 - 1 , as shown in fig5 a & amp ; 6a . at the second station ii - n , the part 70 - 1 is redrawn to form the countersink area 72 and the edge 74 is curled to establish the final outside diameter . this allows the resultant part 70 - 2 to be placed into a belt type transfer system from this operation onward , enabling higher production speeds than can be achieved with other forms of transfer systems . it will be appreciated that the first and second stations can remain separate , however in a production atmosphere that would incorporate an automated transfer system , it may be preferred that stations i - n & amp ; ii - n be combined to allow immediate placement of the parts into a belt , or other similar transfer system . at the third station iii - n , part 70 - 2 is redrawn to obtain additional height of the central section 75 , and in the fourth station iv - n a lip 76 is formed , upon which the curl ( formed in the seventh operation , as later described ) will rest , resulting in part 70 - 3 ( fig5 d & amp ; 6d ). in the fifth station v - n , a hole or opening 78 is pierced through the part , and in the sixth station vi - n opening 78 is extruded upward to obtain the material necessary for the curl on part 70 - 4 ( see fig6 f ). then , in the seventh station vii - n the curled seal rim 30 around the drinking opening is formed . the curl is formed through 360 degrees so the raw edge of the material cannot come in contact with the user &# 39 ; s mouth when drinking directly from the container . this results in the part 70 - 5 ( shown in fig6 g ). the lugs 35 can be added to the upper neck section 25 in a further press station . it is also possible to form such lugs in separate auxiliary equipment which employs the technique of rolling threads or the like in thin - walled metal cylindrical or cup shaped parts . in the additional press station viii - n the part 70 - 5 is placed in a die member 80 which includes cavities 81 corresponding to the desired external configuration and location of the lugs 35 . in a preferred embodiment there will be three or four such cavities ( as before ), which will be aligned around the upper neck section at the desired location of the lugs 35 . a punch , 82 having radially expandable fingers 84 operated by a tapered cam 85 , is inserted into the part 70 - 1 and the wall of the neck section is pressed into the die cavities by expanding the fingers radially outward . fingers 84 have embossing parts 86 configured to the size and shape of lugs 35 and are adapted to mate with cavities 81 . after lugs 35 are so formed , the fingers 84 are retracted , the punch 82 and die 80 separate , and the completed neck part 70 - 5 is removed . in this same station , the wing - like lower rim can be reshaped , as by further curling , preparatory for the seaming operation when the end is attached to a filled can body . alternately , using an auxiliary piece of equipment , the wing - like lower rim or seaming curl will be finish shaped , and lugs 35 will be formed at the same time , using rotary techniques . the part 70 - 5 is grasped in a rotating chuck 90 and rotated about a first axis 92 which coincides with the centerline of the upper neck section 25 . cooperating rotatable rolling ( or ironing ) tools , namely an outer anvil 94 rotating on an axis 95 , and an inner die 96 rotating on an axis 97 , are brought into contact with the wall of the neck section . the anvil and it cooperating die , and their respective rotary drives , are movable toward and away from the chuck / part axis 92 in a radial direction and in a longitudinal direction ; thus these parts can be moved into and out of , and toward and away from the surfaces of , the upper neck section 25 of the chucked part 70 - 5 . these rotary anvil 94 and die 96 tools have the male / female configurations of the lugs 35 formed thereon . when the anvil and die are engaged and rotated with the rotating part 70 - 5 , the lug configurations are pressed into the wall of the upper neck section . thus , the present invention provides methods and apparatus for making the neck and hat member container end . the various punches , dies , and related equipment , associated with the progressive stations disclosed , form a means for performing the various steps described so as to manufacture the neck member and cooperating hat member in presses and related machines in a mass production , environment . fig7 illustrates deformed geometry of the hat or cap at 90 psi , in comparison with approximate undeformed geometry , the deformation being due to application of external vertical axial load on the container due to direct stacking of a second container or can on top of another can ( as in fig1 ). testing and computer modeling indicates the hat or cap will tend to lower to minimum position with doming still present in the hat . the seal 32 will tend to push further into the gap between hat member 12 and the external surfaces of the pouring opening , causing a tightening of the seal . fig8 shows deformed geometry of hat member 12 at 90 psi , compared to approximate undeformed geometry of the hat member . the loading is applied to the center of the hat member and the hat member will tend to flatten due to the moment shown . such deformation may cause some outward movement in the sides of the hat member ( shown exaggerated ). this could , potentially , decompress the o - ring seal somewhat , but even in such a lesser pressurized state there is built - in interference between the seal member , the upper neck region at dome , and the cap . therefore , a container fitted with a seal according to this invention will not lose its sealing , although it may experience some lowering of the hat member as seen in the above described situation ( fig . 7 ) in combination with flattening of the hat member . while the methods herein described , and the forms of apparatus for carrying these methods into effect , constitute preferred embodiments of this invention , it is to be understood that the invention is not limited to these precise methods and forms of apparatus , and that changes may be made in either without departing from the scope of the invention , which is defined in the appended claims . | 1 |
the term “ about ” is used herein to mean approximately , roughly , around , or in the region of . when the term “ about ” is used in conjunction with a numerical range , it modifies that range by extending the boundaries above and below the numerical values set forth . in general , the term “ about ” is used herein to modify a numerical value above and below the stated value by a variance of 20 percent up or down ( higher or lower ). the invention is an unsubstituted quaternary ammonium salt composition with other ingredients that comprises a composition that is non - flammable , alcohol - free , non - stinging , highly protonated , and nondermatropic . the composition has a very high hydronium proton count and is created by a process involving the blending of a premix that comprises a highly protonated , non - corrosive , nondermatropic hydronium carrier and a biocide , added to a predetermined quantity of water until it dissolves . in one embodiment , the present hydronium comprises a proton count of between about 4 × 10 20 and about 5 . 8 × 10 23 . in one embodiment , the present hydronium disposed at a ph of from about 1 . 5 to about 1 . 8 is found suitable for hand sanitizing or any applications requiring contact with human skin while the preferable ph range for hard surface sanitizing or any applications where contact with human skin is not a concern , ranges from about 0 . 5 to about 1 . 2 . in one embodiment , the biocide further comprises one or more quaternary ammonium compounds . the described unsubstituted quaternary ammonium salt composition with other ingredients comprises a blend of an inorganic acid , a sulfate , and water or a blend of organic acid , a sulfate , and water . the quaternary ammonium compound is selected from one or more of the group consisting of benzalkonium chloride , cetylpyridinium chloride , silver chloride adsorbed to titanium dioxide ( initially notified under silver chloride ), cetalkonium chloride , benzyldimethyl ( octadecyl ) ammonium chloride , miristalkonium chloride , dimethyldioctylammonium chloride , hydrogen chloride / hydrocholoric acid , silver chloride , dodecylguanidine monohydrochloride , bromine chloride , dimethyloctadecyl [ 3 -( trimethoxysilyl ) propyl ] ammonium chloride , decyldimethyloctylammonium chloride , benzyldimethyloleylammonium chloride , dimethyltetradecyl [ 3 -( trimethoxysilyl ) propyl ] ammonium chloride , benzylcoco alkyldimethyl chlorides , dicocoalkyl dimethyl , chlorides , bis ( hydrogenated tallow alkyl ) dimethyl chlorides , benzyl - c8 - 18 - alkyldimethyl chlorides , benzyl - c12 - 18 - alkyldimethyl chlorides , di - c6 - 12 - alkyldimethyl chlorides , benzyl - c8 - 16 - alkyldimethyl chlorides , di - c8 - 10 - alkyldimethyl chlorides , benzyl - c10 - 16 - alkyldimethyl chlorides , octenidine dihydrochloride di - c8 - 18 alkyldimethyl , chlorides , benzyl - c12 - 14 - alkyldimethyl chlorides , c12 - 14 - alkyl [( ethylphenyl ) methyl ] dimethyl chlorides . the inorganic acid is selected from one or more of the group consisting of sulfuric acid , hydrochloric acid , nitric acid , phosphoric acid , boric acid , hydrofluoric acid , hydrobromic acid . the organic acid selected from one or more of the group consisting of lactic acid , acetic acid , formic acid , citric acid , oxalic acid , uric acid . the solution may further comprise a skin permeation enhancer or conditioner selected from one or more of the group consisting of natural components and vitamins , minerals , urea or anti - oxidants to enhance the composition &# 39 ; s natural skin moisturizing and protection against the spread of acne and psoriasis . a thickener may be added to make a gel formula solution . the thickener is selected from one or more of the group consisting of xanthan gum , alginic acid , sodium alginate , ammonium alginate , calcium alginate , propylene glycol alginate , propane - 1 , 2 - diol alginate , agar , carrageenan , processed euchuema seaweed , furcelleran , aribinogalactan larch gum , locust bean ( carob gum ), oat gum , guar gum , tragacanth , acadia gum ( gum arabic ), karaya gum , tara gum , gellan gum , sorbitol , mannitol , glycerol , konjac , konjac gum , polyoxethylene ( 8 ) sterate , polyoxyl 8 stearate , polyoxyethylene ( 40 ) stearate , polyoxyethylene ( 20 ) sorbitan monolaurate ( polysorbate 20 ), polysorbate 80 , polyoxethylene sorbitan mono - oleate , polyoxethylene sorbitan monopalminate , polysorbate 40 , tween 40 , polyxethylene sorbitan monostearate , polysorbate 60 , tween 60 , polyoxyethylene - 20 - sorbitan tristearate , polysorbate 65 , tween 65 , pectin , amidated pectin , gelatine , ammonium phosphatides , sucrose acetate isobutyrate , saib , sucrose diacetate hexaisobutyrate , glycerol esters of wood rosins , sodium and potassium pyrophosphates , diphosphates , ammonium phosphate ( diabasic and monobasic ), sodium and potassium triphosphate , triphosphate , sodium and potassium polyphosphates , polyphosphates , beta - cyclodextrine , cellulose ( microcrystalline and powdered ), methyl cellulose , ethyl cellulose , hydroxypropyl cellulose , hydroxypropyl methyl cellulose , methylethylcellulose , carboxymethyl cellulose , sodium carboxymethyl cellulose , crosslinked sodium carboxymethyl cellulose , sodium caseinate , magnesium stearate , sodium , potassium and calcium salts of fatty acids , magnesium salts of fatty acids , mono - and diglycerides of fatty acids ( glyceryl monostearate , glyceryl distearate ), acetic and fatty acid esters of glycerol , acetic acid esters of mono - and diglycerides of fatty acids , lactic and fatty acid esters of glycerol , lactic acid esters of mono - and diglycerides of fatty acids , citric and fatty acid esters of glycerol , citric acid esters of mono - and diglycerides of fatty acids , tartaric and fatty acid esters of glycerol , tartaric acid esters of mono - and diglycerides of fatty acids , diacetyltartaric and fatty acid esters of glycerol , mon - and diacetyl tartaric acid esters of mono and diglycerides of fatty acids , mixed acetic and tartaric acid esters of mono - and diglycerides of fatty acids , sucrose esters of fatty acids , sucroglycerides , polyglycerol esters of fatty acids , polyglycerol esters of interesterified ricinoliec acid , propylene glycol mono - and di - esters , propane 1 , 2 - diol esters of fatty acids , lactylated fatty acid esters of glycerol and propane - 1 , 2 - diol , thermally oxidized soy bean oil interacted with mono - and diglycerides of fatty acids , dioctyl sodium sulphosuccinate , sodium oleyl or stearoyl lactylate stearoyl - 2 - lactylate , calcium stearoyl - 2 - lactylate , stearyl tartrate , sorbitan monostearate , sorbitan tristearate , span 65 , sorbitan monolaurate , span 20 , sorbitan mono - oleate , span 80 , sorbitan monopalmitate , span 40 . the unsubstituted quaternary ammonium salt created by the invention was tested by an independent laboratory and the results recorded for each microbe studied . it is important to note that alcohol - based hand sanitizers with or without the active ingredient bzk does not offer the same results against mrsa , c - diff spores , h1n1 . this product is manufactured according to fda tentative final monograph ( 1974 , 1978 , 1991 , 1994 , 2002 ). all testing is performed by an independent registered laboratory , according to test methods described in aoac official method 961 . 02 ( germicidal spray products as disinfectants ), astme 1053 - 97 ( standard test method for efficacy of virucidal agents intended for inanimate surfaces ), and from astm e2111 - 00 ( standard quantitative carrier test method to evaluate the bactericidal , fungicidal , mycobactericidal and sporicidal potencies of liquid chemical germicides ). the fda does not specify testing protocols for this product . copies of full reports are available upon request . the solution also was graded minimally irritating at 2 . 8 ( non - irritant ) on the standardized draize test scale where 0 is non - irritating and 110 is severe / extreme where skin damage will occur . according to wikipedia website , the draize test is an acute toxicity test devised in 1944 by the food and drug administration ( fda ) toxologists john h . draize and jacob m . spines . initially used for testing cosmetics , the procedure involves applying 0 . 5 ml or 0 . 5 g of a test substance to the eye or skin of a restrained , conscious animal , and then leaving it for set amount of time before rinsing it out and recording its effects . the animals are observed for up to 14 days for signs of erythema and edema in the skin test , and redness , swelling , discharge , ulceration , hemorrhaging , cloudiness , or blindness in the tested eye . the test subject is commonly an albino rabbit , though other species are used too , including dogs . the animals are euthanized after testing if the test renders irreversible damage to the eye or skin . animals may be re - used for testing purposes if the product tested causes no permanent damage . animals are typically reused after a “ wash out ” period during which all traces of the tested product are allowed to disperse from the test site . the fda supports the test , stating that “ to date , no single test , or battery of tests , has been accepted by the scientific community as a replacement [ for ] . . . the draize test ” one embodiment of the invention includes the use of the described unsubstituted quaternary ammonium salt composition with other ingredients which are fully incorporated herein by reference , as the ionic carrier premix . in this embodiment , 10 grams of the described highly protonated , low ph , nondermathropic solution are blended in a 1 : 2 ratio with water , by weight . this blend is then added to 5 . 5 grams of benzalkonium chloride , mixed with 3 grams of urea , and 481 . 5 grams of water . the amount of thickener can vary , depending upon the final intended use . 0 . 5 % to 1 % xanthan gum gives a good consistency for a hand gel . the formula is a composition , which is a highly protonated , supercharged , non - corrosive liquid proton suspending composition . the manufacturing process to create the described unsubstituted quaternary ammonium salt with is well known and beginning as early as the 1980 &# 39 ; s various chemists and inventors have experimented with the nature of this reaction of adding acid to the water . generally speaking , these reactions and resulting compounds have lacked stability and the manufacturing process was extremely expensive for commercialization . however , this invention has created a compound reaction of the several elements for making the described unsubstituted quaternary ammonium salt composition with other ingredients of adding sulfuric acid of at least 88 % purity in a controlled manner to water while vigorously stirring and agitating said solution to control the temperature of the exothermic reaction . it should be understood that the preceding is merely a detailed description of one or more embodiments of this invention and that numerous changes to the disclosed embodiments can be made in accordance with the disclosure herein without departing from the spirit and scope of the invention . the preceding description , therefore , is not meant to limit the scope of the invention . rather , the scope of the invention is to be determined only by the appended claims and their equivalents . | 0 |
the invention discloses a method for detecting an end point in a chemical mechanical polishing process by utilizing either an acoustical detection device alone , or a combination of an acoustical detection device and an optical detection device . in the method for utilizing an acoustical detection device alone , the method can be carried out by first providing a cmp apparatus that is contained in an enclosure ; mounting an acoustical sensor in the enclosure ; initiating a cmp process on a semiconductor wafer for removing an uppermost coating layer ; monitoring an acoustical emission generated by the cmp process and recording a volume of the emission ; and stopping the cmp process when the volume of the acoustical emission changes by at least 30 % of its initial volume . preferably , the end point is taken as the point when the acoustical emission changes by at least 50 % of its initial volume . in the preferred embodiment , the changes occurring in the acoustical emission as a cu layer is polished away from a tan layer results in an acoustical emission drop by at least 30 % of its initial volume . however , in other different interfaces between different material layers , the acoustical emission volume may either increase or decrease by at least 30 % when the interface is reached . the end point may further be determined when the acoustical emission volume changes by at least 5 db from its initial volume . in other words , the acoustical emission volume may either go up by at least 5 db or goes down by at least 5 db . in most cmp processes , a total volume during polishing between about 25 db and about 250 db is normally detected . the present invention method for determining end point in a chemical mechanical polishing process may further be carried out as a dual detection method by utilizing both an optical detection device and an acoustical detection device . under such circumstances , the end point can be determined in the cmp process upon the occurrence of at least one of the two events of either when an optical signal received from the sample surface is indicative of an interface between the uppermost coating layer and an underlying layer , or the acoustical signal generated by the cmp process changes by at least 30 % of its initial value . the present invention novel method provides the benefit that it can be practiced either as an acoustical detection method alone , or practiced as a dual detection method in which the acoustical detection assures the accuracy of the optical detection method . for instance , when a window used for the optical detection is damaged or covered with slurry , the acoustical detection method detects the end point to alleviate any problem caused by the failed optical detection method . it should further be noted that , while the prior art shown in fig2 and 3 are illustrative examples of a rotary type cmp apparatus , the present invention embodiment shown in fig6 and 8 are illustrative of linear - type cmp apparatus . the present invention novel method can be practiced in either type of cmp apparatus achieving the same desirable result as long as an acoustical sensing device can be mounted inside the enclosure for the cmp apparatus , i . e ., adjacent to a polishing pad or polishing belt . referring now to fig6 wherein a present invention apparatus 60 is shown . the apparatus 60 is of the linear - type cmp apparatus operated by two rotating rollers 62 and 64 that rotate in a clockwise direction . onto the surfaces of the rollers 62 , 64 , is stretched a polishing belt with a polishing pad 66 mounted thereon . the rollers 62 and 64 are pushed apart at a suitable tension to keep the polishing pad 66 tightly stretched over the rollers . situated over the polishing pad 66 is a polishing head 68 onto which a wafer 70 to be polished is mounted . underneath the polishing pad 66 , is mounted a support platen 72 for supporting the polishing pad 66 when the polishing head 68 is pushed down onto the pad surface . in the middle portion of the polishing pad 66 , is provided a window ( not shown ) for an optical emission device 74 to project an optical emission therethrough for reflectance by the surface of the wafer 70 . the optical detection method is similar to that shown in the prior art , and thus will not be described in detail . on top of the polishing pad 66 is further provided a pad conditioner 76 which may include a conditioning pad 78 mounted on a conditioning head 80 for the conditioning of the polishing pad 66 during the polishing process . slurry solution 82 is dispensed onto the polishing pad 66 by a slurry dispenser ( not shown ). the present invention novel acoustical end point detection device 84 , as shown in fig6 consists of an acoustical sensing head 86 and a signal receiver / controller 88 . the acoustical sensing head 86 may be suitably a microphone that has suitable sensitivity for monitoring acoustical emission signals during the polishing process and recording the signals by the signal receiver / controller 88 . a linear cmp polishing process is shown in fig7 . note that window 88 provided through the polishing pad 66 is shown in fig7 . the polishing head 68 with the wafer 70 mounted thereon rotates and furthermore , traverses on the polishing pad 66 during the polishing process . the acoustical detection device 84 monitors and records an acoustical emission during the polishing process to produce trace 90 shown in fig8 . it is seen in fig8 that during the beginning pat of the polishing process on a cu layer ( coated on an adhesion layer of tan ), the sound volume is essentially constant when the copper is being removed . after a suitable polishing time has passed , i . e ., between about 1 min . and about 10 min ., the volume of acoustical emission in db decreases through several downward steps to again reach a constant level . the several steps indicate an interface of cu and tan has been reached when islands of cu still existed on the surface of the wafer until all cu has been removed to reach the low plateau of the trace 90 . in the preferred embodiment , a noticeable reduction in the sound volume , such as by at least 5 db was noticed when the cu layer is completely removed to reach the adhesion layer of tan . however , as previously described , in other polishing operations , the sound volume may go up depending on the nature and type of the underlying material below the layer that is being removed . the present invention novel method and apparatus for the dual detection of end point in a chemical mechanical polishing method utilizing both an optical detection device and an acoustical detection device have therefore been amply described in the above description and in the appended drawings of fig6 and 8 . while the present invention has been described in an illustrative manner , it should be understood that the terminology used is intended to be in a nature of words of description rather than of limitation . furthermore , while the present invention has been described in terms of a preferred embodiments , it is to be appreciated that those skilled in the art will readily apply these teachings to other possible variations of the inventions . the embodiment of the invention in which an exclusive property or privilege is claimed are defined as follows . | 1 |
the figure shows a sensor 10 in a sectional diagram through a measurement head . sensor 10 is designed as a planar broad - band sensor having a number of individual layers arranged one above the other , optionally structured , for example , by film casting , punching , screen printing , lamination , cutting , sintering , or the like . production of the layer structure will not be discussed further here as part of the present description because it is already known . sensor 10 is used to determine an oxygen concentration in the exhaust gases of internal combustion engines to obtain a control signal for adjusting a fuel - air mixture with which the internal combustion engine is operated . sensor 10 has nernst measurement cell 12 and a pump cell 14 . nernst measurement cell 12 has a first electrode 16 and a second electrode 18 between with there is a solid electrolyte 20 . electrode 16 is exposed to exhaust gas 24 to be measured through a diffusion barrier 22 . sensor 10 has a measurement orifice 26 which can receive exhaust gas 24 . diffusion barrier 22 extends at the base of measurement orifice 26 , forming a cavity 28 withing which electrode 16 is arranged . electrode 18 of nernst measurement cell 12 is arranged in a reference air channel 30 and is exposed to a reference gas such as air which is applied to reference air channel 30 . solid electrolyte 20 is preferably made of zirconium oxide stabilized with yttrium oxide , while electrodes 16 and 18 are made of platinum , for example . sensor 10 is connected to a circuit arrangement 32 , which is used to analyze signals of sensor 10 and to control the sensor . electrodes 16 and 18 are connected to inputs 34 and 36 to which a detection voltage u d of nemst measurement cell 12 is applied . pump cell 14 is composed of a first electrode 38 and a second electrode 40 between which is arranged a solid electrolyte 42 . solid electrolyte 42 is itself made of zirconium oxide stabilized with yttrium oxide , while again , electrodes 38 and 40 may be made of platinum . electrode 38 is also arranged in cavity 28 and is thus also exposed to exhaust gas 24 through diffusion barrier 22 . electrode 40 is covered with a protective layer 44 which is porous so that electrode 40 is exposed directly to exhaust gas 24 . electrode 40 is connected to an input 46 of circuit arrangement 32 , while electrode 38 is connected to electrode 16 and is jointly connected with it to input 34 of circuit arrangement 32 . sensor 10 also includes a heating device 49 formed by a wave - form heater . heating device 49 receives a heating voltage u h . exhaust gas 24 is in cavity 28 above measurement orifice 26 and diffusion barrier 22 and is thus in contact with electrodes 16 of nemst measurement cell 12 and electrode 38 of pump cell 14 . because of the oxygen concentration present in the exhaust gas on which the measurement is to be performed , an oxygen concentration difference is established between electrode 16 and electrode 18 , which is exposed to the reference gas . electrode 16 is connected by terminal 34 to a current source of circuit arrangement 32 which supplies a constant current . because of an oxygen concentration difference prevailing at electrodes 16 and 18 , a certain detection voltage u d is established . nernst measurement cell 12 operates here as a lambda probe , which detects whether there is a high oxygen concentration in exhaust gas 24 or a low oxygen concentration . it is clear on the basis of the oxygen concentration whether the fuel - air mixture with which the internal combustion engine is operating is a lean or rich mixture . when there is a change from the rich range to the lean range or vice versa , detection voltage u d drops or increases accordingly . with the help of circuit arrangement 32 , detection voltage u d is used to determine a pump voltage u p which is to be sent to pump cell 14 between its electrodes 38 and 40 . pump voltage u p is negative or positive , depending on whether detection voltage u d signals that the fuel - air mixture is in the rich or lean range , so that electrode 40 is switched either as a cathode or as an anode . accordingly , a pump current i p is established and can be measured by a measurement device of circuit arrangement 32 . with the help of pump current i p , oxygen ions are pumped either from electrode 40 to electrode 38 or vice versa . measured pump current i p is used to control a device for adjusting the fuel - air mixture with which the internal combustion engine is operated . in addition , it is assumed that the fuel - air mixture with which the internal combustion engine is operated is in a lean range for a long period of time . therefore , a high oxygen content is established in exhaust gas 24 accordingly and is detected by sensor 10 . a corresponding detection voltage u d is applied over the period of lean operation in accordance with the high oxygen content . circuit arrangement 32 here includes a timer 50 , with which detection voltage u d is sampled and a determination is made regarding the period of time over which this has been at a certain height . timer 50 supplies a signal 52 when detection voltage u d is within a certain value range corresponding to lean operation of the internal combustion engine for a definable period of time , which may be , for example , several minutes , hours , or the like . during lean operation of the internal combustion engine , a cathodic pump current i p flows . due to this cathodic pump current i p , oxygen ions are pumped out of cavity 28 via electrode 38 , so that over a long period of time fewer oxygen ions are pumped out of cavity 28 than enter cavity 28 from exhaust gas 24 through diffusion barrier 22 by cathodic pump current i p . due to the declining pump current of the pump cell , nernst measurement cell 12 detects a fuel - air mixture which is becoming richer . sensor 10 is thus subject to a rich drift . the reason for this is the faulty detection of the oxygen concentration in the cavity . the distribution of the pump current to the internal pump electrode and nemst electrode 38 , 16 changes over time to the detriment of the internal pump electrode , so detected nemst voltage u d no longer corresponds to the concentration ratio between cavity 28 and reference air channel 30 , but instead is falsified by a superimposed polarization voltage . it seems to be increased . therefore , the system establishes a higher oxygen concentration than λ = 1 in the cavity . a switching means 54 which causes a pulse - like reversal of pump current i p is driven by signal 52 generated by timer 50 . thus , although pump current i p is flowing as an anodic current in accordance with the actual measurement of the oxygen concentration in exhaust gas 24 , switching device 54 reverses it briefly to a cathodic pump current i p in a pulsed manner . this causes oxygen ions to be pumped from electrode 38 of pump cell 14 to electrode 40 and thus out of cavity 28 in accordance with this pulse - like reversal . a frequency and a duration of the pulses with which pump current i p is reversed briefly depends on signal 52 , which in turn depends on detection voltage u d . it is thus possible to supply different signals 52 at different oxygen concentrations in exhaust gas 24 and in a different time range within which detection voltage u d is in a certain value range . thus , the frequency and / or pulse duration with which pump current i p is reversed can be made variable . the frequency and pulse duration are adjusted so that only the rich drift of sensor 10 is compensated . according to another embodiment , in particular with a pumped reference , it is possible to provide for brief voltage pulses , which are above the measured nernst voltage and have the same polarity , to be applied to nernst measurement cell 12 . according to detection voltage u d which is then impressed on the nernst measurement cell , a great transport of oxygen ions out of cavity 28 into reference air channel 30 through electrode 16 is established . this also eliminates the polarization on electrodes 16 and 38 due to a declining oxygen ion content in cavity 28 during long - term lean operation . due to the fact that oxygen ions in exhaust gas 24 cannot diffuse subsequently through diffusion barrier 22 as rapidly or cannot be pumped through pump cell 14 into cavity 28 as are pumped out through electrode 16 , there is an activation of electrodes 16 and 38 which compensates for the rich drift . the pump status of the pump cell prevailing in lean operation supports this activation . thus , on the whole , the rich drift during long - term lean operation is eliminated by brief , defined rich operation of sensor 10 . | 6 |
comprehension of the present invention can be gained through reference to the drawings in conjunction with a through review of the following explanation . in order to facilitate a full appreciation of the invention , an overview of the preferred embodiment is initially provided . the overview is followed by more detailed explanation and some significant alternative embodiments . by “ paint ” herein is meant not only oil based artist &# 39 ; s paint but also acrylic paint , watercolor paint , ink , charcoal and graphite and other such liquid , solid , emulsions , suspensions , and thixotropic substances applied to a range of substrates for artistic expression purposes . in a first embodiment , the present invention is a device for applying and manipulating paint on a substrate . for purposes of facilitating comprehension , it may be initially thought of a substitute for the traditional well known bristle brush . however , it is easier to clean and allows novel results in use . as shown in fig1 the device 20 has a handle 22 with a proximal end 24 and a distal end 26 . as will be discussed later , the handle may be formed of wood , preferably varnished or lacquered hardwood , plastic or metal . attached to the distal end 26 of the handle 22 is a ferrule 28 . the ferrule 28 is rigid and in a preferred embodiment may be steel , brass , copper or aluminum or a “ nickel ” plated brass to prevent corrosion or other suitable metallic materials . suitable ferrules could also be formed of plastic . preferably , the ferrule 28 is attached to the distal end 26 of the handle 22 by crimping , as represented by one or more crimps 30 . the ferrule 28 preferably is tubular or barrel shaped and extends beyond the distal end 26 of the handle 22 . most preferably , the ferrule 28 is slightly tapered and is narrower in cross section at its distal end than its proximal end . the extension 32 of ferrule 28 defines a cavity 34 bounded by inner surface 36 , as shown in fig2 . this cavity 34 lies adjacent to and extends from the distal end 26 of the handle 22 . a resilient silicone tip 38 is carried by the cavity 34 . more specifically , the tip 38 has a ferrule connecting portion 39 and a paint contacting portion 40 . the tip 38 is provided with a generally three - dimensional working surface 41 having a maximum cross - sectional diameter 42 that is preferably no larger than the maximum diameter of handle 22 . because the painting tip 38 has dimensional characteristics similar to those of conventional bristle brushes in that the maximum cross - sectional diameter 42 of working surface 41 is not greater than a maximum cross - sectional diameter of handle 22 , the operation of the artist &# 39 ; s tool 20 more closely simulates that of a conventional bristle brush than does a spatula - type tool which has a generally two - dimensional working surface and a width dimension of the working surface that is larger , and usually significantly larger , than the maximum cross - sectional diameter of the handle of the spatula - type tool . the fact that working surface 41 of painting tip 38 is a three - dimensional surface , rather than the two - dimensional surface of spatula - type tools , allows the present invention to place and manipulate the paint in a manner more similar to that of a bristle brush . the surface tension characteristics of the non - porous silicone material from which painting tip 38 is formed , when combined with the three - dimensional characteristics of working surface 41 , allow quantities of paint to be “ carried by ” the painting tip 38 in manner somewhat similar to the way that paint is wicked between and carried by the bristles of a bristle brush . in contrast , if an artist desires to move paint with a spatula - type tool , the paint must be scooped onto the two - dimensional working surface of a spatula . the tip 38 is formed of resilient silicone . the preferred silicone is characterized by low compression set ( i . e . forming tips which do not substantially relax over time even under constant pressure , thus allowing maintenance of the locking relationship within the ferrule over time without the use of adhesives which might deteriorate in the presence of solvents ); a high tear strength ( die b , ppi astm 624 method ) of about 50 - 250 ( i . e . forming tips which show little tendency to rip or tear when an artist is actively painting ); hardness , after cure , of from about 20 - 70 , and preferably from about 30 to 60 , shore a durometer hardness ( astm 2240 method ), with 25 - 40 shore a durometer hardness used to form “ softer ” tips and 45 - 60 shore a durometer hardness material used to form “ firmer ” tips . most preferably , the catalyst use to cure the preferred silicone is platinum based ( which provides greater solvent resistance ). however , less expensive peroxide based catalyst systems are believed to be acceptable to form less demanding tips as might be appropriately supplied to children and beginning artists . a preferred source of such material is medical grade silastic etr tm elastomers q7 - 4735 and q7 - 4750 ( an enhanced tear resistant silicone ) available from dow corning , with q7 - 4735 being used to form “ softer ” tips and q7 - 4750 being used to form “ firmer ” tips . these products are supplied as two - part thermal - setting elastomers . a related product , q7 - 4765 is arguably serviceable but results in too “ firm ” a tip for most painting purposes . these three products are also blendable to formulate intermediate hardnesses and q7 - 4765 may be useful , for example , in such blends . it is expected that less costly commercial products having identical or nearly identical properties to q7 - 4735 and q7 - 4750 will be available from the manufacturer in the near future , as “ medical grade ” nature of these particular materials is somewhat expensive due to the additional quality control required to meet medical standards . the q7 - 4535 and q7 - 4750 products are represented by dow corning as consisting of dimethyl and methylvinyl siloxane copolymers and reinforcing silica . other silicones which are serviceable in the production of tips , yet somewhat less desirable are : fluorosilicones ( very solvent resistant but substantially more costly ); general purpose silastics such as gp - 50 and gp - 30 from dow corning ( sufficient strength but less solvent resistant which prevents extensive applications with oil based paints but does allow use with childrens &# 39 ; paints ); rtv ( room temperature vulcanization types ) from dow corning ; lsr ( liquid silicone rubber ) such as lsr 595 - hc and lsr 590 ( molding may be prohibitively expensive .) a notable quality of all the serviceable materials are the surface characteristics of the molded tips . specifically , dry or drying paint does not appear to stick to the surface which results in remarkably easy cleaning of the tool tips after use . although an unlimited variation in tip shapes is possible , the most useful shapes include the following : taper point , as shown in fig5 ; flat chisel , as shown in fig8 ; cupped chisel , as shown in fig9 ; cupped round , as shown in fig1 ; and angle chisel as shown in fig6 . the cup chisel , shown in fig9 and cup round , as shown in fig1 both include concave surfaces which artists rapidly learn to exploit to move and manipulate fresh undried paint upon a substrate surface . the tips are preferably formed by molding , such as injection - compression modling . alternatively , the tips may be cut from cured silicone . of course , a combination of molding and cutting may also be employed . referring again to fig2 the ferrule connecting portion 39 is expanded within the ferrule cavity 34 to provide locking contact with the inner surface 36 . this expansion is caused by an insert 44 . in a preferred embodiment , the insert 44 may be a screw . the screw is installed by rotational advancement into the ferrule connecting portion 39 of the tip 38 . the longitudinal movement of the insert 44 results in lateral expansion of the material of the tip 38 . if the lateral expansion is sufficient , locking contact is generated between the tip 38 and the ferrule 28 . note that the expansion of the tip 38 , within the ferrule connecting portion 39 , is slightly more pronounced near its proximal end where the installation of the insert 44 is initiated . this effect tends to further improve the locking contact within a preferred tapered ferrule 28 . most preferably , however , a complementary taper can be provided to the ferrule connecting portion 39 of the tip 38 , during tip preparation . in a preferred embodiment , tip 38 is oversized by a range of up to 5 % to enhance the fit of tip 38 within ferrule 28 . a raised ring 43 may be provided on tip 38 to assist in the assembly of tip 38 within ferrule 28 by indicating exactly where tip 38 should be positioned with respect to ferrule 28 . during assembly , ring 43 tends to push tip 38 out slightly once tip 38 is positioned within ferrule 28 at the proper position . in one embodiment , an epoxy - based adhesive is applied to the exposed end of insert 44 to create an adhesive bond between the metal of insert 44 and the metal of an inner wall of ferrule 28 as an added security to keep insert 44 locked in position . the insert 44 need not be a screw . instead , locking contact can be caused by installing other suitable inserts such a nail or other hard insertable body . optionally , the insert 44 may also include one or more barbs or rings , such as those found on flooring nails , or other devices to prevent undesired extraction and unintended unlocking of the tip 38 from the ferrule 28 . most preferably the tip 38 also includes a pilot hole , optimally axially extending from the proximal end of the ferrule connecting portion 40 and terminating at the proximal end of the paint contacting portion 42 . although ferrule 28 and insert 44 are a preferred mechanism for attaching tip 38 to handle 22 , it will be recognized that this attachment may be accomplished in other ways , such as by gluing or adhesively affixing a proximal end of tip 38 to distal end 26 of handle 22 . alternatively , a male protrusion on distal end 26 of handle 22 could be inserted into a corresponding female cavity within tip 38 , or conversely a male protrusion on the proximal end of tip 38 could be inserted into a corresponding female cavity in the distal end 26 of handle 22 . in either case , it would be possible to provide additional mechanical or chemical mechanisms , such as barbs , flanges , latches , screw threads , glue or adhesive , to assist in securing the tip 38 to the handle 22 . preparation of an artist tool of the present invention also constitutes another embodiment of the present invention . specifically , the method includes the initial steps of : providing a handle 22 , such as a wooden paint bristle brush handle ; providing a ferrule 28 , generally such as those used on a bristle brush or a common pencil ,; and providing a tip 38 or any of the variety of tip shapes and hardnesses discussed above . next , the tip 38 is inserted into the ferrule 28 with the ferrule connecting portion 39 of the tip 38 situated in the tip carrying cavity 34 of the ferrule 28 and the paint contacting portion 40 extending distally from the ferrule 28 . then , the ferrule connecting portion 39 of the tip 38 is expanded into locking contact within the tip carrying cavity 34 of the ferrule 28 by installing an insert 44 into the ferrule connecting portion 39 of the tip 38 . preferably , a pilot hole is provided in the tip 38 . a preferred pilot hole or insert cavity is undersized relative to the insert 44 but served to facilitate installation . that is , screws , by way of example , have a tendency to wander during installation and a more uniform locking contact tends to be generated by installation of the insert 44 generally axially , longitudinally , and from proximally toward distally within the ferrule connecting portion 39 . if a screw is used for the insert 44 , providing driving rotation to the screw within a ferrule maybe accomplished by a nut driver or a screw driver . finally , the ferrule 28 is attached to the handle 22 . if the device is to be permanent , a crimp 30 attachment may be employed . crimp attachments can be improved and positively located by providing an encircling groove appropriately adjacent the distal end of the handle 22 . the present invention offers the possibility of interchangeably of the tips 38 if a reversible attachment , such as a female threaded ferrule and a male threaded handle are provided . in such an arrangement , an artist can be provided with a reduced quantity of handles and an array of tips 38 . the tips 38 may be interchanged in a reduced quantity of ferrules , or in the alternative , each tip may have a dedicated ferrule and the tips with dedicated ferrules interchanged on a reduced quantity of handles . in such systems , an array of tips may be provided for an artist , either interchangeable separate tip , tips with dedicated ferrules , or complete artist &# 39 ; s tools . although an artist may readily recognize the various shapes available for employment , efficiency is enhanced by providing an inert distinct color indicia to signify the different hardnesses of the available tips . such color indicia can be mixed with the tip material prior to molding to easily achieve this result . in yet another alternative , the present invention allows for simple repair of a damaged artist &# 39 ; s tool by replacement of either a tip or a tip and dedicated ferrule combination . in a most preferred embodiment 120 of fig1 , an integral insert 144 extends from and is integral with a handle 122 . preferably , the integral insert 144 and the handle 122 are formed of molded thermoplastic plastic material , although they could be formed from metal or wood . the integral insert 144 includes a flute 145 , most preferably four radially projecting flutes 145 . these flutes 145 serve to reduce or prevent rotation of the tip 138 relative to the insert 144 . additionally , barbs 146 are present to inhibit inadvertent separation of the tip 138 from the integral insert 144 . elbows 147 on the flutes 145 similarly contribute to preventing expulsion of the integral insert 144 . further , it should be pointed out that the ferrule 128 may be crimped , for example at crimps 131 to further tighten the locking of the ferrule 128 to the tip 138 . preferably , a pilot hole or insert cavity 143 is provided in the tip 138 . the preferred insert cavity 143 is longitudinally oriented within the ferrule connecting portion 139 of the tip 138 . most preferably , the integral insert 144 and the insert cavity 143 have shapes generally complementary to each other while the integral insert 144 is transversely oversized relative to the insert cavity 143 so as to expand the ferrule connecting portion 140 of the tip 138 against the interior surface 136 of the cavity 134 of the ferrule . 128 . the highly desirable quality of embodiment 120 maybe understood when considered as a permanent assembly with multiply redundant attachment systems between the tip 138 to the handle 122 . that is , the tip 138 is held firmly in a number of ways . first , it is locked against the inner surface of the ferrule 128 due to outward expansion , thereby preventing both separation or rotation . second , barbs 146 and elbows 147 also prevent longitudinal movement subsequent to installation of integral insert 144 and contribute to preventing rotation . third , the ferrule 128 is crimped to both the handle 122 and the tip 138 . finally , flutes 145 inhibit rotation . the only remaining significant limitation of this permanent device is the structural quality of the material forming the tip 138 . the multiply redundant attachments become even more remarkable in light of another embodiment of the present invention , a method of forming an artist &# 39 ; s tool such as that depicted in fig1 . the handles 122 are first provided . it is well within the skill of the art to form such handles 122 with integral inserts 144 by injection molding . similarly , ferrules 128 can be prepared from thin metal tubing , and optionally , worked to provide a slight taper by techniques well within the skill of the art . tips 138 of varying shapes and hardnesses can also be molded and or cut from commercial silicone materials previously mentioned . with the tip 138 inserted in the ferrule 132 , the integral insert 144 and handle 122 are longitudinally installed in the insert cavity 143 and the proximal portion 132 of the ferrule 128 , respectively . finally , the ferrule 128 is attached to the distal end of the handle 122 . preferably , the attachment is by crimping and most preferably may be accompanied by crimping the ferrule 128 to the tip 138 as well . in another method of this invention , the integral insert 144 can be first installed in the tip 138 and the ferrule 128 subsequently forced into place and crimped . in an alternative embodiment shown in fig1 , a series of longitudinal slits 150 can be created in tip 138 to enhance the wicking and paint carrying capability of the present invention . the depths of slits 150 can be cut entirely through tip 138 , or only part way throught tip 138 . similarly , the length of slits 150 can be any desired length relative to the length of tip 138 . it is also possible to create a pair of complementary sets of slits , one on each side of tip 138 and leave a center , non - sliced portion therebetween . in addition to creating slits 150 by cutting or slicing tip 138 , it is also possible to remove a portion of the material of tip 138 to create each slit 150 . the paint wicking and carrying capability is enhanced due to the mechanical nature of slits 150 and due to the increased surface area of tip 138 on which the paint can be carried . slits 150 can also be used to create a different type of mark or stroke with the present invention . in conclusion , it can be readily recognized that the present invention , in a number of embodiments provides a new artist tool , a method suitable for large scale economical production of a durable artist &# 39 ; s tool or for interchangeable tips from an array of tips . because numerous modifications may be made of this invention without departing from the spirit thereof , the scope of the invention is not to be limited to the single embodiment illustrated and described . rather , the scope of the invention is to be determined by appended claims and their equivalents . | 1 |
now , the embodiment of this invention will be described in detail below with reference to the accompanying drawings . in the following description , the component elements possessing an identical or similar function will be denoted by the like reference numerals unless in the presence of a special reason . fig1 illustrates a unit display device 1 which partakes in the construction of the image display apparatus of this invention . when the image display apparatus to be constructed is fated to assume a tetragonal display region having a large image plane , the unit display devices 1 are severally disposed from the left lower corner toward upward , rightward and obliquely rightward and wired . when this procedure is repeated on each of the unit display devices , the image display apparatus having a necessary display region is constructed . though the display device 1 is depicted as possessing four inputs , it is required to have at least one input . the inside structure of the unit display device 1 partaking in the construction of the image display apparatus of this invention is illustrated in fig2 . the unit display device 1 illustrated in fig2 comprises a receiving part 2 for simultaneously receiving a plurality of image signals of the form of an image signal packet , a processing part 3 for dividing the image signal packet into the interior and the exterior of display range and processing the data on the position for starting display of that packet ( address ) of the image signal packet outside the display range , a transmitting part 4 for outputting the processed image signal packet , and a display part 5 for displaying the image signal packet judged to fall in the display range . the construction of fig2 enables expansion of the display range by causing a plurality of such unit display devices to be mutually connected . while various methods are available for realizing the display part that serves to display the image signal packet falling in the display range , the method disclosed in japanese patent no . 3520318 directed to an image synthesizing and processing system , for example , may be adopted for this realization . in case display of two image signal packets at the same position is required , the content of display , namely the kind of image to be displayed , is decided by giving to the display part a synthetic control command data prepared in advance or a synthetic control command data synthesized from the relevant image signal packet . an embodiment of the image display apparatus according to the present invention will be described . fig3 illustrates an image display apparatus 20 obtained by connecting five unit display devices 21 to 25 of this invention individually provided with four inputs and input - output terminals of upper , right upper and right sides and consequently enabled to acquire a display image plane of a rectangle lacking the right upper part . the unit display devices have their respective display - limiting positions input and memorized in advance therein . fig3 depicts the flow of the images of a video camera 11 , tuners 12 and 13 , a digital camera 15 and a personal computer 16 as inputs partly via a hub 14 . the input signals from these component devices are invariably in the form of “ an image signal packet having designated the position for starting display ” which will be specifically described herein below . from the personal computer , two , i . e . one elliptic and one quadrilateral , signals are output . the input signals may be entered into the image display apparatus via any of the input terminals thereof . when the input terminals are not sufficient in number , the insufficiency may be coped with by branching the relevant wire by means of the hub 14 . in the case of the image signal which has a larger number of pixels than one image display device can display , the digital camera 15 in fig3 , for example , when handing the image signal having such a number of pixels , causes this image signal to be automatically broken by the information of the position for starting display of the image signal and displayed in four image display devices . when the image of a popular song broadcast received by the tuner 13 and the image of a person photographed by the video camera 11 are so displayed as to allow the positions of their display to overlap , it is made possible to obtain an image illustrating a scene as though the photographed person was dancing on a stage together with the person appearing in the popular song broadcast . the image received by the tuner 12 of fig3 is displayed on the unit display device 23 . the image signal in one line of this display is illustrated in fig4 . the following description will be made with attention focused on the image signal indicated by a horizontal line drawn across an image plane . it is assumed that the position for starting display of the image signal of this one line falls at ( 1310 , 400 ), i . e . the right end of the line of ( x , y ), and the image plane of the image display device measures 640 dots in width and 480 dots in height . the left lower image display device judges this image signal packet to fall outside the range of image display , alters the value of the x coordinate to 670 (= 1310 − 640 ) resulting from deducting the value of the size of the image plane , and outputs this result via the right output terminal . the second image display device which has received this image signal packet similarly alters the value of the x coordinate to 30 (= 670 − 640 ) resulting from deducting the value of the size of the image plane and outputs the result via the right output terminal . the third image display device which has received this image signal packet , owing to the fact that the position for starting display falls in the range of display , divides the image signal packet into the part inside and the part outside the range of display ( the part outside the range is empty in the illustrated case ) and displays the part inside the range in the display part . the automatic transfer of the image signal packet in the upper direction has the same mechanism as above . the vertically and bilaterally connected image display devices altogether complete an image exhibiting a matching property . fig5 illustrates a mechanism for enabling an image of a digital camera , for example , to be displayed as divided in four unit display devices as in an example of the image display apparatus of this invention . the following description will be made with attention focused on the image signal indicated with a horizontal line in the image plane . it is assumed that the position for starting display ( x , y ) of the image signal of this one line falls at ( 50 , 900 ), the image has a length of 1024 dots , and the image plane of the image display device measures 640 dots in width and 480 dots in height . the left lower image display device judges this image signal packet to fall outside the range of image display and alters the value of the y coordinate to 420 (= 900 − 480 ) resulting from deducting the value of the size of the image plane . further , since the width exceeds the size of the image plane , this image display device divides the image signal packet into image signal packets having image lengths of 590 (= 640 − 50 ) dots and 534 (= 1024 − 490 ) dots and fixes the position for starting display ( x , y ) of the latter signal packets at ( 50 , 0 ). the former one of the divided image signal packets is output via the output terminal for the upper side of the display device 21 . the latter one of the divided image signal packets is output via the output terminal for the right upper side of the display device 21 . the upper and the right upper image display devices which have received these image signal packets , owing to the fact that the positions for starting display both fall in the range of display , divide the image signal packets each into a part inside and a part outside the range of display ( the part outside the range is empty in this case ) and display the parts inside the range in the display part . fig6 illustrates one example of the procedure to be followed in causing an image received by the tuner 12 to be displayed by the display device 23 in accordance with the user &# 39 ; s instructions . the tuner 12 comprises a radio receiving part for receiving a television broadcast and outputting such an image signal packet as allows an origin ( 0 , 0 ) to fall on the left lower side and a packet processing part for processing a position for starting display in accordance with the external instructions from the user . since the tuner 12 is consequently enabled to output such an image signal packet as allows an origin ( 0 , 0 ) to fall on the left lower side , the output is displayed in the image display apparatus 20 as illustrated in fig5 . the case in which the user of this image display apparatus 20 instructs the display position of his own choice by the use of a mouse , for example , will be described below . when the user designates ( 1310 , 450 ) as the display position of the left upper side of an image , for example , the click he gives to the mouse causes the designated data to be transmitted to the tuner 12 . the packet processing part of the tuner 12 which has received the designated data adds ( 1310 , 50 ) to the position for starting display of the image signal packet output by the radio receiving part so as to allow coincidence of the position ( 0 , 400 ) of the left upper side of the output image of the tuner 12 with the designated position ( 1310 , 450 ) and outputs the result of this addition . in the television broadcast image plane of fig4 , the position ( x , y )=( 0 , 350 ) for starting display of the image signal from the radio receiving part in one line indicated by a horizontal line is altered by the packet processing part to ( 1310 , 400 ) and output in the altered form . though the display part of fig2 is assumed to have one display image plane in the foregoing description , an alignment having a deviating phase as shown in fig7 ( b ) may be obtained by repeating such a unit display device as shown in fig7 ( a ), for example . in this case , the unit display device as shown in fig7 ( a ) may be configured by the method of this invention or by the conventional method . further , this unit display device has only to produce an output for use in each of the directions possessing translational objectivity . a distinction button so to speak can be established by designating an optional region on a display and providing this region with a button , the depression of which results in enhancing the resolution of an image in that region , and rendering the image in that region distinct or , in the case of a moving image , this distinction button can be established by using means to heighten the refresh rate of the image instead of or in conjunction with the enhancement of the resolution . as regards this concept , the practice of varying the resolution of an image wholly in conformity with instructions has been in vogue heretofore . the adoption of this option , in an environment in which the communication band as utilized for a network is restricted , enables the whole communication band to be suppressed to a low level while allowing a necessary part of an image to be displayed with high definition and ensures ideal response and accomplishes provision of service at a low communication charge . for the purpose of realizing this option , an apparatus as the source of transmission of an image or a projected image is instructed to send the data exclusively in the designated region with high definition by the use of a circuit of fig8 or fig9 . the source of transmission transmits high - definition data containing the coordinates of the relevant part . as a result , it is made possible to increase the amount of the data and enhance the resolution in the designated part while the resolution in the remainder of the region is kept at a suppressed level . a method for sending such partial high - definition data as mentioned above , when the high - definition data is in a rectangular shape , consists in first giving notice of the information concerning the position of the origin of a rectangle ( the right upper apex , for example ), the length of the rectangle and the resolution and subsequently sending the data exclusively ( the sequence of sending the data is properly decided as from the right upper side toward the left and , when the left side is reached , again from the right in the first row directly below , for example ), with the result that the rectangular range will be successfully displayed . when the resolution of the data in this case falls short of the resolution of the display apparatus , the shortage may be properly complemented . in the recognition of disposition of a multiplicity of image planes by a method using connecting ports corresponding to relevant positions , when a multiplicity of image planes are used wholly as a large image plane , it is necessary that the individual display device be so prepared as to recognize their positional relations and function collectively . preferably , this preparation is effected by a simple adjustment . the display device to be connected to another display device , for example , necessitates preparation of four connection ports for use at vertical and bilateral points , uses as the origins the coordinates of the display device that has entered an image signal , obtains image data resulting from rewriting the image signal into position data by subtracting the number of pixels of the display device in the vertical and lateral directions in accordance with the connecting ports of the display device in the vertical and bilateral directions from the origins , and transmits the image data . simultaneous input to a plurality of display devices is also feasible , on the condition that the image signal devices individually have origins of their own . the positions for display of images that are obtained by this method are initialized values . the user is allowed afterward to alter these positions for display of the images to suit his convenience . in this case , the user has only to alter the position data of images while the positions of the origins on the display device side are kept intact . in accordance with the method proposed above , the simultaneous display in the plurality of display devices is accomplished by merely connecting the display devices to the vertical and bilateral ports in confornity with the positions of the image planes without requiring any special procedure for the recognition of dispositions . in the recognition of the dispositions of a multiplicity of image planes by a method using a camera , all the connected display devices are enabled to comprehend automatically the information of their own positions ( also detect the resolution ) by connecting a camera to any of the display devices as illustrated in fig1 ( a ), keeping the whole group of display devices cast in that display image , and issuing to that display device instructions to effect automatic recognition of dispositions . after the display device has been connected , it is made to exchange the information such as of the id and the resolution proper to the device and have the new information registered . the display device , on receiving instructions to effect automatic recognition of dispositions , sends to the display devices of varying ids including itself a projected image capable of discriminating them from the other display devices ( indicating the display devices required to be discriminated in red and the other display devices in blue , for example ) and detects the position of the device by processing the camera image . by informing all the display devices of the result of detection , the individual displays are enabled to know the information of their own positions . since this function resides wholly on the display device side , the camera may be of an ordinary grade . in the recognition of dispositions of a multiplicity of image planes by a method using id display , the display devices are so adapted that when instructions to effect automatic recognition of disposition is issued to any of the display devices through a circuit illustrated in fig1 ( b ), the other display devices are caused to output pertinent numbers . meanwhile , the display device that has received the instructions to effect automatic recognition of disposition is adapted to show the group of icons of the display devices containing corresponding numerals . then , the user is enabled to recognize the dispositions of the multiplicity of image planes by arranging by remote control these icons in the actual positional relation of the display devices . these icons are enabled to reflect their actual sizes by dint of display information , such as the resolution , for example . thus , the recognition of dispositions can be realized without requiring a camera . though the individual displays are mutually connected and are consequently exchanged in information , they are ignorant of their positional relations . the user , therefore , is required to teach them the positional relations by using a representative display device . | 7 |
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