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referring now to the drawings , wherein like reference numerals designate identical or corresponding parts throughout through the several views , and more particularly to fig4 thereof , in fig4 the reference ( 16a ) designates an input device ( intel 8212 by intel corp .) which receives output signals of the terminal detectors ( 3a )-( 3d ), the down counter ( 20 ) and the speed control device ( 19 ); ( 16b ) designates a central processing unit ( cpu ) ( intel 8085a by intel corp .) of a micro - computer ; ( 16c ) designates a read - only memory ( rom ) ( intel 2716 by intel corp .) in which programs and fixed data are memorized ; ( 16d ) designates a random access memory ( ram ) ( intel 2114a by intel corp .) which memorizes data such as the results of processing ; ( 16e ) designates a timer for trap period control ( intel 8155 by intel corp . ); ( 16f ) designates an output device ( intel 8212 by intel corp .) for outputting an output signal from the cpu ( 16b ). in fig5 vdi , vdi + 1 , vdi + 2 . . . vdi + p2 . . . vdi + n . . . vdi + i - 1 , vdi + i , vdi + i + 1 . . . vdi + p1 . . . designate addresses corresponding to the residual distances ; d c0 , d c1 , d c2 , d cb . . . d cn . . . d ci - 1 , d ci , d ci + 1 . . . d ca . . . designate slowdown command data corresponding to the addresses . in fig6 the reference vsp designates a processed terminal speed command ; vsa designates an acceleration command thereof , vsd designates a slowdown command thereof ; ( 01 )-( 04 ) designate operation modes , ( 01 ); a wait mode ; ( 02 ): an acceleration mode ; ( 03 ): constant speed mode ; and ( 04 ): a deceleration mode . in fig7 to 13 , the references ( 31 ), ( 32 ), ( 41 )-( 44 ), ( 51 )-( 54 ), ( 61 )-( 65 ), ( 71 )-( 86 ), ( 91 )-( 95 ) and ( 101 )-( 104 ) designate serial operations of the digital processor ( 16 ). when the start command is fed from the control device ( 19 ) through the input device ( 16a ) into cpu ( 16b ) of the processor ( 16 ), the terminal speed command vsp shown in fig6 is produced by operation of a terminal slowdown command operation program memorized in rom ( 16c ), to output the data from the output device ( 16f ) to d / a converter ( 17 ). the terminal speed command signal vsp produced is characterized by the initial signal vso larger than the normal speed command signal vn in the wait mode ( 01 ), so that the normal speed command signal vn can be always selected from the comparator circuit ( 18 ) so as to prevent an erroneous operation of the comparator circuit ( 18 ). when the start command is input , the operation in the acceleration mode ( 02 ) is performed . that is , d / a converter ( 17 ) outputs the acceleration command vsa which increases at an acceleration which is slightly larger than the gradient ( acceleration ) of the normal speed command signal vn and smaller than the acceleration of the true speed va 1 , va 2 of the car ( 4 ) in fig3 . when the acceleration command vsa reaches to the predetermined speed vsm larger than the rated speed v 1r , the operation in the constant speed mode ( 03 ) is performed to maintain the terminal speed command vsp to the predetermined speed vsm . when the first terminal detector ( 3a ) is actuated by the cam ( 6 ), the pulses corresponding to the predetermined distance l 1 are preset in the down counter ( 20 ) which initiates subtraction upon receiving the output pulses of the pulse generator ( 11 ). the contents of the down counter ( 20 ) correspond to the residual distance from the present position of the car ( 4 ) to the top floor ( 1 ). when the first detector ( 3a ) is actuated , operation in the slowdown mode ( 04 ) commences and the slowdown command vsd is operated and output as follows . that is , the residual distance data corresponding to the contents of the down counter ( 20 ) is input through the input device ( 16a ) and the slowdown command corresponding to this data is extracted from rom ( 16c ) and output via the output device ( 16f ). when the second terminal detector ( 3b ) is actuated by ascending of the car ( 4 ), the pulses corresponding to the predetermined distance l 2 are preset in the down counter ( 20 ) to calibrate the residual distance . thus , the slowdown command vsd is calibrated as shown in fig6 . in the same manner , the pulses corresponding to the predetermined distances l 3 , l 4 are preset by the actuations of the third and fourth terminal detectors ( 3c ), ( 3d ). the slowdown command vsd having high distance accuracy is operated and output . referring to the flow charts of fig7 to 13 , the operations will be further illustrated . in the step ( 31 ) shown in fig7 the initial set is automatically given by connection of the power source to the processor ( 16 ) to shift to the trap waiting step ( 32 ). the initial set of the ram ( 16d ) is given in the step ( 41 ) shown in fig8 and the stack pointer is set in the step ( 42 ) and the trap mask is released in the step ( 43 ) and the trap period control timer ( 16e ) is started in the step ( 44 ). when the trap is input from the timer ( 16e ) to cpu ( 16b ) in the step ( 51 ) shown in fig9 the acceleration command vsa is operated . the down counter ( 20 ) is preset in the step ( 52 ) to extract and to operate the slowdown command vsd , and the terminal speed command vsp is operated in the step ( 54 ). in the step ( 61 ) shown in fig1 , it is determined whether the starting command is output or not . when the starting command is not output , the acceleration command vsa is kept at vso as the datum in the wait mode ( 01 ) in the step ( 62 ). when the starting command is output , it is shifted to the step ( 63 ) to compare the acceleration command vsa with the predetermined vsm . in the case of vsa & lt ; vsm , the sum of the predetermined increase component dva and the acceleration command vsa is used as the new acceleration command vsa in the step ( 64 ). that is , the operation of the acceleration mode ( 02 ) is performed in the step ( 64 ). when the acceleration command vsa increases to be vsa ≧ vsm , the acceleration command vsa is kept in the predetermined value vsm in the step ( 65 ). in the step ( 71 ) shown in fig1 , the condition of the flag s 1 is elected . when it is not set , as shown in figure , the steps ( 72 )-( 74 ) are performed . when it is preset to &# 34 ; 1 &# 34 ; these steps are not performed and operation is shifted to the step ( 75 ). in the step ( 72 ), the operation of the first terminal detector ( 3a ) is determined . when it is actuated , it is shifted to the step ( 73 ) whereas when it is not actuated , it is shifted to the step ( 75 ). in the step ( 73 ), the predetermined distance datum l 1 obtained by actuating the first terminal detector ( 3a ) is preset in the down counter ( 20 ). after actuating the first terminal detector ( 3a ) the flag s 1 is set to &# 34 ; 1 &# 34 ; in the step ( 74 ) in order to perform the steps ( 72 )-( 74 ) only once . in the same manner , when the second terminal detector ( 3b ) is performed at the first and second terminal acceleration in the steps ( 75 )-( 78 ), the predetermined distance datum l 2 is preset into the down counter ( 20 ). in the steps ( 79 )-( 82 ), the predetermined distance datum l 3 is preset into the down counter ( 20 ) by the actuation of the third terminal detector ( 3c ). in the steps ( 83 )-( 86 ), the predetermined distance datum l 4 is preset into the down counter ( 20 ) by the actuation of the fourth terminal detector ( 3d ). the state of the flag s 1 is determined in the step ( 91 ) shown in fig1 . when the flag s 1 is not set to &# 34 ; 1 &# 34 ; , which corresponds to no actuation of the first terminal detector ( 3a ), the slowdown command vsd is kept in correspondence to the predetermined datum vsm in the step ( 92 ). when the flag s 1 is set to &# 34 ; 1 &# 34 ;. corresponding to actuation of the first terminal detector ( 3a ), the steps ( 93 )-( 95 ) are performed . in the step ( 93 ), the residual distance to the top floor ( 1 ) as the datum of the down counter ( 20 ) is input and memorized as the residual distance rds in the corresponding address of the ram ( 16d ). in the step ( 94 ), the sum of the top address vd 1 of the slowdown command data memorized in the rom ( 16c ) and the residual distance rds is set in the index register hl . in the step ( 95 ), the slowdown command datum is extracted from the address given by the index register hl and memorized as the slowdown command vsd in the predetermined address of the ram ( 16d ). in the step ( 101 ) shown in fig1 , the acceleration command vsa operated in the step ( 51 ) is compared with the slowdown command vsd operated in the step ( 53 ). in the case of vsd & gt ; vsa , the acceleration command vsa is memorized as the terminal speed command vsp in the predetermined address of the ram ( 16d ) whereas in the case of vsd ≦ vsa , the slowdown command vsd is memorized in the step ( 103 ) by the same manner . in the step ( 104 ), the terminal speed command vsp is output to the d / a converter ( 17 ) to complete the step ( 54 ). thus , the processor ( 16 ) performs the steps ( 61 ), ( 62 ) shown in fig1 before feeding the starting command to the processor ( 16 ) by the speed control device ( 19 ) whereby the initial speed vso as the constant bias datum as shown in fig6 is output to the d / a converter ( 17 ). when the starting command is fed , the acceleration command vsa increases each constant increase datum dva to the predetermined datum vsm in each trap period in the steps ( 63 )-( 65 ) and the command having the waveform in the acceleration mode ( 02 ) or the constant speed mode ( 03 ) shown in fig6 is output to the d / a converter ( 17 ). when the car ( 4 ) starts ascending driving from a middle floor , the terminal detectors ( 3a )-( 3d ) are not actuated . the step ( 52 ) is not performed . in the steps ( 91 ), ( 92 ) shown in fig1 , the slowdown command vsd is kept in the same datum vsm the same as the acceleration command vsa . when the car ( 4 ) reaches near the top floor ( 1 ), the first terminal detector ( 3a ) is actuated . this , in the steps ( 71 )-( 74 ) shown in fig1 , the datum corresponding to the residual distance l 1 to the top floor ( 1 ) is preset at this time and the flag s 1 is set to &# 34 ; 1 &# 34 ;. in the step ( 91 ) shown in fig1 , the flag s 1 is set to &# 34 ; 1 &# 34 ;. thus , the extraction operation of the slowdown command vsd in the steps ( 93 )-( 95 ) is started . at this time , the contents of the down counter ( 20 ) must be l 1 whereby , the firstly extracted datum is the slowdown command dc l1 corresponding to the residual distance rds . the residual distance rds reduces depending upon the ascending of the car ( 4 ) whereby the slowdown command vsd is changed as d cl1 → . . . d ci → d ci - 1 → . . . . the aforementioned problem will be illustrated . in the step ( 101 ) shown in fig1 , the slowdown command vsd is compared with the acceleration command vsa . when the slowdown command vsd decreases to be vsd & lt ; vsa , the operation mode ( 04 ) is given . in the step ( 103 ), the slowdown command vsd is set as the output vsp to the d / a converter ( 17 ). thus , the waveform reducing depending upon the residual distance as shown in fig6 ( a ) is given as the terminal speed command after the actuation of the terminal detector ( 3a ). when the car ( 4 ) approaches to the top floor ( 1 ), the second terminal detector ( 3b ) is actuated . thus , in the steps ( 75 )-( 78 ) shown in fig1 , the datum corresponding to the residual distance l 2 at that time is preset in the down counter ( 20 ). that is , the residual distance as the datum of the down counter ( 20 ) is calibrated at the position of the actuation of the second terminal detector ( 3b ) whereby the position accuracy is improved and the landing accuracy at the top floor ( 1 ) is improved . the datum extracted in the step ( 53 ) shown in fig1 is calibrated to the slowdown command d c12 corresponding to the residual distance rds = l 2 from the position d cn . when the third and fourth terminal detectors ( 3c ), ( 3d ) are actuated in the same manner , the datum l 3 , l 4 is preset in the down counter ( 20 ) whereby the slowdown command vsd is calibrated as shown in fig6 ( a ) to give the slowdown command having high position accuracy . the acceleration a in the determination of the positions and the number of the terminal detectors ( 3a )-( 3d ) can be calculated from the gradient of the acceleration command vsa shown in fig6 ( a ) which is substantially the same as the gradient of the normal speed command signal vn during acceleration and is smaller than the increase rate of the true speed va 1 - va 2 of the car in fig3 . thus , the positions of the terminal detectors ( 3b ), ( 3c ) can be placed farther the top floor ( 1 ) than the positions shown in fig3 . therefore , the number of the terminal detectors ( 3a )-( 3d ) can be smaller than that of the conventional apparatus . for example , when the acceleration of the normal speed command signal vn is given as 0 . 9 m / s 2 , the gradient of the acceleration command vsa of the terminal speed command signal vsp can be about 1 . 0 m / s 2 . in the case of the elevator having the rated speed of 240 m / min , the number of the terminal detectors ( 3a )-( 3d ) which is sufficient is 5 which is smaller than that of the conventional apparatus by 3 . the terminal speed command signal vsp just after the start , is the constant bias datum vso . even though the gradient of the acceleration command vsa is the same as the gradient of the normal speed command signal vn , there is no possibility to give vsp ( vn in the normal driving ). therefore , the number of the terminal detectors ( 3a )-( 3d ) can be further decreased . as described , in accordance with the present invention , the terminal detectors are placed at positions to provide the acceleration command for increasing from the starting of the car which is lower than the acceleration of the car caused in the starting during the saturated fault of the normal speed command and the terminal slowdown command signal generated at the time reaching to the normal slowdown position in the rated speed driving is equal to the acceleration command datum and the slowdown command for decreasing depending upon the distance to the terminal floor is operated after the actuation of the terminal detectors to output the lower signal among the acceleration command datum and the slowdown command datum as the terminal slowdown command signal whereby the car can be safely slowed down to land it at the terminal floor even though the number of the terminal detectors is small . obviously , numerous modifications and variations of the present invention are possible 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 otherwise than as specifically described herein .
1
in fig1 a - b - c - d - e - f - a represents the operating envelope on a saturated discharge temperature vs . saturated suction temperature graph for a compressor employing r - 22 in a compound cooling configuration . the line b - e represents the boundary between single stage and two - stage operation . the boundary is established based on sump or interstage pressure limited by thrust washer and bearing load as well as oil viscosity . specifically , b - c - d - e - b represents the envelope where single stage operation is more effective and a - b - e - f - a represents the envelope where two - stage operation is more effective . the stippled region , h , represents the region of the operating envelope where suction modulation applied according to the teachings of the present invention can assist in pulldown . compressor 10 has a suction inlet 24 and a discharge 26 which are connected , respectively , to the evaporator 60 and condenser 62 of a refrigeration system . economizer 70 and expansion device 61 are located between evaporator 60 and condenser 62 . suction inlet 24 branches into line 24 - 1 , which , in turn branches into lines 24 - 3 and 24 - 4 which feed the cylinders of the banks of first stage 112 and line 24 - 2 which contains check valve 28 and connects with the crankcase 22 . the first stage 112 discharges hot , high pressure refrigerant gas into line 30 which contains 3 - way valve 32 . depending upon the position of 3 - way valve 32 , the hot high pressure gas from line 30 is supplied either to discharge 26 via line 26 - 1 or to the crankcase via line 34 . gas from the crankcase is drawn via line 36 into the cylinders of the second stage 114 which defines a third bank where the gas is compressed and delivered to discharge line 26 via line 26 - 2 . microprocessor 50 controls the position of 3 - way valve 32 through operator 33 responsive to one or more sensed conditions . pressure sensor 40 senses the pressure in crankcase 22 which is a primary indicator of the operation of compressor 10 since midstage pressure is equal to the square root of the product of the absolute suction and discharge pressures . microprocessor 50 receives zone information representing the set point and temperature in the zone ( s ) being cooled as well as other information such as the inlet and outlet temperatures and / or pressures for compressor 10 , as exemplified by sensor 51 , as well as ambient temperature and condenser entering air temperature . microprocessor 50 controls 3 - way valve 32 through operator 33 to produce two - stage or single stage operation . two - stage operation results when 3 - way valve 32 connects lines 30 and 34 . line 34 leads to the crankcase 22 . gas supplied to line 24 from the evaporator 60 is supplied via lines 24 - 3 and 24 - 4 to the first stage 112 and the gas is compressed and supplied to line 30 and passes via 3 - way valve 32 and line 34 into the crankcase 22 . the gas in the crankcase is then drawn into the second stage 114 via line 36 and the gas is further compressed and directed via lines 26 - 2 and 26 to the condenser . flow of second or high stage discharge gas is prevented from entering the crankcase 22 via line 26 - 1 by 3 - way valve 32 and flow of suction gas into the crankcase 22 via line 24 - 2 is prevented by the back pressure in the crankcase 22 acting on check valve 28 . parallel single stage operation results when 3 - way valve 32 connects lines 30 and 26 - 1 . gas supplied to line 24 from the evaporator 60 is supplied via lines 24 - 3 and 24 - 4 to the first stage 112 and the gas is compressed and supplied to line 30 and passes via 3 - way valve 32 , line 26 - 1 and line 26 to the condenser 62 . gas in the crankcase 22 is at suction pressure so that gas is able to flow from line 24 , through line 24 - 2 and check valve 28 into the crankcase 22 . gas from the crankcase 22 is drawn into the second stage 114 , compressed and discharged via line 26 - 2 into common discharge 26 . once compressor 10 is in operation , the microprocessor 50 will cause 3 - way valve 32 to switch between two - stage and parallel single stage operation essentially in accordance with the appropriate operating envelope , as exemplified in fig1 . specifically , the pressure sensed by pressure sensor 40 is compared to a fixed value to determine whether two - stage or single stage operation is appropriate and 3 - way valve 32 is appropriately positioned . fig2 illustrates the use of suction modulation for capacity control . suction line 24 - 1 divides into lines 24 - 3 and 24 - 4 which respectively feed the two banks of first or low stage 112 . line 24 - 1 contains infinitely variable solenoid valve 44 having coil 45 . valve 44 functions as a suction modulating valve . when capacity control is needed , as sensed by microprocessor 50 through the zone information , coil 45 is actuated by microprocessor 50 causing valve 44 to close thereby reducing the mass flow of refrigerant entering line 24 - 1 from evaporator 60 and reducing compressor capacity . this approach allows greater capacity control because the mass flow of refrigerant entering line 24 - 1 can be reduced in small increments when the compressor 10 is operating in either the single or two - stage mode . as is conventional , economizer 70 is located between condenser 62 and expansion device 61 . basically , economizer 70 is a heat exchanger with flow in line 27 from the condenser 62 being divided into two paths 27 - 1 and 27 - 2 , respectively . the first path is for liquid refrigerant which passes from condenser 62 via lines 27 and 27 - 1 through economizer 70 where it is further cooled thus increasing system capacity . the second path is for liquid refrigerant which passes from condenser 62 via lines 27 and 27 - 2 where it is expanded by expansion device 72 causing further cooling of the liquid refrigerant passing through economizer 70 via line 27 - 1 with the gaseous refrigerant exiting economizer 70 via line 27 - 2 being supplied to line 34 of compressor 10 . economizer operation is only suitable for two - stage operation . accordingly , economizer operation is only possible when microprocessor 50 causes operator 75 to open normally closed valve 74 . as discussed above , the present invention addresses the problem of pulldown of the cooled space when it is above set point . limiting factors include : maximum engine power output which can be addressed by unloading the compressor , engine coolant temperature , system head pressure and compressor discharge pressure and temperature . typically , when faced with operating in the region h of fig1 prior art units would be unable to pulldown the box temperature or would shut down on a safety . if the zone set point is in the low temperature range , microprocessor 50 will try to shift compressor 10 to the two - stage operation as soon as possible on pulldown . in normal operation of the compressor 10 shifting from single stage to two - stage operation during pulldown with high ambient temperature is limited by the midstage or crankcase pressure which is sensed by sensor 40 . by controlling valve 44 during pulldown at high ambient temperature , the suction pressure at compressor 10 can be effectively reduced as will power draw from the engine and the discharge temperature and pressure from compressor 10 due to less gas being compressed which results in a lower crankcase pressure sensed by sensor 40 . with the resulting lower crankcase pressure , compressor 10 will shift to two - stage operation responsive to the zone set point . once compressor 10 has shifted to two - stage operation , zone demand will still be unsatisfied so that extra system capacity can then be achieved by introducing economizer 70 into the system to give what is analogous to the turbo boost on a car engine . economizer operation will be initiated by microprocessor 50 actuating actuator 75 to open valve 74 . once economizer operation is initiated during pulldown , the flow via line 27 - 1 and economizer 70 is subcooled substantially via the flow through line 27 - 2 , expansion device 72 and economizer 70 . the subcooling provided to the flow in line 27 - 1 substantially increases cooling capacity in evaporator 60 and more than compensates for the loss of potential cooling capacity in the flow that is diverted into line 27 - 2 and injected midstage , or into line 34 , of compressor 10 . the extra cooling capacity of the subcooled liquid in line 27 - 1 allows the temperature of the cooled space to be reduced more quickly than if the compressor 10 were operating in the single stage mode . in response to zone demand , microprocessor 50 will continually try to open modulation valve 44 within the limits of unit safeties , thus increasing flow to compressor 10 results in increased system cooling capacity . except for the switchover to two - stage operation during pulldown at high ambient , the use of an economizer , and the use of an infinitely variable solenoid for capacity control the present invention would operate the same as that described in u . s . pat . no . 5 , 577 , 390 . microprocessor 50 is connected to a plurality of sensors and receives inputs representing the sensed ambient temperature , condenser entering air temperature , zone temperature , and zone set point . microprocessor 50 is also connected to crankcase pressure sensor 40 and sensor 51 which is exemplary of a plurality of sensors for sensing the inlet and outlet temperatures and / or pressures for compressor 10 . microprocessor 50 compares the sensed zone temperature and zone set point and , if the sensed ambient or condenser entering air temperature is on the order of 100 ° f ., or above , the sensed zone temperature exceeds the zone set point by 5 ° f ., or more , and the first , second and third banks of compressor 10 are in single stage operation , microprocessor causes the performing of the serial steps of : reducing the capacity of the first stage 112 which defines the first and second banks and thereby the second stage 114 which defines the third bank to reduce crankcase pressure ; switching over from single stage to two - stage operation of compressor 10 ; and , enabling economizer 70 whereby capacity is increased and the pulldown is speeded up . although a preferred embodiment of the present invention has been illustrated and described , other modifications will occur to those skilled in the art . it is therefore intended that the present invention is to be limited only by the scope of the appended claims .
5
the composition of the invention includes sulfur and milk sugar . sulfur has the following properties : atomic weight , 32 . 97 ; atomic number , 16 ; density , 2 . 07 grams per cubic centimeter ; boiling point , 444 . 6 ° c . sulfur is a fine , yellow , somewhat greenish and gritty powder , having a slight odor and a faintly acid taste . it is insoluble in water and is slightly soluble in alcohol , varying depending upon the temperature and the physical form of the sulfur itself . sulfur exists in three forms : crystalline , amorphous , and as a soft or oily substance . it is mostly abundantly obtained from native sulfur found in italy and sicily , but is widely distributed in nature in combination with many metals forming sulfides . the composition of the invention is made according to methods used by homeopathic pharmacopoeia . the composition is prepared according to french pharmacopoeia , &# 34 ; the first liquid hahnemanian dilution ( first lm or first 50 , 000 ) is obtained after the hahnemanian third centecimal &# 34 ;. there are three types of scales in homeopathy whereby the medication is diluted or ground so that its concentration will be lowered : 1 / 10 decimal scale ; 1 / 100 centesimal scale ; 1 / 50 , 000 fifty - thousandth scale or lm scale ( in roman numerals l = 50 and m = 1000 , which means 50 , 000 ). in the decimal scale , 1 part of the medicinal substance is mixed with 9 parts alcohol or water to dilute , or milk sugar to grind , whereby a 1 / 10 substance is obtained . the resulting product is called first decimal . in the centesimal scale , 1 part of the medicinal substance is mixed with 99 parts alcohol or water to dilute , or milk sugar to grind , whereby a 1 / 100 substance is obtained . the resulting product is called first centesimal . if 1 part of the first centesimal is mixed with 99 parts alcohol or water to dilute , or milk sugar to grind , we will obtain a 1 / 10 , 000 substance . this resulting product is called second centesimal . if 1 part of the second centesimal is mixed with 99 parts alcohol or water to dilute , or milk sugar to grind , we will obtain a 1 / 1 , 000 , 000 substance . this resulting product is called third centesimal , and so on thereafter as far as this scale is concerned . in the fifty thousandth scale ( 1 / 50 , 000 or lm scale ) in which the first 50 , 000 or first lm is prepared out of the third centesimal , the procedure is the following : we take 1 part of the 1 / 1 , 000 , 000 concentration in the bottle containing the third centesimal and mix it with 500 parts of 90 % alcohol . then we take 1 part from this mixture and mix it with another 100 parts of alcohol , thereby obtaining a dilution 50 , 000 times lower than the former ( third centesimal ). this resulting product is stored in a bottle labeled as follows : 0 / 1 , or first lm , or first fifty - thousandth . if we take 1 part from the bottle where the 0 / 1 , of first lm , or first fifty thousandth is stored and mix it with 500 parts and then with 100 parts , we will again obtain a dilution 50 , 000 times lower than the previous one . this result should be labeled as follows : 0 / 2 , or second lm , or second fifty - thousandth , and so on thereafter . see , e . g ., the homeopathic pharmacopoeia of the united states , 8th ed ., vol . i , 1979 ; farmacopeia homeopatica brasileira , first ed ., 1976 ; pharmacotechnie et monographies des medicaments courants , vol . ii , 1979 ; farmacopea homeopatica of dr . wilmar schwabe , leipzig , 1929 . to be able to make the above - mentioned dilution , the sulfur must first be ground ( see organon of medicine of samuel hahnemann , ¶ 270 ) until the one one - millionth attenuation ( third centesimal grinding ) is attained . approximately five centigrams of sulfur is first ground according to the following grinding technique : a glazed porcelain mortar , the bottom of which has been turned dull with fine and moist sand , is used . after dividing five grams of milk sugar in three equal parts , to obtain approximately 1 . 67 grams per part , the first 1 . 67 grams is poured into the mortar . approximately five centigrams of the sulfur substance , reduced to powder , is added to the top of this excipient to form a first mixture . the milk sugar used for dynamization should be of prime quality and perfectly pure . dynamization is the dilution of medications followed by 100 blows over a thick book or object bound in leather . in a preferred embodiment one obtains milk sugar that is crystallized over yarn . the sulfur to be dynamized is mixed for a while with the milk sugar powder with a spatula , preferably made of porcelain . then the first mixture is strongly ground for approximately six to seven minutes with a pounding mortar , also preferably porcelain , the bottom of which should also be dull . the first mixture from the bottom of the mortar , as well as the one adhering onto the pounding mortar , must be thoroughly scraped off and mixed using the spatula for three to four minutes to form a homogeneous mass . the mass is ground by exerting strong pressure for approximately six to seven minutes . then the ground mass is again scraped off the bottom of the mortar and the pounding mortar and mixed for approximately three to four minutes . the second 1 . 67 grams of the powdered milk sugar must then be added to the first mixture and mixed for a while with the spatula to form a second mixture . once again the same force will be used to grind the second mixture for approximately six to seven minutes and once again all the second mixture adhered to the bottom of the mortar and the pounding mortar must be scraped off and mixed for approximately three to four minutes . the second mixture is then ground again for an additional approximately six to seven minutes , and then scraped off and mixed for another approximately three to four minutes . the last 1 . 67 grams of the powdered milk sugar is then added to the second mixture and the material is mixed with the spatula , forming a third mixture . as in the previous steps , the third mixture is vigorously ground for approximately six to seven minutes , scraped off and mixed again for approximately three to four minutes , and finally ground for approximately six to seven minutes , followed by thoroughly scraping off all the mass to blend it carefully with the contents of the mortar . the powder thus prepared must be kept away from the sunlight and daylight in a small , well - covered jar on which a label is pasted bearing the name of the substance , sulfur , and the number &# 34 ; 100 &# 34 ; ( one one - hundredth attenuation ) to indicate the first result . to attain the one ten - thousandth attenuation , approximately five centigrams of the powder marked as &# 34 ; 100 &# 34 ; are poured into the mortar with approximately 1 . 67 grams of powdered milk sugar to form a &# 34 ; first 100th &# 34 ; mixture . this is mixed with the spatula and the above procedure is followed , carefully and vigorously grinding each one - third twice for approximately six to seven minutes , followed by scraping off and mixing for approximately three to four minutes before adding the second 1 . 67 grams of milk sugar to form a &# 34 ; second 100th &# 34 ; mixture and then the third 1 . 67 grams of milk sugar to form a &# 34 ; third 100th &# 34 ; mixture . every time that another one - third of the powdered milk sugar is added , the operation must be repeated . once the process is completed , the ground powder is put in a jar , carefully covered and labeled as &# 34 ; 10 , 000 &# 34 ;. using the same procedure described above , approximately five centigrams of the one - ten thousandth preparation is mixed with approximately 1 . 67 grams of powdered milk sugar to form a &# 34 ; first 10 , 000th &# 34 ; mixture , a &# 34 ; second 10 , 000th &# 34 ; mixture , and a &# 34 ; third 10 , 000th &# 34 ; mixture , thereby lowering the concentration to the one - millionth attenuation , so that each five centigrams of the powder contains one one - millionth of the five centigrams of the initial substance . in summary , each of the three preparations , to reach the third centesimal grinding , requires approximately six to seven minutes of grinding six times and approximately three to four minutes of scraping and mixing six times . overall , approximately one hour of work is necessary per each degree of grinding . following the first grinding that lasted one hour , in each five centigrams of powder , the preparation contains one one - hundredth ( 1 / 100 ) of the starting substance . following the second operation , there will remain one ten thousandth ( 1 / 10 , 000 ) of the initial substance . following the third and last operation , there will be one one - millionth ( 1 / 1 , 000 , 000 ) of the primitive substance . the next step is to dissolve approximately five centigrams of the powder ground to the one one - millionth concentration ( third centesimal grinding ) in approximately five hundred drops of a solution prepared with one part 90 % alcohol and four parts distilled water . ethyl alcohol should be used . then , one drop of this mother solution is added into a small jar containing one hundred drops of 95 % alcohol . once the small jar is carefully covered , it is hand - shaken vigorously one hundred times against a resilient and elastic object , for instance , a thick leather - bound book . this liquid constitutes the first degree of dynamization of the medicament . this medicamentous dynamization in alcohol is placed in a small container , such as a cylindrical thimble - shaped container , made preferably of glass or porcelain , the bottom of which should be pierced with a small hole to saturate globules that are intended to be treated . the globules are small cane sugar bits of such a size that one hundred of them will not exceed five centigrams of weight . the dynamized medicament , as a 95 % alcoholic solution , is poured over the globules to thoroughly soak them , and the liquid percolates through the pierced bottom of the container . the container is then turned over and shaken so that the globules fall over filter paper where they are spread out to quickly dry . once the globules are dry , they are placed in another jar that is immediately covered and labeled &# 34 ; i &# 34 ;, for instance , to indicate the first degree of pharmaco - dynamic power . in order to obtain the next dynamization , a drop of water is put in another jar where only one of the small &# 34 ; i &# 34 ; globules is added to dissolve . after adding one hundred drops of 95 % alcohol , it is dynamized by the same procedure described above , and strongly shaken one hundred times . this medicamentous dynamization in alcohol is used in the same manner to saturate five hundred new small granules that are also quickly spread over filter paper , dried and then kept in a clean and well - covered glass jar away from the heat and the daylight . this jar should be labeled &# 34 ; ii &# 34 ;, for instance , to indicate the second degree of power . the same operation is repeated once more to obtain a dynamization in alcohol of one one - hundredth the concentration of the concentration achieved during the second dynamization set of steps . globules from this step are then dissolved in one hundred drops of alcohol at 95 % concentration and shaken one hundred times and then dried . these globules , when saturated prior to drying , represent the fourth degree of dynamization . the concentration of sublimate sulfur ( washed ) to 0 / 4 , of fourth fifty thousandth , or 4 lm is 1 . 6 × 10 - 25 . the concentration of milk sugar ( pure ) and alcohol ( 90 °) is irrelevant because these substances are used merely as a vehicle for the entire process . the globules obtained from the fourth degree of dynamization have been administered to horses showing symptoms of anhidrosis , and the horses were cured of the disease . horses have been treated with this medicamentous dosage in miami , fla . ( eleven horses ); panama city , panama ( twenty - five horses ); and guayaquil , ecuador ( thirty - one horses ). almost all the horses treated were thoroughbred racehorses . ninety - nine point three percent ( 99 . 3 %) of the horses ( sixty - seven horses ) treated were cured . these dramatic cures , in most cases , have been evaluated and certified by veterinarians , trainers , and race course owners and managers . all of the horses treated and cured , except one removed for breeding , subsequently won several races . horse i was a four - year old horse successfully performing as a racehorse until three years of age . at three years of age it began to have unsuccessful performances , developed agitated respiration even at rest , and ceased to sweat while racing , exercising or training . its skin became dry and scaly , its coat dull , and its hair began to fall off its face . treatment with sulfur 0 / 4 l . m . ( four fifty - thousandths ) was established . five milliliters of the medicament , 0 / 4 lm sulfur , were administered three times a day , half an hour from taking any other substance or feed , by suctioning the container ten times at each intake . thirty days later , the horse began to sweat after exercising and breathing improved . thirty days later after the last administration of the medicament , the horse participated once again in a race and its performance was very good . horse ii was a seven - year old horse with excellent pedigree which for five years had participated in races with incredible success . it began to have breathing difficulties even at rest , stopped sweating , its skin became dry and brittle , and its coat became dull and brittle . after taking the medicament , 0 / 4 lm sulfur , for one month and in the same manner as administered to horse i , horse ii began to sweat abundantly and in a foamy manner , and its breathing was no longer agitated . horse ii was again able to race . although its performance on the race track was not the best for its age , being cured of anhydrosis , it was used as a breeder due to its pedigree . horse iii was a four year old horse used in racing , having performed excellently . it ceased racing for one year as it developed agitated respiration , even at rest , and did not sweat during training or exercising . its skin was dry and brittle and its coat was dull and straw - like . after taking the medication for thirty days , 0 / 4 lm sulfur , the horse began to sweat profusely and the coat , skin and respiration improved . after thirty days from the last administration of the medicament , the horse returned to the race courses and won several races . medication was administered as described above with respect to horse i . from the foregoing description those skilled in the art will appreciate that all of the objects of the present invention are realized . a composition and method of treating equine anhidrosis has been shown and described which alleviates the dangerous symptoms associated therewith and allows horses to successfully return to racing activities . while specific embodiments have been shown and described , many variations are possible . this invention can be used on all living beings that are liable to suffer this disease . an example is dairy cattle because the disease can affect milk production . the same dosages and powers should be used for all treatments . having described the invention in detail , those skilled in the art will appreciate that modifications may be made of the invention without departing from its spirit . therefore , it is not intended that the scope of the invention be limited to the specific embodiments illustrated and described . rather , it is intended that the scope of the invention be determined by the appended claims and their equivalents .
0
depending on the meaning given to q the general formula i represents a molecule having or containing an ab or bab configuration wherein b represents the organic mesogenic moiety and a represents the siloxane portion . for example when q is alkyl , alkenyl or aryl the molecule will have the ab structure . when q represents the group --( ch 2 ) n om &# 39 ; the molecule will be of the bab configuration . when l represents ## str7 ## the molecule will consist of a plurality of ab structures linked to a cylic siloxane . in the general formula hereinabove the r groups are preferably n - alkyl containing 1 to 5 carbon atoms , the preferred terminal group t is cn and the preferred ranges of x and n are from 1 to 4 and from 6 to 11 respectively . the siloxane - containing liquid crystals of the invention can be prepared by the reaction between a diorganosiloxane oligomer having not more than 11 silicon atoms and a hydrogen atom bonded to one or both terminal silicon atoms and an alkenyl - terminated mesogen in the presence of a suitable hydrosilylation catalyst , for example a platinum compound or complex . this is represented schematically below for the ab and bab cases ## str8 ## when l represents the cyclic siloxane structure ## str9 ## the liquid crystal may be prepared by first reacting a methylalkenyl , for example methylvinyl , cyclic siloxane with a siloxane oligomer , for example tetramethyldisiloxane , having terminal silicon - bonded hydrogen under conditions whereby one sih per molecule reacts with each alkenyl group . the product is then reacted with the mesogen having terminal unsaturation in the manner illustrated above . the siloxane - containing liquid crystals of this invention can be characterised for their structure and phase types employing known techniques , for example 29 si nmr , x - ray scattering , optical microscopy , differential scanning calorimetry , dielectric relaxation , rheology and optical spectroscopy . the introduction of the siloxane unit acts to suppress the crystalline phase of the mesogenic structural elements and can replace them by a glass phase with a very low glass transition temperature t g thereby improving the response times . further it has been discovered that the smectic phases have an enhanced structural order that has improved the resistance to mechanical shock and may serve to improve the grey - scaling capability . in one embodiment of the invention the group q may contain a dye moiety . this dye moiety may be pleochroic , fluorescent or optically non linearly active , thereby allowing coloured and / or functional materials to be produced . equally such dye structures chemically linked to the siloxane - containing molecules or not may be included as guest into liquid crystalline host . preferred dyes as guests are for example anthraquinone , azo or perylene structures . an advantage of the siloxane compounds of this invention is that they exhibit smectic phases without requiring the additional presence of other liquid crystal materials . however , if desired , they may be mixed between themselves or with other low molar mass or polymeric liquid crystals to improve or otherwise modify bulk properties . they may for example be mixed with known low molar mass ( lmm ) liquid crystals . when used this way they may usefully modify the elastic constants , viscosity coefficients and optical and dielectric properties of the lmm materials . when mixtures of these types are made improvements can be made to the operating temperature range , the viscosity and the multiplexibility . it is preferred that when used this way the lmm material contains at least one compound having the same or a closely related structural group to m and / or m &# 39 ;, for example when m is ## str10 ## then a preferred liquid crystal liquid material contains compounds such as those described in british patent 1 433 130 for example of general formula ## str11 ## where t = 0 or 1 and r &# 39 ; is alkyl or alkoxy , or the siloxane side chain polymers of the type disclosed in gb - a - 2 146 787 . the liquid crystal materials of this invention find application in a variety of devices employing a liquid crystal display . in the most common display type the smectic material is disposed between a pair of substrates which may be of glass or a suitable polymeric material . the inner surfaces are coated with a transparent conducting film , for example indium tin oxide , and an aligning agent . the thickness of the liquid crystal material , usually 1 to 100 μm is defined by spacers which may be for example polymeric films , glass fibres , microbeads or may be photoetched . the conducting film may cover the whole of the inner surface of the substrates or may be etched into a suitable pattern such as a dot matrix or seven segment display . regions of the film may then be addressed by electrical , magnetic or thermal ( e . g . laser ) means to effect a change in texture of the material and thereby display the required information . it has been found that in both the clear and light scattering states the siloxane - containing liquid crystals of this invention are particularly resistant to mechanical shock . it has been further discovered that combinations of fields may be applied , such as electrical and thermal , to allow selective erasure and storage of information so that the materials are particularly suited for optical data recording and storage applications . the thermal source may be a low powered laser and it has been found that suitable choice of laser energy and / or electric field allows grey scale to be achieved . the compound 4 - cyano - 4 &# 39 ;- hexenyloxybiphenyl ( 3 . 40 g ), prepared by the reaction of 6 - bromohex - 1 - ene with 4 - cyano - 4 &# 39 ;- hydroxybiphenyl , was charged to a 2 - necked round bottom flask fitted with stirrer , dropping funnel , nitrogen purge and reflux condenser . to the flask was also added toluene ( 45 . 0 ml ) and , as catalyst , a complex formed between divinyltetramethyldisiloxane and chloroplatinic acid . the catalyst was added in sufficient quantity to provide 8 . 8 × 10 - 5 moles pt ( as metal ) per mole of sih in the pentamethyldisiloxane reactant . the mixture was then heated to 55 ° c . at which temperature pentamethyldisiloxane ( 2 . 00 g , 10 % excess sih to mesogen ) was added from the dropping funnel over a period of 30 minutes . a slight exotherm occurred . the mixture was maintained at 60 ° c . for one hour and then raised to reflux temperature for a further 24 hours . when the reaction mixture had cooled the toluene and excess siloxane were removed employing a rotary evaporator to leave the compound ## str12 ## purification was effected by dissolving the compound in hexane . the insoluble unreacted mesogenic compound was removed by filtration and the hexane then removed by volatilisation at elevated temperature . analysis of the oligomeric product by infra - red spectroscopy indicated disappearance of the sih peak at 2180 cm - 1 . the product was examined by conventional differential scanning calorimetry and polarising microscope techniques to investigate the formation and nature of a mesophase . for the microscopic examination the sample was placed btween two glass slides with a fixed spacing ( 7 μm ) and subjected to several heating and cooling cycles , the change of temperature being controlled at a rate of 2 ° c . per minute . a smectic a phase was observed up to 43 . 8 ° c . and the sample became isotropic at 48 . 9 ° c . employing the procedures described in example 1 pentamethyldisiloxane was reacted with 4 - cyano - 4 &# 39 ;- decenyloxybiphenyl ( 4 . 10 g ), prepared by the reaction of 10 - bromodec - 1 - ene with 4 - cyano - 4 &# 39 ;- hydroxybiphenyl . the product ## str13 ## was purified as described in example 1 and examined by dsc and polarising microscope . the product exhibited a smectic a phase in the range 39 . 4 ° c . to 47 . 5 ° c . and became isotropic at 61 . 3 ° c . the procedure of example 1 was repeated except that the pentamethyldisiloxane was replaced with 1 , 1 . 1 . 3 . 3 . 5 . 5 - heptamethyltrisiloxane ( 3 . 00 g , 10 % excess sih to mesogen ). after purification of the product it was found to exhibit a smectic a phase up to 45 ° c . and became isotropic at 58 ° c . employing the procedure of example 1 , 4 - cyano - 4 &# 39 ;- hexenyloxybiphenyl ( 4 . 19 g ) was reacted with 1 . 1 . 3 . 3 . 5 . 5 . 7 . 7 . 9 . 9 - decamethylpentasiloxane ( 3 . 00 g , 1 : 1 ratio sih to mesogen ). after purification the product ## str14 ## where x = ## str15 ## showed a smectic a phase up to 46 . 5 ° c . and became isotropic at 56 . 7 ° c . the procedure of example 1 was repeated to react together 4 - cyano - 4 &# 39 ;- decenyloxybiphenyl ( 14 . 90 g ) and tetramethyldisiloxane ( 3 . 00 g , 1 : 1 ratio sih to mesogen ). purification was carried out by dissolving the reaction product in dichloromethane , adding methanol , separating the methanol layer and finally volatilising the dichloromethane at elevated temperature . the purified product ## str16 ## where x = ## str17 ## showed a smectic a phase up to 99 . 4 ° c . and became isotropic at 102 . 1 ° c .,
2
to provide a better understanding of the magnetoresistive ( mr ) sensor according to the invention , some of the operating principles of an mr sensor will be reviewed with the aid of fig1 and 2 . the mr sensor according to the invention is provided with transverse as well as longitudinal bias , and the resulting bias profile is such as to render the sensor with optimal sensitivity and side - reading characteristics . the desired shape of the bias profile , will be described with the aid of fig1 relative to the transverse bias profile and with the aid of fig2 with respect to the longitudinal bias profile . fig1 ( a ) is a sketch showing the quiescent magnetization , m , at some skew angle relative to the sense current , i , through the mr sensor 10 . the plot of fig1 ( b ) shows that the transverse magnetization , my , varies linearly with bias strength , hy , when hy & lt ; hu , where hu is the total anisotropy ( induced + shape ) of the mr sensor . when hy ≧ hu , then my = ms and the mr sensor is saturated . the relationship between the resistance r of the mr sensor and the transverse magnetization my is given by ## equ1 ## c mr is the magnetoresistance coefficient which depends on the material used , and this constant is typically 2 to 3 × 10 - 2 for permalloy , for example . the plot shown in fig1 ( c ) shows that the sensor &# 39 ; s resistive signal , δr / r , depends in a quadratic fashion on my . sensitivity , as measured by the slope of this response curve increases monotonically with my until my = ms . at saturation , the sensitivity drops to zero . the sketch of fig1 ( d ) shows that the excitation , originating from magnetic charges in the medium 11 , is largest at the lower edge of the mr sensor 10 . on moving up on the sensor stripe , the flux leaks to the adjacent shields 12 , and excitation decreases . as shown in fig1 ( e ) typically , the excitation is not a &# 34 ; small signal input &# 34 ; but , at least at the lower stripe edge , causes excursions over a substantial portion of the sensor &# 39 ; s operating range . the excitation vanishes at the upper edge , h . considering the bias dependence of sensitivity , and , the profile of excitation , it follows that maximum sensitivity is obtained by locally biasing the sensor to the largest skew permissible without the combined bias and excitation producing saturation . the plot in fig1 ( f ) shows the bias profile for maximum output signal . bias skew increases in accord with the decreasing excitation . with such a bias profile , the excursions of transverse magnetization across the stripe , remain just short of saturation as is shown in fig1 ( g ). fig2 illustrates relationships helpful in understanding the desired longitudinal bias profile . the longitudinal bias must be strong enough to retain the sensor in a single domain state , as is required for the suppression of barkhausen noise . however , the stronger the longitudinal bias , hx , the lower the sensitivity of the mr sensor . typically , the applied longitudinal bias field , ha , is uniform , as indicated in fig2 ( a ), so that the effective bias field , he , being the sum of the applied and the demagnetizing field , hd , peaks about the center of the sensor . the resulting concave sensitivity profile , s , is undesirable since the magnetic head would have a sensitivity that is lowest over the center of the track and highest about the edges of the track . a more advantageous convex sensitivity profile , fig2 ( b ), is attainable with a bias field that increases in strength toward the ends of the sensor . such bias renders the sensor single domain , while leaving its center segment at maximum sensitivity . this is the sensitivity profile that is provided by the present invention . the present invention includes the addition of elongated or &# 34 ; comb &# 34 ; attachments 14 to the mr sensor 10 as is shown in fig3 . an elongated vertical comb attachment 14v , as shown in fig3 ( a ), provides transverse bias while the elongated horizontal attachment or comb 14h of fig3 ( b ) provides longitudinal bias . both bias components are obtained from a configuration like the one shown in fig3 ( c ) in which both horizontal combs 14h and vertical combs 14v are provided on the same mr sensor 10 . the combs 14 are contiguous with and made of the same material as the mr sensor element 10 . it was found that these comb extensions 14h , 14v , when magnetized along their long axis , exert a magnetostatic bias on the mr sensor much like each extension was a permanent magnet . the extensions do , in fact , behave much like permanent magnets in that they exhibit a large hysteresis to magnetization reversal . this hysteresis can easily be ten times larger than the intrinsic coercive force of the sensor material . as the extensions 14 are made of a soft - magnetic material , typically permalloy , such hysteresis may be surprising but is explainable considering their geometry . the long , narrow , extensions have a large shape anisotropy which imposes a substantial magnetostatic energy barrier to magnetization reversal . fig4 shows the effects of transverse extensions . these mr characteristic curves were measured versus a varying transverse field , hy , plus a constant longitudinal field , hx , to retain a single domain magnetization . the three curves show plots of δr / r vs hx for different sensor geometries . curve ( a ) shows the response of a 25 μm wide stripe without extensions ( as a reference ). curve ( b ) shows the response of transverse extensions on both sides of the mr stripe , and curve ( c ) shows the response of transverse extensions only on one side of the stripe . it can be observed from curves ( b ) and ( c ) that the sensor is put into either a positive or a negative state of internal transverse bias , depending on whether the applied field is reduced to zero from positive or from negative saturation . the sensor remains in that state until , at some threshold , ht , of reversed field , the bias state reverses . the curves demonstrate that a transverse bias condition producing a linear response characteristic can be obtained simply by means of the transverse attachments to the sensor geometry . test data on specific embodiments of the comb mr structure has shown that this structure is capable of providing a self - sufficient bias . the question of whether the bias is self - sufficient involves two issues , bias permeance and the level of bias than can be achieved . bias permeance requires the reversal threshold ht to be larger than any disturbing fields seen by the comb structure . the disturb fields may be environmental or originate from the storage medium . whatever their external value , the strength of such fields will be much reduced at the comb location , at least within the usual mr configuration employing magnetic shields as shown in fig6 . the amplitude of this residual disturb field has to be compared to the reversal threshold for ht . typically , ht is in the tens of oe . for example , one specific embodiment similar to fig4 has 2 . 4 μm wide extensions and a reversal threshold of about 30 oe . narrower extensions , 1 . 4 μm wide , have a reversal threshold of about 5 oe . although these values appear safe relative to the expected amplitudes of disturb fields , there remains the concern that repetitive disturb cycles may degrade the bias condition in some fashion . testing was done regarding the possibility of such an occurrence , and no degradation of bias was found after 30 , 000 disturb cycles , even with disturb amplitudes just below ht . bias sufficiently too , depends on comb geometry . as is suggested in fig3 the magnetization , m , is roughly perpendicular to the mr sensor where the comb extension meets the sensor . between extensions , m tends to be parallel to the mr sensor . along the sensor &# 39 ; s upper edge , the average skew angle is determined by the width to spacing ratio of the extensions . on moving downward from the upper edge , the biasing flux from the comb extensions leaks to the adjacent shields . this results in the familiar hyperbolic decay of the transverse bias condition , the same as the decay of the excitation coming from the lower edge , just in the opposite direction . the measured response characteristics reflect , of course , this bias averaged over the height of the mr stripe . such measurements show that the average bias increases with the width to spacing ratio of the comb extensions , and decreases with the height of the mr stripe . one specific embodiment having a geometry similar to fig4 having a nominal width / spacing ratio of 1 . 7 and a 4 μm high mr stripe , exhibits an average internal bias of 15 oe for the one - sided configuration fig4 ( c ) and 30 oe for the two - sided configuration fig4 ( b ). corresponding quiescent skew angles are 14 deg . and 28 deg . respectively , based on a measured shape anisotropy of 64 oe . the degree of bias permeance and sufficiency is hence dictated by geometry and limited by resolution of the fabrication process . bias permeance improves with a decreasing width of the extensions , while bias sufficiently improves with an increasing width / spacing ratio . these competing requirements can both be satisfied only by having small spacings between extensions . in a specific embodiment , the mr sensor has a geometry such as that shown in fig3 ( c ), and a section view of this sensor is shown in fig6 . in this embodiment a plurality of horizontal combs 14h and a plurality of vertical combs ( not shown in fig6 ) are provided on the same mr sensor 10 , and electrical conductor leads 16 ( shown in dashed line in fig3 ( c )) are provided to conduct the read signal to the external read circuits ( not shown ). the mr sensor 10 is positioned to face the magnetic recording medium 20 and is preferably flanked by soft - magnetic shields 12 , but in some cases the shields can be omitted . in the specific embodiment , the mr sensor was fabricated having the geometry of fig3 ( c ) and fig6 and having the following dimensions , and this sensor had suitable performance characteristics . the sensor has an mr stripe height of 3 μm , and comb extensions that are 50 μm long , and 2 . 5 μm , wide with a spacing between comb extensions of 1 μm . by evaluating embodiments having varied values in the relevant geometric parameters , it was concluded that the length to width ratio of the comb extensions should be at least 10 , and that the ratio of the width of the comb extensions to their spacing should be at least two . the comb configuration need not necessarily be used as a self - sufficient bias method . it can also , at no expense , be used to improve upon some other bias provisions . there is no reason , in principle , why the comb configuration cannot be used to enhance any of the bias techniques discussed in the prior art section of this application . for example , it may be used in combination with exchange bias . in this case ( see fig7 ), the sensor consists of a sandwiched mr sensor 10 and exchange bias film 18 , both patterned together to the same geometry such as that shown in fig3 ( a ), for example , fig5 compares response characteristics of two identical comb configurations , one with and one without exchange bias . without exchange bias , as shown in curve ( a ), we have the familiar transverse response , indicating an average , comb - induced bias field of 15 oe . with exchange bias , which , in effect , acts just like a superpositioned dc magnetic field , the loop is offset relative to hy . the amount of offset equals the transverse component of exchange bias . since the direction of exchange bias is adjustable , one can adjust relative bias components in the transverse and the longitudinal direction . in the present example , the bias direction was set at 85 deg . from the x - axis . the curve shows a resulting transverse bias of 32 oe and one would hence estimate a 3 oe longitudinal component . while the invention has been particularly shown and described with reference to a preferred embodiment thereof , it will be understood by those skilled in the art that various other changes in the form and details may be made therein without departing from the spirit and scope of the invention .
6
with reference to fig1 a , a cross - section of a substrate 101 includes a first oxide layer 103 a . the first oxide layer 103 a is partially etched through in a small region to form an oxide window 105 . ( note that the oxide window may also be fully etched through , followed by a brief reoxidation period to regrow a thin silicon dioxide film within the oxide window 105 if silicon is chosen for the substrate 101 .) the oxide window 105 is formed by techniques known to one of skill in the art . below the oxide window 105 , a first drain region 107 is formed by diffusing or implanting a semiconductor dopant through the oxide window 105 . in a specific exemplary embodiment , the substrate 101 is a p - type silicon wafer or p - type well . the first oxide layer 103 a is approximately 200 å thick with the oxide window etched to be approximately 40 å - 70 å thick . the first oxide layer 103 a may be formed by a thermal oxidation technique . alternatively , the first oxide layer 103 a may be deposited by any of a variety of techniques such as chemical vapor deposition ( cvd ), low - pressure cvd ( lpcvd ), plasma - enhanced cvd ( pecvd ), or plasma - assisted cvd ( pacvd ). in fig1 b , a first polysilicon layer 109 a is formed over the first oxide layer 103 a . an oxide - nitride - oxide ( ono ) layer 111 a is then formed over the first polysilicon layer 109 a . a blanket layer of photoresist ( not shown ) is formed over the ono layer 111 a . the layer of photoresist is then exposed ( e . g ., photolithographically patterned ), developed , and etched to form an etched first photoresist mask 113 ( fig1 c ). in a specific exemplary embodiment , the ono layer 111 a is formed to be approximately 80 å thick while the first polysilicon layer 109 a is formed to be about 1000 å to 1500 å thick . layers underlying the etched first photoresist mask 113 are etched with various techniques and / or chemistries to form an etched ono layer 111 b , an etched first polysilicon layer 109 b ( thus forming a polysilicon pedestal ), and an etched first oxide layer 103 b . etching of listed underlying layers can occur through various wet - etch techniques ( e . g ., the first oxide layer 103 a may be etched in hydrofluoric acid , such as contained in a standard buffered oxide etch ( boe ), or orthophosphoric acid ) or dry etch techniques ( e . g ., reactive - ion - etching ( rie )). such etching techniques are known in the semiconductor art . the etched first photoresist mask 113 is stripped and a first blanket conformal oxide layer 115 a is deposited ( fig1 d ) to a thickness of , for example , 80 å to 200 å . a pronounced vertical structure of fig1 d including the etched first oxide layer 103 b , the etched first polysilicon layer 109 b , and portions of the ono layer 111 b and the blanket conformal oxide layer 115 a form a basic structure for a floating gate memory cell , described in more detail , infra . a blanket nitride layer 117 a is then deposited ( fig1 e ) over the conformal oxide layer 115 a . the blanket nitride layer 117 a may be deposited , in a specific exemplary embodiment , to a thickness of 500 å to 1500 å . a second blanket oxide layer ( not shown ) is deposited , patterned , and etched to create an oxide spacer 119 . the etching is typically performed using an rie process , thus removing primarily those portions of the second blanket oxide layer that are substantially parallel ( i . e ., horizontal portions ) to an uppermost surface of the substrate 101 . the rie process thus leaves substantially intact vertical portions of the second blanket oxide layer . therefore , the oxide spacer 119 is self - aligned with a given feature . further , the spacer allows an etch or alignment step surrounding the given feature to be below a photolithographic limit of resolution since the etch or alignment is now based merely on a thickness of the second blanket oxide layer and a step - height of a proximate structure . additionally , other semiconductors or dielectric materials may be used to from a spacer or spacers . since the size of the spacer is dependent on the thickness of chosen film layers , spacers may be created as thin as approximately 30 å or less . here , a thickness of the oxide spacer 119 is chosen to etch back portions of the blanket conformal oxide layer 115 a and the nitride layer 117 a which are not underlying the oxide spacer 119 . for film thicknesses listed in the specific exemplary embodiments given herein , the oxide spacer 119 is approximately 1000 å . in fig1 g , a highly selective reactive ion etch is chosen to etch the blanket nitride layer 117 a thus creating the etched nitride layer 117 b . a skilled artisan will recognize that various chemistries may be chosen which will readily etch , for example , an oxide layer while leaving a nitride layer essentially intact ( or vice versa ) or , in other embodiments , etch a nitride layer while leaving a silicon dioxide layer intact . therefore , etches of one layer may be performed while leaving adjacent layers intact , thus avoiding tedious and critical timing steps . layers comprised of materials dissimilar to the layer being etched thus serve as an etch stop . with reference to fig1 h , a selective etch is used to remove the oxide spacer 119 and form an etched conformal oxide layer 115 b . ( note that , depending on etch chemistry used , either the oxide spacer 119 or the conformal oxide layer 115 a may be etched prior to the other . in either case , the etched nitride lay 117 b serves as an etch mask for the conformal oxide layer 115 a .) also , notice an uppermost oxide layer of the ono layer 111 b has also been etched away , leaving an oxide - nitride layer 111 c . in fig1 i , a second oxide layer 121 followed by a second polysilicon layer 123 a have been deposited . the second polysilicon layer 123 a will form one of the electrodes for the floating gate memory cell , described in more detail , infra . a third oxide layer 125 a is then conformally deposited ( fig1 j ). a second layer of photoresist ( not shown ) is formed over the third oxide layer 125 a . the layer of photoresist is then exposed ( e . g ., photolithographically patterned ), developed , and etched to form an etched second photoresist mask 127 ( fig1 k ). in a specific exemplary embodiment , the second oxide layer 121 is formed to be approximately 50 å to 80 å in thickness . the second polysilicon layer 123 a is about 1500 å thick while the third oxide layer 125 a is approximately 1000 å to 2000 å thick . the etched second photoresist mask 127 serves as an etch mask to etch the third oxide layer 125 a . once the third oxide layer 125 a is etched , an etched third oxide layer 125 b is produced ( fig1 l ). the etched third oxide layer 125 b is produced using a selective etchant such that the underlying second polysilicon layer 123 a serves as an etch stop . with reference to fig1 m , the etched second photoresist mask 127 is removed . a conformal blanket layer of nitride ( not shown ) is deposited , followed by a predominantly vertical etch ( e . g ., rie ) producing nitride spacers 129 on vertical sidewalls of the etched third oxide layer 125 b . the nitride spacers 129 , in one embodiment , are approximately 500 å to 1000 å thick and serve to produce a fine - resolution etch mask for the underlying second polysilicon layer 123 a . the nitride spacers 129 are thus used to produce an etched second polysilicon layer 123 b ( fig1 n ). using dissimilar materials for spacers , etch masks , and etch stops simplifies an entire fabrication process flow by eliminating etch - time as a predominant factor and relying instead on etch selectivity . thus , difficult to control time - critical etch steps are eliminated . in fig1 o , source regions 131 and a second drain region 133 are formed by diffusing or implanting a semiconductor dopant through the second oxide layer 121 where portions of the etched second polysilicon layer 123 b have been etched through . an isolated portion of the etched second polysilicon layer 123 b ( the pedestal on the left side of fig1 o , located between the second drain region 133 and one of the source regions 131 ) will serve as a gate for the select transistor . the etched first polysilicon layer 109 b serves as a floating gate for the memory transistor while the remaining portion of the etched polysilicon layer 123 b ( i . e ., that portion surrounding the floating gate ) will form the control gate of the memory transistor . thus , fig1 o represents a nearly completed eeprom memory cell fabricated in accordance with an exemplary embodiment of the present invention . considering an uppermost surface of the substrate to lie in an x - y plane and a thickness of various film layers ( i . e ., a “ height ” of fabricated features to lie in a z - direction , one can see that any device fabricated in accordance with the present invention benefits from scaling capabilities in all three spatial dimensions . at least three criteria should be considered . first , minimal lateral feature sizes with design rules less than the photolithographic limit may be accomplished in various x - y planar levels through a use of spacers . thus , utilization of design rules far smaller than may be achieved through conventional lithography may be accomplished by fabricating spacers ( for example , using a variety of materials such as oxide , nitride , or polysilicon ) to define device geometries on underlying semiconducting layers . lateral device geometries then relate to a thickness , rather than a width , of a deposited dielectric layer . second , a use of dissimilar materials on adjacent layers and / or between main layers and spacers eliminate critical timing issues and may be adjusted through a judicious use of various selective chemistries . thirdly , differing z - heights , especially for polysilicon or electrode connection levels minimize or alleviate potential electrical shorting or other deleterious effects ( e . g ., such as parasitic coupling ) which occur more readily when such features are at a uniform height . in the foregoing specification , the present invention has been described with reference to specific embodiments thereof . it will , however , be evident to a skilled artisan that various modifications and changes can be made thereto without departing from the broader spirit and scope of the invention as set forth in the appended claims . for example , skilled artisans will appreciate that other types of semiconducting and insulating materials other than those listed may be employed . additional particular process fabrication and deposition techniques , such as low pressure chemical vapor deposition ( lpcvd ), ultra - high vacuum cvd ( uhcvd ), and low pressure tetra - ethoxysilane ( lpteos ) may be readily employed for various layers and still be within the scope of the present invention . although the exemplary embodiments describe particular types of dielectric and semiconductor materials , one skilled in the art will realize that other types of materials and arrangements of materials may also be effectively utilized and achieve the same or similar advantages . also , the substrate itself may be comprised of a non - semiconducting material , for example , a quartz reticle with a deposited and doped polysilicon layer followed by an anneal step ( e . g ., rapid - thermal annealing ( rta ) or an excimer laser annealing ( ela )). additionally , although the exemplary embodiments are described in terms of an eeprom memory cell integrated circuit device , a person of ordinary skill in the art will recognize that other integrated circuit devices may readily benefit from the fabrication process described herein as well . the specification and drawings are , accordingly , to be regarded in an illustrative rather than a restrictive sense .
7
there are provided pharmaceutically active compounds of the formula ## str6 ## wherein : r 1 is substituted or unsubstituted divalent aliphatic group of 1 to 16 carbon atoms , suitably lower alkyl such as methyl , ethyl , n - propyl , iso - propyl , isobutyl , n - pentyl , n - decyl , or cycloalkyl such as cyclopentyl , cyclohexyl , cycloheptyl . the substituents are mono or poly and are selected from the group consisting of lower alkyl such as methyl , ethyl , n - propyl , iso - propyl , isobutyl , n - pentyl , n - decyl , or cycloalkyl such as cyclopentyl , cyclohexyl , cycloheptyl , aryl , suitably phenyl , napthyl , tetrahydronapthyl , indanyl , indenyl , benzofuranyl , benzopyranyl , and aralkyl such as benzyl and phenethyl , r 3 is selected from the group consisting of same group of values as r 5 , if desired it may also form , with the nitrogen to which it is are attached , a saturated heterocycle of 4 - 8 carbon atoms such as pyrrolino , piperidinocer pyrrolidino , r 5 is selected from the group consisting of substituted and unsubstituted alkyl of 1 - 10 carbon atoms such as methyl , ethyl , n - propyl , iso - propyl , isobutyl , n - pentyl , n - decyl , or cycloalkyl such as cyclopentyl , cyclohexyl , cycloheptyl , aryl , suitably phenyl , naphthyl , tetrahydronaphthyl , indanyl , indenyl , benzofuranyl , benzopyranyl , biphenylyl , heterocycloalkyl such as tetrahydrofuranyl , pyrrolidinyl , piperidyl and morpholinyl , wherein the substituents are mono or poly and are selected from the group consisting of lower alkyl , such as methyl , ethyl , n - propyl , iso - propyl , isobutyl , n - pentyl , halo lower alkyl such as trifluoromethyl or cycloalkyl such as cyclopentyl , cyclohexyl , or cycloheptyl , lower alkenyl , such as ethenyl , n - propenyl , iso - propenyl , isobutenyl , n - pentenyl , lower alkynyl , such as ethynyl , n - propynyl , iso - propynyl , isobutynyl , n - pentynyl , nitro , lower alkoxy , such as methoxy , ethoxy , n - propoxy , iso - propoxy , isobutoxy , n - pentoxy , lower alkoxycarbonyl , such as formyloxy , acetoxy , propionyloxy , and butyryloxy , phenyl loweralkyl , such as benzyl , phenyl , phenoxy , mono and polyhalophenyl , mono and polyhalophenoxy , wherein the halo group is fluoro , chloro or bromo , which may also serve as mono and poly substituents for the above named aryl moieties . r 6 and r 7 may be the same or different and are hydrogen or alkanoyl , suitably formyl , acetyl , propionyl , and butyryl . if desired they may also form , with the nitrogen to which they are attached a saturated heterocycle of 4 - 8 carbon atoms such as pyrrolidyl , piperidinyl or pyrrolidinyl . the pharmaceutically acceptable salts and addition salts thereof and the hydrates of said salts and addition salts . also included are the mono and diacyl derivatives thereof , suitably alkanoyl or aralkanoyl derivatives such as acetyl and benzyl derivatives . the compounds of formula i of the present invention may be synthesized by a number of routes of which the following is of most general applicability and is preferred . in this multi - step process , some of the intermediates may be commercially available , however for the sake of completeness , the following process description commences with readily commercially obtainable starting materials . where it is intended to form a compound wherein y is oxygen or sulfur and q is 1 , the starting material is an alkanol , a phenol or a mercaptan ( ii ). where the starting material is an alkanol , there is utilized an excess of the alkanol and the desired quantity to be reacted is treated with one equivalent of alkali metal sodium to form the alkali metal salt in alkanolic solution . in the case of mercaptans or phenols there is utilized an excess of aqueous alkali , suitably sodium hydroxide , which forms the appropriate sodium salt at ambient temperatures in a few minutes . there is then added an excess , suitably a 2 - fold excess of a dihaloalkane over the calculated amount of alkali metal salt , the position of the halo groups determining the length of the r 1 moiety . the mixture is heated under reflux for from about 1 to about 4 hours . a further excess of alkali is added and the reaction mixture held at between 50 ° and 70 ° c . for about 1 / 2 hour . the mixture is cooled , the lower organic layer separated , washed , and distilled under reduced pressure to give water , unreacted dihaloalkane and the desired r 5 oxy or thioalkyl halide ( iv ). acetohydroxamic acid is converted into the corresponding alkali metal hydroxamate ( v ) by addition of alkanoic , suitably an ethanolic solution of alkali metal hydroxide such as sodium or potassium hydroxide . the oxy or thioalkyl halide ( iv ) produced as above , is then added and the mixture heated under reflux , suitably from about 4 to about 8 hours and cooled . precipitated alkali metal halide salt is removed by filtration , the solvents removed under reduced pressure and the residue dissolved in a polar , water miscible , organic solvent , suitably acetone solution , again filtered and concentrated under reduced pressure to yield the corresponding oxy or thioalkyl acetohydroxamate ( vi ). where q is 0 , for example where r 5 - r 1 is benzyl , the corresponding r 5 - r 1 halo compound ( iv ) such as benzyl bromide , may be commercially obtained and this is then reacted directly with the alkali metal acetohydroxamate as described above . the acetohydroxamate ( vi ) is taken up in an alkanol , to which is added an excess of dilute mineral acid , suitably hydrochloric acid , the mixture heated under reflux for about 2 to about 6 , suitably from 4 hours , the solvents removed under pressure and the residue extracted with dry diethyl ether . the solvent is then removed under reduced pressure and the residue recrystallized from an alkanol , suitably ethanol or isopropanol , to give the desired alkyloxyamine hydrochloride ( vii ). the alkyloxyamine hydrochloride ( vii ) is taken up in an alkanol and treated with concentrated aqueous hydrochloric acid until the solution is clearly acidic . the appropriate omega - substituted dicyandiamide , for example , a lower alkyl dicyandiamide ( vii ), is added in excess . the mixture heated under reflux for about 2 to about 6 hours , the solvents removed by evaporation under reduced pressure to yield the desired alkoxy omega - substituted iminodicarbonimidic diamide hydrochloride ( i ). this oil , upon treatment and trituration with anhydrous ether , gives a solid precipitate which may be recrystallized , suitably from ethyl acetate , as the hydrate . where reagent ( viii ) is a mono omega - substituted dicyandiamide carrying no substitution on the remaining imino nitrogen , then r 7 in compound ( viii ) is hydrogen and the thus obtained product of formula i will carry no substituents on the n 2 and n 4 nitrogens , that is to say , r 6 and r 7 will be hydrogen . where both nitrogens of the imino groups are substituted , then r 7 will be other than hydrogen . where it is desired either to place the same substituent on both the n 2 and n 4 nitrogens or , where r 7 is other than hydrogen , to place a different substituent on the n 2 nitrogen , the hydrochloride hydrate ( i ) is suspended in a suitable water immiscible reaction inert organic solvent , suitably ethyl acetate , shaken with an excess of aqueous alkali , suitably aqueous sodium hydroxide , the organic layer separated , dried , and heated under reflux for from about 1 to about 4 hours with an excess of a suitable acylating agent , for example acetyl chloride . after completion of the reaction , the volatile components are removed under reduced pressure to yield the desired n 2 acylated compound . as illustrated above , where r 7 has a value selected from the r 5 group a different synthetic route is desirable . the methodology is that of curd , f . h . s , et al j . chem soc . 1630 - 45 ( 1948 ) and davidson , j . s ., chemistry and industry , 1977 - 8 ( 1965 ). the r 3 isothiocyanate ( xxxi ) is added to a suspension of sodium cyanamide in alkanol , such as ethanol , which precipitates the sodium salt of n - cyano - n &# 39 ;- r 3 thiourea ( xxxii ) which is filtered off , washed with alkanol . methyl iodide is added with rapid stirring at ambient temperature . the product separates . the suspension is cooled in an ice bath , the solids filtered off and washed with water and dried to give n - cyano - n &# 39 ;- r 3 - s - methylisothiourea ( xxxiii ). the isothiourea ( xxxiii ) is added to an alkanolic solution of r 7 amine and the mixture heated for 4 hours in a pressure bottle at about 50 ° c . the resulting clear solution is gradually diluted with water ( 75 cc ) and product crystallizes out to give the dicyano r 3 , r 7 diamide ( xxxiv ). this can then be reacted with the hydroxylamine hydrochloride salt ( viii ) as described previously to obtain the desired compound ( i ). the compounds of the present invention may be made in the form of the monohydrohalic acid addition salts and / or the solvated compound , for example the hydrochloride hydrate or the hydrobromide . other salts may be made however by simple reaction of a base with acid and may be desirable in order to modify the properties of the product such as its toxicity , taste , physical form or rate of release into the body . for example the compounds may be made in the form of the picrate , saccharinate , acetate , acid maleate , acid phthalate , succinate , phosphate , nitrobenzoate , stearate , mandelate , n - acetyl - glycinate , pamoate , sulfonate , di - sulfonate , cyclohexyl sulphamate , citrate , tartrate , or gluconate . stable salts are normally formed with a ratio of one molecule of n , n &# 39 ; poly - substituted imidodicarbonimidic diamides to 1 or 2 molecules of monobasic acid ( or more than one molecule of compound 1 in the case of polybasic acids ) but the possibility of having basic groups as substituents in r 5 for example means that further quantities of acid may be combined with the disubstituted imidodicarbonimidic diamide in some cases . in addition the above molecules may contain various hydrated forms with molecules of water or other solvent included in the molecular formula of the stable entity . the presence of the imino biguanide nitrogens on the molecule create the possibility of forming acyl derivatives by reaction with appropriate substrates . there is disclosed an improved mode of prophylaxis and treatment of infections by one or more of plasmodia ; mycobacteria ; toxoplasmosis and pneumocystis organisms ; and agents causing nocardia infections . the n , n &# 39 ;- substituted asymmetrical biguanides of formula i of the present invention and / or salts and / or derivatives have antimalarial and antibacterial activity as well as effectiveness against some fungi , protozoans , parasites and viruses . additionally , the n &# 34 ; and n &# 39 ;&# 34 ; substituted derivatives of formula i exhibit like activities . in particular , these n , n &# 39 ;- substituted asymmetrical biguanides and salts , as well as their n &# 34 ; and n &# 39 ;&# 34 ; substituted derivatives exhibit antiparasitic activity including activity against the plasmodia of malaria , p . falciparum exhibit antimicrobial activity against mycobacteria including but not limited to m . avium intercellulare , m . avium complex , m . tuberculosis , m . leprae and toxoplasma gondii and pneumocystis organisms such as p . carinii associated with but not limited to immunocompromised patients . in addition , these compounds have activity against nocardia infections . these compounds can also be potentiated in combination with sulfonamides or sulfones to improve the biological spectrum and potency of these compounds of formula i . our use data have been confirmed by additional extensive animal studies supported by the u . s . department of the army . it is our finding that the novel compounds of the present invention show high levels of effectiveness when given orally , as compared to the related triazine derivatives which are known to be poorly absorbed . unlike the related triazine derivatives , this novel series of compounds need not be administered by injection to observe activity comparable to or exceeding other known antimalarial drugs . the method of testing for activity against human malaria parasites is described in detail by l . h . schmidt , am . j . trop . med . & amp ; hygiene , 1978 , 27 : 718 - 737 . the detailed methods include all aspects of animal treatment , infection and evaluation of drug efficacy . the testing is carried out by in vivo screening in a system accepted as the standard for identifying effective antimalarial compounds in humans . the test system utilizes night monkeys ( aotus , trivergatus ) native to columbia . the monkeys are infected with various selected strains of malaria by means of an intravenous inoculation of 5 × 10 6 trophozoites . these trophozoites are obtained directly from p . falciparum infections isolated from humans and the infectious organisms are well characterized with respect to their response to medication . the aotus system is unique in that it makes possible the evaluation of human falciparum malaria . the drugs are administered to the monkeys via stomach tube , and the usual schedule of testing involves daily dosing of the test animals for seven days . activity is determined by the clearance or the eradication of the malarial infection . in table 1 . provided , the activity of title compound jpc7776 , n -[ 3 -( 2 , 4 , 5 - trichlorophenoxy ) propoxy ]- n &# 39 ;-( 1 - methylethyl ) imidodicarbonimidic diamide , is compared to two known antimalarial drugs and is tested comparatively in the highly drug resistant vietnam smith strain of plasmodia falciparum . jpc7776 elicited a clearcut dose response with 8 / 8 animals treated with 3 . 0 mg / kg daily for three days showing clearance of parasites ( 100 % response ). three of eight subjects were cured ( 37 . 5 %). higher doses produced higher cure rates of 75 % and 100 % at doses of 30 . 0 and 150 . 0 mg / kg . comparison with proguanil or cycloguanil up to 150 mg / kg for three days showed no activity ( 0 % response ). table 1______________________________________activity of jpc7776 againstplasmodium falciparum infectionsmalaria dose mg / kg primary treatmentsstrain total daily cleared cured______________________________________smith 0 . 3 0 . 1 0 / 4 0 / 4 3 . 0 1 . 0 8 / 8 3 / 8 30 . 0 10 . 0 7 / 8 6 / 8 1 died early 150 . 0 50 . 0 3 / 3 3 / 3activity of proguanil , againstplasmodium falciparum infectionssmith 3 . 0 1 . 0 0 / 2 0 / 2 30 . 0 10 . 0 0 / 2 0 / 2 150 . 0 50 . 0 0 / 2 0 / 2activity of cycloguanil , againstplasmodium falciparum infectionssmith 3 . 0 1 . 0 0 / 2 0 / 2 30 . 0 10 . 0 0 / 2 0 / 2 150 . 0 50 . 0 0 / 2 0 / 2______________________________________ comparative tests in vivo in mice against plasmodium have been carried out . confirming tests conducted under the auspices of the u . s . department of the army demonstrate favorable oral activity . results demonstrate the superior bioavailability and effectiveness of jpc7776 via the oral route as compared to its corresponding triazine wr99210 and the antimalarial proguanil . these data in table 2 show the number of cures and the effective dose curing 50 % of infected animals ( ed - 50 ) when drugs were administered in peanut oil via the subcutaneous route ( sq ) or when administered as a single oral dose ( po ). premature deaths of animals ( earlier than five days post infection ) are considered as indications of toxicity . table 2 summarizes the reduced toxicity of jpc7776 in this screening test and the superior oral efficacy . a second widely recognized standard test is also presented in table 3 demonstrating a direct comparison of subcutaneous ( sq ) versus oral ( po ) dosage of p . berghei in mice . these tests systems are described in detail in publications by l . rane and d . s . rane , 9th int . congr . trop . med . malaria . ( 1973 ) 1 : 281 (# 406 ) and ( 2 ) t . s . osdedne , p . b . russell and l . rane , j . med . chem . 1967 . 10 : 431 . in this methodology , groups of 5 or 10 mice are infected with a standard inoculum of a blood - induced p . berghei infection and are treated with a single subcutaneous dose ( 9 ng / kg ) of test drug suspended in peanut oil or a single oral dose of test drug suspended in hexamethyl cellulose and tween . the animals are then observed for a maximum of thirty days . control animals normally live between 6 and 7 days . for a drug to be considered effective , test animals must survive at least twice as long as untreated infected control animals . animals surviving for thirty days are considered cured . table 2______________________________________activity of jpc7776 , triazine wr99210 andproguanil against p . berghei infections . comparison of injected vs . oral doses 50 % cures ; 50 % cure ; injected oral po ed - 50 ; test drug sq ed - 50 ; mg / kg mg / kg______________________________________jpc7776 498 567 ( 7 / 10 cures @ 640 ) not toxictriazine 245 no cures @ 640wr99210proguanil no cures no cures , toxic @ & gt ; 160______________________________________ table 3______________________________________comparative oral and subcutaneousefficacy of jpc7776 given to mice infectedwith p . berghei : enhanced survival and cures survival untreated time survival ( days ) ( days ) cures (%) ______________________________________sc dose ; trial 140 mg / kg 11 . 6 6 . 5 0 / 5 0 % 160 n / a ( 30 )* 6 . 5 5 / 5 * 100 % 640 8 . 0 6 . 5 4 / 5 * 80 % sc dose ; trial 2 20 7 . 4 6 . 5 0 / 5 0 % 40 8 . 8 6 . 5 0 / 5 0 % 80 11 . 8 6 . 5 0 / 5 0 % 160 16 . 3 * 6 . 5 2 / 5 * 40 % 320 n / a ( 30 )* 6 . 5 5 / 5 * 100 % 640 n / a ( 30 )* 6 . 5 5 / 5 * 100 % po dose ; trial 1 40 8 . 8 6 . 5 4 / 5 * 80 % 160 15 . 2 * 6 . 5 0 / 0 0 % 640 10 . 0 6 . 5 4 / 5 * 80 % po dose ; trial 2 20 7 . 0 6 . 5 0 / 0 0 % 40 7 . 4 6 . 5 0 / 0 0 % 80 12 . 4 6 . 5 0 / 0 0 % 160 15 . 4 * 6 . 5 0 / 0 0 % 320 22 . 5 * 6 . 5 3 / 5 * 60 % 640 n / a ( 30 ) 6 . 5 5 / 5 * 100 % ______________________________________ * denotes active with survival greater than 2 × controls or cures based on 30 day animal survival . table 4 below provides comparative data for the efficacy of jpc7776 against various strains of malaria as tested in vitro with and without a sulfonamide to determine the benefits , if any , of such coadministration with the compounds which are the subject of this invention . the results shown below , measured as the in vitro dose to inhibit 50 % growth ( id - 50 ) of the malarial parasites grown in standard culture , ( c . s . genther and c . c . smith , j . med . chem . 1977 . 20 : 237 - w243 ) are presented in nanograms per milliliter ( ng / ml ). these data show that the intrinsic activity of jpc7776 is potentiated from 4 to 19 fold ( see id - 50 values ) by sulfonamides in the presence of certain drug resistent parasites . table 4______________________________________potentiation of jpc7776 bysulfonamides in malarial parasitesinhibited in vitro . potentiation factor * jpc776 id - 50 jpc7776 id - 50 without sulfa - with sulfa - methoxazole methoxazoleparasite ( ng / ml ) ( ng / ml ) factor______________________________________african 19 . 41 4 . 88 4fcb 540 . 81 28 . 46 19______________________________________ * potentiation factor is the ratio of 50 % inhibition value ( id50 ) of test drug without sulfonamide divided by the id50 against the same parasite using an equivalent standard value of sulfonamide . evaluation of drugs for activity against pneumocystis carinii is carried out in the widely recognized and well defined testing system developed and published by dr . walter t . hughes . it is widely referred to and is a generally accepted method clearly defined in the literature as to animal maintenance , infection , treatment protocol and evaluation by autopsy and survival of efficacy . a description of the methodology described by w . hughes et al . is found in antimicrob . agents chemother . 1988 , 32 : 623 - 625 . in this method rats are immunosuppressed with high doses of glucocorticosteroids while being protected from bacterial infection by concurrent administration of the antibiotic tetracycline . in a standard evaluation animals are immunosuppressed with steroids and various doses of test compounds are administered for six weeks during which time unprotected animals will develop pneumocystis pneumonitis . the percentage of animals free of the disease represents the effectiveness of a selected dose of test drug . when the animals are immunosuppressed and treated according to the accepted methodology it is normal to observe 75 % or more of the test subjects spontaneously developing pneumocystis . a customary method to produce pneumocystis in the animals is to administer 2 mg of dexamethasone and 50 mg tetracycline hydrochloride per liter of drinking water . the test compounds are integrated in the food . for the positive treatment control compound sulfamethoxazole - trimethoprim ( smx / tmp ) is fully effective to protect the animals from pneumocystis when given at a dosage of 250 mg / kg smx in combination with 50 mg / kg of tmp . another widely used fully effective compound is dapsone at a dosage of 125 mg / kg . table 5 demonstrates the effectiveness of jpc7776 as compared to these known active treatments which are used in treating and preventing pneumocystis infections in humans . jpc 7776 is 100 % effective and is effective as dapsone which is a recommended antipneumocystis drug in humans . table 5______________________________________prevention of pneumocystiscarinii ( pcp ) infectiontreat - daily # # in - effi - ment dose treated fected cacy______________________________________jpc7776 25 mg / kg 10 / 10 0 / 10 100 % dapsone 125 mg / kg 10 / 10 0 / 10 100 % smx / tmp 250 / 50 mg / kg 10 / 10 0 / 10 100 % none -- 10 / 10 10 / 10 0 % ______________________________________ testing of new drugs for activity against mycobacterial infections is carried out in vitro and in vivo in well defined laboratory procedures which have been widely published . the method used to test for biological activity against growing mycobacterium avium complex ( mac ), mycobacterium tuberculosis ( mtb ) and mycobacterium kanasii ( mk ) are described by a . h . gonzalez et al . in j . antimicrob . chemother . 1989 , 24 : 19 - 22 ; s . majumder and m . h . cynamon , amer . soc . for microbiology mtgs , u - 4 , may 1992 , abstract . activity in vitro was determined against clinical isolates of mac , mtb and mk using a broth dilution method . mycobacteria were grown for several days in 7h10 broth , ph 6 . 6 , with 10 % oadc enrichment and 0 . 05 % tween 80 . serial two - fold dilutions of antimicrobial drugs were prepared in 7h10 broth at 128 μg / ml and less . cultures containing a final concentration of approximately 2 . 5 × 10 4 to 6 . 3 × 10 5 cfu / ml were incubated on a rotary shaker at 37 ° c . for 7 days and read where the minimum inhibitory concentration was defined as the mic at the lowest concentration without visual turbidity . jpc7766 in these studies was compared to known active antimicrobial drugs proguanil ( pg ), cycloguanil ( cg ), sulfamethazine ( sm ) and / or dapsone ( dds ). the results are considered favorable at concentrations below 64 μg / ml and are shown in table 6 . jpc7776 tests as superior to the other drugs . table 6______________________________________activity of jpc7776 and other drugs againstmycobacterium isolates m . avium ( mac ), m . tuberculosis ( mtb ) and m . kanasii ( mk ). [ concentrations ( mic ), μg / ml , to inhibit growth in vitro ] isolate jpc7776 dds pg cg smid μg / ml μg / ml μg / ml μg / ml μg / ml______________________________________mac 101 16 16 & gt ; 128 -- & gt ; 128mac lpr 32 32 128 & gt ; 128 32mac far 32 64 64 -- 16mk picciano 8 -- -- 64 64mtb h . sub . 37 r . sub . v 8 -- -- 64 64mtb 311 16 -- -- 64 64______________________________________ the present invention also provides pharmaceutical compositions comprising as active ingredient a compound according to the present invention together with a pharmaceutically acceptable carrier . the water solubility of the hydrochloride of the parent compound and most other salts are not very great , so when solutions are required it may often be necessary to add solubilizing agents to the water , choose non - aqueous solvents , or find a more soluble salt or prepare very dilute solutions . oral formulations are preferred and this invention has the advantage over related products of being readily absorbed by mammals in sufficient levels to make the compounds of the present invention orally active as therapeutic agents . formulations for oral or injected use are based on sufficient solubility as to allow the therapeutic agent to enter solution in the stomach or in an injectable medium . the drug formulations will include tablets , pills , capsules , sachets , granules , powders , chewing gums , suspensions , emulsions and solutions : particularly preferred for oral use are tablets and capsules of all varieties and microbe - free solutions for injection or infusion . where appropriate and necessary the formulations may include diluents , binding agents , dispersing agents , surface - active agents , lubricating agents , coating materials , flavoring agents , coloring agents , controlled release formulations , sweeteners or any other pharmaceutically acceptable additives , for example , gelatin , sodium starch glycolate , lactose , starch , talc , magnesium stearate , microcrystalline cellulose , povidone , hydrogenated or unsaturated oils , polyglycols , syrups or other aqueous solutions . where the formulations are tablets or capsules and the like the formulations may be presented as premeasured unit doses or in multidose containers from which the appropriate unit dose may be withdrawn . the injectable form may be an aqueous or nonaqueous solution , suspension or emulsion in a pharmaceutically acceptable liquid , e . g . sterile pyrogen - free water or parenterally acceptable oils or mixture of liquids which may contain bacteriostatic agents , antioxidants or other preservatives and stabilizers , buffers ( preferably but not limited to a physiological ph range of 6 . 5 - 7 . 7 , solutes to render the solution isotonic with the blood , thickening agents , suspending agents or other pharmaceutically acceptable additives . such forms will be presented in unit dose form such as ampules or disposable injection devices or in multi - dose forms such as a bottle from which the appropriate dose may be withdrawn , or as a solid form or concentrate which can be used to quickly prepare an injectable formulation . all formulations for injection are preferable as sterile and pyrogen free . suppositories containing the compound will also contain suitable carriers , e . g . cocoa butter , polyglycols or other state - of - the - art carriers . in addition to standard pharmaceutical additives there may be included within formulations of the compound other therapeutic agents , particularly including other antimalarials and antiinfectives . the preferred dosage range is between 0 . 5 and 10 mg / kg / day . the range is quite large because the physician must use his judgement on whether the dosage is prophylactic and if given to an infected subject , on what the level of infection is . when given as tablets the tablets may contain 25 - 250 mg of active material . a mixture of 39 . 5 grams ( 0 . 20 mol ) of 2 , 4 , 5 - trichlorophenol and 33 ml of 25 % aqueous sodium hydroxide were combined and stirred at ambient temperature for 15 minutes at which time 80 grams ( 40 . 7 ml , 0 . 4 mol ) 1 , 3 dibromopropane were added . the reaction mixture was refluxed for 2 hours at which time an additional 51 ml 14 percent aqueous sodium hydroxide was added and the reaction mixture held at 50 °- 70 ° c . for 30 minutes . upon cooling the lower layer was separated and washed five times with water . the residual organic layer was distilled at 1 mm given several fractions and gave on distillation water and dibromopropane at 30 °- 40 ° c ., and the product which distilled between 120 °- 157 ° c . fifty grams of a colorless oil was collected which solidified on standing to yield 79 % of 3 -( 2 , 4 , 5 - trichlorophenoxy ) propyl bromide ( xii ). acetohydroxamic acid ( 8 . 5 grams , 0 . 13 mol ) was added to 110 ml of an ethanolic solution of sodium hydroxide ( 4 . 0 grams , 0 . 1 mol ). the 3 -( 2 , 4 , 5 - trichlorophenoxy ) propyl bromide ( xii ) ( 31 . 8 grams , 0 . 1 mol ) was added and the mixture refluxed for 6 hours and cooled to room temperature . the solution was filtered and evaporated , the residue dissolved in 100 ml acetone and the solution filtered and concentrated to yield 16 . 0 grams ( 51 %) of 3 -( 2 , 4 , 5 - trichlorophenoxy ) propyl acetohydroxamate ( xiii ), melting point 102 °- 104 ° c . the acetohydroxamate ( xiii ) ( 31 . 3 grams , 0 . 1 mol ) was dissolved in 120 ml of methanol . hydrochloric acid ( 30 ml of a 12 % solution ) was added and the mixture refluxed for 4 hours . the residue was evaporated to dryness under vacuum , washed with dry diethyl ether and recrystallized from isopropyl alcohol ( 90 ml ) giving 15 . 5 grams ( 58 . 7 %) 3 -( 2 , 4 , 5 - trichlorophenoxy ) propyloxy amine hydrochloride ( xiv ), melting point 158 °- 168 ° c . the hydroxylamine hydrochloride ( xiv ) ( 10 grams , 0 . 0267 mol ) in 160 ml ethanol was treated with 6n aqueous hcl until the solution was acidic . isopropyl dicyanodiamide ( 4 . 4 grams , 0 . 0347 mol ) was added and the mixture heated at reflux for 4 hours at which time the solvent was evaporated off . the resulting solid material was soluble in water and ethyl acetate and the resulting oil was treated with anhydrous ether to give a solid precipitate that was filtered , washed with ether and dried . the resulting white solid , recrystallized from ethyl acetate after charcoaling yielded 2 . 0 grams of the titled compound ( xv ) as a monohydrate with a melting point of 100 ° c . ; in accordance with the above procedure but where , in place of 1 , 3 - dibromopropane there is utilized methylene dibromide , 1 , 2 - dibromoethane , 1 , 4 - dibromobutane or 1 , 5 - dibromopentane there is obtained the corresponding methoxy , ethoxy , butoxy or pentoxy analogue respectively . in accordance with the above procedure but where , in place of 1 , 3 - dibromopropane there is utilized 1 , 2 - dibromopropane , 1 , 3 - dibromo - 2 - methoxypropane , 1 , 4 - dibromo - 2 - ethoxybutane or 1 , 5 - dibromo - 3 - ethoxypentane there is obtained the corresponding 2 - methylethyl , 2 - methoxypropoxy , 2 - ethoxybutoxy or 3 - ethoxypentoxy analogue respectively . in similar fashion to the synthesis of ( xv ) 2 , 5 - dichlorothiophenol ( 35 . 8 grams , 0 . 2 mol ) was treated with sodium hydroxide ( 40 ml of 20 % aqueous solution ) and then combined with 1 , 3 - dibromopropane ( 160 grams , 0 . 8 mol ) and refluxed for 4 hours . the mixture was cooled , the aqueous layer separated and neutralized with 20 % sodium hydroxide solution , and the lower layer washed five times with water and distilled at 1 mm hg . the main fraction was collected between 130 °- 145 ° c . as a colorless oil ( 50 grams , 84 %) of 2 , 5 - dichlorothiophenoxy propyl bromide ( xvi ) is further reacted with acetohydroxamic acid as described previously in example 1 and hydrolyzed to give the 3 -( 2 , 5 - dichlorothiophenoxy ) propyloxamine hydrochloride ( xvii ) which is then reacted with isopropyl dicyanodiamide as described previously in example 1 to give the title compound ( xviii ). in accordance with the above procedure but where , in place of 2 , 5 - dichlorothiophenol , there is utilized n - propyl mercaptan , cyclohexyl mercaptan , and 3 - tetrahydropyranol there is obtained the corresponding n - 3 -( 1 - propylthio -, cyclohexylthio -, and n - 3 - tetrahydropyranyloxy ) propyloxy - n &# 39 ;-( 1 - methylethyl ) imidodicarbonimidic diamide hydrochloride . in similar fashion to the synthesis of ( xv ), 4 - chlorothiophenol ( 28 . 9 grams , 0 . 2 mol ) was treated with sodium hydroxide ( 40 ml of 20 % aqueous solution ) and then combined with 1 , 3 - dibromopropane ( 160 grams , 0 . 8 mol ) and refluxed for 4 hours . the mixture was cooled , the aqueous layer separated and neutralized with 20 % sodium hydroxide solution , and the lower layer washed five times with water and distilled at 1 mm hg . the main fraction was collected between 120 °- 130 ° c . as a colorless oil ( 47 . 5 grams , 90 %) which crystallized on standing to give 4 - chlorothiophenoxy propyl bromide ( xix ) is then further reacted with acetohydroxamic acid as described previously in example 1 and hydrolyzed to give the 3 -( 4 - chlorothiophenoxy ) propyloxamine hydrochloride ( xx ). this in turn is reacted with isopropyl dicyanodiamide as described previously in example 1 to give the title compound ( xxi ). in accordance with the above procedure but where , in place of isopropyl dicyanodiamide , there is utilized n &# 34 ;- phenyl - n - isopropyl dicyanodiamide or other n &# 34 ;- substituent such as methyl , ethyl or phenylmethyl , there is obtained the corresponding n - 3 -( 4 - chlorothiophenoxy ) propoxy n &# 39 ;&# 34 ;- phenyl or methyl , ethyl or phenylethyl , n &# 39 ;-( 1 - methylethyl ) imidodicarbonimic diamide hydrochloride . where it is desired to form the n &# 34 ;, n &# 34 ;&# 39 ;- dialkanoyl or respective monoalkanoyl derivatives of the foregoing unsubstituted derivatives in fig1 the latter are treated in the manner set forth in example 4 below , such that an appropriate 1 : 1 molar ratio or an acid chloride or anhydride for mono - substituted or 2 : 1 molar ratio for the disubstituted derivatives allows the product to be obtained . n -[ 2 -( 2 , 4 , 5 - trichlorophenoxy ) propoxy ]- n &# 39 ;-( 1 - methylethyl ) imidodicarbonimidic diamide hydrochloride hydrate ( xv ) ( 1 . 0 gram , 0 . 002 mol ) was suspended in ethyl acetate ( 20 ml ) and shaken with 0 . 1 ml of 25 % aqueous sodium hydroxide solution . the organic layer was separated and dried ( magnesium sulfate ), 0 . 1 ml of acetyl chloride added and the mixture refluxed for 2 hours . the subsequent mixture was concentrated to give 0 . 5 grams ( 47 %) of the title compound ( xxii ) as white crystals , melting point 160 °- 170 ° c . a mixture of 39 . 5 grams ( 0 . 20 mol ) of 2 , 4 , 5 - trichlorophenol was dissolved in 40 ml of 20 % aqueous sodium hydroxide and added dropwise to refluxing dibromoethane ( 85 . 8 ml , 1 mol ) over 1 hour . the mixture was refluxed for 2 hours and allowed to cool to room temperature . upon cooling the lower layer was separated and washed four times with water . the residual organic layer was distilled at 1 mm to give the main fraction between 145 °- 155 ° c . as colorless oil ( 51 . 4 grams , 85 %) which was 2 -( 2 , 4 , 5 - trichlorophenoxy ) ethyl bromide ( xxiii ). the trichlorophenoxy ethyl bromide ( xxiii ) ( 30 . 4 g , 0 . 1 mol ) was added to acetohydroxamic acid ( 8 . 5 grams , 0 . 13 mol ) in 110 ml of ethanolic sodium hydroxide ( 4 . 0 grams , 0 . 1 mol ) as described previously in example 1 and the mixture refluxed for 6 hours , cooled to room temperature , filtered , the ethanol evaporated and the residue dissolved in acetone ( 100 ml ) the solution filtered and concentrated to yield 19 . 2 grams ( 68 %) of 2 -( 2 , 4 , 5 - trichlorophenoxy ) ethyl acetohydroxamate ( xxiv ), melting point 160 °- 162 ° c . the acetohydroxamate ( xxiv ) was hydrolyzed to the 2 -( 2 , 4 , 5 - trichlorophenoxy ) ethoxy amine hydrochloride ( xxv ) as described for the corresponding propyl acetohydroxamate ( xiii ). the ethoxyamine hydrochloride was reacted with isopropyl dicyanodiamide as previously described in example 1 to give the n -[ 2 -( 2 , 4 , 5 - trichlorophenoxy ) ethoxy ]- n &# 39 ;-( 1 - methylethyl ) imidodicarbonimidic diamide hydrochloride ( xxvi ). 2 , 4 , 5 - trichlorobenzyl bromide ( xxvii ) ( 16 . 1 g , 0 . 1 mol ) is added to acetohydroxamic acid ( 8 . 5 grams , 0 . 13 mol ) in 110 ml of ethanolic sodium hydroxide ( 4 . 0 grams , 0 . 1 mol ) as described previously in example 1 and the mixture refluxed for 6 hours , cooled to room temperature and filtered . the ethanol evaporated and the residue dissolved in acetone ( 100 ml ) the solution filtered and concentrated to yield 2 -( 2 , 4 , 5 - trichlorobenzyl ) acetohydroxamate ( xxviii ). the acetohydroxamate ( xxviii ) is hydrolyzed to the 2 , 4 , 5 - trichlorobenzoxy amine hydrochloride ( xxix ) as described for the corresponding propyl acetohydroxamate ( xiii ). the benzoxyamine hydrochloride ( xxix ) was reacted with isopropyl dicyanodiamide as previously described in example 1 to give the n -( 2 , 4 , 5 - trichlorobenzoxy )- n &# 39 ;-( 1 - methylethyl ) imidodicarbonimidic diamide hydrochloride ( xxx ). p - chlorophenyl isothiocyanate ( xxxia ) ( 50 . 7 grams ) is added to a suspension of sodium cyanamide ( 19 . 2 g ) in ethanol ( 30 ml ) with stirring which slowly dissolves and precipitates the sodium salt of n - cyano - n &# 39 ;- p - chlorophenylthiourea ( xxxiia ) which is filtered off , washed with ethanol and dried to yield 36 . 2 grams which are suspended in 200 ml of ethanol and combined with 37 . 6 grams of methyl iodide with rapid stirring at ambient room temperature . the product separates as heat is evolved . the suspension is cooled in an ice bath , the solids filtered , washed with water and dried to give n - cyano - n &# 39 ;- p - chlorophenyl - s - methylisothiourea ( xxxiiia ). in accordance with the above procedure but where in place of p - chlorophenyl isothiocyanate there is utilized the corresponding methyl , ethyl , iso - propyl , propyl and benzyl derivative , there is obtained the corresponding n - cyano - n &# 39 ;- methyl , ethyl , iso - propyl , propyl and benzyl - s - methylisothiourea . the s - methylisothiourea ( xxxiiia ) prepared as above is added to an ethanolic solution of methylamine ( 79 . 4 ml containing 4 . 2 g methylamine ) and the mixture heated for 4 hours in a pressure bottle at 50 ° c . the resulting clear solution was gradually diluted with water ( 75 cc ) and product crystallizes out , is filtered off to give the desired dicyanodiamide ( xxxiva ). in accordance with the above procedure but where in place of methylamine there is utilized the corresponding phenyl , ethyl , iso - propyl , propyl and benzyl amine , there is obtained the corresponding dicyan - n &# 39 ;- phenyl , ethyl , iso - propyl , propyl and benzyl diamide . the dicyanodiamide ( xxxiva ) is then reacted with n - 3 -( 2 , 4 , 5 - trichlorophenoxy ) propoxyamine hydrochloride ( xiv ) as described previously in example i to yield the title compound . one tablet contains 25 mg - 500 mg of active ingredient depending upon the specific organism being treated , due to differential sensitivity of the infectious microbe . ______________________________________ 25 mg . 50 mg . 100 mg . 250 mg . 500 mg . ______________________________________active 25 mg . 50 mg . 100 mg . 250 mg . 500 mg . ingredientmicro - 100 mg . 150 mg . 200 mg . 250 mg . 300 mg . crystallinecellulosepovidone 10 mg . 25 mg . 25 mg . 50 mg . 75 mg . k 29 - 32sodium 20 mg . 30 mg . 40 mg . 50 mg . 60 mg . starchglycolatemagnesium 3 mg . 5 mg . 8 mg . 10 mg . 13 mg . stearatetotal 158 mg . 260 mg . 373 mg . 610 mg . 948 mg . weight100 , 000 15 , 800 g . 26 , 000 g . 37 , 000 g . 61 , 000 g . 94 , 800 gtablets______________________________________ the formulation is for production of 100 , 000 tablets ( 15 . 8 - 94 . 8 kg ). the tablets will be coated with hydroxypropyl methylcellulose , color , titanium dioxide , polyethylene glycol 6000 and carnuba wax to approximate weight 2 - 5 % of the tablet weight .
8
a slider 100 of general classical structure is evident in fig1 . this slider 100 comprises a base 110 , two lateral flanges 10 , 120 , 130 and a central bead 140 . the lateral flanges 120 , 130 and the central bead 140 define in combination two channels 150 , 160 , in part at least not parallel . these channels 150 , 160 join at one end of the slider 100 , as in fig2 . the channels 150 , 160 join together the closing elements 200 , 300 , respectively . the specialist understands that as it is moved the slider 100 , according to the direction of motion , separates the closing profiles 200 , 300 , as shown in fig1 , or on the contrary carries the latter engaged , as shown in fig2 . the attached figures illustrate two closing elements 200 , 300 extruded onto films 250 , 350 , constituting the sachet proper . as a variant , and in a manner known per se , the closing elements 200 , 300 could be made initially separately , then connected and fixed onto the films 250 , 350 by any appropriate means , for example by thermal welding . according to the embodiments illustrated in the attached figures , the two closing elements 200 , 300 comprise support bulges 210 , 310 , each of which carries a closing element as such 212 , 312 respectively of complementary male and female type . by way of variant , such elements 212 , 312 could be replaced by any equivalent means , for example structures with hooks or complementary hook and loop fastener type such as those sold under the trademark velcro . as mentioned earlier , according to the present invention the slider 100 comprises , on the apex of the slider 100 opposite the base 110 , at least one flexible lip 145 , 146 placed opposite a lead angle 216 , 316 provided on a closing element 200 , 300 , according to a configuration , such that any attempt to pull back the slider 100 results in autolocking hanging of the lip 145 , 146 . more precisely again , preferably within the scope of the present invention , the closing device comprises two lips 145 , 146 cooperating respectively with a lead angle 216 , 316 provided on each of the two elements 200 , 300 . the lead angles 216 , 316 are provided on the inner face of the closing elements 200 , 300 . the lips 145 , 146 are oriented towards the base 110 by moving away from a plane of symmetry 0 - 0 parallel to the direction of translation of the slider and passing through the plane of symmetry of the central bead 140 . fig3 shows that if the attempt is made to pull back the slider 100 , the lead angles 216 , 316 stress the lips 145 , 146 . the lips 145 , 146 then are underpinned and deformed , their apex being brought closer to the lateral flanges 120 , 130 ( moving away from the base 110 by deformation accompanied by a pivoting movement about the zone connecting the lips 145 , 146 at the apex of the central bead 140 ). this ends in autolocking , where the closing elements or the films 250 , 350 are wedged between the apex of the lips 145 , 146 and the flanges 120 , 130 . the specialist will understand that simultaneously this produces a seal between the two film elements 250 , 350 inside the slider 100 . the height of the lips 145 , 146 , illustrated under reference e 1 in fig3 , is preferably greater than a width e 2 , illustrated in the same fig3 , of the free opening formed between the apex of the central bead 140 and the free end of the flanges 120 , 130 . consequently , owing to this arrangement , it is guaranteed that during an attempt to pull back the slider 100 the apex of the lips 145 , 146 rests against the films 250 , 350 . in the case as shown in fig1 to 3 , the lateral flanges 120 , 130 have a flared sole plate 121 , 131 at their free end , more precisely , the lips 145 , 146 are stressed against the flanks of these sole plates 121 , 131 during an attempt to pull back the slider 100 . fig4 illustrates a variant embodiment according to which the lips 145 , 146 have a length even greater , such that their apexes do not rest against the flanks of the sole plates 121 , 131 but against lead angles 123 , 133 formed between the flanks of the sole plates 121 , 131 and the flanges 120 , 130 , and directed towards the base 110 . the specialist will understand that this arrangement further reinforces the locking effect on the underpinned lips 145 , 146 , at the same time limiting the stress by separating the lateral flanges 120 , 130 . fig5 shows another variant embodiment according to which it is provided with lips 125 , 135 , 145 , 146 simultaneously on the lateral flanges 120 , 130 and on the central bead 140 . these lips 125 , 135 and 145 , 146 cooperate with lead angles 215 , 315 , 216 , 316 provided respectively on the outer faces and on the inner faces 20 of the bulges 210 , 310 of the closing elements . according to the embodiment shown in fig5 , the lips above 125 , 135 and 145 , 146 are situated substantially on the same level and have substantially identical lengths and suppleness . so their apexes come into mutual contact on either side of the films 250 , 350 when the slider 100 is stressed or pulled back . on the contrary fig6 and 7 show pairs of lips 125 , 135 and 145 , 146 , respectively , having different lengths . according to the embodiment shown in fig6 , the longest lips 145 , 146 are solid with the central bead 140 . conversely , according to the embodiment shown in fig7 , the longest lips 125 , 135 are solid with the inner faces of the lateral flanges 120 , 130 in the two cases of the embodiments illustrated in fig6 and 7 , the longest lips are placed on the interior of the slider relative to the shortest lips . the specialist will understand that in this case , the outer face of the longest lips comes into contact with the apex of the shortest lips during an attempt to pull back the slider . fig8 shows another variant embodiment according to which the lateral flanges 120 , 130 are fitted , in the vicinity of their free end opposite the base 110 , and on their inner face , with substantially rigid flanges 122 , 132 . these flanges 122 , 132 each define an inclined facet 124 , 134 forming a ramp which converges towards the plane symmetry 0 - 0 by moving away from the base 110 . two lips 145 , 146 solid with the end free of the central bead 140 opposite the base 110 are placed on the interior of these ramps 124 , 134 . the lips 144 , 146 converge towards the base 100 by moving away from the plane of symmetry 0 - 0 . the ramps 124 , 134 define in combination with the lips 145 , 146 channels 128 , 138 which converge by moving away from the base 110 . the specialist will comprehend from studying fig8 that the channels 128 , 138 cause the films 250 , 350 to approach one another and ensure contact between the latter at the level of a zone referenced 290 in fig8 . such a structure obviously improves the sealing property of the device . in addition , the specialist will comprehend that this sealing is further reinforced when an attempt is made to pull back the slider , with the lips 145 , 146 30 tending to accentuate the effort and convergence of the films 250 , 350 . scrutiny of the attached figures will clarify that the slider 100 is preferably fitted on the outer face of the base 110 with two tappets or lugs 112 , 114 substantially adjacent to the flanges 120 , 130 . in a manner known per se , such tappets 112 , 114 , when they are caused to approach one another , stress the flanges 120 , 130 to move apart and consequently accentuate the width of opening of the channels 150 , 160 to facilitate engagement of a slider on the closing elements 210 , 220 . the lips 125 , 135 , 145 , 146 can be made from the same material as the essential material of the slider 100 , or from a different material . they are preferably made from a supple material such as polyethylene or ethylene copolymer . it is understood that the present invention is not limited to the particular embodiments described hereinabove but extends to any variant in keeping with its basic idea .
8
fig1 a schematically illustrates the components of a portable computing device 100 , which is an exemplary device used to illustrate the features of the present invention . the portable computing device 100 may take the form of a smartphone , a personal digital assistant ( pda ), an e - reader , a tablet computer etc . the portable computing device 100 includes a processor 102 that is able to transmit control messages to , receive status information from , and transmit data to and from components within the portable computing device 100 that are connected to a system bus 104 , where these components may include a non - volatile storage device 106 , random access memory 108 , user input interface 110 , network interface 112 and graphics processing component 114 . the processor 102 , which in this embodiment is a microprocessor , processes instructions stored in the random access memory ( ram ) 108 that have been loaded from the non - volatile storage device 106 which could be for example a flash memory or a hard disk drive . these instructions are in the form of computer software in the form of one or more programs that implement an operating system 118 and a client program . the ram 108 is also used by programs running on the processor 102 as a means of storing and accessing data in the form of electronic signals where the data is used during the execution of the programs . the operating system 118 is computer software in the form of a program or set of programs whose instructions are loaded from non - volatile storage 106 by the processor 102 and executed when the portable computing device 100 is turned on . the operating system 118 may start further programs automatically and / or may allow a user to start further programs , for example by the user using a user interface provided by the operating system 118 . the operating system 118 enables the sharing of the processing power provided by the processor 102 between the programs ( e . g . 120 ) running on the processor 102 . the operating system 118 provides a programmatic interface for programs running on the processor 102 allowing them to request functionality from the operating system 118 . this programmatic interface may take the form of procedures , i . e . system calls , which a program running on the processor 102 may use in order to invoke the operating system 118 and request it to provide desired functionality . in response to receiving a request for functionality the operating system 118 may transmit control messages to , receive status information from , transmit data to and / or receive data from components ( e . g . 106 , 108 , 110 , 112 , 114 , 116 ) connected to the system bus 104 in order to provide the requested functionality , and may also return data to the requesting program as a result . the operating system 118 may provide a file system for storing , modifying and accessing files held in non - volatile storage 106 . this file system may be accessible to other programs running on the processor 102 via the programmatic interface provided by the operating system 118 . the operating system 118 may also provide database access procedures for creating , accessing and modifying databases managed by the operating system 118 ( e . g . databases held in non - volatile storage 106 ). these database access procedures may also be accessible to other programs running on the processor 102 via the programmatic interface provided by the operating system 118 . the portable computing device 100 includes a graphics processing component 114 that is able to render graphics in accordance with commands made by programs running on the processor 102 and output these to a touch - screen display 116 which may reside within the portable computing device 100 . in alternative embodiments of the invention the touch - screen display 116 may be an external component connected to the portable computing device 100 via a composite video , component video , video graphics array , digital visual interface , or high - definition multimedia interface connection . programs running on the processor 102 can process user input obtained from a user input interface 110 that receives user input from a user input device or devices ( not shown ). the user input devices may include a touch - screen interface of the touch - screen display 116 . alternatively or in addition user input devices may include a keypad , keyboard , mouse and / or remote control which may be incorporated within the portable computing device 100 or may be connected to it via a wired or wireless connection . fig2 shows an external view of an exemplary embodiment of the portable computing device 100 . in this embodiment the portable computing device includes a touch - screen display 116 that may be touched by a user using a finger 200 in order to provide touch - screen user input that is received by the user input interface 110 and then processed by one or more programs running on the processor 102 . alternatively a stylus or other device may be used to provide the touch input . the touch - screen interface of the touch - screen display 116 may use any of a number of different known touch - sensing technologies including capacitive sensing technologies such as mutual capacitance or self capacitance , where a number of capacitive sensor elements detect touch input to the touch - screen interface . the portable computing device 100 also includes a network interface 112 ( or a plurality of such interfaces ) that allows programs running on the processor 102 to transmit and receive data to and from a number of other devices and systems via a communications network 140 ( or a plurality of such networks ). fig1 b schematically illustrates communication links that may be made by the portable computing device 100 using the network interface 112 . the network interface 112 ( or a plurality of such interfaces ) may allow programs running on the processor 102 to transmit and receive data to and from a number of other devices and systems via a communications network 140 ( or a plurality of such networks ). the network interface 112 ( or the plurality of such interfaces ) may include a radio access network interface ( or a plurality of such interfaces ) that is able to communicate with a wireless access node 146 such as a base station or a wireless access point that provides access to a communications network 140 ( or a plurality of such networks ). the network interface 112 ( or plurality of such interfaces ) may be able to connect to the wireless access node 146 using one or more of a number of radio access technologies including global system for mobile communications ( gsm ), universal mobile telecommunications system ( umts ), long term evolution ( lte ), fixed wireless access ( such as ieee 802 . 16 wimax ), and wireless networking ( such as ieee 802 . 11 wifi ). these communications network 140 and / or wireless access node 146 may also provide access to the internet . the network interface 112 ( or the plurality of such interfaces ) may also include a modem and / or an ethernet card or interface for use with a corresponding communications network ( or networks ) 140 such as the internet and / or a private data communications network . the operating system 118 may provide messaging procedures for sending and receiving messages such as short messaging services ( sms ), multimedia messaging services ( mms ) and e - mail via the wireless access node 146 and / or the communications network 140 by using the network interface 112 . these messaging procedures may be accessible to other programs running on the processor 102 via the programmatic interface provided by the operating system 118 . the operating system 118 may include a networking program that allows communication between programs running on the processor 112 and external devices via the network interface 112 and communications network 140 ( or plurality of such networks ) using networking protocols such as ( for example ) the transmission control protocol ( tcp ) or the user datagram protocol ( udp ). external devices which can be communicated with via the communications network 140 may include a remote data processing device such as a network operations centre ( noc ) 150 . the networking program and / or networking procedures may be accessible to other programs running on the processor 102 via the programmatic interface provided by the operating system 118 . the noc 150 may be a computer server ( or a plurality of computer servers ) with a network interface via which the noc 150 may be connected to the communications network 140 . the network interface of the noc 150 may also allow the noc 150 to communicate via a communications network 142 with other remote data processing devices such as one or more enterprise servers 170 , 172 , 174 that are connected to an enterprise network ( not shown ). the one or more enterprise servers 170 , 172 , 174 may be a computer server ( or a plurality of computer servers ) that reside within the enterprise network . the communications network 142 via which the noc 150 may access the one or more enterprise servers 170 , 172 , 174 may be the same communications network as the communications network 140 via which the portable computing device 100 may access the noc 150 and / or may include the internet . in order to access content and services provided by remote data processing devices such as the noc 150 and one or more enterprise servers 170 , 172 , 174 a user of the portable computing device 100 may use a client program 120 on the portable computing device 100 . the client program 120 may be pre - loaded onto the portable computing device 100 before purchase of the portable computing device 100 by the user . alternatively the client program 120 may be downloaded and installed onto the portable computing device 100 by the user , for example by the user using an application store program provided by the operating system 118 to download ( and install ) the client program 120 from an application store server via the communications network 140 . the user may use the operating system 118 to start the client program 120 once it is installed on the portable computing device 100 . the client program 120 may include a number of components that are configured to allow the user to access services provided by remote data processing devices such as the noc 150 and one or more enterprise servers 170 , 172 , 174 . these components of the client program 120 may include a rendering engine 122 , core services 124 , service plugins 126 , application services 128 and applications 130 . these components may use the programmatic interface provided by the operating system 118 ( i . e . system calls ) to request functionality from the operating system 118 ( for example to access the file system , send / receive messages , use the network interface 112 , etc ). the client program 120 may comprise a rendering engine 122 that is able to parse hypertext mark - up language ( html ) documents ( and / or variant document types such as extensible html or extensible mark - up language ) and display these on the touch - screen display 116 of the portable computing device 100 by using the graphics processing component 114 in order to display one or more user interfaces . the rendering engine 122 may also be able to interpret cascading style sheets ( css ) documents when displaying html documents in order to use these to determine how the html documents should be presented ( i . e . in terms of layout , colours , fonts , etc ). when displaying html documents the rendering engine 122 may make use of functionality provided by the operating system 118 in order to display user interface elements with a look and feel consistent with that of the operating system 118 . the rendering engine 122 may include a resource management component that manages the retrieval of documents via the communications network 140 ( e . g . from the one or more enterprise servers 170 , 172 , 174 and / or from the noc 150 ) and the storage of these documents in non - volatile storage 106 for later re - use ( i . e . caching ). documents that the rendering engine 122 may retrieve and cache may include html , css , javascript , images , video and any other documents that may be needed in order to render an html document parsed by the rendering engine 122 . the rendering engine 122 may be configured to interpret javascript programs embedded in html documents and / or may be configured to interpret javascript programs contained in javascript files . the rendering engine 122 may be configured to parse plain - text javascript programs and / or javascript programs that may have been pre - compiled into javascript byte - code . pre - compiled javascript byte - code provides several advantages over plain - text javascript as it is less computationally expensive to interpret ( and hence also requires less power to interpret ), and requires less storage ( and less transmission bandwidth ) than plain - text javascript . the rendering engine 122 allows javascript programs ( i . e . either pre - compiled or plain - text ) that are interpreted by the rendering engine 122 to interact with html documents displayed by the rendering engine by executing programmatic functions and accessing programmatic variables and objects relating to those html documents i . e . by accessing the document object models ( doms ) of those documents . the client program 120 may comprise core services 124 that provide a programmatic javascript interface for javascript programs interpreted by the rendering engine 122 to request functionality from the operating system 118 , for example by wrapping ( in javascript ) the system calls provided by the operating system 118 and / or by providing javascript functions , variables and objects that allow direct interaction with the operating system 118 . thus javascript programs interpreted by the rendering engine 122 may perform any of the operations that could be performed by a program programmed to run natively on the portable computing device 100 . examples of functionality that the core services 124 may expose to javascript programs interpreted by the rendering engine include : file system operations for interacting with the file system provided by the operating system 118 , database operations for interacting with a database engine ( or engines ) provided by the operating system 118 , messaging operations for sending , receiving and accessing e - mails and messages ( e . g . sms and mms ), and other operations described in further detail below . the client program 120 may comprise service plugins 126 that , like the core services 124 , provide a javascript interface for javascript programs interpreted by the rendering engine 122 to request functionality from the operating system 118 . the service plugins 126 however may not be included with the client program 120 when it is first installed on the portable computing device 100 , but instead may later be retrieved from the one or more enterprise servers 170 , 172 , 174 or noc 150 in order to provide a javascript interface for additional functionality not made available by the core services 122 . the rendering engine 122 may be configured to run a number of application services 128 and applications 130 that may each consist of javascript programs ( interpreted by the rendering engine 122 ) providing programmatic functionality and html documents ( parsed by the rendering engine 122 ) providing one or more user interface . the applications 130 may be used to display user interfaces and provide programmatic functionality to allow a user to access services provided by remote data processing devices such as the noc 150 and one or more enterprise servers 170 , 172 , 174 . the application services 128 may be used to provide services running in the background of the applications 130 , such as accessing client program 1120 updates provided by the noc 150 and / or one or more enterprise servers 170 , 172 , 174 , installing new applications 130 , service plugins 126 , etc ., and making applications 130 that the user is entitled to use accessible via a user interface provided by the client program 120 . the applications 130 may include a catalogue application that provides a user interface allowing the user to enter identification and authentication details ( e . g . a username and password ) for transmission to the noc 150 . the authentication user interface of the catalogue application may be the first user interface that is displayed to a user when the client program 120 is started . once a user has entered identification and authentication details using this user interface these details may be transmitted to the noc 150 in order to identify and authenticate the user , as is described in greater detail below . the catalogue application may also provide a user interface to the user that allows other applications 130 to be started and / or new applications 130 to be acquired from the noc 150 and / or one or more enterprise servers 170 , 172 , 174 . applications 130 besides the catalogue application may provide the user with means for securely accessing content and services provided by remote data processing devices . the content and services accessible to a user of the client program 120 via the applications 130 may be controlled remotely by administrators of the remote data processing devices ( such as the noc 150 and / or one or more enterprise servers 170 , 172 , 174 ). general access to the one or more enterprise servers 170 , 172 , 174 and the enterprise network from the communications network 142 ( e . g . the internet ) may typically be prevented by a firewall 160 placed between the communications network 142 and the enterprise network such that all network traffic that passes between the communications network 142 and enterprise network can be monitored and ( optionally ) discarded if it does not satisfy the firewall &# 39 ; s criteria . for example the firewall 160 may be configured to only allow network connections between the noc 150 and one or more enterprise servers 170 , 172 , 174 , and to discard all other network connections from the communications network 142 to the one or more enterprise servers 170 , 172 , 174 and / or the enterprise network . the one or more enterprise servers 170 , 172 , 174 may provide access to enterprise services including enterprise email services for storing , sending and receiving email , enterprise file sharing services for storing and retrieving files , enterprise database services for accessing and modifying an enterprise database ( or databases ), and enterprise personal information management ( pim ) services for accessing and modifying personal information such as contact lists , calendars , task lists , etc . each of these services may be provided by the one or more enterprise servers 170 , 172 , 174 and / or by one or more other servers within the enterprise network to which the one or more enterprise servers 170 , 172 , 174 may connect in order to provide access to those services . the noc 150 may be used by applications 130 of the client program 120 to access the one or more enterprise servers 170 , 172 , 174 and the services they provide via the communications network 140 , i . e . from outside the enterprise network and the firewall 160 . in order to do this the user of the client program 120 is first identified and authenticated by the noc 150 and / or one or more enterprise servers 170 , 172 , 174 , by the user entering his identification and authentication details in the user interface provided by the catalogue application . once the user has entered his identification and authentication details into the catalogue application they may be transmitted by the catalogue application to the noc 150 over a secure ( e . g . encrypted ) data connection established over the ( relatively insecure ) communications network 140 . once the user has been identified and authenticated by the noc 150 the client program 120 may maintain a data connection between it and the noc 150 in order to allow communication between the client program 120 ( i . e . and its components e . g . 122 , 124 , 126 , 128 , 130 ) and the noc 150 . this data connection may be a secure connection over the data communications network 140 . the applications 130 may use the data connection between the client program 120 and the noc 150 to send data to the noc 150 which the noc 150 may forward to the one or more enterprise servers 170 , 172 , 174 . the applications 130 may also use the data connection between the client program 120 and the noc 150 to receive data from the noc 150 which the noc 150 has received from the one or more enterprise servers 170 , 172 , 174 . thus the noc 150 may act as a relay between the applications 130 of the client program 120 and the one or more enterprise servers 170 , 172 , 174 . by sending data to and receiving data from the one or more enterprise servers 170 , 172 , 174 in this way the applications 130 may access the enterprise services as described in greater detail for exemplary applications 130 below . the data connection between the client program 120 and the noc 150 may also be used to ‘ push ’ information received from the one or more enterprise servers 170 , 172 , 174 to applications 130 of the client program 120 , as is described in more detail below . the network interface of the noc 150 may also allow the noc 150 to communicate via a communications network 144 with other remote data processing devices such one or more third party computer servers 180 , 182 , 184 . the communications network 144 via which the noc 150 may access the one or more third party computer servers 180 , 182 , 184 may be the same communications network as communications network 140 via which the portable computing device 100 may access the noc 150 and / or may include the internet . the noc 150 may provide the applications 130 with access to the third party computer servers ( via the data connection between the client program 120 and the noc 150 ). the one or more third party computer servers 180 , 182 , 184 may provide internet services that may be maintained by third parties . the internet services may include internet - based email services such as hotmail or gmail , internet - based social networking services such as facebook or twitter , internet - based pim services such as google calendar , etc . the noc 150 may alternatively or additionally provide one or more of these services internally e . g . within a computer server ( or computer servers ) of which the noc 150 is comprised . the noc 150 may regularly poll , or register for occasional update notifications from , the internet services for updates ( such as new emails , new facebook updates , etc .) associated with the user of the client program 120 , and if any updates are available information relating to these may be transmitted to the client program 120 via the communications network 140 . the data connection between the client program 120 and the noc 150 may be used by the noc 150 to ‘ push ’ information received from internet services to the applications 130 of the client program 120 , as is described in greater detail below . the client program 120 may access a secure database that may be held in volatile storage 106 that is used to store information relating to the user . the secure database may also be used to store cached information received by the client program ( and any of its components ) from the noc 150 and / or one or more enterprise servers 170 , 172 , 174 . by storing information in a secure database the client program 120 ensures that only it can access information stored within the secure database , thus the user ( or a person who has gained unauthorised accessed to the portable computing device 100 ) is prevented from accessing such information using other programs of the portable computing device 100 . the client program 120 may be configured to receive instructions from the noc 150 and / or one or more enterprise servers 170 , 172 , 174 to remove information from the secure database or to delete the secure database entirely . the noc 150 and / or one or more enterprise servers 170 , 172 , 174 may be configured by an administrator to transmit such instructions to a client program 120 running on a portable computing device 100 by storing a flag indicating that such instructions should be transmitted . the noc 150 and / or one or more enterprise servers 170 , 172 , 174 may be configured to transmit such instructions to the client program 120 of a particular portable computing device 100 by storing the international mobile equipment identity ( imei ) of that portable computing device 100 with the flag indicating that such instructions should be transmitted . when the client program 120 is started it may be configured to contact the noc 150 ( and , if necessary , the one or more enterprise servers 170 , 172 , 174 ) and transmit the imei of the portable computing device 100 to the noc 150 and / or one or more enterprise servers 170 , 172 , 174 . the noc 150 and / or one or more enterprise servers 170 , 172 , 174 may then respond with instructions to the client program to delete the secure database if a flag indicating such instructions should be transmitted to the portable computing device 100 with that imei number has been stored at the noc 150 and / or one or more enterprise servers 170 , 172 , 174 . this allows an administrator to ensure that the secure database is immediately deleted on starting of the client program 120 in the event that a person gains unauthorised access to a portable computing device 100 or a previous user loses authorisation to access the noc 150 and / or one or more enterprise servers 170 , 172 , 174 . by providing a client program 120 , noc 150 and one or more enterprise servers 170 , 172 , 174 configured in the manner described above a number of advantages may be obtained as follows . firstly , the applications 130 may be easily ported to different portable computing devices with different operating systems , processors etc . without re - writing the program code of the applications 130 , as the applications comprise javascript and html documents which are interpreted or parsed by the rendering engine 122 of the client program 120 . in order to use the client program 120 on a new portable computing device the rendering engine , core services 124 and service plugins 126 may be tailored to the operating system , processor ( etc ) of the new portable computing device . however it may be not necessary to tailor an update to an existing application 130 or a new application 130 to different portable computing devices . a common set of functionality and user interfaces may thus be provided by the applications 130 across a range of different portable computing devices . secondly , the system described allows the applications 130 to securely access the noc 150 and one or more enterprise servers 170 , 172 , 174 over the communications network 140 , whilst ensuring that the one or more enterprise servers 170 , 172 , 174 and enterprise network are not generally accessible via the communications network 142 . the noc 150 , which serves as an access point to the enterprise network for the client program 120 , remains outside the firewall 160 and hence if the noc 150 fails or is compromised the one or more enterprise servers 170 , 172 , 174 , enterprise network and the content they contain remain secure and inaccessible via the communications network 142 . thirdly , by maintaining a secure data connection between the client program 120 and the noc 150 and using this connection to ‘ push ’ updates from the one or more enterprise servers 170 , 172 , 174 and / or internet services to the applications 130 , the client program 120 need not regularly poll the one or more enterprise servers 170 , 172 , 174 and / or internet services for updates or new content . instead the applications 130 can be informed of updates or new content available at the one or more enterprise servers 170 , 172 , 174 when they become available . in addition the noc 150 can poll the internet services for updates or new content on behalf of the applications 130 , and inform the applications 130 when they become available . this reduces the battery power , processing power and communications bandwidth that would otherwise be consumed by the portable computing device 100 if the applications 130 polled the noc 150 , one or more enterprise servers 170 , 172 , 174 and / or internet services for updates . each application of the applications 130 may be configured to provide a workspace service that provides functions for accessing , creating , and editing workspace data objects . as described in greater detail below , examples of workspace data object include an email , contact entry , calendar entry , task entry , document , message or information stored by a social network , etc . each workspace data object may include a number of characteristics , examples of which are given below . in alternative embodiments of the invention each application of the applications 130 may be configured to provide one or more workspace services , where each workspace service provided by an application provides functions for accessing , creating , and editing a different type of workspace data object . the applications 130 may include an email application for accessing , editing , sending and receiving emails . the email application may thus provide a workspace service for accessing , creating , and editing workspace data objects that are emails and that include characteristics such as email subject , email attachments , email body , recipients , sender , date sent , etc . in order to send and / or receive emails the email application may use the enterprise email services and or internet - based email services via the data connection maintained between the client program 120 and the noc 150 as described above , with the noc 150 communicating with the internet services and / or one or more enterprise servers 170 , 172 , 174 if required . copies of emails accessed , sent and / or received via the noc 150 , internet services and / or one or more enterprise servers 170 , 172 , 174 may be cached by the email application in the secure database of the client program 120 . the applications 130 may include a contacts application for accessing and editing one or more lists of contacts . each list of contacts may comprise contact entries , where each contact entry comprises characteristics relating to a contact which may include the contact &# 39 ; s name , information relating to how that contact may be contacted via e - mail , telephone , social networks , etc , the contact &# 39 ; s postal address , company name , etc . the contacts application may thus provide a workspace service for accessing , creating , and editing workspace data objects that are contact entries . the applications 130 may include a calendar application for accessing and editing one or more calendars . each calendar may comprise calendar entries , where each calendar entry may include characteristics such as a calendar entry subject , a location associated with the entry , start and end times for the calendar entry , a list of contacts associated with the entry , etc . the calendar application may thus provide a workspace service for accessing , creating , and editing workspace data objects that are calendar entries . the applications 130 may include a tasks application for accessing and editing one or more tasks lists . each task list may comprise task entries , where each task entry may include characteristics such as a task subject , a task due date , a list of other entities such as contacts , emails or documents associated with the task , etc . the tasks application may thus provide a workspace service for accessing , creating , and editing workspace data objects that are task entries . the applications 130 may include a document manager application for accessing and editing one or more documents . each document may comprise one or more document types including formatted text , spreadsheets , drawings , images , presentations , audio and / or video , and each document may include document characteristics associated with each of these document types . each document may also include characteristics including who owns , has created , and / or has access to the document . the document manager application may thus provide a workspace service for accessing , creating , and editing workspace data objects that are documents . the applications 130 may include a messaging application for accessing , editing , sending and receiving messages . each message may comprise characteristics such as a message type indicating whether the message is an sms message , mms message , instant message , etc , as well as who the message was sent from / to , the content of the message , when it was sent , etc . the messaging application may be configured to use the network interface of the portable computing device to send and / or receive these messages . instant messages may be sent and / or received via instant messaging services available via the communications network 140 such as windows live messenger , aim , etc . the message application may thus provide a workspace service for accessing , creating , and editing workspace data objects that are messages . the applications 130 may include a social networks application for accessing one or more social networks which may include social networks such as facebook , myspace , twitter , etc . the social networks application may access social networks made available by the internet - based social networking services . the social networks application may thus provide a workspace service for accessing , creating , and editing workspace data objects that include characteristics such as messages and / or information sent to or received from a social network . the workspace data objects that may be accessed , created and / or edited by the workspace service ( or workspace services ) provided by each application of the applications 130 may include workspace data objects stored by remote data processing devices such as the noc 150 , internet services and / or one or more enterprise servers 170 , 172 , 174 . these workspace data objects stored by the noc 150 , internet services and / or one or more enterprise servers 170 , 172 , 174 may be accessed , created and / or edited by an application 130 using the data connection maintained between the client program 120 and the noc 150 as described above , with the noc 150 then communicating with the internet services and / or one or more enterprise servers 170 , 172 , 174 if required . the contacts application , calendar application and tasks application may , for example use this method to access , create and edit workspace data objects stored in the enterprise pim services and / or internet - based pim services . copies of one or more of the workspace data objects may be cached in the secure database of the client program 120 . the applications 130 may allow the user to provide identification and authentication information for use in accessing the internet services . this identification and authentication information may be stored by the applications 130 in the secure database of the client program 120 and used by the applications 130 when the internet services need to be accessed . the identification and authentication information may also be associated with the user and stored by the noc 150 so that it can access the internet services on the user &# 39 ; s behalf when necessary . the email application , contacts application , tasks application , calendar application , document manager application , message application , social networks application and other applications 130 may be configured to provide one or more user interfaces allowing the user to control the functions provided by these applications as described above . these user interfaces may be described in the form of html documents and rendered by the rendering engine 122 as described above . as described above the applications 130 of the client program 120 may be configured to provide functions for editing workspace data objects . these may include functions for associating a first workspace data object with a first workspace service and for providing a workspace service editor for editing a second workspace data object . for example , the first workspace data object could be an email that is provided by the workspace service of the email application , and the first workspace service could be the workspace service provided by the tasks application . the second workspace data object may be populated with at least some data from the first workspace data object according to the association of the first workspace data object with the first workspace service . for example , the second workspace object could be a new task entry in the tasks application which is populated with information from an email ( i . e . the first workspace data object in this example ) according to the association of the email with the workspace service provided by the tasks application ( i . e . the first workspace service in this example ). characteristics of the association of the first workspace data object with the first workspace service may be determined by touch - screen user input in a plurality of user interface configurations . in order to allow characteristics of this association to be easily entered by a user of the portable computing device 100 despite the relatively small size of the touch - screen display 116 , the plurality of user interface configurations may require relatively little user input to the plurality of user interface configurations , as is described in greater detail below . fig3 illustrates steps typically performed by applications 130 of the client program 120 in order to allow characteristics of the association of a first workspace data object with a first workspace service to be entered by a user of the portable computing device 100 . firstly , a first user interface configuration may be displayed by a first application of the applications 130 ( step 300 ). the first user interface configuration may be one of the plurality of user interface configurations into which touch - screen user input may be entered in order to characterise the association of the first workspace data object with the first workspace service . the first user interface configuration may be one of the user interfaces displayed by the first application during use of the first application by the user , and it may be displayed by the first application during provision of a workspace service for reviewing workspace data objects . for example , the first user interface may be displayed by the email application during normal use of the email application by the user to review a list of emails sent and / or received by the user . in the first user interface configuration the first application may display selectable elements in a plurality of areas of the touch - screen display 116 , including a first display area in which at least one selectable element is displayed corresponding to a workspace data object , and a second display area in which at least one selectable element is displayed for the selection of a workspace service . alternatively the at least one selectable element may include a plurality of selectable elements , where each selectable element corresponds to a different workspace data object . the first application may connect to a remote data processing device such as the noc 150 , internet services and / or one or more enterprise servers 170 , 172 , 174 ( e . g . using the data connection maintained between the client program 120 and the noc 150 as described above ), in order to receive one or more workspace data objects from the remote data processing device during the provision of a workspace service for reviewing workspace data objects . each workspace data object in the one or more workspace data objects may correspond with one of the selectable elements in the at least one selectable element ( or plurality of selectable elements ). in this way the one or more workspace data objects may be updated at the portable computing device 100 during the provision of a workspace service for reviewing workspace data objects . an example of a first user interface configuration is shown in fig4 a , which is an exemplary screen displayed by the email application . the first user interface displayed in fig4 a includes a first display area , indicated by the dashed box 400 , in which a number of selectable elements 402 , 404 , 406 , 408 are displayed . each of the selectable elements 402 , 404 , 406 , 408 correspond to a workspace data object , in this case an email that may have been sent or received by the user . the first user interface also includes a second display area , indicated by the dashed box 420 , in which a number of selectable elements 422 , 424 , 426 are displayed . each of the selectable elements 422 , 424 , 426 may allow the selection of a workspace service , for example selectable element 422 allows the selection of the workspace service provided by the contacts application , selectable element 424 allows the selection of the workspace service provided by the calendar application , and selectable element 426 allows the selection of the workspace service provided by the tasks application . once the first user interface configuration has been displayed by the first application , touch - screen user input may be received by the client program 120 from the user input interface 110 ( step 302 ). this touch - screen user input may be due to user input to the touch - screen display 116 and / or may include one or more of several different inputs that are described in detail below . in response to the touch - screen user input received in the first user interface configuration a second user interface configuration may be displayed ( step 304 ). the second user interface configuration may be one of the plurality of user interface configurations into which touch - screen user input may be entered in order to characterise the association of the first workspace data object with the first workspace service . the second user interface configuration may be displayed by a second application of the applications 130 . the second application is in one embodiment the same application as the first application and in other embodiments a different application . in the second user interface configuration a plurality of display areas may be displayed in the touch - screen display 116 . the plurality of display areas may include the first display area and the second display area originally displayed in the first user interface configuration . however in the second user interface configuration at least one new selectable element may be displayed in at least a part of at least one of the first display area and the second display area of the first user interface configuration . the at least one new selectable element displayed in the second user interface configuration may be determined according to the touch - screen user input received in the first user interface configuration , as is described in greater detail below . the at least one new selectable element may include a plurality of new selectable elements . once the second user interface configuration has been displayed , touch - screen user input may be received from the user input interface 110 ( step 306 ). this touch - screen user input may be due to user input to the touch - screen display 116 . the touch - screen user input may involve the selection of one of the at least one new selectable element , and may include one or more of several different inputs or gestures that are described in detail below . by selecting one of the at least one new selectable element the touch - screen user input that is received in the second user interface configuration may determine a characteristic of the second workspace data object , as is described in greater detail below . the steps outlined in fig3 and the description above allow a number of alternative embodiments of the invention that enable the association of a first workspace data object with a first workspace service and the determination of a characteristic of a second workspace data object . a number of examples of these alternative embodiments are described in detail below . a first exemplary embodiment of the invention will now be described within the context of the steps of fig3 . initially , in accordance with step 300 described above , a first user interface configuration may be displayed by a first application of the applications 130 . touch - screen user input may then be received in the first user interface configuration from the user input interface 110 in accordance with step 302 . this touch - screen user input may include a first user input action for selecting a selectable element in the first display area . the selectable element selected by the first user input action may correspond with a first workspace data object which is thereby selected by the first user input action . for example , in the first user interface configuration shown in fig4 a the first user input action may select selectable element 406 in the first display area 400 . the selected selectable element 406 corresponds with a workspace data object that is an email which may therefore be selected as the first workspace data object . touch - screen user input received in the first user interface configuration in step 302 may include a second user input action for selecting a selectable element in a different display area to the first display area . the second user input action may be received after the first user input action . the selectable element in a different display area selected by the second user input action in step 302 may be used by the applications 130 to determine the at least one new selectable element that is displayed in the second user interface configuration in step 304 of fig3 , described above . the second user input action may , for example , select a selectable element in the second display area , and may thereby select the first workspace service which is the workspace service that corresponds to the selectable element selected by the second user input action . for example , in the first user interface configuration shown in fig4 a the second user input action may select selectable element 424 in the second display area 420 . the selected selectable element 424 corresponds with a workspace service provided by the calendar application which may therefore be selected as the first workspace service . the first user input action received in step 302 may include a press input received from the touch - screen display 116 and caused by the user pressing on the touch - screen display 116 at the position of a selectable element in the first display area ( for example selectable element 406 ) of the first user interface configuration . the second user input action received in step 302 may include movement input received from the touch - screen display 116 in response to the user moving his finger on the touch - screen display 116 . this movement input may begin at the position of the selectable element in the first display area ( for example selectable element 406 ) of the first user interface configuration . the movement input may pause , for at least a predetermined time period ( such as one second ) at the position of a selectable element in the second display area ( for example selectable element 426 ) of the first user interface configuration . in response to the detection of touch - screen user inputs received in the first user interface configuration in step 302 a second user interface configuration may be displayed in accordance with step 304 . the second user interface may be displayed by a second application , which could be the same application as the first application or a different application . in the second user interface configuration at least one new selectable element may be displayed in accordance with step 304 . the at least one new selectable element may be displayed in at least a part of the first display area , and may replace at least one selectable element displayed in the first display area of the first user interface configuration . the at least one new selectable element may correspond with an action ( or actions ) that the workspace service provided by the second application may be able to perform with the first workspace data object . for example , where the first workspace data object is an email and the second application is the email application , the at least one new selectable element may correspond with actions such as forwarding the email , or replying to the email . in another example , where the first workspace data object is an email and the second application is the calendar application , the at least one new selectable element may correspond with actions such as creating a new meeting relating to the email at one of several dates . in another example , where the first workspace data object is a contact entry and the second application is the email application , the at least one new selectable element may correspond with actions such as creating a new email addressed to the contact , or forwarding the contact entry to another contact . the at least one new selectable element may alternatively correspond with a workspace data object ( or objects ) that the workspace service provided by the second application allows the access , creation or editing of . the second application may allow an association between the workspace data object ( or objects ) that the at least one new selectable element correspond with and the first workspace data object . for example , where the first workspace data object is a file and the second application is the contacts application , the at least one new selectable element may correspond with contact entries that the first workspace object may be sent to ( e . g . in an email ) or associated with . an example of a second user interface configuration is shown in fig4 b , which is an exemplary screen displayed by a second application which in this case is the calendar application . the second user interface displayed in fig4 b includes a first display area , indicated by the dashed box 430 , in which a number of selectable elements are displayed including selectable element 432 . these selectable elements form the at least one new selectable element that is displayed in the second user interface configuration , and replace the at least one selectable element that was displayed in the first display area of the first user interface configuration , which in this example was the first display area 400 of the first user interface configuration shown in fig4 a . once the second user interface configuration has been in step 304 , touch - screen user input may be received in the second user interface configuration from the user input interface 110 in accordance with step 306 . this touch - screen user input may include a third user input action to select one of the at least one new selectable element ( or plurality of new selectable elements ) displayed in the second user interface configuration . for example , in the second user interface configuration shown in fig4 b the third user input action may select the new selectable element 432 in the first display area 420 . by selecting one of the at least one new selectable element the touch - screen user input ( e . g . the third user input action ) that is received in the second user interface configuration may determine a characteristic of a second workspace data object . the second workspace object may be a new workspace object that is created by the second application in response to touch - screen user input received in the second user interface configuration . for example , the second workspace object could be a new calendar entry created by the calendar application in response to touch - screen user input received in the second user interface configuration . the second workspace object may alternatively be an existing workspace object that is edited by the second application in response to touch - screen user input received in the second user interface configuration . for example , the second workspace object could be an existing calendar entry edited by the calendar application in response to touch - screen user input received in the second user interface configuration . the touch - screen user input that is received in the second user interface configuration may determine a characteristic of the second workspace data object . for example , the touch - screen user input in the second user interface configuration may include a third user input action selecting a selectable element that corresponds to a date in a calendar , such as the date represented by selectable element 432 in the first display area 430 of the second user interface configuration shown in fig4 b . the date represented by the selected selectable element may determine a characteristic for the second workspace data object such as the start and / or end time for a new calendar entry created by the calendar application . the second workspace data object may be populated with at least some data from the first workspace data object according to the association of the first workspace data object with the first workspace service . for example for a second workspace data object that is a calendar entry , characteristics such as the subject and / or list of contacts associated with the second workspace data object may be populated with data from the first workspace object . if the first workspace object is for example an email , the subject of the second workspace object may be set the same as the subject of the first workspace object , and the list of contacts associated with the second workspace object may be set as the recipients of the first workspace object . the second application may connect to a remote data processing device such as the noc 150 , internet services and / or one or more enterprise servers 170 , 172 , 174 ( e . g . using the data connection maintained between the client program 120 and the noc 150 as described above ), in order to transmit the second workspace data object to the remote data processing device during the provision of the workspace service for editing workspace data objects provided by the second application . in this way the second workspace data object , characteristics of which have been determined by touch - screen user input , may be updated at the remote data processing device . the third user input action received in step 306 may include movement input received from the touch - screen display 116 in response to the user moving his finger on the touch - screen display 116 . this movement input may end at the position of one of the at least one new selectable element in the first display area ( for example selectable element 432 ) of the second user interface configuration . the touch - screen user input in the plurality of different user interface configurations may be in the form of continuous movement input to the touch - screen display 116 between the different user interface configurations . for example movement input may continue through the first user input action , second user input action and third user input action , without the user removing his finger ( or other input device ) from the touch - screen display 116 . the continuous movement input may include at least one pause , for a pre - determined time period , at the position of a selectable element and / or an at least one new selectable element in at least one of the plurality of different user interface configurations . in response to touch - screen user input received in the second user interface configuration ( e . g . the third user input action ), a workspace service editor may be displayed to allow the user to edit the second workspace data object . the workspace service editor may be displayed by the second application that may have created the second workspace object in response to the touch - screen user input received in the second user interface configuration . fig4 c shows an exemplary screen displayed by the calendar application ( i . e . the second application ), which includes a workspace service editor , indicated by the dashed box 440 , for editing a second workspace data object that has been created by the calendar application in response to touch - screen user input received in the second user interface configuration such as the one shown in fig4 b . the workspace service editor may comprise a number of fields 442 , 444 , 446 , 448 , 450 , that can be edited by the user and that correspond to characteristics of the second workspace data object . the workspace service editor may comprise one or more selectable elements , indicated within the dashed box 460 , that correspond to actions that the user may perform with the second workspace data object , such as for example saving changes made by the user to the characteristics of the second workspace data object to the secure database of the client program 120 and / or a remote data processing device . a second exemplary embodiment of the invention will now be described within the context of the steps of fig3 . the second embodiment may proceed according to the steps performed by the first embodiment of the invention described above . however in the first user interface configuration of the second embodiment , the second user input action received in step 302 may be received before the first user input action . the second user input action received in step 302 may include movement input received from the touch - screen display 116 in response to the user moving his finger on the touch - screen display 116 . this movement input may begin at the position of a selectable element in the second display area ( for example selectable element 426 ) of the first user interface configuration . the first user input action received in step 302 may include movement input received from the touch - screen display 116 in response to the user moving his finger ( or other input device ) on the touch - screen display 116 . this movement input may pause , for at least a predetermined time period ( such as one second ) at the position of a selectable element in the first display area ( for example selectable element 406 ) of the first user interface configuration . as in the first embodiment , in response to the touch - screen user input received in the first user interface configuration in step 302 a second user interface configuration may be displayed in accordance with step 304 . the second user interface may be displayed by a second application , which may be the same application as the first application or a different application . in the second user interface configuration the at least one new selectable element displayed in accordance with step 304 may be displayed in at least a part of the second display area ( rather than in the first display area as in the first embodiment ). the at least one new selectable element may replace at least one selectable element displayed in the second display area of the first user interface configuration . an example of a second user interface configuration is shown in fig4 d , which is an exemplary screen displayed by the second application which in this case is the calendar application . the second user interface displayed in fig4 d includes a second display area , indicated by the dashed box 470 , in which a number of selectable elements 472 , 474 , 476 are displayed . these selectable elements form the at least one new selectable element that is displayed in the second user interface configuration , and replace the at least one selectable element that was displayed in the second display area of the first user interface configuration , which in this example was the second display area 420 of the first user interface configuration shown in fig4 a . once the second user interface configuration has been displayed by the second application in step 304 , touch - screen user input may be received by the second application from the user input interface 110 in accordance with step 306 . this touch - screen user input may include a third user input action to select one of the one new selectable element ( or plurality of new selectable elements ) displayed in the second user interface configuration . for example , in the second user interface configuration shown in fig4 d the third user input action may select the one new selectable element 474 in the second display area 470 . as in the first embodiment , by selecting one or more of the at least one new selectable element the touch - screen user input ( e . g . the third user input action ) that is received in the second user interface configuration may determine a characteristic of a second workspace data object . the third user input action received in step 306 may include movement input received from the touch - screen display 116 in response to the user moving his finger on the touch - screen display 116 . this movement input may end at the position of one of the at least one new selectable element in the second display area ( for example selectable element 474 ) of the second user interface configuration . the touch - screen user input in the plurality of different user interface configurations may be in the form of continuous movement input to the touch - screen display 116 between the different user interface configurations in accordance with the first embodiment . in response to touch - screen user input received in the second user interface configuration ( e . g . the third user input action ), a workspace service editor user interface may be displayed to allow the user to edit the second workspace data object , in accordance with the first embodiment . the first and second embodiments of the invention offer flexibility to the user when entering touch - screen user input for associating a first workspace data object with a first workspace service , as the user may select the first workspace data object first ( from the first display area in the first embodiment ), or the first workspace service first ( from the second display area in the second embodiment ). a third exemplary embodiment of the invention will now be described within the context of the steps of fig3 . the third embodiment may proceed according to the steps performed by the first embodiment of the invention described above . however the second user input action received in the first user interface configuration of the third embodiment is for causing the at least one new selectable element to be displayed , and touch - screen user input in the second user interface configuration is used to select the first workspace service using the one new selectable element . initially , in accordance with step 300 described above , a first user interface configuration may be displayed by a first application of the applications 130 . touch - screen user input may then be received by the first application from the user input interface 110 in accordance with step 302 . an example of a first user interface configuration according to this embodiment is shown in fig5 a , which is an exemplary screen displayed by the email application . the first user interface displayed in fig5 a includes a first display area , indicated by the dashed box 500 , in which a number of selectable elements including selectable element 502 are displayed . each of the selectable elements correspond to a workspace data object , in this case an email that may have been sent or received by the user . the first user interface also includes a second display area , indicated by the dashed box 510 , in which a number of selectable elements including selectable element 510 are displayed . each of the selectable elements allows the selection of a workspace service . touch - screen user input received in the first user interface configuration in step 302 may include a second user input action for selecting a selectable element in a different display area to the first display area . the second user input action may be received after the first user input action . the selectable element in a different display area selected by the second user input action in step 302 may be used by the applications 130 to determine the at least one new selectable element that is displayed in the second user interface configuration in step 304 of fig3 , described above . the second user input action may , for example , select a selectable element in the second display area , and may thereby cause at least one new selectable element to be displayed in the second user interface configuration . for example , in the first user interface configuration shown in fig5 a the second user input action may select selectable element 512 in the second display area 510 . selectable element 512 may be associated with at least one workspace service not currently displayed in the second display area 510 . the first user input action received in step 302 may include movement input in accordance with the first embodiment . the second user input action received in step 302 may then include movement input in accordance with the first embodiment . in response to the touch - screen user input received in the first user interface configuration in step 302 a second user interface configuration may be displayed in accordance with step 304 . the second user interface may be displayed by the client program 120 which may be configured to display the workspace services displayed in the second display areas of the plurality of user interface configurations . in the second user interface configuration at least one new selectable element displayed in accordance with step 304 may be displayed in at least a part of the second display area , and may replace at least one selectable element displayed in the second display area of the first user interface configuration . an example of a second user interface configuration according to the third embodiment is shown in fig5 b , which is an exemplary screen displayed by the email application ( first display area 500 ) and client program ( second display area 510 ). the second user interface displayed in fig5 b includes a second display area , indicated by the dashed box 520 , in which a number of selectable elements 522 , 524 , 526 are displayed . these selectable elements form the at least one new selectable element that is displayed in the second user interface configuration , and replace the at least one selectable element that was displayed in the second display area of the first user interface configuration , which in this example was the second display area 510 of the first user interface configuration shown in fig5 a . once the second user interface configuration has been displayed by the second application in step 304 , touch - screen user input may be received from the user input interface 110 in accordance with step 306 . this touch - screen user input may include a third user input action to select one of the at least one new selectable element ( or plurality of new selectable elements ) displayed in the second display area of the second user interface configuration . for example , in the second user interface configuration shown in fig5 b the third user input action may select the new selectable element 524 in the second display area 520 . the touch - screen user input in the second user interface configuration may select the first workspace service , which is the workspace service that corresponds to the selected one new selectable element . the first workspace service may be provided by a second application of the applications 130 . the second application may be the same application as the first application or it could be a different application . by selecting one of the at least one new selectable element , the touch - screen user input ( e . g . the third user input action ) that is received in the second user interface configuration may determine a characteristic of a second workspace data object . the second workspace object may be a new workspace object that is created by the second application in response to touch - screen user input received in the second user interface configuration . for example , the second workspace data object could be a new message created by the messaging application in response to touch - screen user input received in the second user interface configuration . the touch - screen user input that is received in the second user interface configuration may determine a characteristic of the second workspace data object . for example , the touch - screen user input in the second user interface configuration may include a third user input action selecting a selectable element that corresponds to a workspace service , such as the workspace service of the messaging application represented by selectable element 524 in the first display area 520 of the second user interface configuration shown in fig5 b . the messaging application may determine a characteristic for the second workspace data object such as the type of message for a new message created by the messaging application . for example the type of message characteristic of the second workspace data object may be determined as an sms message by the messaging application . the second workspace data object may be populated with at least some data from the first workspace data object according to the association of the first workspace data object with the first workspace service . for example for a second workspace data object that is a message , characteristics such as the subject and / or message text of the second workspace data object may be populated with data from the first workspace object . if the first workspace object is for example an email , the subject of the second workspace object may be set the same as the subject of the first workspace object , and the message text of the second workspace object may be set as email body of the first workspace object . the second application may connect to a remote data processing device , in order to transmit the second workspace data object to the remote data processing device in accordance with the first embodiment . the third user input action received in step 306 may include movement input received from the touch - screen display 116 in response to the user moving his finger on the touch - screen display 116 . this movement input may end at the position of one of the at least one new selectable element in the second display area ( for example selectable element 524 ) of the second user interface configuration . the touch - screen user input in the plurality of different user interface configurations may be in the form of continuous movement input to the touch - screen display 116 in accordance with the first embodiment . in response to touch - screen user input received in the second user interface configuration ( e . g . the third user input action ), a workspace service editor user interface may be displayed to allow the user to edit the second workspace data object . the workspace service editor may be displayed by the second application that may have created the second workspace object in response to the touch - screen user input received in the second user interface configuration . the third embodiment of the invention thus allows a number of workspace services to be associated with the first workspace object , even if some of those workspace services may not initially be displayed in the workspace service area due to a lack of space on the touch - screen display 116 . a fourth exemplary embodiment of the invention will now be described within the context of the steps of fig3 . the fourth embodiment may proceed according to the steps performed by the first embodiment of the invention described above . however after touch - screen user input is received in the second user interface configuration to select said one new selectable element , one or more further user interface configurations may be displayed . initially , in accordance with step 300 of the first embodiment , a first user interface configuration may be displayed by a first application of the applications 130 . an example of a first user interface configuration according to this embodiment is shown in fig6 a , which is an exemplary screen displayed by the document manager application . the first user interface displayed in fig6 a includes a first display area , indicated by the dashed box 600 , in which a number of selectable elements 602 , 604 , 606 , 608 are displayed . each of the selectable elements 602 , 604 , 606 , 608 correspond to a workspace data object , in this case a document that has been created by or shared with the user . the first user interface also includes a second display area , indicated by the dashed box 620 , in which a number of selectable elements 622 , 624 , 626 are displayed . each of the selectable elements 622 , 624 , 626 allows the selection of a workspace service , for example selectable element 622 allows the selection of the workspace service provided by the contacts application . touch - screen user input may then be received by the first application from the user input interface 110 in accordance with step 302 of the first embodiment . in response to the touch - screen user input received in the first user interface configuration in step 302 a second user interface configuration may be displayed in accordance with step 304 of the first embodiment . an example of a second user interface configuration is shown in fig6 b , which is an exemplary screen displayed by a second application which in this case is the contacts application . the second user interface displayed in fig6 b includes a first display area , indicated by the dashed box 630 , in which a number of selectable elements are displayed including selectable element 634 . these selectable elements form the at least one new selectable element that is displayed in the second user interface configuration , and replace the at least one selectable element that was displayed in the first display area of the first user interface configuration , which in this example was the first display area 600 of the first user interface configuration shown in fig6 a . once the second user interface configuration has been displayed by the second application in step 304 , touch - screen user input may be received from the user input interface 110 in accordance with step 306 of the first embodiment . for example , the touch - screen user input in the second user interface configuration may include a third user input action selecting a selectable element that corresponds to a contact entry , such as the contact entry represented by selectable element 634 in the first display area 630 of the second user interface configuration shown in fig6 b . the contact entry represented by the selected selectable element may determine a characteristic for the second workspace data object such as the start and / or end time for a new calendar entry created by the calendar application . in response to the touch - screen user input received in the second user interface configuration , at least one further user interface configuration may be displayed . the at least one further user interface configuration may be displayed by the second application . the at least one further user interface configuration may comprise a plurality of further user interface configurations , each of which may be displayed in sequence in response to touch - screen user input . in each further user interface configuration of the at least one further user interface configuration at least one new selectable element may be displayed . the at least one new selectable element may be displayed in at least part of a different display area to the at least one new selectable element displayed in the previously displayed user interface configuration , which may be the second user interface configuration or one of the at least one further user interface configurations . for example , if in the second user interface configuration at least one new selectable element was displayed in at least a part of the first display area , then at least one new selectable element may be displayed in at least part of the second display area and replace at least one selectable element displayed in the second display area . alternatively , if in the second user interface configuration at least one new selectable element was displayed in at least a part of the second display area , then at least one new selectable element may be displayed in at least part of the first display area and replace at least one selectable element displayed in the first display area . the above example and alternative may be extended in a similar way to the display of a second further user interface configuration after the display of a first further user interface configuration , where each of these further user interface configurations form part of the at least one further user interface configuration . the at least one new selectable element displayed in each further user interface configuration may correspond with an action ( or actions ) that the workspace service provided by the second application may be able to perform with the first workspace data object and the selected at least one new selectable element selected in the second user interface configuration . for example the selected one new selectable element is the second user interface configuration may correspond with a selected workspace data object , and the at least one new selectable element in each further user interface configuration may correspond with actions that the second application may perform on the first workspace data object and the selected workspace data object . an example of a first further user interface configuration is shown in fig6 c , which is an exemplary screen displayed by a second application which in this case is the contacts application . the second user interface displayed in fig6 c includes an action display area , indicated by the dashed box 640 , in which a number of selectable elements are displayed including selectable element 646 . these selectable elements form the at least one further selectable element that is displayed in the first further user interface configuration , and replace the at least one selectable element that was displayed in the second display area of the first and second user interface configuration , which in this example was the second display area 620 shown in fig6 a and 6 b . an example of a second further user interface configuration is shown in fig6 d , which is an exemplary screen displayed by a second application which in this case is the contacts application . the second user interface displayed in fig6 d includes an action display area , indicated by the dashed box 650 , in which a number of selectable elements 652 , 654 , 656 , 658 are displayed . these selectable elements form the at least one new selectable element that is displayed in the second further user interface configuration , and replace the at least one new selectable element that was displayed in the second display area of the second user interface configuration , which in this example was the first display area 630 shown in fig6 b and 6 c . once a further user interface configuration of the at least one further user interface configurations has been displayed by the second application , touch - screen user input may be received in that further user interface configuration from the user input interface 110 . this touch - screen user input may include a further user input action to select one of the at least one new selectable element displayed in that further user interface configuration . for example , in the first further user interface configuration shown in fig6 c the further user input action may select the further selectable element 646 in the second display area 640 . in another example , in the second further user interface configuration shown in fig6 d the further user input action may select the further selectable element 654 in the second display area 650 . by selecting one of the at least one new selectable element the touch - screen user input ( e . g . the further user input action ) that is received in a further user interface configuration may determine a characteristic of a second workspace data object . for example , the touch - screen user input in the at least one further user interface configuration may include a further user input action selecting a selectable element that corresponds to the action of sending an email based on the first workspace object and the selected at least one new selectable element , such as the action represented by selectable element 646 in the second display area 640 of the second user interface configuration shown in fig6 c . the selected at least one selectable element may determine that the email body characteristic for the second workspace data object may be set to contain the at least some data from the first workspace object . the user input action received in each further user interface configuration may include movement input similar to that of the first embodiment . the touch - screen user input in the plurality of different user interface configurations may be in the form of continuous movement input to the touch - screen display 116 in accordance with the first embodiment . in response to touch - screen user input received in a further user interface configuration , a workspace service editor user interface may be displayed to allow the user to edit the second workspace data object . the fourth embodiment of the invention thus allows a number of different actions based on the association of the first workspace data object and first workspace service to be entered by the user . these actions may allow further characteristics of the second workspace object to be determined from the association of the first workspace object and first workspace service . the above embodiments are to be understood as illustrative examples of the invention . further embodiments of the invention are envisaged as follows . it is to be understood that further user interface configurations in accordance with the fourth embodiment may also be displayed before the display of a workspace service editor ( if appropriate ) in the second embodiment and / or the third embodiment . in alternative embodiments of the invention the touch - screen user input in the plurality of different user interface configurations need not be in the form of continuous movement input to the touch - screen display 116 . for example , one or more of the user input actions entered in the plurality of different user interface configurations may include the user tapping at the position of a selectable element on the touch - screen display 116 . additionally or alternatively one or more of the user input actions entered in the plurality of different user interface configurations may include the user removing his finger from the touch - screen display 116 after moving his finger to the position of a selectable element in order to perform a drag and drop input action . it is to be understood that the plurality of user interface configurations of the embodiments of the invention described above may in alternative embodiments not be displayed from within one or more applications 130 that are pre - compiled and / or interpreted javascript programs or similar , but could instead be displayed from within any program or programs configured to run on the portable computing device 100 . such programs may be configured to communicate with one or more remote data processing devices such as the noc 150 , cloud services and / or enterprise server 170 as described above . such programs may be may be configured to provide a workspace service that provides functions for accessing , creating , and editing workspace data objects as described above . it is to be understood that any feature described in relation to any one embodiment may be used alone , or in combination with other features described , and may also be used in combination with one or more features of any other of the embodiments , or any combination of any other of the embodiments . furthermore , equivalents and modifications not described above may also be employed without departing from the scope of the invention , which is defined in the accompanying claims .
7
embodiments of the present invention provide an advertisement scheme for use with interactive content , such as for example video games , entertainment software , or any other type of interactive content . in some embodiments , during game play , the game slows down , then stops , and a commercial is played . the user may be given an indication or other warning that a commercial is coming . by way of example , the indication may comprise a slowing down of the game play . this way , when the game slows down , the user knows to get ready for a commercial , the game then stops , and the commercial is played . after the commercial , the game resumes ( i . e . starts again ). in some embodiments the game may resume by slowly starting again , which allows the user to remember where he or she was in the game . referring to fig1 , there is illustrated a method 100 that operates in accordance with an embodiment of the present invention . the method 100 , which may be used in advertising , may be used in any interactive entertainment system or any content where the user interacts with the content . the method 100 begins in step 102 where the playing of interactive content is initiated . in some embodiments , an optional step 104 may be used to provide the user with an indication that the playing of the interactive content will be suspended . in some embodiments , the indication may comprise a slowing down of the playing of the interactive content . for example , in some embodiments , the interactive content may be played in slow motion before being suspended . in other implementations , the slowing down of the content may be gradual so that the speed at which the interactive media is played is decreased until the playing of the interactive media is suspended . various transmission mechanisms may optionally be used to couple player minds out of ( and back into ) the game environment . for example , in some embodiments , the indication provided in optional step 104 may comprise displaying a warning message , a notice , bell , audio signal , visual signal , audio - visual signal , or some other indication that alerts a user of an upcoming break , such as a commercial break , in the playing of the media content . fig2 a , 2 b , 2 c and 2 d illustrate example suspension indications that may be used in accordance with embodiments of the present invention . namely , in fig2 a the game playing on client display device 210 may be gradually slowed down . in fig2 b a warning message 212 that the game play is about to stop may be displayed on the client display device 210 . in fig2 c a visual warning signal such as a blinking light 214 may be used to indicate that game play is about to stop . in fig2 d an audio signal played through speakers 216 connected to the client device may be used to indicate suspension of playing of media . in step 106 ( fig1 ) the playing of the interactive content is suspended . according to some embodiments , the playing of content may be suspended at predefined times . in other embodiments , suspension of playing of interactive content may , occur randomly . during step 106 when the playing of the interactive content is suspended , in some embodiments , a stop point may be recorded referring to the point at which the playing of the media content was suspended . this stop point may be the time within the media content where the playing of the content is suspended , or other such identifiers that may be used to identify the point within the media content at which the playing is suspended . in step 108 an advertisement is displayed . by way of example , the advertisement may be similar to a traditional tv commercial , or may comprise some other type of advertisement . for example , fig3 illustrates an example advertisement 308 played on client display device 310 . in this example the advertisement 308 is for “ best brand soda ” having the slogan “ you &# 39 ; ve got to try it ”?. in some embodiments , the advertisement may be preselected , randomly chosen , selected based on demographics , selected based on a user profile or other criteria , or selected by some other process . in embodiments where interactive content is played on several client devices ( discussed below ), commercial advertisements may be played on one or more or all client devices . in some embodiments , the advertisement may be played on the whole screen . thus , when the playing of interactive content is suspended , a commercial or other advertisement is played . in some embodiments , a portion of the content may be replayed before resuming the playing of the interactive content . for example , as shown in optional step 110 ( fig1 ), at least a portion of the interactive content is rewound prior to the resuming playing of the interactive content . that is , a portion of the game may be rewound to replay the last few seconds or minutes slowly to allow the user to begin playing again . in some embodiments , the recorded stop point is used , so that a portion of the content before the content is played back in either normal speed or slow motion up to the stop point and normal playing of content is resumed after the stop point . in some embodiments , an indication may be provided alerting the user that playback of the content is about to resume before resuming playing of the content . the indication may be a notice , an audio indication such as a bell , an audio visual signal , or other such indications . in some embodiments , objects , targets , scenes , players , scores , or other such information may be highlighted or animated to bring focus into key elements of the interactive content at the time of resuming playing of content . fig4 a and 4b illustrate example resuming indications that may be used in accordance with embodiments of the present invention . namely , in fig4 a a warning message 412 that the game play is about to resume may be displayed on the client display device 410 . in fig4 b the rank 414 , score 416 and / or object 418 , such as an automobile , may be highlighted or animated to bring focus into those elements of the interactive content at the time of resuming playing of content . next , in step 112 ( fig1 ) the playing of the interactive content is resumed . in some embodiments a signal scheme may trigger and coordinate the resuming of playing of content to establish a safe and fair transition . various transition mechanisms may be used to transition from a suspended state to resuming playing of the content . in some embodiments , the speed of the content may be increased until the speed returns to its normal speed . in some embodiments , the speeding up may be gradual to insure an effective transition . embodiments of the present invention may be used in stand alone games or in network gaming environments . referring to fig5 , there is illustrated a system 500 that may be used in implementing a network gaming environment in accordance with an embodiment of the present invention . in the system 500 , a plurality of players are able to interact with each other , such as for example in a network game . this may be accomplished by each player operating a client device 502 that has access to a network 504 , such as for example the internet . in some implementations , the gaming network may be synchronized using a signaling scheme where a signal is sent to all players on the network to suspend and play a game . additionally , signals may be sent to facilitate slowing down or speeding up the playing of the content at the same time to provide a fair and simultaneous game play environment . other synchronization schemes utilizing recording stop points and time stamps may be used in some embodiments . in network gaming one or more players may all see the same or different commercials when game play stops . in embodiments where different commercials are played synchronization schemes may be used to ensure that regardless of the commercial that is playing on each client device the game stops and resumes at the same time . such synchronization schemes may also be used to ensure that the game stops and resumes in a similar manner at all client devices to ensure a fair playing environment . in some embodiments , where a game is played over a network , suspension of the content , and optionally an indication , may be initiated when the server transmits a message to all game clients coordinating the state change . for example , in a network gaming framework , a signal may be transmitted to some or all players to indicate a break and to coordinate the break in all player units . in some embodiments , the signal scheme may trigger and coordinate game functions across the game environment to establish a safe and fair transition from active game play to a pause state . in some implementations , the points at which the suspending of the playing of the media takes place is pre - recorded and suspending of the content is initiated when the players encounter a stop point within the content . in some implementations , where media content is being played simultaneously on several client playback devices , a signal scheme , or other schemes , may be used to coordinate the suspension of the content on all devices . in other embodiments , the playing of the content may be suspended at random points . in some implementations a signal scheme may be used to send a signal causing all client devices to suspend playing of the content on all client apparatuses . in embodiments where the content is displayed to multiple clients , the same advertisement may be played on all client devices , while in other embodiments different advertisements may be played on some or all of the client devices . the advertisements that are played on client devices may be randomly assigned to different devices , or in some implementations , the advertisements specific to some or all of the client devices , based on a user profile or other criteria , may be sent to those devices . the methods and techniques described herein may be utilized , implemented and / or run on many different types of computers , graphics workstations , televisions , entertainment systems , video game systems , dvd players , dvrs , media players , home servers , video game consoles , and the like . referring to fig4 , there is illustrated a system 400 that may be used for such implementations . however , the use of the system 400 is certainly not required . by way of example , the system 600 may include , but is not required to include , a central processing unit ( cpu ) 602 , a graphics processing unit ( gpu ) 604 , digital differential analysis ( dda ) hardware 606 , a random access memory ( ram ) 608 , and a mass storage unit 610 , such as a disk drive . the system 600 may be coupled to , or integrated with , a display 612 , such as for example any type of display , including any of the types of displays mentioned herein . the cpu 602 and / or gpu 604 may be used to execute or assist in executing the steps of the methods and techniques described herein , and various program content and images may be rendered on the display 612 . removable storage media 614 may optionally be used with the mass storage unit 610 , which may be used for storing code that implements the methods and techniques described herein . however , any of the storage devices , such as the ram 608 or mass storage unit 610 , may be used for storing such code . either all or a portion of the system 600 may be embodied in any type of device , such as for example a television , computer , video game console or system , or any other type of device , including any type of device mentioned herein . while the invention herein disclosed has been described by means of specific embodiments and applications thereof , numerous modifications and variations could be made thereto by those skilled in the art without departing from the scope of the invention set forth in the claims .
6
fig1 is a diagram showing a configuration of an image transfer system according to a first embodiment of the present invention . a digital camera 101 and a computer apparatus 103 are connected to each other through a cable 102 . the digital camera 101 that functions as an image creation apparatus includes a photography apparatus 104 , a memory card 105 , and an image transfer apparatus 106 for transferring image data . a disk apparatus 107 and a display apparatus 108 are connected to the computer apparatus 103 , which functions as an image processing apparatus . image display software 109 is operated on the computer apparatus 103 , and an image file recorded in the disk apparatus 107 is displayed on the display apparatus 108 . fig2 is a diagram showing an example of a data structure of the image file recorded by the digital camera 101 . data of the image file includes a header part 201 and an image data part 202 . in the header part 201 , a group number 203 and an intragroup serial number 204 are recorded as grouped image information . the intragroup serial number 204 is a unique number in grouped images having similar group numbers . in the digital camera 101 of the first embodiment , a user must set operation in a grouped image photography mode before photographing images . in each of the images photographed in the grouped image photography mode , the aforementioned information is automatically written in the header part 201 . the grouped images taken according to the first embodiment are those photographed by panorama photography , continuous photography , interval photography , auto - bracketing photography , and the like . hereinafter , these images will be described as grouped images . fig3 shows a display example in which the image display software 109 is displayed on the display apparatus 108 . the screen includes a menu 301 , a directory area 302 , and a thumbnail area 303 . in the directory area 302 , directories within the disk apparatus 107 are displayed in a hierarchical manner . when one of the directories displayed in the directory area 302 is selected , a list of thumbnail images of reduced image files present within the directory of the disk apparatus 107 is displayed in the thumbnail area 303 . in fig3 , a directory 0001 is selected . in the image display software 109 , grouped image information written in the header part of each of the image files present within the disk apparatus 107 is not analyzed , but the files present in the disk apparatus 107 are organized by using file names and directory names , and displayed . for a file system installed in the computer apparatus 103 , for example , a general - purpose file system provided by an existing operation system can be used . fig4 is a flowchart showing a processing flow when the image transfer apparatus 106 transfers an image file recorded in the memory card 105 to the disk apparatus 107 . contents of the flowchart are stored as program codes in an optional storage medium ( not shown ) in the digital camera 101 , and read and executed by a cpu or the like of the digital camera 101 . first , in a step s 401 , the image transfer apparatus 106 obtains a list of all images to be transferred which have been recorded in the memory card 105 . in the image list , at least file names of the images and serial numbers corresponding to the image file names are described . the process ends when there is no image to be transferred . next , in a step s 402 , the image transfer apparatus 106 decides a directory name d in the disk apparatus 107 for storing the images after their transfer . this directory name is decided based on setting made by user , a date , and the like . for example , the directory name d is dlimages . subsequently , in step s 403 , the image transfer apparatus 106 designates a first image as a current transfer target , i . e ., an image whose serial number n is “ 1 ” in the image list . the image transfer apparatus 106 obtains a file name f of the image of the current transfer target from the memory card 105 in step s 404 , and checks whether or not the image of the current transfer target has been photographed as a grouped image in step s 405 . if the image is a grouped image , the process proceeds to step s 406 . if the image is not a grouped image , the process proceeds to step s 408 . in the case of the image of the serial number “ 1 , ” for example , a file name f is set to sta — 0234 . jpg . in step s 406 , the image transfer apparatus 106 obtains the group number 203 and the intragroup serial number 204 from the header part 201 of the image file of the current transfer target , and stores them as g and n respectively . in the case of the image of the serial number “ 1 , ” a shown in fig2 , the group number g is 00001 , and the intragroup serial number n is 001 . in a subsequent step 407 , the image transfer apparatus 106 decides a file name at a transfer destination when the grouped image is transferred . a file name including a directory in the disk apparatus 107 of the transfer destination is decided to be d ¥ g ¥ nf based on the g ( group number 203 ) and the n ( intragroup serial number 204 ), the image storing directory name d , and the file name f of the image in the memory card 105 . here , “¥” is a delimiter indicating a directory . in the case of the image of the serial number 1 , the file name d ¥ g ¥ nf including the directory is dlimages ¥ 00001 ¥ 001sta — 0234 . jpg . similarly , in step s 408 , when an image other than the grouped image is transferred , the image transfer apparatus 106 decides that a file name including a directory is d ¥ f in the disk apparatus 107 of the transfer destination . after the file name is decided in the disk apparatus 107 of the transfer destination through the aforementioned procedure , in step s 409 , the image transfer apparatus 106 transfers the image stored in the memory card 105 to the disk apparatus 107 with the decided name . after the transfer processing ends , in step s 410 , the image transfer apparatus 106 checks whether or not the image of the current transfer target is a last image of transfer targets recorded in the memory card 105 . if transfer of the last image has been finished , the image transfer apparatus 106 ends the processing . if the last image is not yet transferred , a next image is specified as a current transfer target in a step s 411 , then the process returns to step s 404 . the image transfer apparatus 106 transfers the images according to the aforementioned procedure , so that the grouped image information recorded in the header part 201 of the image file stored in the memory card 105 can be correlated to the directory name or the file name in the disk apparatus 107 . accordingly , the image display software 109 can provide the grouped images in a classified state to the user without analyzing the grouped image information recorded in the header part 201 of the image file . this is shown in the display example of fig3 . fig5 is a diagram showing a configuration of an image transfer system according to a second embodiment of the present invention . a digital camera 501 and a computer apparatus 503 are connected to each other through a cable 502 . the digital camera 501 that functions as an image creation apparatus includes a photography apparatus 504 , a built - in flash memory 505 , and an image transfer apparatus 506 for transferring image data . a disk apparatus 507 and a display apparatus 508 are connected to the computer apparatus 503 , which functions as an image processing apparatus . image display software 509 is operated on the computer apparatus 503 , and an image file recorded in the disk apparatus 507 is displayed on the display apparatus 508 . fig6 is a diagram showing an example of a file structure in the built - in flash memory 505 of the second embodiment . in the flash memory 505 , there are a dcim directory 601 and a misc directory 602 , and there is a 100 canon directory 603 as a subdirectory in the dcim directory 601 . in the 100 canon directory 603 , an image photographed by the photography apparatus 504 is stored in a jpeg file form . a mark file 604 having grouped information recorded therein is present in the misc directory 602 . fig7 shows an example of contents of the mark file 604 . in the mark file , one grouped image section 701 is present for each set of images , and a plurality of grouped image sections are present if there are plural sets of grouped images . at the top of the grouped image section , a group number 702 is described . subsequently , file names 703 including directories of images belonging to the sets are described , images being arranged one by one . according to the digital camera 501 of the second embodiment , after photographing images , a user can select a plurality of images present in the built - in flash memory 505 , and designate the selected images as a new set of grouped images . by this operation , a grouped section is added to the mark file 604 , and a designated image file name is described therein . in the grouped image section 704 thus added , a group number 705 is described , and file names 706 including directories of images belonging to the set are described , the images being arranged one by one . fig8 shows a display example of a screen in which the image display software 509 is displayed on the display apparatus 508 . the screen includes a menu 801 , a directory area 802 , a sort button 803 , and a thumbnail area 804 . in the directory area 802 , directories in the disk apparatus 507 are displayed in a hierarchical manner . when one of the directories displayed in the directory area 802 is selected , a list of thumbnail images of reduced image files present within the directory of the disk apparatus 507 is displayed in the thumbnail area 804 . in fig8 , a directory trip is selected . a plurality of sort buttons are arranged in the sort area 803 . by clicking the sort buttons 805 in order of file names , image files displayed in the thumbnail area 804 are sorted and displayed in ascending order of the file names . by clicking the sort buttons 805 in order of the file names again , the image files displayed in the thumbnail area 804 are sorted and displayed in a descending order . similarly , there are a date order sort button 806 and a type sort button 807 which can respectively sort thumbnails of the thumbnail area 804 in order of thumbnail updates or in order of types of image file forms . in the image display software 509 , grouped image information written in the header part of each of the image files present in the disk apparatus 507 is not analyzed , but the files present in the disk apparatus 507 are organized and displayed using attributes of file names , directory names and the like . fig9 is a flowchart showing a processing flow when the image transfer apparatus 506 transfers an image file recorded on the memory card 505 to the disk apparatus 507 . contents of the flowchart are stored as program codes in an optional storage medium ( not shown ) in the digital camera 501 , and read and executed by a cpu or the like of the digital camera 501 . first , in step s 901 , the image transfer apparatus 506 obtains a list of all images recorded in the built - in flash memory 505 to be transferred . in the image list , at least file names of the images and serial numbers corresponding to the image file names are described . the process ends when there is no image to be transferred . next , in step s 902 , the image transfer apparatus 506 decides on a directory name d in the disk apparatus 507 for storing the images after their transfer . this directory name is decided based on settings made by the user , a date , and the like . for example , the directory name d is trip . subsequently , in step s 903 , the image transfer apparatus 506 designates a first image as a current transfer target , i . e ., an image whose serial number n is “ 1 ” in the image list . the image transfer apparatus 506 obtains a file name f and a file update t of the image of the current transfer target from the memory card 505 in step s 904 , and checks whether or not the file name f is included in the mark file 604 in step s 905 . if in step s 905 it is determined that the file name f is included in the mark file 604 , the image transfer apparatus 506 obtains , in step s 906 , a file name l recorded in a head of a grouped image section which includes the file name f of the mark file 604 . subsequently , in step s 907 , the image transfer apparatus 506 obtains an update of the file l , and replaces a value of the update t obtained in step s 904 with this value . then , in step s 908 , the image transfer apparatus 506 obtains a group number g of the grouped image section including the file f from the mark file 604 . subsequently , in step s 909 , the image transfer apparatus 506 adds a character string “ st ” and group number to the head of the file name f obtained in step s 904 , rewrites the file name f in a form of & lt ; group number & gt ; _f , and then proceeds to step s 910 . if it is determined in step s 905 that the file name f is not included in the mark file 604 , the image transfer apparatus 506 directly proceeds to step s 910 . the image transfer apparatus 506 transfers a file from the built - in flash memory 505 to the disk apparatus 507 in step s 910 , then changes an update of the file transferred to the disk apparatus 507 to t in step s 911 . in step s 912 , the image transfer apparatus 506 changes the transferred file name to f . if an image regarding a serial number “ 1 ” is a file name img — 0001 . jpg , a group number 001 within the built - in flash memory 505 , the transferred file name is set to st001_img — 0001 . jpg . subsequently , in step s 913 , the image transfer apparatus 506 checks whether or not the image of the current transfer target is a last image of transfer targets recorded in the built - in flash memory 505 . if transfer of the last image has been finished , the image transfer apparatus 506 ends the processing . if the last image is not yet transferred , in step s 914 , a next image is specified as a current transfer target , and then the process returns to step s 904 . the image transfer apparatus 506 transfers the images according to the aforementioned procedure , so that the grouped image information recorded in the mark file 604 stored in the built - in flash memory 505 can be correlated to the file name and the file update in the disk apparatus 507 . the image display software 509 sorts files in order of file names or file updates , so that grouped images are always displayed in continuous positions . this is shown in the display example of fig8 . in other words , the image display software 509 can provide the grouped images in a classified state to the user without analyzing the grouped image information recorded in the mark file 604 . according to the second embodiment , the grouped image information recorded in the mark file 604 is correlated to the file name and the file update in the disk apparatus 507 . however , similar effects can be obtained only by adopting either the file name or the file update . as described above , the present invention can be also achieved by providing a storage medium , which stores program codes of the software for realizing the functions of the embodiments , to the system or the apparatus , and causing a computer ( cpu or mpu ) of the system or the device to read and execute the program codes stored in the storage medium . in this case , the program codes read from the storage medium realize themselves the aforementioned functions of the embodiments , and the storage medium storing the program codes constitutes the present invention . as such storage medium for supplying program codes , for example , a floppy disk ( registered trademark ), a hard disk , an optical disk , a magneto - optical disk , a cd - rom , a cd - r , a magnetic tape , a nonvolatile memory card , or a rom can be used . further , the functions of the embodiment are realized not only by the execution of the program codes read by the computer , but also realized by an operating system ( os ) or the like which is operated on the computer and executes real processing in part or in whole based on instructions of the program codes . this aspect is also within the invention . furthermore , the program codes read from the storage medium can be written in a memory installed in a function expansion board inserted into the computer or a function expansion unit connected to the computer . based on instructions of such program codes , a cpu or the like provided in the function expansion board or the function expansion unit executes real processing in part or in whole , thereby realizing the aforementioned functions of the embodiments , which is also within the invention . while the present invention has been described with reference to exemplary embodiments , it is to be understood that the invention is not limited to the disclosed embodiments . the scope of the following claims is to be accorded the broadest interpretation so as to encompass all modifications and equivalent structures and functions . this application claims priority from japanese patent application no . 2004 - 220386 filed jul . 28 , 2004 , which is hereby incorporated by reference herein in its entirety .
7
fig1 - 6 indicate the construction of the spot welding machine of the present invention concerning the embodiments of the present invention . fig1 reference numeral 1 indicates a main body of the spot welding machine of the present invention . the main body of said spot welding machine 1 is comprised a welding stand 2 , a holding portion 3 disposed above said welding stand 2 to hold an earth cable at the secondary side and a spot welding portion 4 disposed in the front side of said welding stand 2 . the earth cable holding portion 3 at said secondary side is constructed such that the holding portion of the angled form fixed above the welding stand 2 , a cylinder 6 for holding earth cable supported vertically at the side surface of the wall above the cylinder supporting element 5 , a lower arm ( fixed arm ) 11 for clamping an electric conductive detachable plate which is projected horizontaly from the upper end of the holding portion of the cylinder supporting element 5 ( toward left side in fig1 ), an upper arm ( rotatable arm ) 8 to clamp the electrode conductive detachable plate rotatably provided in the vertical direction by the cylinder rod 6a of the cylinder 6 for holding earth cable , said upper arm 8 being axially supported at the supporting member 5 by means of a hinge pin 7 at its middle portion of the back side and an earth cable terminal 9 at secondary side which is axially connected rotatably in left and right direction by means of a hinge portion 10 laterally from the upper arm 8 . the terminal 9 of the secondary side earth cable is integrally united through the electric conductive detachable plate 12 and the connection member 14b at one end . at the lower side of the end portion of the upper arm 8 , there is provided between a lower arm 11 and a pressing member 14a , the electric conductive detachable plate 12 ( a connecting electric conductive plate to connect the automobile door as a work to the secondary earth cable terminal 9 ). there is provided a first positioning pin 13 in the upper top portion of the lower arm 11 at the position while the electric conductive plate 12 faces to the pressure member 14a above the lower arm 11 to engage said first pin 13 with a first positioning hole 12a disposed in the electric conductive detachable plate 12 . as shown in fig1 said electric conductive detachable plate 12 is held by the spot welding machine main body 1 by inserting the first positioning pin 13 into the first positioning hole 12a . holding of the electric conductive detachable plate 12 is continued by action of a robot arm 81 in the material handling robot side until a work clamper 85 of a material handling tool ( jig ) 80 shown in fig2 clamps an automobile door 50 ( pressed work ) from the work conveying line and return to the upper portion of the spot welding machine main body 1 for welding operation and the work clamper 85 is clamped by an electric conductive detachable plate clamper 88 of a material handling tool side 80 . fig2 shows a construction of the material handling tool 80 suspended from the robot arm 81 via a robot wrist 82 and an adapter 82a . the material handling tool 80 is composed of a material handler 83 supported by the adapter 82a of the robot wrist 82 , a work clamper 85 supported under the material handler 83 via a cylinder 84 for clamping the work , an electric conductive element 87 which functions as an earth electrode provided against a work clamp arm 86 under a supporting bracket 91 , an electric conductive detachable plate clamper 88 provided on the tip end of said material handler 83 , an electric conductive plate 89 underneath the electric conductive detachable plate clamper 88 and an electric conductive earth connection plate 90 to connect the electric conductive plate 89 to the electric conductive element 87 . the work clamper 85 is constructed to rotatably support the work clamp arm 86 in the vertical direction via a hinge pin 92 under the supporting bracket 91 fixed to the material handler 83 . the tip end of the clamp arm 86 is inserted through a service hole 55 of a inner panel 51 of the automobile door 50 . a cylinder rod 84a of the work clamping cylinder 84 extends and the inner panel 51 is set to clamp and fix said automobile door 50 as shown in the figure . the electric conductive plate 89 of the electric conductive detachable plate clamper 88 is electrically connected to the inner panel 51 . in fig2 reference numerals 93a - 93c , and 97 indicate insulation members . the electric conductive detachable plate clamp 88 of the material handling tool side 80 is provided with a clamp piece 96 confronting with the electric conductive plate 89 having a second positioning pin 98 like the first positioning pin 13 in the holding portion 3 of the spot welding machine main body 1 . the clamp piece 96 is actuated downward by a clamp cylinder 95 . as shown with an imaginary line at the back side of the electric conductive detachable plate 12 via the insulation member 97 , the second positioning pin 98 is inserted through the second positioning hole 12b of said electric conductive detachable plate 12 . at the same time , clamping at the holding portion 3 is released . in this process the earth cable terminal 9 of the welding transformer is connected to the , inner panel 51 of the automobile door 50 . afterward , the material handling robot is actuated to take down the material handling tool 80 to the welding gun portion . a spot welding machine portion 4 disposed in front of the welding stand 2 is supported by a pole 19 supported in the vertical direction by upper and lower connecting members 17 and 18 , a guide rail 20 of a predetermined length fixed in the vertical direction in front of the supporting pole 19 , an electrode supporting arm 24 slidably supported in the vertical direction along the upper portion of the guide rail 20 , a back bar supporting arm 35 slidably supported in the vertical direction along the guide rail 20 with its end under the electrode supporting arm 24 and a supporting member 21 horizontally projected from the supporting pole an electrode supporting arm lifting cylinder 22 ( electrode lifting mechanism ) of which a cylinder rod 22a going through the back bar supporting arm 35 and a supporting member 37 projected from the supporting arm 19 . the spot welding machine portion 4 is further constructed by a back bar supporting arm lifting cylinder ( back bar supporting arm lifting mechanism ) 38 being connected to the back bar supporting arm 35 with a cylinder rod 39 , an electrode adapter 26 fixed on the supporting arm 24 via insulation member , a spot electrode 27 provided under the electrode adapter 26 , a first and a second flexible electric conductive plates 28 , 29 connected to the back of the electrode adapter 26 , an electric conductive connection plate 30 of an angle form connecting the second electric conductive plate 29 to a connection terminal 31 of a power cable 32 of the welding transformer , and a connection plate supporting member 34 to connect the connection plate 30 to the upper end of the supporting pole 19 via an insulation members 34a . in the meantime , as shown in fig3 at the portion confronting the spot electrode 27 of the back bar supporting arm , there is provided a back bar 61 freely follows along the contour of an outer panel 52 of the automobile door 50 . the back bar 61 is elastically supported on the back bar supporting arm 35 via the free mechanism of a spherical joint 65 and a compression spring 66 . in fig3 reference numeral 62 indicates a back bar mounting adapter , reference numeral 63 , 64 indicate a first and a second antirotation members , reference numeral 67 indicates an adjusting bolt and reference numeral 68 indicates an adjusting nut . degree of compression pressure of the compression spring 66 to the spherical joint 65 is changed by releasing the adjusting nut 68 to rotate the adjusting bolt 67 and a following pressure of the back bar 61 to the door outer panel 52 is freely adjusted . there is provided an engagement piece 25 at the back end of the electrode supporting arm 24 . in fig4 when weight of the electrode supporting arm 24 is loaded to the hemming portion 53 of the automobile door 50 , there is provided a balance cylinder 42 to eliminate the weight load to the hemming portion 53 by supporting the engagement piece 25 by actuation of the cylinder rod 41 . further reverting to fig1 reference numeral 100 indicates a air source which supplys free air pressure and free air flow to the electrode supporting arm lifting cylinder 22 and the back bar supporting arm lifting cylinder 38 , respectively . said air source 100 is connnected to the electrode supporting arm lifting cylinder 22 via a solenoid valve 101 providing with a port and b port , a first air pressure adjusting valve 102 and a first air flow adjusting valve 103 . the air source 100 is also connected to the electrode supporting arm lifting cylinder 22 via the magnetic electrode valve 101 and a second air flow adjusting valve 106 . further , said air source 100 is connected to the back bar supporting arm lifting mechanism 38 via the magnetic electrode valve 101 , the second pressure adjusting valve 104 and the third air flow adjusting valve 105 . it is also connected to the back bar supporting arm lifting cylinder 38 via the magnetic electrode valve 101 and a fourth air flow adjusting valve 107 . on the other hand , the air source 100 is connected to the balance cylinder 42 via a third air pressure adjusting valve 108 . now , as shown in fig1 the hemming portion 53 of the automobile door 50 is set at the welding position when the material handling tool 80 comes down to the spot electrode portion . in this position the magnetic electrode valve 101 is located in the a port side . one side of the electrode supporting arm lifting cylinder 22 is in exhausting condition and the other side is in pressing condition . the back bar supporting arm lifting cylinder 38 is in adverse condition . accordingly , said supporting arms 24 , 35 are in opened condition . on the other hand , when connection of air source 100 of the electromagnetic control valve 101 is changed from a port to b port , line l 1 is converted to pressing condition and line l 2 is converted to exhausting condition . afterward , air pressure in line l 1 is adjusted to a predetermined pressure at the first air pressure control valve 102 and then it is fed to the electrode supporting arm lifting cylinder 22 . on the other hand , air in the other side is exhausted , being controlled by the second air flow control valve 106 . the back bar supporting arm lifting cylinder 38 is actuated in adverse condition . accordingly , the electrode supporting arm 24 comes downward and the back bar supporting arm 35 synchronously goes upward . the back bar 61 contacts to the back side of the hemming portion 53 of the automobile door 50 . air pressure and air flow are precisely controlled by means of the second air pressure valve 104 , the third air flow control valve 105 at pressure side and the fourth air flow control valve 107 at exhausting side , so as to keep contacting pressure of the back bar 61 in optimum soft condition . as shown in fig4 the electrode supporting arm 24 comes down and the spot electrode 27 contacts the upper surface of the hemming portion 53 and then a predetermined clearance s is formed between the stopper 35a , 35a of the lower portion of the back bar supporting arm 35 and the stopper 40a , 40a of the upper portion of the supporting plate 40 of the electrode supporting arm lifting cylinder 22 . if such clearance s is not formed , the weight of the electrode supporting arm 24 is not loaded to the hemming portion 53 . on the other hand , if such clearance s is enlarged beyond the predetermined value , the weight of the electrode supporting arm 24 is loaded to said hemming portion 53 . when the above weight is loaded , the balance cylinder 42 is actuated to receive that lead . accordingly , the hemming portion 53 at work side is not loaded with the weight and is spot welded . a constant air pressure which is possible to keep balance against the electrode weight is supplied at anytime by means of the third air pressure control valve 108 providing with a relief function of the pressure line l 2 . the electrode supporting arm lifting cylinder 22 actuates slightly to generate an optimum spot welding pressure . then the spot electrode 27 proceeds spot welding . the optimum spot welding pressure is adjusted by means of the third air pressure control valve 102 . fig2 it is further preferable to combine the work clamper 85 which has earthing function and the work clamper 85 &# 39 ; which has no function of earthing as sown in fig6 . in fig6 reference numerals 93d , 93e indicate insulation members . reference numeral 91 &# 39 ; a indicates a clamp piece at the supporting bracket 91 &# 39 ; side . as aformentioned , the spot welding machine of the present invention can expand versatility of the jig at robot side and shorten the necessary length of the earth cable as well as decreasing construction cost . the working space factor at the circumference of the spot welding machine is improved as well as decreasing total cost . it is also possible to offer high quality products while leaving no pressed spot welding trace .
1
the invention is described hereafter in greater detail with reference to the accompanying drawings , which are provided without limitation , and in which [ 0012 ] fig1 is a diagram which schematically shows a first embodiment of the invention . in accordance with a first embodiment , the invention first consists in inserting a recall to a file situated on a web server in an electronic message . once the message is read — or displayed — by the recipient , this file is automatically recalled in a well - known manner , whereby a record is generated in the server log file . bu further selecting the log file , it is possible to learn whether the message has been read , or anyway displayed . further , it will be understood that if the file — typically an image file , possibly transparent — is created with a specific name on the server , and referenced as such in the electronic message , this will constitute a sort of receipt notice . the solution may be used exactly as described above . however , in order to make it accessible to a wider public , it shall be complemented by a client / server software solution . creating files to be recalled by the e - mail message on the server — including name creation algorithms , creating a record in a database , allowing to determine the correspondence between the file recall in the log file and the reference to the actual message ( sender data , message reference , send data , etc .) posting a confirmation e - mail to the sender — or providing this information by any means whatever ( e . g . by secure access to the database through on - line consultation interfaces ), the technical implementation of the first level solution may be illustrated by the following example : html code to be inserted in the electronic message & lt ; img src = http :// www . e - mail - receipt . net / custlmages / xxyyzzz123456 . gif & gt ; the server domain name “ e - mail - receipt . net ” is obviously provided as an example . according to a second embodiment , an advantageous simplification of the system is proposed , which is shown in fig2 . it shall be noted that , in this figure , the steps 1 , 2 and 3 may be reversed . in this case , the message is created immediately before step 3 , instead of step 1 . the simplification consists in inserting , in the html tag & lt ; img & gt ;, instead of a reference to an image file , the address of a page ( url ) whose parameter is a unique code . this code corresponds to a previously created record , whereby the system may select this record and send its issuer the confirmation that the corresponding message was actually viewed by the recipient . this allows to avoid the log file analysis part . therefore , the receipt sending process is immediate . the solution may be used exactly as described above . however , in order to make it accessible to a wider public , it shall once more be complemented by a client / server software solution . hence , a site , e . g . http :// e - mail - receipt . net may be created to implement the invention . this site allows a user connected to a network , e . g . the internet , who subscribes to the service ( as a client ) to : manage his / her profile ( first name , second name , password , e - mail address , defaults , etc . ), create new receipt notices ( by entering the subject / reference , expiration date , maximum number of receipts to be sent via e - mail , receipt visible by the recipient yes / no , etc .) and obtain the code to be inserted in the message . store his / her acknowledgements ( have them sent via e - mail and clear them from the server ). as shown above , in the secure part of the web site , the system user may create his / her own receipts . particularly , he / she may enter the desired subject / reference of the receipt he / she will receive via e - mail . he / she may also change default settings , e . g . the receipt time - out , the maximum number of e - mail messages to be sent , etc . when the user submits this form , a page appears which contains a code to be inserted in his / her message . the user may easily copy the code and paste it in message source code ( if the client software allows to do so ), or use the option “ insert image ” and paste therein the url of the request ( e . g . : http // e - mail - receipt . net / confirm . cfm ? id = xxyyzzz123456 ) the user enters the following instruction in a html electronic message in the first example , the user simply needs to create a record containing a unique number ( id ), the sender reference and the subject , and insert the code in the e - mail message to be sent . when the e - mail message is opened , the tag will be interpreted by the e - mail client of the recipient and the page will be recalled on the server . the software will simply have to search for the record that is referenced in the page recall ( id = xxyyzzz123456 ) and to give the sender referenced therein , a confirmation that his / her e - mail message has been actually opened . the main advantage of the solution proposed by the invention is that the read receipt is transmitted automatically , with no recipient intervention . an additional advantage is that the confirmation process is started by the sender , who can obviate the problem that the recipient might be unwilling to confirm receipt . it shall be noted that the system proposed by the invention does not affect privacy more than prior art solutions , as the information provided is already recorded in the log file of e - mail servers . this means that there is already a third party who is able to access this information ( generally the mail isp , for private mail , and the edp department or manager , for professional mail ). in fact , the information on the receipt delivering server is almost totally confidential , both for the sender and the recipient . the information known by the server only consists of a reference , a read date and time and an ip address . the e - mail address of the recipient is not required for proper process execution . the message content will not even transit through it . it shall be understood that the server database , possibly selectively accessible to the sender - client , may count the number of times that the electronic message has been opened by the recipient . the sender may enter a maximum number of receipts to be accounted on the server for a predetermined message . the server bill may depend on the number of transmitted receipts . it shall be also understood that , if the recipient opens the message offline and cancels the automatic connection attempt , the receipt request will not be sent over the network . users - recipients may advantageously install a program allowing to delay the request transmission until the next connection to the network . it shall be noted that one aspect of the invention proposes to insert a recall to a page or script , in lieu of an image file , in an htmp & lt ; img & gt ; tag . for instance , this tag might be : this novel aspect may be implemented independently of the automatic receipt notice system of this invention .
7
data transfer in the present invention is illustrated among computer systems using a communication network . a communication network of the present invention includes at least one computer system at each of several network nodes . each node is coupled by a link from time to time for communication with other nodes of the network . each link includes conventional computer communication technology of the type including , for example , local area , wide area , dedicated telephone , or satellite services and including conventional data communication hardware and software . the popular computer networks known as the internet , world wide web , and national information infrastructure are examples of such a communication network having nodes possibly at physically separate locations and addressed by a node address , for example a uniform resource locator ( url ), a name from a domain name system ( dns ), or an internet protocol address ( ip ). communication network 100 of fig1 includes computer systems , each shown in a block , that communicate for data transfer . communication of messages is illustrated by one or more lines between blocks , though it is apparent that one communication link between any two blocks is sufficient for any number of message lines . practice of variations of the invention is independent of whether such a link is maintained continuously , as in a dedicated line , or is maintained for the duration of the message as in some public multiple access facilities . communication technology provides known mechanisms and computer software for message transfer . this technology surrounds the message content data with other data that provide a mechanism for various purposes including tracking messages , synchronizing equipment , and assuring accurate and secure transfer of message content data . in the description that follows , digital works are transferred between nodes . the term “ content ,” therefore , refers to a digital work or a portion thereof . network 100 includes content acquisition node 102 , content managing node 104 , provider preparation node 106 , content providing node 108 , content requesting node 110 , authorizing node 112 , banking node 114 , event reporting node 116 , and reconciling node 118 . in operation , for content to be transferred on request to any of perhaps millions of content requesting nodes , the content is first received from a source and formatted for storage on one or more of perhaps thousands of content providing nodes . initially , a content developer , publisher , or distributor provides digital works , for example multimedia files , to content acquisition node 102 for encoding in a format efficient for storage and access by content managing node 104 . content is conveyed on line 130 as it becomes available for management by content managing node 104 . content from content managing node 104 is conveyed on line 132 and then made unique to each content providing node 108 by formatting processes performed by provider preparation node 106 . content providing node 108 receives content from time to time from provider preparation node 106 on line 134 . to request a data transfer in a preferred embodiment for the internet , a user or consumer at content requesting node 110 uses a network browser , such as microsoft internet explorer , and follows an internet link ( clicks on a portion of an html file display ), causing a message in http format to be conveyed on line 136 to content providing node 108 . content providing node 108 forwards the request on line 138 to authorizing node 112 . if the request is valid , authorizing node 112 creates a permit and sends it on line 146 to content requesting node 110 . a permit is a message created to uniquely respond to the request from a particular content requesting node . using portions of the permit , content requesting node 110 requests on line 136 particular files from content providing node 108 . in response , such particular files are conveyed on line 148 to content requesting node 110 , completing the data transfer . accounting for the above described transfer of content includes , for example , receiving payment from the user of content requesting node 110 , making payment for distribution services to at least the operator of content providing node 108 , and making payment to one or more owners of rights in the content . these accounting transactions find accurate basis in a reconciliation of reports from a variety of network nodes and reported at separate times during the data transfer process . for example , when authorizing node 112 receives the request and queries an access authority data base on content managing node 104 via lines 140 and 142 , content managing node 104 logs the query and reports the log on line 156 from time to time to reconciling node 118 . with knowledge of the identity of content requesting node 110 , an identity of the user , and a price of the requested work for a requested purpose ( for example , copy or preview ), authorizing node confirms a debit of an account kept on banking node 114 by messages conveyed on line 144 . banking node 114 logs the debit and reports the log on line 154 from time to time to reconciling node 118 . when the data transfer begins and again when at least some of the data has been transferred , content requesting node 110 reports on line 150 to event reporting node 116 . event reporting node 116 logs the events and from time to time reports the log on line 152 to reconciling node 118 . by comparing reports received on lines 152 , 154 , 156 , and possibly 158 ( from content providing node 108 ), reconciling node distinguishes valid complete data transfers from incomplete transfers and from events that could indicate intentional interference with the integrity of network 100 . for each valid complete transfer , reconciling node allocates revenues generated from the debits of users &# 39 ; accounts , discussed above with reference to line 144 . reconciling node then initiates funds transfers with messages to banking node 114 on line 160 for payments of , for example , distribution fees and royalties . each node of network 100 may represent more than one conventional computer system that performs , inter alia , methods of the present invention . multiple computers or multiple data storage devices may be necessary for maintaining a particular node &# 39 ; s functions operational in periods of high network traffic . such multiple computers may be at various physical locations , provided that only one network node address ( for example , an ip address ) is associated with each node . a method of the present invention for preparing content for storage on a content providing node includes separation of content and map information . when content is divided for convenience into several files in a conventional file storage system , map information identifies the particular files from the entire inventory on the storage system and the order of presentation of the files for reconstituting a particular work . separation of content and map information facilitates security measures without unduly compromising rapid provision of a work or performance of a work on a content requesting node . for example , as shown in fig2 content acquisition node 102 encodes ( using conventional data formatting and compression technology ) contract items associated with the work and encodes the work itself . when the work is primarily an audio recording , contract items may additionally include : name of the album , producer , label , publisher , mail order company , publishing year , bar code , album and track distribution levels , title of a track , performers , authors , composers , isrc code for the title , language , track number , duration , extract start and end times , number of allowed copies , price to preview ( listen ), price to make copy , rights collecting societies , authorized distribution areas , album cover picture , liner notes , other graphics , music style , associated country , and possibly pictures associated with the recording and text to be shown while the work is being played . receiver processes 204 and 206 ( using conventional communication and data storage technology ) on content managing node 104 , receive the encoded contract items and content and store each respectively on access authority data base ( aadb ) 208 and content masters store 210 . when a particular content providing node 108 is identified , works to be provided by that node are selected from content masters store 210 and scrambled by process 214 ( using conventional data security technology ). scrambling is a preferred ( though weak ) form of encryption that allows some security without unduly burdening data transfer or use of the work when requested . the scrambled result of a work is combined with a header , which includes encrypted data from access authority data base 208 , to form one or more content files . content files 217 are transferred for storage on store 216 of content providing node 108 . process 212 prepares map files 218 for transfer and storage on store 216 . descriptors of the work , of the content files , and of content providing node 108 are obtained from aadb 208 and formatted and encrypted by process 212 ( using conventional data formatting and encryption technology ). some or all of the descriptors , alone or in combination , may be subject to rigorous encryption . the map file permits content file locations to be random or at least unpredictable in store 216 , substantially decreasing the likelihood of unauthorized access without the system performance penalties associated with encrypting a content files 218 on store 216 . in a preferred embodiment for an audio recording , the map file includes a version number of a group of content files and a node address and pathname to each content file of the group . the node address corresponds to the unique node address of the content providing node for which content files are being prepared . each node address and pathname is encrypted separately . each content file of the group provides a different level of sound quality for the same audio material . different levels of quality provide , for example , flexibility in meeting the audio fidelity of different content requesting nodes . fig1 illustrates an example map file data structure 1300 when instantiated in memory at provider preparation node 106 . fig1 illustrates an example data structure 1400 of a header of a content file when instantiated in memory at provider preparation node 106 . content files 217 and map files 218 are organized for convenient access on store 216 using a conventional file system such as a directory system , shadowed physical drives , or a raid system . as indicated by ellipsis in fig2 many content acquisition nodes may supply content to content managing node 104 . many content providing nodes may be supplied with content files from content managing node 104 . due to differing security and traffic support requirements , it is preferred to operate network 100 with physically separate nodes 104 and 106 . in a variation , the functions of nodes 104 and 106 may be combined on one node or combined with content acquisition node 102 . various methods of the present invention for data transfer use to advantage ( a ) the cooperation of several network nodes , ( b ) linking a request through a registered node , ( c ) creating a permit using data from multiple sources , ( d ) using encryption , current time of day , or encryption keys based on unique properties of a node , and / or ( e ) providing unique structures and separate access to content files and map files . these features , inter alia , accomplish validating the request , validating the permit , and validating the data transfer operation itself . when validation is unsuccessful , data transfer is stopped , preserving the integrity of network 100 . the integrity of network 100 may be compromised by unauthorized copying , transfer , or use of a digital work . for example , as shown in fig3 a data transfer begins at content requesting node ( crn ) 110 . there a consumer or service user obtains a listing of titles , each title for a digital work . process 302 ( using a conventional browser and operating system ) responds to user input , for example a mouse switch closure (“ click ”) when an on - screen cursor points to a portion of an html page identifying a title , and in the conventional manner generates a message 303 to content providing node ( cpn ) 108 . process 304 ( using conventional http message technology ) forwards the request 305 to authorizing node ( an ) 112 . fig1 illustrates an example request data structure 1500 when instantiated in memory at authorizing node 112 . in a variation , process 304 determines the price to be billed for the request type and title and includes price and price currency with the forwarded request . price information is stored in file 306 which is available for editing by the operator of content providing node 108 . in a preferred embodiment , validate payment process 310 obtains price information via the associated map file from each content file after the validity of the request has been determined . process 308 validates the request by denying further processing to requests that do not meet predetermined criteria . in one variation , shown in fig6 process 308 includes the steps beginning at step 600 . at step 602 , the node address of content providing node ( cpn ) 108 is obtained from access authority data base ( aadb ) 208 . at step 604 , the cpn node address as provided in request 305 is compared to the cpn node address as provided from aadb 208 . if a match is found , control passes to step 606 , else to step 608 where the request is ignored . at step 606 , the node address of the calling page ( which contains the link that was followed by process 302 ) is compared to the cpn node address provided by aadb 208 . if a match is found , the request is considered valid and control passes to process 310 , else to step 608 where the request is ignored . process 310 ( using conventional data base and communication technology ) validates payment by the user by confirming that the user ( via pay price process 310 ) has made a proper debit on the user &# 39 ; s account . if a debit cannot be confirmed , request 305 is ignored . if confirmation of the debit transaction is successful , control passes to process 312 . process 312 creates a permit by combining information from more than one source . in one variation , shown in fig7 process 312 includes the steps beginning at step 700 . at step 702 , a map file 315 for the requested content is obtained either from the request or from store 216 on content providing node 108 . at step 704 , content providing node address , content price , and price currency are obtained from request 305 . at step 706 , local date and time are obtained from the authorizing node 112 . these data items are arranged , for example , in data structure 1600 instantiated in memory of authorizing node 112 , as illustrated in fig1 . at step 708 some or all data in permit data structure 1600 are encrypted to provide permit 313 . at step 710 , permit 313 is sent to content requesting node 110 . process 314 validates the permit by stopping the transaction for permits that do not meet predetermined criteria . in one variation , shown in fig8 process 314 includes the steps beginning at step 800 . at step 802 , that portion of the permit that is encrypted is decrypted . at step 804 , the syntax of each content file location ( content . cpn . node address . pathname ) is checked . the several pathnames in the permit provide ready access to the content file matching the sound quality level specified in request 305 ( see fig1 , request . sound . quality ). if the syntax check fails , control passes to step 810 to stop the transaction . otherwise control passes to step 806 where the content requesting node address provided in permit 313 is compared to the node address of content requesting node 110 . if no match , control is transferred to step 810 . if a match is found , control passes to step 808 , the current date and time on content requesting node 110 is compared to the date and time value stamped by authorizing node ( an ) 112 on permit 313 ( an . date . time ). if the current time is more than a predetermined amount ( for example , 5 minutes ) after an . date . time , then control passes to step 810 and the transaction stops . otherwise , control passes to step 812 and , in due course , to process 316 . process 316 reports the start of a data transfer between content providing node 108 and content requesting node 110 . generation of the report may occur before data transfer actually starts or during an initial phase of data transfer . a start report is made to one or more event reporting nodes as specified by a list on content providing node 108 . the report is transmitted by packet message techniques on a separate port so as to avoid interference with the data transfer itself which may be underway on another port . the two ports may share the same communication hardware such as a single line to an internet service provider , as is well known in applications of tcp / ip . for other communication hardware and software configurations , concurrent ports may be arranged on two or more hardware communication links . in one variation , shown in fig9 process 316 includes the steps beginning at step 900 . at step 902 , one or more event reporting node addresses are obtained from list 318 on content providing node 108 . at step 904 , a port is opened for each event reporting node on list 318 . in a preferred embodiment , ports 1000 through 1016 are used , although other port numbers may be equivalently accommodated by the communication software on content requesting node 110 . if no event reporting node successfully responds after attempts have been made to couple it for communication , then either the transaction is stopped or the transaction continues without the capability to generate reports . at step 906 , a port is opened for reporting to content managing node 104 , using the next available port number from the range 1000 through 1016 . at step 908 , information from request 305 is obtained and placed in a data structure in memory . fig1 illustrates a start report data structure 1700 when instantiated in memory at content requesting node 110 . for data structure 1700 , such data includes the content requesting node address , the username and password , and the price , currency , and specified sound quality . at step 910 , data from permit 313 is added to the start report data structure . for data structure 1700 , such data includes the content file location for the specified sound quality level , i . e . a corresponding content . cpn . node . address . pathname . quality . level . at step 912 , data from the content file header is added to the start report data structure . for data structure 1700 , such data include the title , artist , copyright , duration , id . code . type ( whether isrc , iswc , or etc . ), the id . code . number , the content providing node address , and a file number ( a serialized number assigned by encoding process 202 ). at step 914 , local values of the content requesting node are added to the start data structure . for data structure 1700 , such values include a transaction number for discriminating reports from the same user , the current date and time , an encryption key unique to the content requesting node , and values from which the country in which content requesting node 110 is located . these later values include in one variation of the present invention , the time zone , the language identified by the operating system of node 110 and the keyboard identified by the operating system of node 110 . country location is important to allocating royalties under the laws that vary from one jurisdiction ( country ) to another . at step 916 , the report is placed in final format using conventional techniques and at step 918 it is sent to each event reporting node , for example node 116 , and to content managing node 104 . process 320 obtains and uses the requested content files . after a content file header has been received by process 320 , the transaction may be stopped if contents of the header do not compare favorably with the permit . in one variation , a summary report is prepared before data transfer of all requested files is complete . in a second variation , a duration of use of the files is measured and reported in a summary report , prepared and sent after all files have been received or usage is determined to be substantially completed . in the later case , shown in fig1 , process 320 includes the steps beginning at step 1000 . at step 1002 , a port is opened for content provider node file transfer ( in addition to ports opened for reporting as discussed above ). at step 1004 , the header of the requested content file is obtained . the pathname to this content file is provided in permit 313 for a corresponding sound quality of content requesting node 110 . after decrypting the pathname itself , at step 1006 , the header of the specified content file is decrypted . at step 1008 , if the content providing node address in the obtained content file header does not match the content providing node address as permitted , the transaction stops at step 1010 . otherwise , control passes to step 1012 . at step 1012 , the usage mode as permitted is compared to the usage mode as requested . the user specifies a usage mode at the time of picking a title for a digital work to facilitate calculation of an appropriate price . for example , in many cases , the price for previewing a work ( as in listening to a portion of an audio work ) is less than the price for making a copy of a work for unlimited use . if the requested and permitted usage modes both indicate a copy is to be made , that is , the data transferred will be stored for repeated use , then control passes to step 1202 on fig1 . otherwise , control passes to step 1102 of fig1 . steps 1102 through 1108 obtain all subsequent blocks of the requested content file and , after each block is received , perform the digital work according to the data in that respective block . unscrambling of the data may be required . performance or preview may be , for example one or more of the following : playing audio , showing visual , performing multimedia , or executing computer program digital works . for example , when an audio file is being received , unscrambling is performed and the resulting data may be played without interruption . at step 1110 , information from several sources is combined to form a summary report . one purpose of the summary report is to indicate for purposes of reconciliation , the duration the digital work was being performed . fig1 illustrates a summary report data structure 1800 when instantiated in memory at content requesting none 110 . for summary report 328 , data items from start report structure 1700 ( having the same names ) are formatted in summary report data structure 1800 . at step 1112 , the summary report is sent through ports opened in steps 902 and 904 to one or more event reporting nodes . the transaction is completed at step 1114 . if at step 1012 , a copy of the work has been permitted , control passes to step 1202 . at step 1202 , a destination file for receiving the digital work is opened on the content requesting node 110 . at step 1204 , an encryption key is prepared using conventional data security technology . at step 1206 , the content file header is obtained and written to the destination file . at steps 1208 through 1214 , each block of the requested content file is obtained , encrypted , and written to the destination file . at step 1216 , the destination file is closed . at step 1218 the transaction is completed . from time to time , reports are generated by various nodes for checking the integrity of network 100 and for allocating revenues received by debiting user accounts as described with reference to fig3 process 310 . five reports are provided in network 100 . access report 332 is provided by content managing node 104 from queries of aadb 208 initiated by authorizing node processes 308 through 312 . fig1 is a memory map of data structure 1900 of an access report record when instantiated in memory of content managing node 104 or reconciling node 118 . report 342 is provided by banking node 114 from debit transactions requested by process 310 of authorizing node 112 . fig2 is a memory map of a data structure of a debit report record when instantiated in memory of banking node 114 or reconciling node 118 . reports 326 and 328 respectively provide the start and summary information from content requesting node 110 . data structures 1700 and 1800 correspond to a single record of the start report and summary report respectively when instantiated in memory of reconciling node 118 . finally , report 336 may be generated by content providing node 108 . each report consists of multiple records , each record having multiple fields . because these reports have some fields in common , comparison of the data in identical fields (“ reconciliation ”) provides the basis for distinguishing valid complete transactions from interrupted and unauthorized transactions . for example , an access report record 1900 , debit report record 2000 , start report 1700 , and summary report 1800 each include a tracking field for the value : request . crn . node . address . transaction . number . by noting whether all four records having the same value for this tracking field have been received at reconciling node 118 , conclusions about network integrity and allocation of funds can be reliably made . a method for reconciling reports of the present invention includes accommodations for high volume event report processing . in addition , reconciled reports may be used to identify nodes having suspect operations and thereby provide a way of detecting unauthorized copying and use of digital works . in combination with the operation of the aadb 208 , unauthorized use may be blocked . for example , if unauthorized transactions frequently involve the same content providing node address , that node address may be deleted from the list of registered content providing nodes by an appropriate operation on aadb 208 . when a content requesting node makes a request through the link at the offending content providing node address , the request will be denied at the authorizing node . an example of a reconciliation method of the present invention is illustrated in fig4 . event reporting node 116 receives start report 326 and summary report 328 at high traffic levels from numerous content requesting nodes . each report is logged as an event by process 402 using conventional database technology . logged events are stored for a time in events data base 404 . synchronization of multiple parallel event reporting nodes may result in additional database transactions by event reporting node 116 as to records in events data base 404 . from time to time records from events data base 404 are provided to reconciling node 118 . process 406 , using conventional data base technology , accomplishes the comparison of records having one or more respective field values that are identical . in one variation , the tracking field is used exclusively . table 502 in fig5 identifies results of reconciliation for several combinations of reports being reconciled . if for a given tracking field value ( or at a given time , date , content requesting node , and content providing node ), reports a 332 , b 342 , c 326 , d 328 , and possibly e 336 have been logged , then a group of messages accomplishing a normal request and payment for data transfer can be inferred to have been completed successfully . allocation of earnings by process 408 follows the identification of such a reconciliation result . if on the other hand , no report is received for reconciliation having the given common field values , then it can be suspected that software on one or more nodes of network 100 may have been manipulated , compromising network integrity . due to the large number of content requesting nodes and the lack of physical controls that could protect software on such nodes from being manipulated , it is likely that at least some of the failures to receive all expected reports may be a consequence of content requesting node software manipulation . in cases 508 and 510 , some or all requested data transfer might have been successful ; however , allocation of earnings may not be justified when there remains a possibility that a user of the respective content requesting node may insist that the debit to his account be reversed . allocation of earnings by process 408 is consummated by generating , according to conventional banking messaging and data base technology , requests for funds transfer by process 410 in banking node 114 . as described in detail above , network 100 overcomes the problems of the prior art and provides a basis for accurate allocation of earnings to the owners of rights in digital works stored on systems of the present invention or transferred according to methods of the present invention . these and other benefits are provided with lesser system performance penalties than heretofore possible . the present invention has been described in the preferred embodiments . several variations and modification shave also been described and suggested . other embodiments , variations , and modifications known to those skilled in the art may be implemented without departing from the scope and spirit of the invention as recited in the claims below .
6
fig1 comprises a schematic representation of a housing 10 which encloses the apparatus of the present invention . the housing 10 is shown as being generally rectangular in configuration , but it is obvious that any appropriate , contemporary style housing may be used . the housing 10 includes an instruction plate 12 on which are printed instructions for use of the apparatus . sequentially , after reading the instructions , a user inserts coins in a coin receptor 14 which is disposed on the top of the housing 10 . for illustrative purposes herein , two quarters are required to actuate the apparatus of the present invention and accordingly a user inserts two quarters sequentially into the coin receptor 14 . after the quarters have been inserted , the user is then directed to four time - select switches which are preferably located beneath the instruction plate 12 . the time selector switches include a thirty - minute or one - half hour selector switch 20 , a sixty - minute or one - hour selector switch 22 , a one - and - one - half hour or ninety - minute selector switch 24 , and a one - hundred - twenty or two - hour time selector switch 26 . the user may select any of the time periods by actuating or depressing any one of the switches 20 , 22 , 24 , or 26 . it will be noted that regardless of the time selected , the cost is the same , namely fifty cents or two quarters . at the lower portion of the housing 10 , and beneath the time selector switches , are three digital readout indicators , including an hour readout indicator 30 , a tens of minutes readout indicator 32 , and a minutes readout indicator 34 . the readout indicators indicate the time remaining after the coins have been inserted into the coin receptor 14 and the appropriate time selected by depressing one of the time selector switches 20 , 22 , 24 , or 26 . three conductors are shown extending between an interface circuitry block 38 for connection to the readout digits 30 , 32 , and 34 . the interface circuitry will be discussed below . fig2 is a schematic representation of a coin selector switch 40 which is employed internally of the apparatus and is associated with the optoisolators illustrated schematically in fig4 and also illustrated in conjunction with the schematic diagram comprising fig5 . the coin selector switch 40 is connected to terminal b and the switch may be rotated to connect with either terminal c , terminal d , terminal e , or terminal f . the terminals c , d , e , and f , respectively represent the insertion of a single quarter , two quarters , three quarters , or four quarters . that is , by selecting or connecting the switch 40 to the appropriate terminal c , d , e , or f , the installer / proprietor may pre - select the number of coins required to operate the timer apparatus . as indicated in fig2 and as discussed herein , switch 40 is connected to terminal d which determines that two quarters ( fifty cents ) are required to operate the apparatus . the significance of terminal b and terminals c , d , e , and f will be explained in detail below . fig3 is a schematic diagram of power supply apparatus 50 usable with apparatus of the present invention . a pair of batteries 52 and 54 are connected in parallel with a monolithic voltage regulator integrated circuit 56 . the batteries 52 and 54 may be any appropriate voltage source , such as a pair of lantern batteries . the integrated circuit 56 is in turn connected with terminal a which comprises the power supply for the apparatus of the present invention . it will be noted that by using lantern batteries for batteries 52 and 54 , the circuitry apparatus of the present invention should last for many months under virtually continuous use . the circuitry , including the integrated circuits and other circuit components involved in the apparatus of the present invention have been chosen , in part , for their low power consumption . as will be noted in conjunction with figs . 4 and 5 , terminal a , the voltage source or supply , is connected to the circuitry at a plurality of different , required , locations . the voltage regulator 56 may be a 7805 ic . fig4 is a schematic representation of a pair of infrared led optoisolators connected together and used in conjunction with the coin receptor apparatus 14 , shown schematically in fig1 . fig4 accordingly comprises an optical coin identification circuit 60 . the circuit 60 includes a light emitting diode and a phototransistor . the optoisolators 62 and 72 are connected together , as shown in fig4 with the anodes of the light emitting diodes ( led &# 39 ; s ) connected to a common terminal a , the power supply terminal ( see fig3 ) and the cathodes of the led &# 39 ; s also connected together and to a ground . the ground is also common to the emitters of the phototransistors . the collectors of the phototransistors are in turn connected to voltage supply terminal a through appropriate resistors , and also through a pair of diodes and resistors to terminal g . in practice , the coin receptor 14 is adjusted with respect to the optoisolators 62 and 72 such that only the outer edge of a quarter breaks the light beam between each led and its phototransistor . in this manner , a false triggering of the apparatus or enabling of the apparatus will not occur by using a coin other than a quarter . the transistors in the optoisolator are always in their &# 34 ; on &# 34 ; state . however , the output is blocked by diodes 64 and 74 , which are respectively tied to the phototransistors in the optoisolators 62 and 72 . with the output of the transistors blocked , terminal g is &# 34 ; off &# 34 ;. it is only when both optoisolator 62 and 72 have their respective light beams broken by appropriate coins , such as quarters as discussed herein , will terminal g see a positive voltage . accordingly , only a quarter coin will provide a positive voltage output to terminal g by breaking the light beam in the optoisolators . fig5 is a schematic circuit diagram of the timing apparatus of the present invention . as indicated above , the particular components represented in fig1 , 3 , and 4 are also represented in fig5 . the various components are shown in fig5 as required to illustrate the functioning of the present invention . the schematic circuit diagram of fig5 is generally designated by reference numeral 36 . as shown in fig5 four discrete integrated circuit modules are used in the apparatus of the present invention . one of the integrated circuit packages is a shift register 100 , typically a 4015 ; one is a dual timer ic 110 , typically a 556 ; one is a quad , two - pole and - gate integrated circuit 120 , typically a 4081 ; and the last one is a timer 130 , typically a 555 . in the following discussion , where necessary , a particular pin of one of the ic modules will be identified by number . in operation , the optoisolator 60 is connected to terminal g , which is in turn the input terminal to pin 9 of the shift register ic 100 . the input to pin 9 from terminal g produces a pulse which is in turn seen at terminals c , d , e , and f which are connected to the respective pins 10 , 3 , 4 , and 5 of the shift register 100 . it will be noted that terminals c , d , e , and f are in turn connected by a switch 40 to terminal b in the coin select circuitry discussed above in conjunction with fig2 . terminal b is in turn connected to pin 8 of one - half of the dual timer ic 110 , designated herein as timer half 112 . the first coin inserted into the coin receptor 14 produces an output pulse on terminal g which is seen at terminal c , but terminal c is not connected to the switch 40 . the second coin inserted into the optoisolator 60 produces another output pulse on terminal g which results in a pulse seen at terminal d because of the shifting action of the shift register 100 . with switch 40 connected to terminal d , the pulse seen at d is in turn transmitted through switch 40 to terminal b and pin 8 of the timer half 112 of dual timer 110 . the input to terminal 8 triggers the startup circuit at timer half 112 of the dual timer 110 . the timing circuit of one - half of the dual timer 110 is preset for a period of fifteen seconds and accordingly the initial timer portion of 110 , designated by reference numeral 112 , is &# 34 ; on &# 34 ; for fifteen seconds after being triggered . while timer half 112 is &# 34 ; on &# 34 ; for fifteen seconds , output from pin 9 of timer half 112 turns on an scr designated by reference numeral 42 , and the output from pin 9 of timer half 112 also turns on switching transistor 44 . the switching transistor 44 turns on the selector swtiches 20 , 22 , 24 , and 26 to allow the user of the apparatus to select the appropriate time by depressing one of the momentary switches 20 , 22 , 24 , or 26 , illustrated in fig5 and also in fig1 . it will be noted that one of the selector switches 20 . . . 26 must be depressed within the fifteen second time interval during which the half timer 112 is &# 34 ; on &# 34 ; because transistor 44 turns &# 34 ; off &# 34 ; at the expiration or termination of the fifteen second time period when the half timer 112 turns off . if no time is selected furing that fifteen second time period by the expiration of one of the selector switches 20 . . . 26 , two additional coins must be inserted in order to reactivate the apparatus by again triggering the half timer 112 . the switches 20 . . . 26 are connected respectively to the gates of four scr &# 39 ; s are in turn connected to input pins of the quad , two pole and - gate ic 120 . the input to ic 120 from the scr &# 39 ; s 80 , 82 , 84 , and 86 provides the bias for one side of the respective discrete and - gates within ic 120 in accordance with the respective connections . that is , scr 84 , when turned on by switch 24 , is connected to pin 2 of ic 120 , and pin 2 comprises one - half of a single and - gate within ic 120 . similarly , when switch 22 is closed , scr 82 is turned on to provide a bias to input pin 6 of ic 120 which is connected to one - half of another and - gate . in a similar fashion , scr &# 39 ; s 80 and 86 are respectively turned on by switches 20 and 26 to provide a bias to pins 9 and 12 of ic 120 which each comprise one - half of two additional and - gates . thus an input to terminal b , connected to pin 8 of timer half 112 of timer 110 results in a limited , fifteen second , time period during which the appropriate , desired time interval may be selected by a user by selecting any one of the switches 20 , 22 , 24 , or 26 . the depression of the switches , which are momentary switches , as indicated above , spring biased to the &# 34 ; off &# 34 ; position , results in the turning on of one of the scr &# 39 ; s , respectively 80 , 82 , 84 , and 86 , and the turning on of one of the scr &# 39 ; s results in an input to one - half of an and - gate in ic 120 . at the same time , the second half of dual timer 110 , comprising a timer half 114 , is activated . the timer half 114 comprises an electronic clock which produces a substantially constant output at a frequency of one millihertz , or once each 16 . 67 minutes . that is , the output of timer half 114 comprises a positive pulse lasting sixteen and two - thirds minutes , and a negative pulse lasting sixteen and two - third minutes , for a total cycle of 331 / 3 minutes . the timer half 114 is turned on by the output of scr 42 through a switching transistor 116 connected to pin 4 of timer half 114 of the dual timer 110 . the transistor 116 is normally on . when it is momentarily turned off , as will be described below , the timer ic 110 is reset . with each positive transistion of the one millihertz pulsed output from pin 5 of timer half 114 of pin 1 of shift register 100 , there is one shift of the shift register 100 with respect to pins 2 , 11 , 12 , and 13 , and the output from the pins 2 . . . 13 is appropriately transmitted to the complementary pins 1 , 5 , 8 , and 13 , respectively , of and - gate ic 120 . if both complementary pins of and - gate ic 120 are biased on equally , then the output from the and - gates to the pins 4 , 3 , 10 , and 11 of the ic 120 through diodes connected to each output pin is &# 34 ; on &# 34 ; to transistor 46 . if there is no equal bias on the complementary pins of each and - gate , then the respective and - gates are &# 34 ; off &# 34 ;. with respect to the and - gate ic 120 , the complementary pins for the four and - gates included in ic 120 comprise input pins 2 , 6 , 9 , and 12 , and pins 1 , 5 , 8 , and 13 . the output pins from the four and - gates include pins 4 , 3 , 10 , and 11 . the time period initially selected is , as described above , manifest by the actuation of one of the switches 20 . . . 26 , which results in the turning on of one of the corresponding scr &# 39 ; s 80 . . . 86 . as previously indicated , each scr is connected to one of a pair of inputs of and - gates within ic 120 . accordingly , the actuation of a switch and the turning on of an scr results in an input to one - half of an and - gate . the other halves of the respective and - gates are tied to one of the pins 2 , 11 , 12 , or 13 of ic 100 . as the shift register ic 100 receives an input from the clock timer half 114 in ic 110 , the second inputs to the four and - gates and consecutively turned on by the outputs from the shift register ic 100 . the four and - gates will consecutively receive an input , but only the and - gate receiving a signal from an scr will provide an output in response to the consecutive outputs from the shift register 100 . accordingly , at the end of the preselected time period , an output will result from one of the and - gates in ic 120 through a blocking diode to the base of transistor 46 . if one of the and - gates is &# 34 ; on &# 34 ;, then there will be an output through a diode from one of the and - gate outputs 4 , 3 , 10 , or 11 , to the base of transistor 46 which causes transistor 46 to turn on . when transistor 46 turns on and conducts , timer 130 , which comprises an integrated circuit , is turned on . ic timer 130 comprises a reset circuit having a timing out period of ten seconds after being triggered . when the ic 130 turns on , four different occurrences transpire substantially simultaneously . one occurrence is that the scr &# 39 ; s 80 , 82 , 84 , and 86 are turned off , which in turn causes the and - gates in ic 120 to turn off . the scr &# 39 ; s 80 , 82 , 84 , and 86 are turned off when a switching transistor 88 is turned off by the output from pin 3 of ic 130 through conductor 132 to the base of the transistor 88 , which turns the transistor 88 off . the second occurrence is that the shift register 100 is reset through conductors 134 , 135 , and 136 extending between pin 3 of ic 130 and pins 6 and 14 of ic 100 . the third occurrence which transpires when reset timer ic 130 turns on is the resetting of both sides of timer ic 110 . timer halves 112 and 114 of ic 110 are reset by the output of pin 3 of ic 130 through conductor 134 to the base of a switching transistor 116 , which turns the transistor 116 off . the fourth occurrence is the turning on of an audio output element 140 , which may be any of the oscillators , well - known in the market , such as the mallory sc 628p . audio element 140 is turned on by the output from pin 3 of ic 130 through conductors 132 and 133 . the ic 130 is in an &# 34 ; on &# 34 ; state for ten seconds , after which time it turns off , causing the audio element 140 to also turn off and , at the same time , allows transistors q2 and q4 to return to their normal &# 34 ; on &# 34 ; state . it will be noted that transistors 44 , 88 , and 116 are switching transistors and accordingly may be referred to simply as &# 34 ; switches &# 34 ;. however , transistor 46 is a high current switch , whose purpose is to switch the high current required for timer ic 130 , as opposed to the simple &# 34 ; on &# 34 ; and &# 34 ; off &# 34 ; function of transistors 44 , 88 , and 116 . when timer ic 130 turns off , the timer apparatus is then ready for the next customer or user who inserts a pair of quarters into the coin receptor 14 , shown in fig1 . between ic &# 39 ; s 100 and 120 are four conductors , namely conductor 102 extending between pin 2 of ic 100 and pin 1 of ic 120 , conductor 104 extending between pin 11 of ic 100 and pin 5 of ic 120 , conductor 106 extending between pin 12 of ic 100 and pin 8 of ic 120 , and conductor 108 extending between pin 13 of ic 100 and pin 13 of ic 120 . each of the conductors 102 , 104 , 106 , and 108 includes a terminal connection designated respectively as terminals h , i , j , and k . the terminals h , i , j , and k are connected to interface circuitry 38 , shown as a block in fig1 between the circuitry 36 of fig5 and the visual display indicated in fig1 . the interface circuitry 38 preferably comprises a total of seven well known integrated circuit chips plus three led digits . the integrated circuit chips are a counting chip , three latching chips , and three driver chips . all seven ic &# 39 ; s are well known in the art and perform well known functions . for example , the counting chip receives its input information from the terminals h , i , j , and k with respect to the time selected by the procedure outlined above . the latching chips hold the last piece of information between the clock pulses produced by the counting chip . the three drivers take the information in binary coded decimal ( bcd ) form , and convert the information to seven segment display form which in turn is used for the respective three digits or numerals 30 , 32 , and 34 . it will be noted that while there is only one counting chip needed , there are three latching chips and three driver chips , one for each of the three digits or numerals . the three numerals 30 , 32 , and 34 , illustrated in fig1 comprise seven segment display led &# 39 ; s for visual readout . as indicated previously , the apparatus of the present invention counts down rather than up . accordingly , when the apparatus is activated , the maximum time selected appears first as information in terms of hours , ten minutes , and minutes , on the numerical display characters 30 , 32 , and 34 , respectively . the numerical characters or digits in turn count down from the maximum time selected to the end of the selected time period . fig6 is a schematic diagram of an analog switch integrated circuit , such as a 4016 , which may be used in the apparatus of fig6 to replace transistors 44 , 46 , and 88 . it will be noted in fig5 that the three connections for each of the transistors 44 , 46 , and 88 , namely the base , emitter , and collector , have been given an alphabetical or letter designation . the base of transistor 44 has been designated with reference letter o , the emitter of transistor 44 with letter p , and the collector of transistor 44 with letter q . the collector , emitter , and base of transistor 88 have been designated respectively by letters l , m , and n . the base , collector , and emitter of transistor 46 have been respectively designated by leters r , s , and t . in fig6 the respective terminals of the ic 150 are shown with the respective letters connected to the identified pins of the 4016 chip . in addition to the circuit connections , other pins of the chip are also indicated as being connected to ground and to a voltage source through a biasing resistor . it will be noted in the schematic diagrams that only certain components have been specifically identified with reference numerals . for example , various components , such as various conductors , the two capacitors , the four diodes , the two variable resistors , and the various fixed resistors in fig5 have not been specifically identified . their use in the circuitry is well known and understood . for example , the two capacitors comprise timing capacitors , and the variable resistors comprise timing resistors , both of which functions are well known and understood . the diodes comprise blocking diodes , and the fixed resistors comprise biasing resistors , again both of which functions are well known and understood . while the principles of the invention have been made clear in illustrative embodiments , there will be immediately obvious to those skilled in the art many modifications of structure , arrangement , proportions , the elements , materials , and components used in the practice of the invention , and otherwise , which are particularly adapted for specific environments and operative requirements without departing from those principles . the appended claims are intended to cover and embrace any and all such modifications , within the limits only of the true spirit and scope of the invention . this specification and the appended claims have been prepared in accordance with the applicable patent laws and the rules promulgated under the authority thereof .
6
a schematic of a standard ice resurfacing machine is shown in fig1 . main body ( 10 ) encloses an internal combustion motor or electric motor for propelling the unit and powering other components . it also encloses a storage tank for ice shavings , tanks for wash water and ice making water , and an operator &# 39 ; s seat and controls ( 11 ). the sled or conditioner ( 12 ) is attached to main body ( 10 ) by hydraulic arms ( 13 ). fig1 shows only some of the components of conditioner ( 12 ). a horizontal conveyor ( 14 ) for moving ice shavings to the center and throwing them onto a vertical conveyor ( 9 ) is placed forward of shaving blade ( 15 ) mounted to draw bar ( 16 ). remaining elements of the conditioner are not shown . fig2 - 4 show the flow of ice cuttings during operation . horizontal conveyor ( 14 ) collects ice cuttings generated by cutting blade ( 15 ). the helical flights ( 18 ) are oriented so that cuttings are swept from the outside toward the center , where slinger paddles ( 19 ) throw the cuttings at the open mouth ( 21 ) of vertical conveyor assembly ( 9 ). the flights ( 22 ) of a vertical auger or conveyor carry the cuttings upward to the top ( 23 ) of the conveyor , where they are engaged by the vertical slinger paddles ( 24 ) and flung into the storage tank . the problem with ice build - up in front of the horizontal conveyor is shown in fig5 - 8 . as seen in fig5 , a spray of loose ice cuttings is constantly thrown out of the front side of the horizontal conveyor by both the slinger and the centrifugal effect caused by the conveyor &# 39 ; s rapid spinning . some cuttings bounce off the vertical conveyor housing and others fall on the ice in front of the machine . under certain environmental conditions , ice cuttings form clumps instead of remaining as a fine powder . these clumps may be thrown forward as shown in fig6 . if clumps do not fall within the space between the auger flights of the horizontal conveyor , the clumps will be struck by the leading edge of a flight , pushing the clump forward . if clumps are not ingested by the conveyor , they may be combined with thrown ice particles and other clumps to form a build - up that increases in size and weight as the machine moves forward . fig7 and 8 show an example of build - up in front of the horizontal conveyor . the ice build - up under the most adverse operational conditions , such as slush on the ice or extreme cold , can become solid enough to support very high pressures exerted by the horizontal conveyor , resulting in a build - up that obstructs the conveyor system , compromising the quality of the resurfacing run . it is possible for the blockage to exert enough force that the machine &# 39 ; s rubber - tire - on - ice traction cannot overcome it , resulting in a stopped machine and an aborted conditioning run . in one embodiment of present invention shown in fig9 - 11 , the horizontal conveyor ( 14 ) uses a double flight design , with two helical auger flights ( 31 , 32 ) winding around the conveyor &# 39 ; s central shaft , ( 33 ) and two slinger paddles ( 34 , 35 ) used in the central slinger section . this new design does not use a circular cross section , and does not use a constant auger flight radius . instead , the conveyor is bisected length wise into two halves along the axis of the conveyor &# 39 ; s central shaft . the two conveyor halves have semi - circular cross sections , and create an overall shape of two hypothetical half cylinders of different radius , with each half covering 180 degrees of the 360 degrees of rotation around the conveyor &# 39 ; s central shaft . the semi - circular cross sections of the two half cylinders share a common radius center ( 36 ) along the axis of the conveyor &# 39 ; s central shaft ( 33 ). the two halves differ from each other only in that they have different cross sectional radii , with the radius of one half being slightly smaller than that of the other half . consequently , the conveyor can be described has having a larger radius half , ( 37 ) and smaller radius half , ( 38 ) separated from each other by a bisecting plane ( 39 ) extending along the axis of the conveyor &# 39 ; s central shaft ( 33 ). the difference in length between the larger and smaller flight radii used by the new conveyor design is the conveyor &# 39 ; s “ radius differential ”. the size of the radius differential is exaggerated in fig1 for visual clarity . in this embodiment , as each flight winds around the shaft , the flight uses the radius of the half that it is winding through , changing cross sectional radius as its rotation causes it to cross from one half into the other . the conveyor does not use one cross sectional radius exclusively on one of the two flights winding around the central shaft , and a different radius exclusively on the other flight . both flights use both the larger and smaller radii as they twist around the central shaft , winding back and forth between the larger and smaller radius “ sides ” of the conveyor . at all points along the length of the central shaft , one flight is using the larger flight radius ( 37 ) when the other flight is using the smaller flight radius ( 38 ). there is no point along the new conveyor &# 39 ; s length at which both of the two flights use the same flight radius . as a result , every part of any ice cuttings buildup being pushed by the new conveyor is subjected to contact with flights alternating between the larger and smaller flight radii . there is no point along the new design conveyor &# 39 ; s length where the ice cuttings buildup is subjected to contact with only one flight radius . every part of an ice cuttings buildup is alternately swept by flights of both the larger and smaller flight radii . in order to remain balanced while spinning , the conveyor half using the smaller flight diameter radius is also equipped with counter weights ( 40 ) attached to the non - thrusting side ( the side of each flight that does not push ice cuttings ) of each flight , close to the flight &# 39 ; s outer edge . in one embodiment the weights ( 40 ) are attached to the smaller diameter flights exactly in the middle of the smaller diameter half of the conveyor with respect to the smaller diameter half &# 39 ; s degrees of rotation around the central shaft . the weights compensate for the slightly lower weight of the conveyor flight flanges on the side of the conveyor using the smaller radius . the placement and size of any counterweights will depend on the dimensions of the particular auger , and may readily be determined by one of ordinary skill in the art . the design of this new horizontal ice cuttings conveyor forces any ice cuttings buildup that may front in front of the conveyor into the space swept by the conveyor flights by using the principle of “ positive displacement ”. positive displacement of the ice cuttings occurs when the spinning flights of the horizontal conveyor are physically forced into the space occupied by the ice cuttings . because two solid objects cannot occupy the same space , the ice cuttings must be displaced , or moved aside , by the intruding conveyor flight . thus the ice cuttings are “ positively displaced ”, meaning they must be displaced and moved by the conveyor flights . this new horizontal ice cuttings conveyor creates positive displacement of the ice cuttings buildup because edges of the conveyor pushing an ice cuttings buildup forward over the ice surface alternate between using the larger and smaller flight radii once each conveyor revolution . the process the alternating flight radii create is best illustrated by examining what would happen to a hypothetical , fully formed ice cuttings buildup , complete with a solidified and compacted face for the conveyor to push against , if it were placed in front of the new conveyor design . see fig1 - 16 . as the conveyor rotates , the continuous transition of the flight edges between using the larger and smaller flight radii creates a repeating sequence of four distinct events that results in the rapid break up and removal of the ice cuttings buildup . the four events repeat each time that the conveyor completes one revolution . in the first of these four repeating events , show in fig1 , the hypothetical ice cuttings buildup is in front of the conveyor &# 39 ; s larger radius lengthwise half . once in place , the buildup will initially be pushed over the ice surface just as it is pushed forward by the conventional conveyors currently in use that have a circular cross section . the buildup is initially pushed over the ice by the spinning edges of the larger radius conveyor flights rubbing against the ice cuttings buildup the second of the four repeating events , shown in fig1 , is for the conveyor to quickly remove all contact with and physical support for the entire ice cuttings buildup . as the new design conveyor rotates the conveyor flights pushing the ice cuttings buildup switch from the larger flight radius to the smaller flight radius . this transition produces an empty gap ( 41 ) very suddenly between the ice cuttings buildup &# 39 ; s face and the spinning conveyor flight edges . the size of the gap is equal to the radius differential between the larger and smaller flight radii . the sudden creation of this gap removes the continual contact and support that conventional conveyors with circular cross sections provide to the face of the ice cuttings buildup . this temporarily removes the continual “ spine - like ” structural support that conventional horizontal conveyors with circular cross sections provide to the ice cuttings buildup . the third of the four repeating events , shown in fig1 , is to move part of the buildup into the space that must be swept by the flights on the larger radius lengthwise half of the conveyor . this is accomplished by quickly closing the gap in between the body of the ice cuttings buildup and the flight edges of the conveyor on the smaller radius lengthwise conveyor side almost immediately after the gap forms , and while the smaller radius side is still the side in position to push against the ice cuttings buildup . because the ice re - surfacing conditioner is in continual forward motion , the conditioner naturally pushes forward to close the gap between the ice cuttings buildup and the edges of the conveyor &# 39 ; s spinning flights . the gap is small enough that the normal rate of forward motion of the conditioner easily closes the gap in the time available before the larger diameter lengthwise half of the conveyor can rotate back into contact with the ice cuttings buildup . as a result , the gap is closed by the conditioner &# 39 ; s forward motion and the ice cuttings buildup is back in contact with , and being pushed forward by the edges of the conveyor flights on the lengthwise side of the conveyor with the smaller flight radius . when being pushed forward by the lengthwise half of the conveyor using the smaller flight radius , the body of the ice cuttings buildup is closer to the conveyor &# 39 ; s central shaft than when it is being pushed by the lengthwise half of the conveyor using the larger flight radius . as a result , when it is being pushed by the smaller radius conveyor half , part of the ice cuttings buildup lies inside space that will be swept by the lengthwise half of the conveyor using the larger flight radius . the fourth of the repeating events , shown in fig1 , is for the larger radius lengthwise half of the conveyor to rotate back into contact with the ice cuttings buildup , taking a “ forced bite ” out of the buildup . just before the larger radius lengthwise half of the conveyor rotates back into contact with the ice cuttings buildup , the buildup is in contact with and being pushed forward by the smaller radius lengthwise half of the conveyor . in this situation , the part of the ice cuttings buildup that is closest to the conveyor lies inside part of the space that must be swept by the flights on the larger radius lengthwise half of the conveyor . this creates a “ positive displacement ” relationship between the ice cuttings buildup and the larger radius conveyor half . as the larger radius lengthwise half of the conveyor rotates back into contact with the ice cuttings buildup , the outer edge of the conveyor flights must pass through the same space occupied by the closest part of the ice cuttings buildup . see fig1 . as a result , the conveyor is forced to take a bite out of the ice cuttings buildup , shearing off and removing the cuttings that make up the closest part of the ice cuttings buildup &# 39 ; s face . the four events repeat with each complete revolution of the conveyor . consequently , a portion of the ice cutting buildup is removed with each revolution of the conveyor , repeating until the entire ice cuttings buildup is removed from in front of the conveyor . since the horizontal conveyor normally spins at a several hundred revolutions per minute , the new design horizontal conveyor can eliminate a very large ice cuttings buildup in only a few seconds . a large difference in flight radius between the two lengthwise halves of the conveyor , or “ radius differential ” is not needed . the radius differential between the two lengthwise halves only needs to be large enough to cause the conveyor to remove enough of a forming ice cuttings buildup with each revolution that the flow of ice cuttings into the front side of the conveyor is never obstructed . a flight radius differential between the two lengthwise halves of the conveyor of 1 / 16 th to ¼ th of an inch ( 1 . 5 mm to 6 . 5 mm ) should be more than enough to prevent an ice cuttings buildup from obstructing the front of the horizontal conveyor . there are several advantages to using the smallest radius differential possible that will still prevent the formation of an obstructing ice cuttings buildup . these include ease of conveyor manufacture while maintaining proper conveyor balance , achievement of the smoothest conveyor rotation and most even power consumption possible while actually removing any ice cuttings buildup , having the largest possible total conveyor flight surface area to achieve the most efficient removal of ice cuttings possible , and keeping the conveyor &# 39 ; s power consumption as smooth as possible during normal collection and removal of the ice cuttings resulting from ice shaving . various alternative embodiments of the present invention will also be effective . a single - flight auger conveyor , rather than the preferred double - flight auger , may be employed . configuration of the differential radius cross section may also be varied . fig1 shows one such variation . transition ( 42 ) between the smaller radius portion ( 38 ) and the larger radius portion ( 37 ) remains abrupt , but there is not another abrupt transition after 180 ° of rotation . instead , the radius if the flight continuously variable from the small radius ( 38 ) to the large radius ( 37 ). the flight may be configured so that the gradual change from the small radius to the large radius takes place over an entire rotation ( 360 °), a half rotation ( 180 °) or something in between . a transitional change from small radius and large radius may also be carried out in less than a half rotation . as shown in fig1 , for configurations that do have abrupt transitions ( 42 ) from small radius ( 38 ) to large radius ( 37 ) on opposite sides of the flight , those transitions may be more or less than 180 ° apart . this is illustrated by alternate transitions ( 43 , 44 ) in the figure . again , note that in fig1 and 18 the radius differential is exaggerated for illustration . another embodiment of the invention is shown in fig1 , with dimensions exaggerated for clarity . each flight in this embodiment includes a sequence of larger radius ( 37 ) portions and shorter radius ( 38 ) portions with transitions ( 42 ) between . in this embodiment the flights should be arranged so that at any point along the length of the conveyor ( 45 , 46 , 47 ), one flight is using the larger radius and the other flight is using the smaller radius . in this embodiment , the flights change radius every 2 to 6 inches ( 5 cm to 15 cm ). another embodiment is shown in fig2 . in this two - flight configuration , both flights have a circular cross section . one flight has a larger radius ( 37 ) and the other has a smaller radius ( 38 ). again , the radius differential is small , and the figure exaggerates the magnitude of the radius differential . this embodiment maintains the desired positive displacement effect because all points along the length of the conveyor shaft use flights of both radii . consequently , all points along the length of an ice cuttings build - up are alternatively contacted by flights of both radii . generating the desire positive displacement effect . the invention is suitable as a retrofit modification for existing ice resurfacing machines , as the new design conveyor can be dimensioned to match the fittings of the horizontal conveyor on any of the standard resurfacing machines . the foregoing description of a preferred embodiment of the invention has been presented and is intended for the purposes of illustration and description . it is not intended to be exhaustive nor limit the invention to the precise form disclosed and many modifications and variations are possible in the light of the above teachings . the embodiment was chosen and described in order to best explain the principles of the invention and its practical application and to enable others skilled in the art to best utilize the invention in various embodiments and with various modifications as are suited to the particular use contemplated . therefore , it is intended that the invention not be limited to the particular embodiments disclosed for carrying out the invention .
1
fig2 to 4 show a putter in accordance with a primary embodiment of the present invention . as shown in the drawings , the head 10 of the putter according to the present invention has a hollow cylindrical head body having a diameter of 35 mm - 45 mm , preferably 38 mm . in the above head body , a pair of vertical partitions 11a are placed in the front and rear portions inside the head body , thereby forming a central cavity 11 having a volume v 1 . the cavity 11 has either circular or polygonal cross - section . each partition 11a has at least one threaded hole . the above threaded hole of each partition 11a engages with coupling means of a cap 20 , 20a which will be described later herein . the caps 20 and 20a are coupled to the front and rear ends of the head body , respectively . each cap 20 , 20a cooperates with an associated partition 11a in order to form a side cavity having a volume v 2 . as shown in fig2 a handle 12 extends from a given portion of the above head 10 . in the present invention , it is preferable to make the ratio of volume ( v 1 , v 2 ) of the cavities inside the head 10 be v 1 : v 2 = 2 : 1 . however , it should be understood that the volume ratio between the cavities may be changed without affecting the functioning of this invention . in addition , the head 10 may be provided with one or more partitions for forming the cavities . in the above head 10 , both ends of the above cylindrical head body are coupled to the hollow hemispherical caps 20 and 20a . each cap 20 , 20a has the above coupling means engaging with the threaded hole of an associated partition 11a . the above coupling means comprises a rod 21 which axially extends from the center of the inside surface of each cap 20 , 20a . the above rod 21 is at least partially threaded in order to form a screw portion which will be threaded into the threaded hole of the partition 11a . in accordance with the present invention , a plurality of annular weights 26 and 26a may be fitted over the rod 21 of each cap 20 , 20a . each weight 26 , 26a has an inner diameter of larger than the outer diameter of the rod 21 and is used for adjusting the weight of the head 10 . in order to prevent the weights 26 and 26a from suddenly moving on the rods 21 and 21a of the caps 20a and 20a , it is preferable to fit a biasing means or a compression coil spring over each rod 21 , 21a between the inside surface of an associated cap 20 , 20a and the weights 26 and 26a . as shown in fig2 the peak of each hemispherical cap 20 , 20a may be provided with a depression . a transparent tap 24 is fitted in the depression of the above cap 20 , 20a with a label of a putter producer interposed between the tap 24 and depression . in this case , the putter will have an additional effect of showing the putter producer and good appearance . in the present invention , an annular groove having a given depth is preferably formed on the coupling edge of each of the cap 20 , 20a and the body 10 . an o - ring 14 , 14a formed of an appropriate material is fitted over the above annular grooves when the caps 20 and 20a are fitted into both ends of the head 10 . the above o - ring 14 , 14a prevents foreign substances such as moisture , grass and sand from being introduced into the cavity 11 of the head 10 . while putting , a golfer selects one of the putters having different weights in accordance with the putting conditions , such as the putting green conditions , that is , wet green or dry green , golfer &# 39 ; s weight and the weather . while selecting the putters , a golfer selects a putter in accordance with one &# 39 ; s subjective preference . as described above , the putter head 10 of the present invention may be provided with the weights 26 and 26a for adjusting the weight of the putter head 10 as shown in fig2 to 4 . in accordance with the primary embodiment of the invention , each weight has an annular configuration suitable to be fitted over the rod 21 , 21a . however , it should be understood that there exist various polygonal configurations of each weight 26 , 26a which yield the same result as that described for the primary embodiment without affecting the functioning of this invention . each annular weight 26 , 26a has an weight of 5 - 50 g , preferably 15 g . in the present invention , it is preferable to fit 0 - 20 weights 26 and 26a , preferably 10 weights , over each rod 21 , 21a . however , a golfer may freely select the number of the weights 26 and 26a , which will be fitted over the rod 21 , 21a , in accordance with one &# 39 ; s preference . the net weight of the head 10 without having any weight 26 , 26a is 250 - 300 g . in order to install the weights 26 , 26a in the head 10 , the biasing means 27 , 27a is fitted over the rod 21 , 21a of each cap 20 , 20a prior to fitting an appropriate number of weights 26 and 26a over the rod 21 , 21a . after fitting the weights 27 and 27a over the rods 21 and 21a of the caps 20 and 20a , the caps 20 and 20a are tightly fitted into both ends of the head 10 , respectively . of course , the weights 26 and 26a may be exclusively fitted over the rod 21 , 21a of either cap 20 or 20a . the above biasing means 27 and 27a interposed between the inside surfaces of the caps 20 and 20a and the weights 26 and 26a prevent the weights 26 and 26a from moving on the rods 21 and 21 inside the head 10 . in addition , a plurality of o - rings ( not shown ) formed of elastic rubber may be interposed between the weights 26 and 26a in order to prevent noises generated from the weights 26 and 26a while putting . in the present invention , it is preferable to fit the caps 20 and 20a into both ends of the head 10 through screw - type fitting . in order to achieve the above screw - type fitting of the caps 20 and 20a into the head 10 , the fitting edges of the caps 20 and 20a and of the head 10 are preferable provided with threaded portions . of course , the caps 20 and 20a may be fitted into both ends of the head 10 through another method , such as interference fit . in order to make it easy to fit the caps 20 and 20a into both ends of the head 10 , the fitting edge of each cap 20 , 20a is preferably provided with a knurled portion 22 , 22a . the putter head 10 of the present invention is a cylindrical body . with the cylindrical body of the head 10 , the putter head 10 knocks the center of a golf ball regardless of the putting postures of a golfer while putting as shown in fig5 . the putting force of the golfer is thus precisely transmitted to the ball through the putter regardless of the golfer &# 39 ; s putting postures , thereby improving the putting precision of the golfer . as described above , the present invention provides a structurally improved putter . the head of the above putter is a cylindrical body with a cavity . with the cylindrical configuration of the putter head , the putter head knocks the center of a golf ball regardless of the golfer &# 39 ; s putting postures while putting . a plurality of annular weights are provided in the cavity of the head . the number of the weights in the head can be freely changed by a golfer thereby freely adjusting the weight of the head . the above weights are prevented from moving in the cavity by a biasing means . although the preferred embodiments of the present invention have been disclosed for illustrative purposes , those skilled in the art will appreciate that various modifications , additions and substitutions are possible , without departing from the scope and spirit of the invention as disclosed in the accompanying claims .
0
first embodiment . an altsoi embodiment of the invention is now described . a standard soi wafer 10 is provided , which is shown in fig2 and which comprises a handle layer 12 , a dielectric layer 14 usually consisting of silicon dioxide , and a device layer 16 ( see , fig2 a ). such wafers are commercially available from many sources , and are fabricated using wafer bonding , simox technology , smart - cut methods , or other processes . wafers can also be obtained from a large number of vendors of standard semiconductor material , and are sawn and polished to provide precise dimensions , uniform crystallographic orientation , and highly polished , optically flat surfaces . parameters for the three layers of the soi wafer are determined by the user . typically , the handle wafer is of sufficient thickness for handling purposes , without other requirements . the dielectric layer is thick enough for electrical isolation and effective etch - stop action , yet thin enough so as not to cause severe bowing of the soi wafer . the device layer parameters are important , as they will translate directly into properties of the resulting structure . thickness of the device layer determines the device thickness ( including any gap that may be machined between the device and the substrate ). electrical resistivity , carbon and oxygen content , growth technique , crystallographic orientation and other wafer parameters are selected based on the properties requited of the end product . surface finish should be highly polished . the interface between the dielectric and device layers should not have voids . once the soi wafer parameters have been selected and the material obtained , processing of the wafer begins . fig2 shows the primary steps involved in preparing the soi wafer for bonding to a substrate wafer . first the soi wafer is cleaned and patterned for the “ mesa ” etch . here mesas are preserved in the device layer and the background is etched back , so that the final structure , when bonded to a substrate , has regions which are directly bonded ( the mesas ) and regions suspended above the planar surface of the substrate ( i . e ., everywhere else on the wafer ; see , fig2 b ). the mesa etch may be performed using koh or other etchants . in one preferred embodiment , once the mesa etch has been performed , the wafer is cleaned and patterned for the “ structural ” etch ( see , fig2 c ). typically , the structural etch is a deep reactive ion etch ( drie ) process , in which high aspect ratios may be desired ( ayon a a et al ., mat . res . soc . symp . proc . 546 : 51 ( 1999 ); ayon a a et al ., j . vac . sci . tech . b 18 : 1412 ( 2000 )). since the process etches straight down to the dielectric layer , which is bonded everywhere to the device layer , techniques designed to prevent plasma etching problems at the dielectric — device interface become very effective . the micromachining of silicon can be observed by the use of epifluorescence microscopy or by the use of metallurgic microscope . alternatively , the micromachining can be observed by an electron microscope , such as a scanning electron microscope ( sem ). the soi wafer that has been patterned and etched for both the mesa and structural layers is then bonded to a substrate . the substrate can be glass , silicon or other equivalently workable material . in one embodiment , the fabrication steps for a glass substrate 20 are those outlined in fig3 . first , the glass wafer 20 is cleaned and patterned for the electrode pattern . here , the electrode pattern is composed of multilevel metallization . the glass wafer 20 is then recess - etched , and , without removing the photoresist , a blanket sputter of the multilevel metallization is performed . finally , the wafer undergoes “ lift - off ”, where metal not applied directly to the substrate is removed . note that in fig3 d , an additional step has been added ; the formation of access ports 22 in the glass substrate 20 . the advantage for this process step is described below , where the substrate wafer is bonded to the processed soi wafer . these access ports 22 may be etched , or more preferably , mechanically or ultrasonically drilled through the glass substrate . the spacing of these holes is determined by the die size and by the presence and distribution of bonded seals between the soi wafer and the substrate . since the purpose of the access ports is to equalize the pressure between the internal cavities and outside of the wafer sandwich , at least one such port must be positioned within each region sealed by bonding . typically , these regions coincide with the die size , so that each device is isolated from all others by a bonded structure known as a seal ring . once the soi and glass wafers have been processed , they are bonded together . this is usually accomplished by anodic bonding . the remainder of the process sequence is illustrated in fig4 . note that the presence of the access port ensures that the inner cavities are at the same pressure as the external environment . without the access port , the quantity of gas inside the cavity is fixed when the bond is formed . applying the ideal gas law , the pressure inside the cavity p = nrt / v , where n is the number of moles of gas present ( fixed ), v is the volume of the cavity ( fixed ), r is the universal gas constant , and t is the temperature . if the bonding is performed at 300 ° c . and 1 atmosphere , for instance , the pressure inside the cavity at room temperature is ( 293 / 573 ) atm ˜ 0 . 5 atm . therefore , in room ambient , the cavity is in an underpressure situation , while in a vacuum chamber , it is at an overpressure situation . for any specific pressure condition during bonding , once the wafer sandwich has cooled , the pressure inside the cavity can be different from that of the outside world . analysis indicates that such a pressure differential will lead to fracture of the oxide interlayer . use of an access port resolves the problem of the pressure differential . once the wafers have been bonded together , with the device side of the soi wafer bonded to the metallized side of the glass , the handle layer of the soi wafer must be removed . without an access port , this material may be removed in a wet chemical etch or by a dry plasma etch . with the access port present , only the dry process is used . for example , a rie tool may be used to remove the handle silicon layer . one required feature of rie process tool is that it enables the plasma removal to occur with equalized pressure across the oxide dielectric . the other required feature is that plasma gases cannot gain access to the cavity through the port ; otherwise , attack of structural layers would ensue . the final step in the process is removal of the oxide dielectric . in this as well as previous embodiments , removal of the dielectric layer must be performed using a dry plasma etch process , so as not to attack the bulk glass and metallization on the topside of the device . once the dielectric has been removed , the final structure is produced . this structure is expected to have excellent build quality , as it benefits from several significant process improvements : ( 1 ) high material quality through use of virgin soi material rather than highly doped layers ; ( 2 ) very high fidelity drie processing , due to fully bonded device and oxide dielectric layer during the etch process , and newly - developed vendor equipment and processes designed specifically for these applications ; ( 3 ) high quality access port holes , drilled using ultrasonic methods which produce smooth walls without stress concentrations ; ( 4 ) complete flexibility in wafer bonding process , without concern for ambient conditions and resulting pressure differentials ; and ( 5 ) dry plasma etch wafer thinning process , which allows for pressure equalization across oxide dielectric , eliminating possible exposure of device layer to etchant . one group of former methods for fabricating micromachined structures in silicon involves the use of an etch - stop such as heavily - doped boron layers or sige layers . the method of the invention has several distinct advantages over that family of techniques , including increased process flexibility without the requirement for heavy doping , a higher - quality silicon device layer , and improved process control . alternative embodiments . alternate methods for the invention include , but are not limited to ( 1 ) the use of silicon or other crystalline substrates rather than a glass substrate , ( 2 ) anodic bonding using a thin layer of sputtered pyrex ® rather than a full glass wafer , ( 3 ) fusion bonding rather than anodic bonding of the lower handle wafer , etching or other processes rather than ultrasonic drilling , ( 4 ) alternate means for removing the soi handle layer , and ( 5 ) the use of materials other than silicon and silicon dioxide for the device layer and etch - stop layer , respectively . wafers made from pyrex ®, other borosilicate glass , or other glasses can also be procured and inserted into micromachining processes , with alternative processes used to etch the glassy materials . see , published pct patent application wo 00 / 66036 ; kaihara et al ., tissue eng 6 ( 2 ): 105 - 17 ( april 2000 ). plasma etching provides the ability to control the width of etched features as the depth of the channel is increased . wet chemical processes typically widen the trench substantially as the depth is increased , leading to a severe limitation on the packing density of features ( fruebauf j & amp ; hannemann b , sensors and actuators 79 : 55 ( 2000 )). several different plasma etching technologies have been recently developed . one of the available etch processes is know as the bosch process . in another preferred embodiment , the process of bonding the soi wafer and the substrate is performed at a predetermined pressure less than atmospheric pressure , for example , 200 mtorr . thus , some gas can be present in the cavities between the si and the substrate , but the gas pressure is not great enough to cause devices to explode during a subsequent potassium hydroxide ( koh ) etch to remove the handle layer . this step avoids the need for drilling holes in the substrate ports to equalize the pressure between the internal cavities and outside of the wafer sandwich . in a further preferred embodiment , the handle layer of the soi wafer is removed by a relatively fast wet etch , for example , using potassium hydroxide ( koh ). the fast etching of the handle layer is terminated at a predetermined distance , e . g ., about 10 μm , from the sio 2 layer . removal of the rest of the handle layer is preferably done by a relatively slow etch , for example , using tetramethyl ammonium hydroxide ( tmah ). thus , the etch of the rest of the handle layer is preferably performed slowly and stops well at the sio 2 layer . this etch can also be performed using xef 2 , which is a non - ionized gas that has a si : sio 2 etch ration as high as 10 , 000 : 1 . the next step in the process is removal of the sio 2 layer . in this as well as previous embodiments , removal of the sio 2 layer is preferably performed using an rie dry plasma etch process , so as not to attack the bulk glass and metallization on the topside of the device . the sio 2 can be removed in an rie tool using a recipe designed for sio 2 etching . this process can be performed at desired gas pressure , such as 200 mtorr , which is substantially the same as the pressure at which the bonding of the soi wafer and the substrate is performed . thus , a differential pressure is not applied to the sio 2 during the rie etch , allowing the sio 2 to be removed without damaging the device . the previously described method requires the mesa etching and structural etching to be performed before the soi wafer is bonded to a substrate wafer . once the bonding has been performed , the handle layer part of the soi wafer is removed using a wet etch . the wet etch which removes the handle layer must stop on the thin sio 2 layer . if the etch does not completely stop at the sio 2 layer , the etch chemicals would penetrate the device and destroy it . also , the structural etching , which is performed before the soi wafer is bonded to the substrate , defines cavities in the device layer . in these cavities , there is no si underneath the sio 2 to mechanically support the sio 2 layer . during the etching process for removing the handle layer , the etch chemicals may penetrate the sio 2 layer , which has no si support , and destroy the device under the sio 2 layer . [ 0045 ] fig5 illustrates an alternative fabrication method , which is called bonded and etch back silicon - on - insulator ( besoi ). in the besoi method , the structural etching is performed after the soi wafer is bonded to the substrate , and after the handle layer and sio 2 layer are removed . when removing the handle layer , the sio 2 layer is supported by the underlying si across the complete surface of the soi wafer . thus the sio 2 layer functions as a good etch stop , and no etch chemicals penetrate the device region when the handle layer of the soi wafer is removed . the besoi method begins with a standard soi wafer 10 , similar to that used in the previously described soi processes . first , the soi wafer is cleaned and patterned for the mesa etch . the mesa etch may be preformed by several methods , for example , using koh . the glass substrate fabrication steps are similar to the previously described methods , which are outlined in fig3 . in one preferred embodiment , the glass substrate may be provided with access ports to equalize the pressure between the internal cavities and outside of the wafer sandwich . once the soi and glass wafers have been processed , they are anodically bonded , with the device side of the soi wafer bonded to the metallized side of the glass substrate . the bonding process also can be performed under a predetermined pressure , which is less than atmosphere pressure , as described above . the handle layer of the soi wafer is preferably removed by a relatively fast wet etch , for example , using potassium hydroxide ( koh ). the etching of the handle layer is stoped at a predetermined distance , e . g ., about 10 μm , from the sio 2 layer . removal of the rest of the handle layer is preferably done by a relatively slow etch , for example , using tetramethyl ammonium hydroxide ( tmah ). the etch of the rest si is preferably performed slowly and stops well on the sio 2 layer . this etch can also be performed using xef 2 , which is a non - ionized gas that has a si : sio 2 etch ratio as high as 10 , 000 : 1 . the next step in the process is removal of the sio 2 layer . in this as well as previously described embodiments , removal of the sio 2 layer is preferably performed using an rie dry plasma etch process . the sio 2 can be removed in an rie tool using a conventional recipe designed for sio 2 etching . after the sio 2 layer is removed , the device layer is revealed and ready for structural etching . in a preferred form of the invention , the device layer is then etched to define the device preferably by inductively coupled plasma ( icp ), using a surface technology systems plc ( sts ) machine , which prevents charge build - up causing “ footing ”. the structural etching process may etch straight down to the glass substrate . when the icp etch is performed using a prior art process step , positive ions of sf 6 are generated in a region above the soi wafer . these ions are accelerated by a negative potential applied to a bias plate upon which the soi wafer is placed . the sf 6 ions subsequently etch the device layer of the soi wafer . as the device layer is etched away , the underlying glass wafer is exposed . electronic charge from the sf 6 ions may accumulate on the exposed glass . once the exposed glass is positively charged , the positively charged incoming sf 6 ions are repelled . their trajectory is bent such that they may etch and damage the underside of nearby si . a diagram of this prior art process step is shown in fig6 a . in accordance with the present invention , the above described prior art process step is replaced with a new process step , which avoids damage of the underside of the nearby si of the device . with the improved step , the glass substrate is covered with a substantially uniform metal layer , which , during the etch , prevents charge build - up , as shown in fig6 b . typically , gaps in metal layer are necessary to keep metal regions or lines separate . these gaps are preferably placed other than under an operable element which is to be formed by etching the device layer , or placed in areas where damage to the device will not affect the performance of the device . for example , as shown in fig6 b , the area directly underneath the drive or sense fingers of a mems device is covered by metal , and the gap between the si and the metal is placed other than under the finger . the icp etch is performed after the soi wafer is bonded to the glass substrate . the silicon , which is to be removed , is preferably not bonded to the glass , because it is very difficult for the icp etch to remove si , which has been bonded to the glass . to prevent the silicon , which will be removed by icp etch , from bonding to the substrate glass , a few microns of the surface of the silicon are preferably removed before the soi wafer is bonded to the glass wafer . the removal of the silicon can be done in the mesa etch , as shown in fig2 . [ 0055 ] fig7 illustrates another alternative besoi method of the invention , which uses highly doped silicon or other crystalline substrates rather than a glass substrate . as shown in fig7 a second soi wafer is provided to be used as the substrate . the device layer of the second soi wafer is etched straight down to the dielectric layer to form highly doped ( and thus electrically conductive ) “ si runners ”, which can be used as electrically conductive lines and contacts . after the “ si runners ” are formed , the first etched soi wafer is bonded to the second substrate soi wafer . the substrate soi wafer can be used in all previously described methods to replace the glass substrate . uses of the invention . commercial applications for this technology include , but are not limited to , inertial sensors for the automotive and other transport businesses , chemical and biological sensors for the biomedical and environmental monitoring businesses , industrial control sensors , actuators and components for the optoelectronics industry , and components for use in microfluidic applications aimed at biomedical and other technologies . the invention is also useful in the manufacture of an accelerometer . an accelerometer pattern is etched into the soi wafer . guidance for making an accelerometer is provided in u . s . pat . no . 6 , 269 , 696 , “ temperature compensated oscillating accelerometer with force multiplier ”, issued aug . 7 , 2001 to weinverg et al ., incorporated herein by reference . the details of one or more embodiments of the invention are set forth in the accompanying description above . although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention , the preferred methods and materials are now described . other features , objects , and advantages of the invention will be apparent from the description and from the claims . in the specification and the appended claims , the singular forms include plural referents unless the context clearly dictates otherwise . unless defined otherwise , all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs . all patents and publications cited in this specification are incorporated by reference . the following examples are presented in order to more fully illustrate the preferred embodiments of the invention . these examples should in no way be construed as limiting the scope of the invention , as defined by the appended claims . summary . several significant barriers to successful fabrication of the silicon oscillator accelerometer using silicon - on - insulator ( soi ) material have been encountered , necessitating the use of epitaxial material to build acceptable devices . use of soi rather than epitaxial material is strongly preferred for numerous reasons , including process flexibility , radiation hardness , performance , and ip issues . here we show a method for an accelerometer device from soi material . this process , coined the “ alt besoi ” process , appears to overcome current barriers to soi processing . principal advantages of soi vs . epitaxial process . the driving force for using soi material instead of epitaxial material to build the accelerometer is the greatly enhanced process flexibility afforded by the soi process . for high performance , the best crystallographic quality is expected to produce the best devices . device layers on soi wafers can be of any doping level , type , crystallographic quality , etc . by contrast , epitaxial layers must be heavily - doped with boron . high doping concentrations of b are associated with etch pits , extended defects , curvature and strain , all undesirable features for strategic devices . in addition to raw performance considerations , boost requirements require that the accelerometer be radiation hardened against fast neutrons , thermal neutrons and gamma radiation . boron doping reduces hardness against thermal neutrons ; therefore soi material is preferred . more importantly , the glass substrate , whether pyrex ® or hoya sd - 2 , exhibits compaction under fast neutron and gamma irradiation [ c . allred , master &# 39 ; s thesis , mit materials science and engineering department , august 2000 . fabrication of an accelerometer built from sigeb epitaxial material would be difficult to impossible with a silicon - on - silicon process , but would be very compatible with the use of soi material for the device layer . process difficulties with baseline besoi process . fabrication yields for the accelerometer were extremely , low , partly due to the very large (& gt ; 1 cm ) die size , but also due to process problems with the baseline besoi sequence . difficulties with this process are mainly associated with the final step in the process , in which the structural element is etched into the soi device layer using the ( inductively coupled plasma ) icp etching process . etching of the structural element in epitaxial processes occurs prior to bonding to the glass substrate . therefore , the icp etch must penetrate below the line of the sigeb etch stop layer , so that subsequent backside wafer dissolution results in full release . when the icp process stops in a silicon wafer , a phenomenon known as rie lag , shown in fig8 causes wide features to etch deeper than narrow features . however , this over - etch causes no serious harm , since wide features simply penetrates more deeply into the silicon wafer . by contrast , when the icp etch stops on a substrate such as the glass , wide features cannot etch any deeper , and therefore the plasma attacks the underside of released features and forms notches near the silicon — glass interface . this phenomenon in illustrated in fig9 where first sem image shows what comb fingers should look like ( epitaxial process ), while the second sem image shows comb fingers built using the standard besoi process . severe attack of the bottom of the comb fingers ( comb is turned upside down for better visibility ) is evident . new icp etch technology is specifically aimed at reducing notching and underside attack . however , the new technology is most effective when silicon is directly bonded to the non - etching substrate , such as glass or oxide . alternatives attempted to date principally address the notching problem , and entail icp etching down to the buried oxide layer prior to anodic bonding . process difficulties with initial attempts at an alternative soi process . high fidelity etching of the structural layer using an soi wafer requires that the icp process be conducted when the device layer is fully bonded to the oxide dielectric . the most obvious alternative soi process therefore entails icp etching prior to wafer bonding , followed by wafer thinning and oxide removal after the wafer bond . attempts to produce accelerometer devices using the sequence as modified above have not been successful . basically , the oxide etch - stop mechanically fails during wafer thinning , resulting in attack of silicon underneath the etch - stop , and all devices are obliterated . a re - design was performed , in which towers of silicon underneath the etch stop , but not connected to the device , could be inserted to insure mechanical survival during thinning . however , the most serious mechanical problem was the pressure differential between the internal cavities and the ambient . since anodic bonding of the glass substrate is performed at 345 ° c ., the pressure in the cavity at room temperature is , from the ideal gas law , where n is the number of moles , r the universal gas constant , and v the volume , all fixed . since anodic bonding is performed at atmospheric pressure , the internal cavity pressure at room temperature is p =( 293 k /( 273 + 345 ) k ) ˜ 0 . 45 atm . therefore , at room ambient , the cavity will tend to implode , while in a vacuum chamber , the cavity will tend to burst . basic description of new alt besoi process . herein is presented a new , alternative besoi process , coined “ alt besoi .” as the initial prototype alternative processes did , this new process differs from baseline besoi in that icp etching occurs prior to anodic bonding . four salient differences from initial prototype alternative besoi processes are ( 1 ) icp etch is conducted using newly available soi etch technology , ( 2 ) a pressure relief hole is inserted in the glass to eliminate pressure differentials during wafer thinning , ( 3 ) wafer thinning is accomplished using a dry plasma process rather than a wet etch , and ( 4 ) the die layout is adjusted to minimize the spacing between anchored features ( without affecting the actual accelerometer design .) initially , a standard soi wafer is provided , which is similar to that used in both the baseline and prototype alternative soi processes . first , the soi wafer is cleaned and patterned for the mesa etch . the mesa etch may be performed using koh or other etchants . this represents yet - another advantage of the soi process over its predecessors . once the mesa etch has been performed , the wafer is cleaned and patterned for the structural etch . since the process etches straight down to the dielectric layer , which is bonded everywhere to the device layer , technology designed to prevent plasma etching problems at the dielectric — device interface becomes very effective . in one embodiment , the soi wafer , which has been patterned and etched through both the mesa and structural layers , is then bonded to a glass substrate . the glass substrate fabrication steps are outlined in fig3 . first , the glass wafer is cleaned and patterned for the electrode pattern . in this embodiment , the electrode pattern is composed of multilevel metallization . the glass wafer is then recess - etched , and , without removing the photoresist , a blanket sputter of the multilevel metallization is performed . finally , the wafer undergoes “ lift - off ”, where metal not applied directly to the substrate is removed . the advantage of access ports is evident , as the substrate wafer is bonded to the processed soi wafer . these access ports may be etched , or more preferably , mechanically or ultrasonically drilled through the glass . the spacing of these holes is determined by the die size and by the presence and distribution of bonded seals between the soi wafer and the substrate . since the purpose of the access ports is to equalize the pressure between the internal cavities and outside of the wafer sandwich , at least one such port must be positioned within each region sealed by bonding . typically , these regions coincide with the die size , so that each device is isolated from all others by a bonded structure known as a seal ring . once the soi and glass wafers have been processed , they are anodically bonded . the remainder of the process sequence is illustrated in fig4 . note that the presence of the access port ensures that the inner cavities are at the same pressure as the external environment . without this access port , the quantity of gas inside the cavity is fixed when the bond is formed . once the wafers have been bonded together , with the device side of the soi wafer bonded to the metallized side of the glass , the handle layer of the soi wafer must be removed . without an access port , this material may be removed in a wet chemical etch or by a dry plasma etch . with the access port present , only the dry process may be used . for the present example , a rie reactor may be used to remove the handle silicon layer . one required feature of rie process tool is that it enables the plasma removal to occur with equalized pressure across the oxide dielectric . the other required feature is that plasma gases cannot gain access to the cavity through the port ; otherwise , attack of structural layers would ensue . the final step in the process is removal of the oxide dielectric . in this as well as previous embodiments , removal of the dielectric layer must be performed using a dry plasma etch process , so as not to attack the bulk glass and metallization on the topside of the device . once the dielectric has been removed , the final structure is revealed . excellent build quality is expected , based upon the use of the new icp soi etching technology and pressure equalization during thinning . the foregoing description has been presented only for the purposes of illustration and is not intended to limit the invention to the precise form disclosed , but by the claims appended hereto .
1
particular embodiments of the present disclosure are described hereinbelow with reference to the accompanying drawings ; however , it is to be understood that the disclosed embodiments are merely exemplary of the disclosure and may be embodied in various forms . well - known functions or constructions are not described in detail to avoid obscuring the present disclosure in unnecessary detail . therefore , specific structural and functional details disclosed herein are not to be interpreted as limiting , but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present disclosure in virtually any appropriately detailed structure . like reference numerals may refer to similar or identical elements throughout the description of the figures . as shown in the drawings and described throughout the following description , as is traditional when referring to relative positioning on a surgical instrument , the term “ proximal ” refers to the end of the apparatus which is closer to the user and the term “ distal ” refers to the end of the apparatus which is further away from the user . electromagnetic energy is generally classified by increasing energy or decreasing wavelength into radio waves , microwaves , infrared , visible light , ultraviolet , x - rays and gamma - rays . as used herein , the term “ microwave ” generally refers to electromagnetic waves in the frequency range of 300 megahertz ( mhz ) ( 3 × 10 8 cycles / second ) to 300 gigahertz ( ghz ) ( 3 × 10 11 cycles / second ). as used herein , the term “ rf ” generally refers to electromagnetic waves having a lower frequency than microwaves . fig2 - 3 show an electrosurgical pencil constructed in accordance with an embodiment of the present disclosure is shown generally as 100 . electrosurgical pencil 100 includes an elongated housing 102 configured and adapted to support a blade receptacle 104 at a distal end 103 thereof which , in turn , receives a replaceable electrocautery end effector 106 in the form of a loop and / or blade therein . electrocautery blade 106 is understood to include a planar blade , a loop , a needle and the like . a distal end portion 108 of blade 106 extends distally from receptacle 104 while a proximal end portion of blade 106 is retained within distal end 103 of housing 102 . electrocautery blade 106 may be fabricated from a conductive type material , such as , for example , stainless steel , or is coated with an electrically conductive material . the electrosurgical pencil also includes a power board “ p ”, a wireless communication board “ w ”, and a controller board “ c ”. as shown , electrosurgical pencil 100 is coupled to a return pad “ r ” via a cable 112 . cable 112 includes a transmission wire which electrically interconnects return pad “ r ” with return port 111 of electrosurgical pencil 100 . alternatively , the return pad “ r ” can be connected to the generator “ g ”. for the purposes herein , the terms “ switch ” or “ switches ” includes electrical actuators , mechanical actuators , electro - mechanical actuators ( rotatable actuators , pivotable actuators , toggle - like actuators , buttons , etc .) or optical actuators . electrosurgical pencil 100 includes at least one activation switch , e . g ., three activation switches 124 a - 124 c , each of which are supported on an outer surface 107 of housing 102 . each activation switch 124 a - 124 c is operatively connected to a respective switch 126 a - 126 c which , in turn , controls the transmission of rf electrical energy supplied from a power board “ p ” and an electrosurgical generator “ g ” to electrosurgical blade 106 . more particularly , switches 126 a - 126 c are electrically coupled to control loop 116 and are configured to close and / or complete control loop 116 , which causes the controller board “ c ” to send an instruction to the wireless communication board “ w ”. the wireless communication board “ w ” sends a wireless signal using antenna 140 to the electrosurgical generator “ g ” to generate an rf energy field 200 . the rf energy field 200 causes a current to flow though an inductor 150 connected to power board “ p ”. as the current flows through inductor 150 , energy is transmitted to electrocautery blade 106 to perform surgical operation . in an alternative embodiment , the rf energy field 200 can be continuously in an “ on ” mode by selecting a switch on the electrosurgical device 100 or on the electrosurgical generator “ g ”. additionally , switches 124 a - 124 c can be used to supply energy in an operational mode selected by the user without sending information to the electrosurgical generator “ g ”, where the power board “ p ” conditions the rf signal from inductor 150 into the selected operational mode . the operational mode can be cut , ablate , coagulate , or seal depending on the surgical instrument being employed . electrosurgical pencil 100 further includes one or more intensity controllers 128 a and / or 128 b , each of which are slidingly supported in guide channels 130 a , 130 b , respectively , which are formed in outer surface 107 of housing 102 . each intensity controller 128 a and 128 b is a slide - like potentiometer . each intensity controller 128 a and 128 b and respective guide channel 130 a and 130 b may be provided with a series of cooperating discreet or detented positions defining a series of positions to allow easy selection of output intensity from a minimum amount to a maximum amount . the series of cooperating discreet or detented positions also provide the surgeon with a degree of tactile feedback . one of the series of positions for intensity controllers 128 a , 128 b may be an “ off ” position ( i . e ., no level of electrical or rf energy is being transmitted ). intensity controllers 128 a and 128 b are configured and adapted to adjust one of the power parameters ( e . g ., rf energy field , voltage , power and / or current intensity ) and / or the power verses impedance curve shape to affect the perceived output intensity . as shown in fig3 , electrosurgical pencil 100 may include a controller board “ c ”, a wireless communication board “ w ”, and a power board “ p ” within housing 102 . controller board “ c ” receives inputs from the various switches , intensity controller , nubs , potentiometers or the like that may be disposed in housing 102 and outputs a signal to wireless communication board “ w ” that , in turn , sends a wireless signal though antenna 140 to the generator “ g ” to generate rf energy field 200 from a generator side inductor 160 connected to a power source 430 . an inductor 150 is connected to a power board “ p ”, and the rf energy field 200 induces a current to flow through inductor 150 . the power board “ p ” then sends an energy signal to electrosurgical blade 106 . the type of energy signal sent to the electrosurgical blade 106 may be controlled through the controller board “ c ” using switches 124 a - 124 c and / or 128 a - 128 b . alternatively , the electrosurgical pencil 100 may include a rechargeable battery ( not shown ). the battery may be recharged when rf field 200 induces a current to flow through inductor 150 . the battery then supplies the energy signal through the power board “ p ” to the electrosurgical blade 106 . in another embodiment , the electrosurgical pencil 100 may include a capacitor ( not shown ). the capacitor may be charged when rf field 200 induces a current to flow through inductor 150 . the capacitor then supplies the energy signal through the power board “ p ” to the electrosurgical blade 106 . for example , the capacitor may take 20 seconds to charge and provide a 20 second burst of electrical energy to the power board “ p ” to supply to the electrosurgical blade 106 . [ please give a size range of capacitor that may be possible to use ] fig4 discloses a schematic of a wireless rf system 400 to power an electrosurgical device 100 or 510 ( see fig2 and 5 a , respectively ). an electrosurgical device 405 , such as electrosurgical device 100 or 510 , includes a control interface 450 , inductive power circuitry 440 , an inductor 150 , wireless communication circuitry 460 , and / or a device electrode or seal plate 470 . a generator “ g ” includes at least an inductor 160 connected to a power source 430 . the inductor 160 may be a single inductor with an inductance between about xx and xx [ please give a range for the inductance ]. alternatively , inductor 160 may be two or more inductors connected in series or parallel . the inductor 160 generates an rf energy field 200 . [ what is the formula for calculating size of rf energy field and what is the size range of the rf energy field ] the rf energy field 200 causes a current to flow through inductor 150 . the inductor 150 is connected to inductive power circuitry 440 , where the inductive power circuitry filters and / or conditions the rf signal . the rf signal may be conditioned based on the selected mode . the rf signal is then sent to the electrode 106 ( see fig2 ) or seal plate 528 ( see fig5 a ) of the device . the control interface 450 is an interface between an operator and the device 405 . the control interface 450 includes one or more switches , such as switches 124 a - 124 c , that allow the operator to select the mode for operating the device 405 . the control interface 450 is connected to the wireless communication circuitry 460 . the wireless communication circuitry 460 relays the mode selected from the control interface 450 over the wireless communication field 410 to data port 420 in the generator “ g ”. the generator “ g ” then operates in the mode selected by the operator . the mode may be continuously on , selectably on , cut , seal , ablate , or coagulate . for example , the generator “ g ” may provide a rf field 200 with a pulsed waveform , when the surgeon is sealing tissue with the device 10 . alternatively , the generator “ g ” generates the rf field 200 , and the power circuitry 440 conditions an rf signal from the inductor 150 into a pulsed waveform for sealing tissue . the wireless communication board 460 replaces the signal wires needed in the prior art to communicate with the generator “ g ”. the wireless communication circuitry 460 may include a battery ( not shown ) to allow the wireless communication circuitry to send a signal to the generator “ g ” before the generator “ g ” generates the rf field 200 that induces power in the inductive power circuitry 440 . with reference to fig5 a and 5b , an illustrative embodiment of a wireless electrosurgical apparatus , e . g ., a bipolar forceps 510 ( forceps 510 ) is shown . forceps 510 is wirelessly connected to electrosurgical generator “ g ” through rf field 200 for performing an electrosurgical procedure . the electrosurgical procedure may include sealing , cutting , cauterizing coagulating , desiccating , and fulgurating tissue all of which may employ rf energy . the electrosurgical generator “ g ” may be configured for monopolar and / or bipolar modes of operation and may include or be in operative communication with a system ( not shown ) that may include one or more processors in operative communication with one or more control modules that are executable on the processor . the control module ( not explicitly shown ) may be configured to instruct one or more modules to transmit electrosurgical energy , which may be in the form of a wave or signal / pulse to the forceps 10 . forceps 510 is shown configured for use with various electrosurgical procedures and generally includes a housing 520 , a rotating assembly 580 and a trigger assembly 570 . for a more detailed description of the rotating assembly 80 , trigger assembly 570 , reference is made to commonly - owned u . s . patent application ser . no . 11 / 595 , 194 filed on nov . 9 , 2006 , now u . s . patent publication no . 2007 / 0173814 . with continued reference to fig5 a and 5b , forceps 510 includes a shaft 512 that has a distal end 514 configured to mechanically engage an end effector assembly 590 operably associated with the forceps 510 and a proximal end 516 that mechanically engages the housing 520 . in the drawings and in the descriptions that follow , the term “ proximal ,” as is traditional , will refer to the end of the forceps 510 which is closer to the user , while the term “ distal ” will refer to the end that is farther from the user . handle assembly 530 includes a fixed handle 550 and movable handle 540 . in one particular embodiment , fixed handle 550 is integrally associated with housing 520 and handle 540 is movable relative to fixed handle 550 for effecting movement of one or more components , e . g ., a drive wire 533 , operably associated with a drive assembly 534 ( fig5 b ) via one or more suitable mechanical interfaces , e . g ., a linkage interface , gear interface , or combination thereof . drive assembly 534 is in operative communication with handle assembly 530 ( see fig5 a and 5b ) for imparting movement of one or both of a pair of jaw members 525 , 535 of end effector assembly 590 . the drive assembly 534 may include a compression spring ( not shown ) or a drive wire 533 to facilitate closing the jaw members 525 and 535 . drive wire 533 is configured such that proximal movement thereof causes the movable jaw member , e . g ., jaw member 535 , and operative components associated therewith , e . g ., a seal plate 528 , to “ flex ” or “ bend ” inwardly substantially across a length thereof toward the non - movable jaw member , e . g ., jaw member 525 . with this purpose in mind , drive rod or wire 533 may be made from any suitable material and is proportioned to translate within the shaft 512 . in the illustrated embodiments , drive wire 533 extends through the shaft 512 past the distal end 514 , see fig5 a for example . fig6 is a flow diagram of process 600 for operating a device , such as 100 or 510 , within a wireless rf system . the process 600 starts at step 605 , with an operator pressing a switch , such as 124 a - 124 c or 570 , on the handheld device 100 or 510 to select a mode of operation at step 610 . an instruction specifying the mode of operation is sent to the generator “ g ” from the wireless communication board “ w ” to generate the rf energy field 200 according to the specified mode of operation at step 620 . the generator “ g ” generates the rf field at step 630 using inductor 160 . the rf field 200 induces , in step 640 , a current to flow across inductor 150 . the power board “ p ” conditions the rf signal produced from inductor 150 based on the requested operational mode at step 645 . the power board “ p ” then supplies the rf signal to the electrode , seal plate , or other end effector assembly at step 650 . when the operator completes the procedure , the operator depresses the switch , such as 124 a - 124 c or 570 , on the hand held device at step 660 . the process ends at step 680 , when the generator “ g ” receives and executes an instruction sent from the wireless communication board “ w ” instructing the generator “ g ” to stop generating the rf field 200 at step 670 . while several embodiments of the disclosure have been shown in the drawings , it is not intended that the disclosure be limited thereto , as it is intended that the disclosure be as broad in scope as the art will allow and that the specification be read likewise . therefore , the above description should not be construed as limiting , but merely as exemplifications of particular embodiments . those skilled in the art will envision other modifications within the scope and spirit of the claims appended hereto .
0
fig1 a shows in perspective a single - layer corrugated piezoelectric device of the invention ; it shows how a straight bender can be made from merely a single layer of piezoelectric material and the appropriate electrodes . the device is little more than an elongate sheet 11 of piezoelectric material that has been pressed ( or folded ) into a simple corrugated shape with the semi - circular corrugations 12 running the length of the sheet . the sheet has a notional median plane mp shown dashed , and has seven clearly distinct piezoelectric portions , three on one side ( the upper half , as shown ) and four on the other ( the lower half ). the upper three belong to one group that is generally planar , and the lower four belong to the other group . these groups are shown in dashed boxes u and l in fig2 a , b to be discussed below . the sheet has , at the appropriate manufacturing stage , been poled — that is , its piezoelectric crystals have been forced by a strong applied electric field to align themselves pointing along the thickness of the sheet — and formed on the top ( as viewed ) surface of the sheet 11 is a whole series of separate electrodes 13 ( shown in fig1 b only ), while formed on the bottom ( as viewed ) surface is a single continuous electrode 14 . together these make effective pairs of electrodes , and in each such pair &# 39 ; s case a small electric field applied using that pair will cause the piezoelectric material in the corrugation to expand or contract , depending on the direction of the field relative to the poling direction . as shown in fig1 a , the top electrodes 13 are separate but the bottom electrode 14 is a single , continuous electrode . how this works can be understood simply by imagining the continuous one is neutral , say ( it is shown earthed ), and then considering the electrical fields across each alternate corrugation . the applied voltage alternates between adjacent electrode pairs from positive to negative voltage as indicated by the circled plus and minus signs . one such field will be from neutral to plus — upwards , as shown — while the adjacent ones will be from minus to neutral — downwards , as shown . so , even with one of the electrode sets being continuous there can still be set up alternate opposed activation fields ( up , down , up , down , . . . and so on ). if , as shown , the applied activation field alternates between adjacent electrode pairs , so each is in the opposite sense of that of its immediate neighbours either side , then all the corrugations on one side of the sheet 11 ( and thus on one side of the median plane mp ) will suffer the same effect — expansion or contraction , depending on the field direction — while all the corrugations on the other side of the sheet 11 ( and on the other side of the median plane mp ) will suffer the opposite effect . so if , say , all the upper ( as viewed ) corrugations contract , then all the lower corrugations expand , and because the upper and lower corrugations are spaced across the median plane it necessarily follows that the sheet as a whole bends normal to that plane as dictated by these contractions and expansions — namely up , as shown by the dotted lines in fig1 a . were the fields to have been the other way round then the sheet would have bent downwards , instead . in this way a single sheet of piezoelectric material behaves just like a unimorph or bimorph , yet without the need for two layers , and without the concomitant need for , and the problem of , a central electrode . fig2 a , b show two possibilities for poling direction ( the feint short arrow 25 ) and actuating electric field direction ( the heavy long arrows 26 ). in fig2 a the entire sheet has been poled in the same direction 25 , while the electric fields direction 26 alternate , while in fig2 b it is the electric fields 26 which are in the same direction and the poling 25 that alternates . the effect , though , is the same . fig2 a , b also show how the piezoelectric portions are arranged in two essentially planar groups defined by the dashed boxes u and l which are so disposed as to face each other across the median plane and wherein the portions in one group expand while the portions in the other group contract . although the example shown in fig1 and 2 is for a corrugated cross - section , any cross - section that is not linear will work if regions above or below a neutral axis of the cross - section are deformed differently . fig3 a and b show a v - section device of the invention and a u - section device , and fig4 shows a rectangularly - sectioned corrugated device . all these work in much the same way . thus , in fig3 a the median plane runs horizontally ( as viewed ) through the v so that its two tip portions 21 form a generally planar group lying on one side of the median plane mp while its lower v section 22 is the group on the other side . the u - shaped device of fig3 b is much like a “ wide ” version of the v - shaped device of fig3 a , with its two arms 31 forming the generally planar group on one side of the median plane mp and its base 32 the group on the other . the fig4 is a rectangularly - sectioned corrugated device . the upper ( as viewed ) corrugations 41 are in a generally planar group on the opposite side of the median plane mp to the group of its lower corrugations 42 , and in the example shown there is a single bottom electrode ( not shown separately , but earthed / grounded ), while the top electrodes ( again not shown separately ) are alternately plus and minus as indicated by the symbols in the circles . fig5 a and b show ( in perspective ) two “ s ”- bending devices of the invention — that is to say , devices designed , shaped and operated to bend into an s - shape . the advantage of this type of deformation is that it enables devices to be stacked , one on top of the next ( rather like the crease of a piano accordion bellows ), to amplify the movement . for this purpose its is required that the piezoelectric material deform differently in each half of the device — expanding on top at one end while contracting on top at the other . to achieve this in one way , the electrodes are split half way down the device along line 53 , as is the case in the device of fig5 a where line 53 indicates the split electrodes . in a first corrugation 51 , 52 the field direction are indicated by the respective symbols . in an alternative way the direction of the corrugations is changed halfway along , as is shown in fig5 b . also , two s - bending devices can be combined with the free ( distal ) end sections abutting , resulting in a strip of twice the length , and , if the other ( proximate ) ends are fixed , a bulging middle section upon activation . fig6 a , b , c and d show ( in side , perspective and cut - away view ) two different doming corrugated devices of the invention . the device is basically a “ flat ” disc of piezoelectric material . it can be corrugated in either of two different ways — the two fig6 b , c and d show these two types of corrugation , one radial ( 6 b ), the other circumferential ( 6 c , d ). fig6 a shows , from the side , how each device moves upon actuation — moving from a generally flat , planar object ( the solid outline ) to take up a domed shape ( the dashed outline ). either corrugated form can be utilised to achieve this type of shape change . typical dimensions for a domed device of the type shown in fig6 b made from pzt4d would be an outer diameter of 15 mm , a thickness of 20 ìm , and a mass of 27 mg . the dome should then exhibit a corrugation amplitude of 20 ìm , and a corrugation pitch of approximately 0 . 5 mm . with an operating voltage of ± 20v there should be obtained a displacement of ± 0 . 1 mm with a blocking force of 7 mn . fig7 a - d show ( in plan , perspective , side and end view ) a linear strip corrugated device of the invention . the device is a linear strip 71 of piezoelectric material corrugated across rather than along the length of the strip . however , the corrugations 72 are angled ( at about 45 degrees to the long axis a - a of the strip ) rather than straight across ; since the bending action of the device is only along the length of the corrugations 72 , and not perpendicular to them , the angled corrugations 72 have the effect of twisting the strip about its axis a - a . the general sense of the twisting is shown in fig7 b , d ( the latter is what can be seen on actuation looking along the axis in the direction of the axis a - a ; what actually happens might be subtly different , depending on the exact nature of the corrugations ). the geometry represented by fig7 can then be curved into an arc to create a variant that deforms up and down across the plane of the arc . fig8 - 10 show ( in at least plan and perspective view ) three different arcuate strip corrugated devices of the invention . this type of structure , novel and inventive in its own right , demonstrates a device geometry that significantly amplifies the normal relatively small deformation of piezoelectric materials to produce a large displacement . the manner in which such structures works is complex , and not easy to appreciate . the following comments may assist . consider a ( planar ) circular arc 81 , fixed at one end 87 ( as shown in fig8 ). if the arc is deformed into a helix of the same radius , the free end has moved out of the plane of the circular arc . it is this deformation that the structure induces in a corrugated piezoelectric tape that nominally forms part of a circular arc . the same principles apply if considering a spiral curve fixed at one end . this out of plane deformation is achieved if torsion is induced in the arc . as noted , fig8 - 10 show three different curved strip corrugated devices . fig8 shows one in which the corrugations 82 are not straight across the strip but at an angle ( of about 45 degrees ) to the tangent to the curve . these corrugations are straight , and the strip 81 is otherwise flat ; in fig9 , however , the corrugations 92 are themselves arcuate ( albeit generally also at 45 degrees ), while in fig1 the corrugations 102 are straight ( and at 45 degrees ), but the strip has itself been curved / dished to take on a three - dimensional aspect , best seen at the fixed end 107 . arbitrary cross - sections 108 along the device show the superposition of the arcuate strip and any curvature introduced by the corrugations . the reason for curving the corrugations as in fig9 and 10 is to increase the blocking force of the device . it is easy to bend straight corrugations ( as in fig8 ) perpendicularly to the direction of the corrugations , and curving them resists this bending . the fig1 “ out - of - plane ” curve to the corrugations gives the best results , and in addition seems to increase the amount of movement . therefore the geometry shown in fig1 gives the best performing actuators . this geometry can produce a large actuation device pressed from a single layer of piezoelectric material . thus , using pzt4d as the piezoelectric material , and constructing an arcuate strip of outer diameter 15 mm , inner diameter 10 mm , and tape thickness 20 ìm , with corrugation amplitude 0 . 25 mm , corrugation pitch approximately 1 mm , and mass 15 mg , there should be obtained , with an operating voltage of ± 20v , a displacement of ± 0 . 25 mm with a blocking force of 0 . 3 mn . this would be an excellent result . the corrugations shown in the devices of fig8 - 10 are all regular , all at the same angle to the radial direction . an interesting property of the deformation of a circular arc into a helix by the application of a torsion is that the deformation does not increase linearly around the length of the arc . however by suitably varying the angle of the corrugations around the arc , it may be possible to remove this non - linearity . this may have the effect of increasing the efficiency of the device . the actual construction of devices of the invention can , as noted above , be effected in a number of ways . thus , the required corrugated shapes can be embossed into a compliant sheet of piezoelectric material prior to sintering , the required shape simultaneously being cut from the sheet using the same press tool . the devices can then be cured and sintered in appropriately shaped saggers to maintain the shape . after sintering , the electrodes can be applied either by printing or plating ( or a combination of the two ). the printing allows the electrodes to be applied on certain places to delineate the different regions of the device that must deform different . the entire device can then be poled in the same manner , so that each region would need to be activated separately . alternatively , the corrugations can be cut ( sawn ) into a flat sheet of piezoelectric material that has already been sintered ( and possibly poled ). the sawing process creates the required regions above and below the neutral axis of the cross - sections . the geometries produced then have squared corrugations similar to those shown in fig4 , but would of course still operate in the same fashion as those with rounded corrugations . it may be easier to manufacture certain geometries with this approach , since there will be fewer problems with sintering a thicker flat plate than a curved thin sheet . in low volumes , this approach will also reduce the manufacturing cost , since the costs of custom tooling will be reduced . one of the main manufacturing issues associated with corrugated structure devices of the invention is the need for a number of different electrical connections to be made to the device , since there are different regions that must deform differently . one solution to this problem is to connect to the different regions temporarily during poling , so that all the regions of the device can be connected together and be activated with the same voltage during use . this process may require two electrode printing processes ; the second one to join up all the regions after poling .
7
fig1 through 5 detail a simple parallel computing environment with accompanying mechanical assembly and computerized electronic control according to this invention . nevertheless , this description should be considered to apply to any type of lever or stick or control column and yoke . other generalized adaptations include electronic gimbal applications wherein precise positioning with strong position holding and redundant position encoding and control over torque and acceleration and velocity of shaft or other movement is required . fig1 details the schematic diagram of the parallel computing embodied by this invention to control all stick parameters and movement within 1 ms or less with a goal of less than 700 ns wherein each stick has essentially a black box 2 , 4 , and 7 or however many are in the system 6 . each black box has its own processing units and takes as input : sensor information 11 from the control surfaces 18 , the automated flight control system or auto - pilot 10 via bus 9 , other stick output 3 , 5 and 8 via a bus or other broadcast method 1 which includes : torque , acceleration , deceleration , velocity , friction or holding force , the stick shaker , and the stick pusher . all flight parameters : pitot static airspeed , computed gps based ground speed , barometric altitude , gps altitude , vertical speed , magnetic heading , gps ground track , temperature , altitude 12 are fed to each black box by discrete channels 19 , ball left , ball right . . . all of these signals are independently redundant with at least three other independent sensors and three independent and unique signal paths 17 and wherever possible independently written algorithms and sense methods are used in each redundant system . a voting method is used to flag and throw out any possibly failing sensor or sensor signal path . a stick shaker is used to warn the pilot through feel of a near stall condition . a stick pusher is used to warn the pilot through feel by pushing the stick forward when an imminent stall is sensed . a stick shaker 14 has independent sensor input 13 and the stick pusher 16 has independent input 15 as well . the stick shaker and stick pusher are independent systems which feed directly 20 and 21 into the stick black boxes 2 , 4 , and 7 or however many are in the system 6 . fig2 details the flow diagram of the procedure for each stick control processor . each black box acquires all of the parameters ( described by their respective command out vector ) 22 and performs a dot product 23 of the individual stick command direction and force to produce a command for its own stick 24 which it rapidly executes . a new command out vector for the individual stick is prepared 25 . this point in time is a synchronization point wherein all stick black boxes 26 wait at a barrier until all others have reached a point wherein all individual stick black boxes are ready to issue a stick command . this is the synchronization barrier 27 . this command contains the appropriate force on the friction / feel sheet while producing the appropriate torque and trajectory with corresponding activations of the electromagnetic windings on the stick and the windings or electromagnets surrounding the stick . once all of the sticks have reached this barrier all black boxes are said to be in synchronization and broadcast their respective command out vectors 28 . all of this happens in less than 1 ms . a provision is made wherein all sticks can revert to a constant friction force and an open loop dead joystick ( which is much like what is used in normal operation of current “ fly by wire ” transport category aircraft today ) configuration wherein all stick torque and positioning electromagnetics are turned off and simple position encoding is used . fig3 is a cutaway detail of the stick body 29 and enclosure assembly according to this invention wherein neodinium magnets 36 maintain a permanent friction on the stick to prevent it from flopping over when power is removed from the electromagnetics which control the stick movements . a set of electromagnets 38 maintain a holding force on the stick via the feel plate 40 which is variable by control . the feel plate is suspended by ball bearings 37 and 41 and is moved by the universal joint 37 attached to the bottom of the stick . electromagnetic movement is achieved by a plurality of windings which are activated by computer and are separated by an air gap 53 and reside at the surface of a bowl like structure 35 and 39 and the outer portion 51 of the bell like structure at the base of the stick 30 . this inverted bell like structure has three slots 31 wherein bearings 33 , 32 , and 34 remain in a fixed position but allow the shaft or stick 29 to tilt and move the feel plate 40 while remaining secure . position information can be decoded from the relative position of the bearings 32 , 33 , and 34 relative to the bell 30 . redundant position information can also be decoded from the position of the feel plate 40 x and y position . a backup positioning system can be in the form of x , y movement of the feel plane via rack and pinions . fig4 details an exploded partial perspective view of the stick body and enclosure 44 assembly according to this invention . the stick 29 is comprised of an inverted bell like shaped structure 30 on the end of a shaft . the inverted bell like structure 30 contains pluralities of electromagnets positioned around the surface 51 of the inverted bell wherein computer controlled electronics can selectively activate individual electromagnets located in the bell 51 as well as any of the pluralities of electromagnets in the bowl 39 . three slots 50 on the bell allow the stick to tilt in any direction by means of bearings 32 , 33 , and 34 mounted on the retaining plate 43 spokes 42 . a universal joint 37 mounted on the base of the bell moves a heavy steel feel plate 40 which is secured by bearings 37 and 41 mounted on the base plate 45 underneath . neodinium magnets 36 and electromagnets 38 act as bushings securing the plate from above and supplying holding forces to the stick . fig5 details a perspective view of a stick 29 mounted in a mobile phone or tablet 48 case 46 . the bowl assembly is mounted in the case 39 with an air gap 53 separating the electromagnets mounted in the stick base held in place by the retaining plate 43 . control electronics and batteries are housed in the case 49 wherein communication to the tablet or mobile phone is achieved by a touch screen i / o adapter 52 to and from the stick controller . the normal operating mode of the system is not “ control wheel steering ”. a trim system button is present on the stick 47 . with a press of this button 47 the stabilizer is quickly electronically trimmed most efficiently with aircraft equipped with canards or flying tails / stabilators . extra time may be required for aircraft with less efficient elevator designs . depending on the overall aircraft design the trim button 47 may be used to fully trim the aircraft in all axes .
1
the same elements have been referred to with the same references in the different drawings . for clarity , only those elements necessary to the understanding of the present invention have been shown in the drawings and will be described hereafter . in particular , it should be noted that a flat display screen is associated with an external control circuit intended for biasing the rows and columns of the cathode - grid as well as the anode conductors . this control circuit uses conventional electronic circuit techniques and will not be detailed , its structure and operation being within the abilities of those skilled in the art based on the functional indications given hereafter and on the operation desired for the screen . [ 0047 ] fig5 shows the equivalent electric diagram of a second preferred embodiment of the present invention . the representation of fig5 illustrates four screen pixels to better show the conductors common to these pixels . as previously , each pixel includes a current source 20 corresponding to the microtips having their respective tips 24 directed towards the anode ( not shown ). the base of the microtips forms a terminal 21 of the current source connected , via resistor 22 , to a reference voltage terminal 50 adapted to the present invention , which will be described hereafter . the luminance information remains provided by the cathode columns , but it is individualized at the level of the grid of the considered pixel , which includes localized so - called “ pixelized ” grid regions . according to the preferred embodiment of fig5 the terminal of capacitor 26 , which faces terminal 21 , is directly connected to a region 28 ′ of the so - called “ pixelized ” grid and , via a switch 40 ′, to a conductor 51 of the screen cathode . the switches 40 ′ aligned in a direction perpendicular to conductors 51 are simultaneously controlled by having their respective control terminals connected to a line 52 of the grid . however , according to the present invention , the cathode conductor 51 used to convey the luminance control signal is dissociated from conductors 50 organized in meshes and biasing the microtip base . conductors 51 are arranged in columns and are interposed between two columns 50 of reference meshed conductors . according to the present invention , all terminals 50 of resistors 22 are permanently biased to a reference voltage adapted to enabling electron emission when the pixel is addressed . thus , when a switch 40 ′, of a pixel is closed , the grid ( individualized region 28 ′) of this pixel is brought to a control voltage corresponding to a desired brightness imposed on column conductors 51 while the base of the microtips of this pixel is at a fixed voltage . at the end of the addressing line time of conductor 52 , switch 40 ′ is opened , so that one of the terminals of capacitor 26 is in the air . the charge maintained across this capacitor ( that is , the grid voltage maintained on the considered pixel ) maintains the electron emission by the microtip since the voltage of terminal 50 is fixed . it is thus possible to address the next conductor 52 and apply different control signals to conductors 51 for the next line . it should be noted that the emission current is provided by terminal 50 at the fixed voltage , so that the luminance control signal is not affected by the emission . preferably , at the end of a frame ( or of a color sub - frame ), all conductors 52 are simultaneously biased to a state where they turn on all switches 40 ′. during this time , all conductors 51 are addressed to ground , to discharge , during the frame flyback period , all capacitors 26 of the screen pixels and place said screen back to an initial state for the next frame . the implementation of the present invention requires associating , with each pixel ( or sub - pixel ), a switch and a storage element . on this regard , the present invention takes advantage of the fact that the cathode - grid plate is formed based on techniques derived from integrated circuit manufacturing to use thin layer manufacturing methods to form the switches . said switches are , preferably , manufactured in the form of field - effect transistors ( mos ). the storage element ( capacitor 26 ) associated with each pixel is formed by means of the insulating layer separating the cathode from the grid . it has already been provided , for example , in u . s . pat . no . 5 , 814 , 924 , to integrate transistors in the screen cathode - grid , to enable addressing of a screen , the tips of which are not arranged in columns . it should be noted that , although it requires additional components individualized per pixel , the present invention does not increase the surface bulk of a screen pixel . indeed , since the present invention considerably improves the emission capacity of each pixel by allowing emission during the entire frame time , the pixel emission surface area can be reduced for a given lighting . accordingly , the switch and the capacitor can be housed in the surface area thus spared . [ 0057 ] fig6 a and 6b show , respectively in a top view and in a cross - section view along line b - b ′, of fig6 a , an example of forming of a cathode - grid plate implementing the present invention . to make the comparison between the representation of fig6 a and 6b of the present invention and the conventional representation of fig3 a and 3b easier , fig6 a has been set out in the same orientation as fig3 a , that is , the conductors ( 51 ) formed in the cathode conductive level are vertical while the conductors ( 52 ) formed in the grid conductive level are horizontal . as illustrated in fig6 b , a conductive layer ( for example , niobium ) in which not only parallel conductive tracks 51 , but also a meshing 67 for forming conductors 50 for biasing the bases of microtips 2 are formed , is first deposited on a substrate 10 ( for example , glass ). to make the representation of the cross - section view of fig6 b easier , the number of microtips 2 per screen pixel has been arbitrarily reduced to eight , assuming the presence of a single microtip per mesh 31 ( fig6 a ). of course , the pattern of meshes 31 may follow the conventional pattern ( fig3 a ), except for the fact that the surface area occupied by an emissive pixel 60 of a screen according to the present invention can now be smaller than that of a pixel of a conventional screen . the thickness of the niobium layer in which conductors 50 and 51 are formed is , for example , on the order of 2 , 000 å . a semiconductor layer ( for example , amorphous silicon ) is then deposited . this layer aims at forming , on meshing 67 of conductors 50 , resistive pads 61 approximately having the size of a pixel , as well as ( channel ) depletion area 62 of the transistors 40 ′ associated with each pixel . in the preferred embodiment illustrated in fig6 a and 6b , one of the contacts ( corresponding to column 51 ) of the transistor is under the silicon layer constitutive of depletion area 62 . the other contact of the transistor is formed , on this depletion area , in a metal used to form pixel grid region 28 ′. as an alternative , pads 61 and areas 62 may be made of different materials . a layer of an insulator ( for example , silicon oxide sio 2 ) is then deposited and etched according to the pattern , for each pixel , of an area 63 separating the cathode from the grid of emission area 28 ′ of the pixel , and of an area 64 intended for forming the gate oxide of transistors 40 ′. a conductive layer ( grid layer 3 ) is then deposited according to the pattern where it covers insulator areas 63 and 64 . this conductive layer ( for example , niobium with a 4 , 000 - åthickness ), forms grid 65 above the emissive region of the pixel ( region 28 ′, fig5 ) as well as gate 66 of transistor 40 ′ of this pixel . the deposition of this conductive layer forms a step between the emission area and the transistor , to contact depletion area 62 of the transistor . this amounts to connecting one of electrodes 28 ′ of the capacitor 26 formed by insulating area 63 , its other electrode being formed by conductive meshing 67 . it should be noted that , outside of the surface of each pixel , the gates 66 of the different transistors 40 ′ are interconnected in the line direction in fig6 a by conductors 52 . similarly , in the column direction in fig6 a , conductors 51 extend over the entire screen surface and meshings 67 are inter - connected by connection sections 68 . this enables connecting all columns to one of the screen ends without having to provide an additional interconnection level . it should also be noted that , as they are preferentially formed of depletion transistors , switches 40 ′ of a screen according to the present invention are in a normally - on state . therefore , it is necessary to bias them to a more negative voltage than the minimum addressing voltage of conductors 51 , to block them outside the line times intended for them . taking the preceding example of operating voltages of the microtip screen , reference voltage vr of the microtip bases ( conductors 50 ) is − 40 v . the addressing voltage of conductors 51 then ranges between 0 v ( black ) and + 40 v ( white ) according to the deisred pixel brightness . with this choice of voltages , ( selection ) grid conductors 52 are addressed , in a line scanning , that is , during a “ line time ”, with a voltage v 1 of 0 v , the quiescent voltage of the unadressed lines 52 being , for example , − 40 v or less , for switch 40 ′ to be off . [ 0065 ] fig7 shows , in a partial perspective cross - section view , an alternative embodiment of a cathode - grid pixel according to the present invention . according to this alternative , a specific contact 70 is provided for the electrode of capacitor 26 intended to be connected to terminal 50 of interconnection of microtip base biasing resistors 22 . in this case , insulating area 63 is wider , since it is necessary to provide an additional conductive section in meshing 67 with respect to the embodiment of fig6 b . the choice between the embodiment of fig6 b and 7 will depend , in particular , on the capacitance desired for capacitors 26 forming the elements of storage of the luminance control signals . [ 0066 ] fig7 also illustrates an alternative in which the thickness of insulating layer 12 used to form gate oxide 64 and capacitor 26 differs in the two areas 63 and 64 to individualize the sizing of the gate oxide and of the capacitor . the respective sizing of capacitor 26 and of transistor 40 ′ of each screen pixel will depend , in particular , on the need for storage as concerns the capacitor , and on the control voltages as concerns the transistor . this sizing will be within the abilities of those skilled in the art according to the characteristics desired for the screen operation , to the surface area of the pixels , and to the involved voltage levels . further , the frame duration of the screen in operation will of course be taken into account . this duration determines , according to the present invention , the time constant desired for the rc cell of the pixel formed by its storage element ( capacitor 26 ) and its microtip base biasing resistor ( resistor 22 ). it should be noted that the present invention is perfectly compatible with current flat display screen manufacturing methods . in particular , the implementation of the present invention requires no increase in the screen pixel surface area and is campatible with currently - used pixel widths , in particular , in the case of color screens providing one cathode column per color , which is the most constraining case in terms of column width . it should also be noted that the implementation of the present invention requires , as compared to a current manufacturing method , no additional deposition step . if necessary , a mere additional mask will be provided to etch insulating layer 12 enabling formation of the transistor gates , and which is currently only etched to form the microtip holes ( 4 ). this is an advantage of providing a depletion transistor to control the pixel operation . indeed , when the voltage increases on the gate of this transistor , the electrons only pass under this line in the amorphous silicon forming its depletion area . of course , the present invention is likely to have various alterations , modifications , and improvements which will readily occur to those skilled in the art . in particular , in the case where an additional deposition step is not disturbing , the forming of individualized switches for each pixel in the form of normally - off transistors may be provided . further , the lighting gain brought by the implementation of the present invention may be taken advantage of in different ways . for example , advantage may be taken of it to have the screen operate under lower voltages by decreasing the number of microtips . the maximum emission voltage of the pixels may also be decreased . a decrease in the number of tips used to decrease the surface of each pixel may further be provided , to thus improve the screen resolution . to form the transistors , a significant gate width and a small gate length will preferably be provided to reduce the charge and discharge times of the respective pixel capacitors . such alterations , modifications , and improvements are intended to be part of this disclosure , and are intended to be within the spirit and the scope of the present invention . accordingly , the foregoing description is by way of example only and is not intended to be limiting . the present invention is limited only as defined in the following claims and the equivalents thereto .
7
fig1 shows a diagram of a measuring apparatus according to the invention . the apparatus can consist of a measuring unit 1 , a storage unit 2 and a display unit 3 . these communicate with each other using wireless or wired connections . some of the units , or all of them , can be integrated in the same casing or unit . the measuring unit is attached close to the human body , e . g . close to the middle . the measuring unit is typically positioned at some garment of the moving person , like e . g . a piece of clothing , a piece of headwear , the neck , a pocket , or close to the middle , i . e . close to the body &# 39 ; s center of gravity , e . g . at the belt . the display unit is typically located in a clearly visible position . it can be integrated , for example , in a measuring and storage unit , or it can be separate . it can also be part of a watch , a satellite navigator , a mobile terminal , a radio receiver , a player , or the like . any calibration data for the measuring device are stored in one unit or in several units . fig2 shows a view of a measuring unit according to the invention . the measuring unit 1 can comprise an acceleration sensor 4 of 1 to 3 axes , a unit 5 for analysis and diagnostics of the acceleration data , a volatile and a nonvolatile memory 6 , a communication unit 7 , and a power supply 8 , e . g . a battery , an accumulator , a harvester or some similar device . the analysis unit can , for example , be based on a microprocessor or a dsp ( digital signal processor ). the memory stores , for instance , user data , calibration data , measurement data and other log data . the communication unit comprises , for example , a transfer protocol generator , a required interface , or a radio transmitter , a receiver and an antenna . the measuring unit can be positioned fastened close to the human body , like , for example , close to the middle , i . e . close to the body &# 39 ; s center of gravity . the measuring unit is , typically , positioned at the clothing of the moving person , like , for instance , a piece of clothing , a piece of headwear , the neck , a pocket , or the belt . fig3 shows a view of an alternative measuring unit according to the invention . if , in addition to the speed and the distance covered , one wants to know the traveled route , a magnetometer 11 of 2 or 3 axes can be added to the alternative measuring unit for the compass direction to be determined for each step , or once in a while . in the solution according to the invention , the acceleration of the cyclic motion of progress is being measured in one or more directions . from the vertical acceleration values measured during each step cycle , a characteristic maximum acceleration a max occurring during the positive half cycle or the acceleration stage and , respectively , a characteristic minimum acceleration a min occurring during the negative half cycle or the braking stage are being determined . as values of the characteristic maximum acceleration a max and the characteristic minimum acceleration a min accelerations are defined , that clearly differ from zero , whereby the influence of the zero point error in the acceleration sensor or of the coupling of gravitation , caused by inclination , on the metering signal is minimal , since they are clearly lower than the values a max and a min . in the solution according to the invention , the characteristic maximum acceleration a max and the characteristic minimum acceleration a min can be defined , for example , directly as the maximum and / or the minimum of the vertical acceleration value from the raw data measured by the acceleration sensor . alternatively , in the solution according to the invention , the values a max and a min can be defined by filtering the acceleration sensor signal a in analogically by , for example , mechanical damping of the signal a in . further , alternatively , in a solution according to the invention , the values a max and a min can be defined by filtering the acceleration sensor signal a in digitally , by means of , for example , an rc filter . in this case , in the digital filtering , the function used in the first stage filtering could be , for instance : a out = a in /√{ square root over ([ 1 +( f / f 0 ) 2 ])}, where f = frequency and f 0 = the boundary frequency for − 3 db and the values a max and a min can be defined based on this filtered signal as , for example , the maximum and / or the minimum of the filtered acceleration value . further , alternatively , in the solution according to the invention , the values a max and a min can be defined by filtering the acceleration sensor signal a in by means of digital weighting . here , the function to be used in the digital weighting could be , for instance : a out ( n )=( 1 − k )* a out ( n − 1 )+ a in * k , where n indicates the n : th sample and k is the weighting factor . further , alternatively , in a solution according to the invention , the values a max and a min can be defined by using a mean value calculated from the measured acceleration value over times selected during the positive and / or the negative half cycle . the time used up for one step t step is obtained as the time interval between two equivalent points , such a maximum , a minimum , or a point of exceeding or falling below a certain value , on the acceleration graph given by the measured values of vertical acceleration . the time t c spent in ground contact during a step is obtained based on the length of time of zero acceleration in the acceleration graph derived from the measured vertical acceleration values . for running , it has been noted that the speed is proportional to the inverse of the contact time and to the force produced in the take off . since the average vertical acceleration of the body is zero , t c · a max +( t step − t c )· a min = 0 , the speed of locomotion v is obtained based on the characteristic maximum acceleration a max , in other words , where g is the acceleration caused by gravitation , f ref is a reference frequency and the characteristic maximum acceleration a max is the maximum value of the vertical acceleration strongly filtered at , for instance , the boundary frequency f 0 = 6 hz . in running , the characteristic maximum acceleration a max of the middle or some other part of the body is a good measure of the speed of progress . for walking , the speed is obtained based on the characteristic minimum acceleration a min of the vertical acceleration , in other words , the factors k depend , to some extent , on the boundary frequency in the filtering of the acceleration data . in walking , the characteristic minimum acceleration a min of the middle or some other part of the body is a good measure of the speed of progress . in the solution according to the invention , the step length s step can be calculated using the formula : and , correspondingly , the step rate or the cadence f step can be calculated using the formula : in the solution according to the invention , running and walking can be distinguished from each other based on step rate and speed of progress . at low running speeds , a non - linear model can be used , and running and walking can be adapted to each other . in the solution according to the invention , the step count n can be calculated on the basis of the number n of equivalent points , such a maximum , a minimum , or a point of exceeding or falling below a certain value , on the acceleration graph given by the measured values of vertical acceleration . further , in the solution according to the invention , the distance covered s can be calculated as the sum of the step lengths : in the solution according to the invention , a single acceleration sensor of one axis can be used , and thus , implementing the calculations of the formulae presented above is a simple task by means of , for example , a microcontroller . this enables a small , low cost , and low power sensor solution , by means of which a precision sufficient for consumer products is achieved . without individual calibration , the relative error , at distances exceeding one kilometer , is less than 10 %. in the solution according to the invention , an acceleration sensor of many axes can be used as well , and that enables , for example , diagnosing stationary running . in the solution according to the invention , a magnetometer of two axes can also be used , by means of which the length and direction of every step can be obtained . there will be inclination compensation as well , since the inclination of the body is more or less constant . calibration of direction and speed can be done by running a straight line back and forth . in the solution according to the invention , the speed estimate suffers a minimal impact from the zero point error in the acceleration sensor or from gravitation coupling into the metering signal caused by inclination , when using the characteristic maximum acceleration a max and the characteristic minimum acceleration a min , which values are large numbers in comparison with those . the ways of progress , e . g . walking , running , and skiing , can be distinguished from each other based on the characteristic maximum acceleration a max , the characteristic minimum acceleration a min , and / or the step rate . in the solution according to the invention , based on the acceleration values measured during the step cycles , characteristic maximum acceleration and characteristic minimum acceleration values a max and a min for each step cycle are defined , by means of which values the speed , the step rate , the step length , and the distance can be calculated with low power consumption using simple arithmetic , for example by using a polynome . the system , even if not calibrated , provides good precision . in order to improve precision , individual calibration can be made for different modes of progress , e . g . running , walking , pole walking , or cross - country skiing . this can be done over a known distance using one speed or a multitude of speeds . by repeating the calibration , errors in speed and distance caused by stochastic errors are reduced , whereby precision is further improved . new calibration data can be added to the old data by suitable digital filtering . in addition , for further improvement of the precision , information about the characteristic maximum and minimum acceleration values a max and a min can be combined with contact time data , with change in altitude and terrain inclination data obtained from an altimeter , and / or with satellite navigation . a complete step - by - step navigation unit is provided by adding to the step data the compass direction obtained from a magnetometer . the magnetometer can be calibrated , e . g . by rotating about a vertical axis . a direction error in the installation can be calibrated away by , e . g . walking a selected calibration route back and forth . absolute coordinate data is obtained by combining this navigation unit with satellite navigation . precision is further improved by combining the navigation unit with a map database and with an altimeter , since plausibility checks of the coordinates and movement can be made based on the altitude and changes in altitude . by using an acceleration sensor signal perpendicular to the principal metering direction , a measure of the efficiency of locomotion is obtained . in the solution according to the invention , characteristic maximum acceleration and characteristic minimum acceleration values a max and a min and / or maximum and / or minimum acceleration values obtained from an acceleration sensor of one or more axes can be used for estimating the speed of progress of a person . the signal of the acceleration sensor can be suitably filtered by means of mechanical , electronic , analog and / or digital filtering such , that the speed estimate is as exact and reliable as possible . in the solution according to the invention , step time , step rate , step length , and distance accumulated from the steps can be calculated based on the speed and the time interval between consecutive maxima or minima . in the solution according to the invention , walking , running , and skiing , or some other way of progress can be distinguished from each other based on , for example , the maximum and minimum acceleration of the middle of the body , the characteristic maximum and minimum acceleration values a max and a min and / or the step rate . in the solution according to the invention , the parameters for an average person running and walking can be utilized without individual calibration of the measuring system . the measuring system can be calibrated by means of individual calibration for one speed or for a multitude of speeds for a certain way of progress , e . g . running or walking . in the solution according to the invention , the calibration of the measuring system can be repeated such , that new data is combined with the old data by digital filtering . the precision of the measuring system can be improved by combining contact time data with the maximum and minimum acceleration data . in the solution according to the invention , the direction of each step or the direction of the distance covered observed from time to time can be determined by combining the speed estimate with the compass direction obtained from a magnetometer of 2 or 3 axes . a magnetometer and an installation direction error can be compensated for by rotating about a vertical axis and by walking a selected calibration route back and forth . in the solution according to the invention , the efficiency of the locomotion can be estimated by combining with the characteristic maximum acceleration values and the characteristic minimum acceleration values a max and a min and / or with the maximum and minimum acceleration value data , acceleration values measured at right angles to those . by means of the method and device according to the invention , a precision is achieved equal to that of the best methods presented above , by an implementation solution of significantly greater simplicity , utilizing one acceleration sensor without inclination compensation . by means of the method and device according to the invention , the complicated algorithms of prior systems are avoided , and low cost , low power consumption , and small size are achieved . the low power consumption of the method and device according to the invention allows a small battery and gives it long life , or even a battery - free solution based on , for example , recovery of the kinetic energy occurring in the measuring device ( harvesting ). the simple measuring algorithm of the method and device according to the invention allows the computations to be performed entirely in the measuring unit , which reduces the need for data transfer from the measuring unit , and thus , the power consumption of data transmission utilizing radio traffic . the small size of the measuring unit of the solution according to the invention allows the unit to be positioned , for example , at a piece of garment of the moving person , like , for example a piece of clothing , a piece of headwear , the neck , a pocket or close to the middle of the body , i . e . near the center of gravity of the body , at the belt , for instance . the method according to the invention is applicable , for example , to both slow and fast running , to walking at various speeds , pole walking , cross - country skiing , downhill sports , roller skiing , roller - skating and skating . the method and device according to the invention can be used for measuring a moving person &# 39 ; s speed , the step length , and the distance covered , based on maximum and minimum acceleration values of the body , given by an acceleration sensor of one axis for vertical acceleration and / or characteristic maximum and minimum acceleration values a max and a min . in the solution according to the invention , the acceleration signal can be optimally filtered such , that the acceleration signal gives as good a picture of the speed as possible . in the solution according to the invention , the ways of locomotion of the moving person , like walking and running , can be distinguished from each other based on the cadence and the speed of locomotion . in the solution according to the invention the parameters for an average person walking and running can be utilized without any individual calibration of the measuring system . the solution according to the invention enables calibration of the single point measuring system for walking and for running . the solution according to the invention enables diagnosing stationary running by means of a sensor of longitudinal acceleration . the solution according to the invention enables the direction of each step and the distance covered to be determined by means of a compass of two or three axes . the solution according to the invention enables calibration of the installation error of the compass by traveling the same route back and forth .
0
referring now to the drawings , wherein like reference numbers designate like or similar structures throughout the various figures , fig1 through 6 illustrate the first embodiment of the modular shelving storage system of the present invention . fig1 illustrates a preferred embodiment of a modular shelving storage system of the present invention in the form of a knock - down shelving structure 10 . suitable knock - down type shelving systems include the metromax ® shelving system and the super erecta tm shelving system manufactured by intermetro industries , and the like , which typically include a plurality of support posts , e . g ., four , arranged to support one or more shelves at corner assemblies thereof . one example of such a shelving system can be found in u . s . application ser . no . 08 / 893 , 979 , which is incorporated herein by reference . as shown in fig1 the shelving structure 10 generally includes four corner posts 12 and three shelves 14 supported on the posts 12 by adjustable corner supports 16 . the shelving structure 10 optionally may be provided on casters , as shown in fig1 . in the preferred embodiment , each of the shelves 14 is an open or ventilated wire perimeter shelf having right and left sides 18 , a front side 20 and a rear side 22 . each side of the shelf 14 generally comprises an upper rail 24 , a lower rail 26 and a central rail 28 bent back and forth in a serpentine manner between the upper rail 24 and the lower rail 26 . in the preferred embodiment , each of the upper rail 24 and the lower rail 26 may be made of cold rolled steel ( crs ) 1 / 4 wire , the central serpentine rail 28 may be made of cold rolled steel ( crs ) or # 7 gauge stainless steel wire , and the central serpentine rail 28 may be bonded ( e . g ., by welding ) to the upper rail 24 and lower rail 26 at bent portions thereof . however , those skilled in the art readily will appreciate alternative materials and structures for forming the shelves that may be used in other embodiments and applications . the modular storage system of the present invention may include a plurality of divider structures . for example , in the embodiment of fig1 the storage system includes three shelves , two reel storage dividers 30 , two lower stencil storage dividers 32 and an upper stencil storage divider 34 . each reel storage divider 30 comprises right and left reel storage divider beams 36r , 36l and a plurality of reel storage partitions 38 . each stencil storage divider 32 , 34 comprises right and left stencil storage divider beams 40r , 40l and a plurality of stencil storage partitions 42 . as discussed in greater detail below , each reel storage divider 30 is supported at its respective ends on the right and left sides 18 of the open perimeter shelf 14 . of course , the number and location of the reel storage dividers 30 may be varied based on the size of the reel dividers 30 and the shelf 14 . in this manner , a variety of electronic component accessories , such as electronic component storage reels ( shown in phantom in fig1 ), may be accommodated by the modular storage system . in the embodiment shown in fig1 the modular storage system also includes three stencil storage dividers arranged on adjacent shelves . each of the lower stencil storage dividers 32 is adjustable by selectively locating the divider on the right and left sides of the shelf 14 . similarly , the upper stencil storage divider 34 may be selectively located anywhere along the right and left sides 18 of the upper shelf 14 . the upper and lower shelves selectively may be raised and lowered . in this manner , it will be appreciated that a variety of electronic component accessories , such as stencils ( shown in phantom in fig1 ) may be accommodated in the modular shelving system . fig2 a through 2d illustrate a first embodiment of a reel storage divider beam of the present invention . in this regard , fig2 a through 2d illustrate a left side reel storage divider beam 36l . as illustrated in fig1 each reel storage divider 30 comprises a right side reel storage divider beam 36r and a left side reel storage divider beam 36l that are mirror image structures . fig2 a is a top plan view of a reel storage divider beam template 36l prior to folding ; fold lines are shown as dashed lines . as shown therein , the reel storage divider beam 36l generally includes a top surface 44 , an interior side 46 , an exterior side 48 having an exterior side flange 50 , and right and left end tabs 52r , 52l . when assembled , the various sides , flange and tabs are bent at approximately 90 ° angles to form a beam having a generally rectangular cross - section ( see , e . g . fig4 ). the right and left reel beam end tabs 52 ( r , l ) are provided with respective end tab offsets 54r , 54l for receiving respective right and left sides 18 of a shelf 14 , thereby to support the reel storage divider beam 36l on the shelf 14 ( see fig2 b to 2d ). once located at the desired position on the shelf 14 , the tabs 52r , 52l of reel storage beams 36r , 36l optionally may be secured to the shelf 14 by convention means , such as conventional hardware ( including plates , screws and bolts ), nylon wire ties , cable clamps , plastic or metal clips , and the like . alternatively , the tabs 52r , 52l may be permanently secured to shelf 14 , e . g ., by bonding or welding . those skilled in the art readily will appreciate numerous alternative and equivalent means for securing the beams 36r , 36l to the shelf 14 . the top surface 44 of the reel storage divider beam 36 includes a plurality of elongated holes or slots 56 . in a preferred embodiment , slots 56 are arranged periodically at regular intervals along the length of the reel storage divider beam 36 ( e . g ., at 1 inch intervals ), and a plurality of extended slots 56x selectively are also provided at regular intervals ; the extended slots 56x most preferably are provided every fifth slot to facilitate easy visual indexing and alignment of corresponding slots in respective right and left reel storage divider beams 36 ( r , l ). of course , other indicia or structures may be used to provide visual indexing . as discussed in greater detail below , these slots 56 function as locators for a plurality of reel storage partitions 38 . each exterior side 48 includes a plurality of respective locking holes 58 corresponding to slots 56 , 56x . each reel beam interior side 46 comprises a plurality of supporting holes 60 ( r , c , l ) for supporting a reel storage mat 62 suspended between corresponding right and left reel storage divider beams 36r , 36l . in a preferred embodiment , each reel storage divider beam 36 includes 3 reel storage mat supporting holes 60 , i . e ., right , center and left supporting holes 60 ( r , c , l ). however , the number of supporting holes and supports may be varied in accordance with the desired environment or application . as discussed in greater detail below , the size and shape of the slots 56 , 56x , locking holes 58 and mat supporting holes 60 are selected to accommodate mating parts of the divider 30 . in one embodiment , the slots 56 are 0 . 750 inch × 0 . 219 inch , the extended slots 56x are 1 inch × 0 . 219 inch , the locking holes 58 are 0 . 219 inch dia ., and the mat supporting holes 60 are 0 . 250 inch dia . those skilled in the art readily will be able to select the appropriate sizes and shapes for the desired applications . fig3 a through 3c illustrate a reel storage mat 62 of the present invention . as shown therein , the reel storage mat 62 includes a plurality of rails 64 arranged in parallel and extending along the length of the mat 62 , a plurality of cross - bars 66 and a plurality of reel storage mat support projections 68 . the number of rails 64 , cross - bars 66 and support projections 68 will vary depending on the desired width and length of mat 62 , as well as the desired environment . a greater density of rails 64 may be used to prevent smaller objects from falling down between the beams 36 . in the preferred embodiment , the reel storage mat includes three support projections , i . e ., right , center and left support projections 68 ( r , c , l ). the reel storage mat support projections 68 ( r , c , l ) have a spacing which corresponds with the spacing of holes 60 ( r , c , l ) of corresponding right and left reel storage divider beams 36 ( r , l ). fig4 illustrates in cross section a reel storage divider 38 including right and left divider beams 36r , 36l , a partition 38 and a mat 62 . as shown therein , each of right and left beams 36 ( r , l ) is supported at an end thereof on a side 18 of a shelf 14 . more specifically , end tabs 52 of right and left reel storage divider beams 36 ( r , l ,) are bent downwardly from the top surface 44 of right and left beams 36 ( r , l ) to accommodate the side 18 of the shelf 14 in respective end tab offsets 54 ( see also fig2 b to 2d ). a mat 62 is supported between right and left beams 36 ( r , l ), and suspended therebetween , by inserting respective support projections 68 through corresponding supporting holes 60 . in this manner , mat 62 forms a trough between beams 36r , 36l for securely locating and supporting various accessories , such as reels containing electronic components ( shown in phantom in fig4 ). in the present embodiment , each reel storage partition 38 is a generally u - shaped wire hoop including an arm 70 , right and left legs 72r , 72l , and corresponding right and left feet 74r , 74l . to assemble divider 30 , right and left legs 72 ( r , l ) are pinched inwardly , as shown by the arrows in fig4 inserted through respective slots 56 , and then released such that right and left feet 74 ( r , l ) are inserted through respective locking holes 58 in right and left reel storage divider beams 36 ( r , l ). ( see also fig1 wherein front side 20 of shelf 14 is partially cut - away ). in this manner , each reel storage partition 38 is located and locked relative to right and left reel storage beams 36 ( r , l ) so as to support partition 38 in an upright position with the right and left legs 72 ( r , l ) and reel storage arm 70 extending away from right and left reel storage divider beams 36 ( r , l ). similarly , each partition 38 may be removed by reversing this process , and relocated at another position . the size , shape and structure of partition 38 may be selected based on the application . the width of partition 38 is selected to correspond to the width of mat 62 and beams 36r , 36l . by varying the width of mat 62 and partition 38 , the width of the trough formed between the beams 36 may be selected for the desired application . although the partition in the preferred embodiment is a wire hoop , alternative partition structures that accomplish the same functions readily will be apparent to those skilled in the art . fig5 a through 5c illustrate a preferred embodiment of a lower stencil storage divider 32 of the present invention . the lower stencil storage divider 32 generally includes right and left beams 40r , 40l and a plurality of stencil storage partitions 42 . each beam 40 has an open or ventilated structure , including an upper rail 76 , a lower rail 78 and a center rail 80 which is bent back and forth in a serpentine manner between the upper rail 76 and the lower rail 78 . the center rail 80 is bonded to the upper rail 76 and the lower rail 78 at bent portions thereof . right and left beams 40 ( r , l ) also are connected at respective ends by upper end cross - beams 82 and lower end cross - beams 84 . as shown in fig5 a , the upper rail 76 extends further than the lower rail 78 at each end of the beam 40 , such that beam 40 may be supported on a side 18 of shaft 14 . as with the reel storage dividers , once located on the shelf 14 , the stencil storage divider beams 40 optionally may be secured to the shelf 14 by conventional means , including conventional hardware ( plates , screws and bolts ), ties , clamps , clips and the like . alternatively , the beam 40 may be permanently secured to the shelf 14 , e . g ., by bonding or welding one or more of the upper rail 76 , the lower rail 78 , the central rail 80 , upper cross beam 62 or lower cross beam 84 to the shelf 14 . each stencil storage partition 42 includes an arm 86 extending between the right and left beams 40 ( r , l ), and right and left legs 88 ( r , l ) which are supported by respective right and left beams 40 ( r , l ). in the preferred embodiment , right and left legs 88 ( r , l ) are fixed to respective right and left beams 40 ( r , l ) by conventional means , preferably by bonding , and most preferably by welding . in this manner , each stencil storage partition 42 is supported and extends upwardly in a generally vertical direction away from right and left stencil storage divider beams 40 ( r , l ). in the embodiment of fig5 a and 5b , partitions 42 are arranged at periodic intervals along the length of dividers 32 . however , the location of the partitions may be selected to accommodate various accessories having different widths in accordance with the desired application . fig6 illustrates a preferred embodiment of an upper stencil storage divider 34 . referring to fig1 and 6 , the structure of upper stencil storage divider 34 is substantially similar to the structure of lower stencil storage divider 32 ( fig5 a to 5c ); upper stencil storage divider 34 includes right and left beams 40 ( r , l ), each including an upper rail 90 , a lower rail 92 , and a center rail 94 bent back and forth in a serpentine manner between upper rail 90 and lower rail 92 . however , as shown in fig1 and 6 , in upper stencil storage divider 34 , right and left legs 88 of the plurality of stencil storage partitions 42 are supported by ( e . g ., bonded to ) right and left beams 40 ( r , l ) such that each partition 42 extends downwardly in a generally vertical direction away from right and left beams 40 ( r , l ). fig7 a to 7f and fig8 illustrate an alternative embodiment of the reel storage divider of the present invention . in this embodiment , the first and second beams and the mat are provided in the form a single element . fig7 a is a top plan view of a one - piece template 100 for the alternative embodiment of the base of a reel divider prior to folding ; fold lines are shown as dashed lines . as shown therein , the template 100 includes at its center a ventilated webbed portion ( mat ) 102 , right and left interior side beam portions 104r , 104l , right and left top beam surfaces 106r , 106l , right and left exterior side beam portions 108r , 108l , and right and left terminal flange portions 110r , 110l . fig7 b schematically illustrate the reel divider beam template after folding . it will be appreciated that the present embodiment thus provides in a single piece right and left beams each comprising an interior side ( 104r , 104l ), a top beam surface ( 106r , 106l ), and exterior side ( 108r , 108l ), and a terminal flange ( 110r , 110l ). the right and left beams are connected by the ventilated webbed mat 102 . as illustrated in fig7 a , b , c and e , the right and left side beams are formed as mirror image structures . as in the first embodiment , each top side 106 ( r , l ) includes a plurality of slots 112 formed along the length of the beam , and such slots 112 preferably are formed at regular intervals . likewise , each exterior side 108 ( r , l ) of the right and left beams includes a corresponding plurality of locking holes 114 . each interior side 104 ( r , l ) of the right and left beams optionally includes a plurality of visual indices 116 provided at regular intervals along the length of the beam . in the embodiment of fig7 a , the visual indices are defined by small holes formed in the interior sides 104 ( r , l ) of the beams at regular intervals corresponding to every five slots 112 . however , such visual indices may be provided by any suitable indicia , such as embosses , dimples , stickers , and the like , and may be arranged at different intervals as appropriate for the desired application . those skilled in the art readily will appreciate alternative visual indicia and spacing suitable for the desired embodiment or application . the ventilated webbed mat 102 together with right and left interior sides 104 ( r , l ) form a trough . as in the prior embodiment , the width of the trough formed by the ventilated webbed mat 102 and the right and left interior sides 104 ( r , l ) may be varied to suit the appropriate environment or application . for example , the depth and width of the trough may be varied to accommodate a specific size of electronic components , e . g ., reels containing a plurality of electronic devices . more specifically , the width of the ventilated webbed mat 102 , the width of the right and left interior sides 104 ( r , l ) and / or the angle formed between the ventilated webbed mat 102 and the respective right and left interior sides 104 ( r , l ) may be varied . in a preferred embodiment , the angle formed between the ventilated webbed mat 102 and the respective right and left interior sides 104 ( r , l ) is 41 . 6 degrees ( see fig7 e ). of course , those skilled in the art readily will be able to select the respective widths and angles based on the desired environment or application . as in the first embodiment , the reel storage divider 100 of the present embodiment includes a plurality of partitions 118 supported by the respective right and left beams of the reel storage divider 100 . as best shown in fig7 e , in one embodiment each partition 118 is formed by a wire hoop including an arm 120 , right and left legs 122r , 122l , and right and left feet 124r , 124l . as in the prior embodiment , each partition 118 is supported in the right and left beams of divider 100 by pinching the right and left legs 122 ( r , l ) together , inserting the right and left feet 124 ( r , l ) through respective slots 112 in the right and left beams , and then releasing the legs 122 ( r , l ) such that the right and left feet 144 ( r , l ) are inserted through corresponding locking holes 114 . in this manner , it will be appreciated that each partition 118 is supported by the right and left beams by locating and locking the partition legs 122 and feet 124 in the respective slots 112 and locking holes 114 . moreover , as discussed above , each partition may readily be removed by reversing this procedure , and relocated at a different desired location . in the present embodiment , the one - piece reel storage divider 100 is mounted on a shelf 14 using a pair of end brackets 126 . fig8 illustrates one embodiment of an end bracket 126 which includes an end plate 128 , a tab 130 and an offset 132 . each end bracket may be fixed , e . g ., by welding or the like , to respective ends of the one - piece reel storage divider 100 ( see fig7 e and 7f ). each reel storage divider then may be supported on the sides 18 of an open ( ventilated ) shelf 14 in the same manner as in the first embodiment . as shown in fig7 e and 7f , the depth of the trough formed by the ventilated webbed mat 102 and the right and left interior sides 104 ( r , l ) of the trough may extend below the right and left exterior sides 108 ( r , l ) and terminal flanges 110 ( r , l ). it will be appreciated that this configuration provides additional strength and rigidity to the divider structure . each reel storage divider optionally may be secured to the sides 18 of a shelf 14 by conventional means , including conventional hardware ( screws , bolts and plates ), nylon wire ties , cable clamps , clips and the like . the reel storage divider tabs 36 , 130 may be provided , e . g ., with holes or slots 134 for this purpose . each reel storage divider alternatively may be permanently fixed to the sides 18 of a shelf 14 by bonding , e . g ., by welding . as shown in fig1 in a preferred embodiment the stencil storage divider system of the present invention includes two lower stencil dividers 32 and a single upper stencil storage divider 34 , although that arrangement may be varied ( i . e ., by using any combination of one or more lower dividers and one or more upper dividers ) without departing from the scope of the invention . respective stencil storage partitions 42 of the lower stencil storage dividers 32 and upper stencil storage divider 34 are arranged in - line , such that a stencil may be inserted through generally vertical slots defined therebetween ( see stencil shown in phantom in fig1 ). in the knock - down shelving system of the preferred embodiment , it will be appreciated that the height of the respective shelves and the regular spacing intervals of the stencil storage partitions 42 readily may be varied to accommodate stencils having numerous sizes and thicknesses . in the preferred embodiment , each of the shelves 14 , stencil storage divider beams 40 and stencil storage partitions 42 is made of metal , e . g ., stainless steel , using an open wire ( ventilated ) shelving design . it will be appreciated that such structures are strong , stable , durable , easily assembled and easily cleaned . however , those skilled in the art readily will appreciate that other materials , e . g ., molded plastics , may provide particularly utility and advantages in different environments and applications . similarly , in the preferred embodiments the reel storage divider beams 36 , 100 preferably are formed by stamping and machining / bending sheet metal , preferably stainless steel sheet metal . thus , the reel storage divider beams 36 , 100 of the preferred embodiments also are strong , stable , easily and cheaply manufactured , and easy to clean . however , those skilled in the art readily will be able to identify alternative compositions and structures suitable for various alternative embodiments and environments . although specific embodiments of the present invention have been described above in detail , it will be understood that this description is merely for purposes of illustration . various modifications of and equivalent structures corresponding to the preferred embodiments in addition to those described above may be made by those skilled in the art without departing from the spirit of the present invention which is defined in the following claims , the scope of which is to be accorded the broadest interpretation so as to encompass such modifications and equivalent structures .
0
fig4 shows an embodiment of a laser system configured to generate at least one supercontinuum output signal . in the present application the terms supercontinuum and continuum are used interchangeably and refer to a broad spectral bandwidth while retaining a relatively high spatial coherence . those skilled in the art will appreciate that there are a number of applications for continuum generation in diamond or other materials as described below . the continuum generation process described below effectively redistributes the power of a high repetition rate pulse train into a broader spectrum of wavelengths , which may not easily be generated directly with an alternate laser source . one or more of these shifted spectral regions may be selected and used for an application requiring a wavelength other than that of the pump laser . in particular , different spectral regions may be used to selectively excite different fluorescent proteins in high resolution biological imaging . two appropriately spaced portions of a continuum may also be combined in a nonlinear material and a difference signal generated , at a longer wavelength , generally in the infrared . also , if appropriately distributed in time , a spectral continuum may be temporally compressed , using well - known techniques including grating and prism pairs , to produce a much shorter optical pulse . a portion of a continuum spectrum may also be amplified in an optical parametric amplifier ( opa ). the amplified signal may then itself be used in any of the above - mentioned applications . as shown in fig4 , the supercontinuum generation laser system 20 includes at least one pump laser system 22 in optical communication with at least one continuum generator 24 . in one embodiment , the pump laser system 22 is configured to emit sub - picosecond pump signals 26 to the continuum generator 24 . for example , in one embodiment , the pump laser system 22 comprises a diode - pumped solid state oscillator . more specifically , the pump laser 22 may comprise a yb : caf 2 oscillator . in another embodiment , the pump laser system 22 comprises a yb : kgw , yb : kyw , yb : calgo , yb : glass , cr : licaf , cr : lisaf , cr : liscaf , or cr : licagaf oscillator . in yet another embodiment , the pump laser system comprises a ti : sapphire or cr : znse laser system . referring again to fig4 , the pump laser system 22 may be configured to output a pulsed pump signal 26 to the continuum generator 24 having a peak power of about 0 . 2 mw or more . in a more specific embodiment , the pump signal 26 may have a peak power of about 1 mw or more . optionally , the pump signal 26 may have a peak power of about 1 . 5 mw . as such , it is desirable that the pump laser 22 emits a pump signal 26 at a power greater than the self - focusing threshold . self - focusing occurs when the intensity of a beam is sufficiently high in a nonlinear material . at some intensity the effect of the nonlinear index n 2 becomes significant . for a beam with a gaussian spatial profile , the center of the beam is more intense and thus experiences a higher index . the higher index on axis creates a lens that delays the center of the beam and causes the beam to self - focus upon itself . the intensity of the beam then increases further and the beam focusses more tightly until diffraction or other processes provide a limit . the intensity required for this process to begin is called the self - focusing threshold . as such , any variety of laser systems , optical amplifiers , and / or optical oscillators may be used as a pump source provided that the output pump signal 26 is at a peak power sufficient to generate self focusing . further , the pump laser 22 may output a pump signal at a variety of wavelengths . for example , in one embodiment , the pump signal 26 has a wavelength of about 300 nm to about 3000 nm . more specifically , the pump signal 26 may have a wavelength of about 600 nm to about 1800 nm . optionally , the pump signal 26 may have a wavelength of about 750 nm to about 1100 nm . in another embodiment , the pump signal 26 has a wavelength of about 1000 nm to about 1100 nm . as shown in fig4 , 5 a , and 5 b , the continuum generator 24 receives the high power , relatively narrow bandwidth pump signal 26 from the pump laser system 22 and emits a lower power , broad bandwidth continuum signal . for example , fig5 a shows graphically the wavelength characteristics of a pump signal 26 . as shown in fig4 , 5 a , and 5 b , the pump signal 26 consists of a signal wavelength signal having essentially all its energy at 1047 nm . in contrast , the continuum generator 24 receives the pump signal 26 from the pump laser system 22 and emits a broad wavelength signal 28 . in one embodiment , the continuum generator 24 comprises at least one single filament diamond - based device . there are a number of considerations in designing a practical continuum generator 24 . for example , a useful amount of spectral broadening must be produced in the bulk material forming the continuum generator at an intensity below that material &# 39 ; s damage threshold . the spectral broadening necessarily occurs at a very high intensity in a small volume within the solid material and involves some optical loss . such loss often involves heating and damage to the material either within the bulk or at a surface of the continuum generator 24 . the extremely high thermal conductivity of diamond mitigates this local heating within the bulk , even in a static crystal , while its desirable self - focusing threshold ( diamond has a value of about 30 × 10 − 16 cm 2 / w ) allows for significant continuum generation . as such , unlike prior art devices which required the continuum generator to be moved during use , the continuum generator 24 described herein may remain substantially stationary during use . further , the length of the crystal or bulk material forming the continuum generator 24 must be long enough for self - focusing to occur and establish a high intensity optical filament . this filament will be self - terminating , due to other linear or nonlinear optical effects . the crystal must also be long enough such that the exit surface of the crystal is beyond the end of the filament formed therein , to avoid damage to that surface . further , continuum generation in diamond - based continuum generator 24 is also affected by the propagation direction and polarization of the pump beam within the crystal . propagation along a & lt ; 110 & gt ; direction , with polarization in a & lt ; 111 & gt ; direction ( along the carbon - carbon bonds ) provides the production of a stable and efficient continuum output signal near continuum generation threshold . once well above continuum generation threshold ( i . e . 1 . 5 times supercontinuum threshold ) alternative polarizations may be used . given the relatively high fresnel reflection from a normal incidence diamond surface brewster - angle entrance and exit surfaces may be advantageous . thus , a diamond rhomb , with particular crystalline orientation is preferred , although those skilled in the art will appreciate that the shape and dimensions of the bulk material forming the continuum generator 24 may be tailored as desired . alternatively , broadband ar ( anti - reflection ) coatings may be applied to the substantially normal incident surfaces . optionally , any number of alternate materials may be used to form the continuum generator 24 . for example , sic , gan , and / or aln may be used to form the continuum generator . as such , other high thermal conductivity , crystalline materials may be substituted for diamond in forming the continuum generator 24 . fig6 a shows a more detailed schematic diagram of one embodiment of the continuum generation system 20 shown in fig4 . in the present embodiment , the pump laser 22 includes at least one gain medium 34 pumped by a diode pump source 40 . in one embodiment , the gain medium is a solid state material . for example , the gain medium 34 may be yb : caf 2 . in the alternative , the gain medium 34 may be yb : kgw , yb : kyw , yb : calgo , yb : glass , cr : licaf , cr : lisaf , cr : liscaf , or cr : licagaf . optionally , the pump laser 22 may comprise a ti : sapphire or cr : znse laser system . for example , in one embodiment the ti : sapphire laser system used to form the pump laser 22 is configured to output sub - picosecond output pulses . in an more specific embodiment , the ti : sapphire laser system is configured to output 100 fs pulses . referring again to fig6 a , the gain medium 34 may be positioned between a first mirror 36 and at least a second mirror or outcoupler 38 . as such , the first and second mirrors 36 , 38 may cooperatively form a cavity 32 within the pump laser system 22 . further , at least additional supplemental optical element 42 may be positioned within the pump laser system 22 . exemplary optical elements include , without limitations , semiconductor saturable absorber mirrors , mode - locking devices , lens and lens systems , mirrors , prisms , gratings , filters , acousto - optic devices , and the like . in addition , at least one lens or other focusing device may be used to focus the pump signal 26 into the continuum generator 24 . in the illustrated embodiment , the continuum generator 24 is located outside the pump laser system 22 . optionally , the pump laser system 22 and continuum generator 24 may be located within a single housing . as shown in fig4 , the continuum generator 24 emits at least one continuum signal 28 when irradiated by the pump signal 26 . in one embodiment , the continuum generator 24 emits continuum signals 28 at a repetition rate of at least about 1 mhz . in another , the continuum generator 24 emits continuum signals 28 at a repetition rate of at least about 5 mhz . in yet another embodiment , the single filament diamond - based continuum generator 24 emits continuum signals 28 at a repetition rate of at least about 10 mhz . further , the single filament diamond - based continuum generator 24 may be configured to emit continuum signals 28 having an average power of about 1 w or more . in another embodiment , the continuum generator 24 may be configured to emit continuum signals 28 having an average power of about 5 w or more . optionally , the continuum generator 24 may be configured to emit continuum signals 28 having an average power of about 10 w or more . fig6 b shows the wavelength characteristics of a pump signal 26 from a ti : sapphire pump laser system 22 as compared with the continuum signals 28 emitted from the continuum generator 24 shown in fig4 . fig7 shows an embodiment of a laser system 70 which uses a continuum signal as a seed for one or more optical parametric oscillators . as shown , the laser system 70 includes at least one pump laser system 72 to provide at least one pump signal to the continuum generator 100 . exemplary pump laser systems 72 include the diode - pumped solid state pump laser devices described above . in one embodiment a portion of the pump signal is directed by a beam splitter 74 to beam splitter 76 , which in turn directs a portion of the pump signal to a first optical parametric amplifier 78 ( hereinafter first opa 78 ). also , a portion of the pump signal is directed by a reflector 86 to at least a second optical parametric amplifier 88 ( hereinafter second opa 88 ). referring again to fig7 , the beam splitter 74 directs a portion of the pump signal to a focusing device 98 which focuses the pump signal into the continuum generator 100 . at least one continuum signal is emitted from the continuum generator 100 and directed into the first opa 78 and second opa 88 , by the optical elements 104 , 106 respectively . optionally at least additional optical device 80 may be used to condition the pump signal and / or continuum signal prior to irradiating the first opa 78 . similarly , at least additional optical device 90 may be used to condition the pump signal and / or continuum signal prior to irradiating the second opa 88 . in one embodiment , at least one of the first and second opas comprises periodically poled ktp ( ppktp ). in the alternative , at least one of the first and second opas may contain lithium tantalate , periodically poled lithium tantalate ( pplt ), lbo and / or bbo . in another embodiment , the pump signal from pump laser system 72 may be frequency doubled for pumping one or both opas . the embodiments disclosed herein are illustrative of the principles of the invention . other modifications may be employed which are within the scope of the invention . accordingly , the devices disclosed in the present application are not limited to that precisely as shown and described herein .
6
in the production of the alkanoic acids and esters of this invention , one preferably begins with a hydroxyaromatic ketone and reacts it with one of the aforesaid substituted acids or esters under basic conditions . this reaction product is then reacted with a hydroxylamine derivative and then subjected to a beckmann rearrangement in the presence of a catalyst . the resulting product is the desired 2 -( amidophenoxy ) alkanoic acid or ester . this resulting product may then hydrolyzed or alcoholized to obtain the desired 2 -( 4 - aminophenoxy ) alkanoic acid or ester . the reaction sequence may be generalized as : ## str6 ## the preferred embodiment will now be set forth in further detail , and the skilled artisan can well obtain the analogous compounds . an important feature of this invention is to begin the synthesis with a hydroxyaromatic ketone ( i ) or benzaldehyde derivative which is preferably a 4 - hydroxyacetophenone compound . the most preferred compound is 4 - hydroxyacetophenone , as well as its sodium and potassium salts . the hydroxyaromatic ketone is then reacted with one of the aforesaid x - substituted acids or esters which may be optically active or racemic . preferred esters are halogen substituted propanoates such as methyl 2 - chloropropanoate , methyl 2 - bromopropanoate , and ethyl 2 - chloropropanoate , alkyl 2 -[( methylsulfonyl ) oxy ] propanoate and alkyl 2 -[( toluylsulfonyl ) oxy ] propanoate . this reaction proceeds by the williamson &# 39 ; s ether synthesis which is also well known to the skilled artisan . the reaction may take place by refluxing the hydroxyaromatic ketone with the ester in a solvent such as dimethylformamide under basic conditions . the basic conditions may be provided either by use of a base such as an alkali metal or alkaline earth metal hydroxide or carbonate , amines or a hydride such as sodium hydride . alternatively , within the meaning of this invention , the basic media may be provided by using one of the aforesaid salt forms of the hydroxyaromatic ketones , such as 4 - hydroxyacetophenone sodium or potassium salt . alternative solvents for the refluxing reaction non - exclusively include polar protic solvents , e . g ., water or alcohol ; or polar aprotic solvents , e . g ., ketones , ethers , nitriles , and sulfoxides . the reaction may take place at a temperature of from about 0 . 1 to about 100 hours , or more preferably from about 1 to about 50 hours at a temperature of from about 0 ° c . to about 200 ° c . or more preferably from about 25 ° c . to about 200 ° c . the reaction product of this juncture is a 2 -( 4 - acylphenoxy ) alkanoic ester derivative . in the preferred embodiment the foregoing reactants are 4 - hydroxyacetophenone potassium salt and methyl 2 - bromopropionate with refluxing in dimethylformamide . therefore the preferred compound produced is methyl 2 -( 4 - acetylphenoxy ) propionate . in the alternative , instead of the aforesaid substituted ester , one could use a substituted acid of the formula : ## str7 ## wherein r 2 is as described before is conducted prior to the oxidation step . this component is then reacted with an amine such as h 2 n -- r 3 wherein r 3 is oh , o -- so 3 h , where r is as described before . in the most preferred embodiment , hydroxylamine is employed . other preferred amines non - exclusively include hydrazoic acid and hydroxylamine - o - sulfuric acid . the reaction product at this point is a 2 -( 4 - acyliminophenoxy ) alkanoic acid or ester . this component is then subjected to a beckmann rearrangement process which is well known to the skilled artisan per se . this causes a shift of the r 3 group from its carbon bond to a bond with the nitrogen . the rearrangement is conducted with any commonly employed beckmann catalyst . in the preferred embodiment an acid catalyst is used in a suitable solvent . the most preferred acid is sulfuric acid . others non - exclusively include thionyl chloride and polyphosphoric acid . one preferred solvent is acetic acid . alternative solvents non - exclusively include carboxylic acids , esters , nitriles and ethers . the reaction may take place at a temperature of from about 0 . 1 to about 12 hours , or more preferably from about 0 . 5 to about 6 hours at a temperature of from about 40 ° c . to about 130 ° c . or more preferably from about 80 ° c . to about 120 ° c . the reaction product of this juncture is a 2 -( 4 - acetamidophenoxy ) alkanoic acid or ester which in the preferred embodiment is a 2 -( 4 - acetamidophenoxy ) propanoic acid or ester . this latter component may then be hydrolyzed or alcoholyzed . the alcoholysis may be conducted by contacting with alcohols under acidic conditions and elevated temperatures for a period of time sufficient to permit the reaction to approach completion . the amount of alcohol used may be , for example , about 0 . 5 to about 1 , 000 mol equivalents , preferably about 1 to about 100 mol equivalents based on the ester being alcoholized . the acids which may be employed for this purpose are organic acids such as methanesulfonic acid , para - toluenesulfonic acid , mineral acids such as sulfuric , hydrochloric and phosphoric acids , and acidic ion exchange resins . in some instances , it may be desirable to employ a combination of alcohol and water to achieve a measure of solvolysis . the hydrolysis may be conducted by refluxing with alcohols , ion exchange resins and / or acids such as hydrochloric acid and sulfuric acid . hydrolysis may take place at from about 0 . 1 to about 10 hours , or more preferably from about 0 . 5 to about 4 hours at a temperature of from about 20 ° c . to about 200 ° c ., or more preferably from about 60 ° c . to about 140 ° c . the reaction is conducted with an anticipated conversion of from about 90 % to about 99 % with a selectivity of from about 90 % to about 98 %. the solvolysis product is a 2 -( 4 - aminophenoxy ) alkanoic acid or ester which in the preferred embodiment is a 2 -( 4 - aminophenoxy ) propanoic acid or ester . the alcoholysis process of this invention provides for the recovery of the amino product in relatively higher yields . the product may be recovered by conventional purification methods usually involving a combination of crystallization , filtration , washing and distillation in any order deemed advantageous for the system at hand . to a solution of 4 - hydroxyacetophenone potassium salt ( 8 . 8 g , 500 mmol ) in methanol ( 50 ml ) is added methyl 2 - bromopropanoate ( 11 . 08 , 65 . 0 mmol ) dropwise over 30 minutes under nitrogen . the mixture is refluxed under nitrogen for 24 hours during which kbr is accumulated . the reaction is monitored by thin layer chromatography using 100 % ethyl acetate . the reaction is cooled to room temperature and the kbr is filtered out . ethyl acetate ( 50 ml ) is added to give a turbid solution which is refiltered . the reaction product is analyzed by glc and found to yield methyl 2 -( 4 - acetylphenoxy ) propanoate ( 13 . 2 g ). ( m . p . 54 . 8 ° c . ); ir ( kbr ) 1757 . 7 ( vs ), 1666 . 8 ( vs ); 1 h nmr ( cdcl 3 ) delta 1 . 54 ( d , j = 6 . 8 hz , 3h ), 2 . 42 ( s , 3h ), 3 . 64 ( s , 3h ), 4 . 76 ( q , j = 6 . 8 hz , 1h ), 6 . 79 and 7 . 80 ( dd , j = 8 . 0 hz , 4h ). to a solution of the potassium salt of 4 - hydroxyacetophenone ( 25 . 0 g , 0 . 14 mol ) in dimethylformamide ( dmf ) ( 100 ml ) is added methyl 2 - chloropropanoate ( 24 . 5 g , 0 . 20 mol ) over 30 minutes and stirred at 85 °- 90 ° c . for 3 hours under nitrogen . the reaction is filtered to remove kcl and the filtrate is concentrated under reduced pressure to remove dmf and the product analyzed by glc . the product is dissolved in ethyl acetate ( 300 ml ) and extracted with 2n naoh ( 2 × 100 ml ) and water ( 100 ml ). the organic phase is dried and concentrated to give pure methyl 2 -( 4 - acetylphenoxy ) propanoate ( 25 g ) ( yield 64 %). to a solution of the potassium salt of 4 - hydroxyacetophenone ( 25 . 0 g , 0 . 14 mol ) in dmf ( 100 ml ) is added ethyl 2 - chloropropanoate ( 27 . 3 g , 0 . 20 mol ) over 30 minutes and stirred at 85 °- 90 ° c . for 3 hours under nitrogen . the reaction is filtered to remove kcl and the filtrate is concentrated under reduced pressure to remove dmf and the product is analyzed by glc . the product is dissolved in ethyl acetate ( 300 ml ) and extracted with 2n naoh ( 2 × 100 ml ) and water ( 100 ml ). the organic phase is dried and concentrated to give pure ethyl 2 -( 4 - acetylphenoxy ) propanoate ( 30 g ) ( yield 75 %); m . p . 49 . 6 ° c . ; ir ( kbr ) 1747 . 7 ( vs ), 1669 . 8 ( vs ); 1 h nmr ( cdcl 3 ) delta 1 . 18 ( t , j = 7 . 2 hz , 3h ), 1 . 58 ( d , j = 6 . 8 hz , 3h ), 2 . 46 ( s , 3h ), 4 . 15 ( q , j = 7 . 2 , 2h ), 4 . 77 ( q , j = 6 . 8 , 1h ), 6 . 83 and 7 . 84 ( dd , j = 9 . 0 hz , 4h ). a solution of the potassium salt of 4 - hydroxyacetophenone ( 17 . 6 g , 0 . 1 mol ) in dmf ( 50 ml ) is added to a solution of ethyl l - 2 -[( methylsulfonyl ) oxy ] propanoate ( 21 . 5 g , 0 . 11 mol ) in dmf ( 40 ml ) over 15 minutes at 80 ° c . and stirred at 80 ° c . for 2 hours . to the reaction is added ethyl acetate ( 100 ml ) and filtered . the filtrate is concentrated under reduced pressure whereupon the product is analyzed by glc . the product is dissolved in ethyl acetate ( 250 ml ) and extracted with saturated sodium bicarbonate solution ( 2 × 100 ml ) and water ( 2 × 60 ml ). the organic phase is dried and concentrated to give ethyl d4 -( 4 - acetylphenoxy ) propanoate ( 20 . 2 g ). potassium hydroxide ( 17 . 0 g , 0 . 3 mol ) is added to water ( 50 ml ) and allowed to dissolve . the solution is added to 4 - hydroxyacetophenone ( 13 . 6 g , 0 . 1 mol ) to produce the potassium salt of 4 - hydroxyacetophenone . 2 - bromopropanoic acid ( 17 . 0 g , 0 . 11 mol ) is added to the potassium salt of 4 - hydroxyacetophenone to give a yellow suspension . the solution is heated to reflux ( 102 ° c .) during which a yellow solution results . the solution is refluxed for 24 hours and cooled to room temperature . the ph is adjusted to 6 - 7 and extracted with ethyl acetate ( 3 × 100 ml ) and the solution is concentrated under reduced pressure . the aqueous layer is acidified to ph 2 and extracted with ethyl acetate ( 3 × 150 ml ). the solution is concentrated to give 7 . 0 g of a brown liquid which is 2 -( 4 - acetylphenoxy ) propanoic acid at a yield of 34 %. to a solution of the potassium salt of 4 - hydroxyacetophenone ( 8 . 8 g , 0 . 05 mol ) in dimethylformamide ( 25 ml ) is added methyl 2 - bromopropanoate ( 10 . 2 g , 0 . 06 mol ) over 30 minutes and stirred at 80 °- 90 ° c . for 4 hours under nitrogen . the reaction is cooled to room temperature and methylene chloride ( 75 ml ) and water ( 75 ml ) are added . the organic phase is separated , washed with water ( 100 ml ), dried and concentrated to give methyl 2 -( 4 - acetylphenoxy ) propanoate ( 8 . 5 g ) ( yield 76 %). methyl 2 -( 4 - acetylphenoxy ) propanoate ( 7 . 0 g , 31 . 5 mmol ) is combined with 2n naoh ( 20 ml ) and refluxed overnight . water ( 30 ml ) is added to the reaction which is then washed with methylene chloride ( 50 ml ). it is then acidified to ph = 1 with concentrated hydrochloric acid and extracted with ethyl acetate ( 3 × 100 ml ). the organic phase is dried and concentrated to provide 2 -( 4 - acetylphenoxy ) propanoic acid ( 5 . 0 g ) ( yield 92 %): m . p . 104 . 3 ° c ., ir ( kbr ) 3000 ( br , vs ), 2940 ( br , s ), 1754 ( vs ), 1650 ( vs ); 1 h nmr ( cdcl 3 ) delta 1 . 69 ( d , j = 6 . 8 hz , 3h ), 2 . 55 ( s , 3h ), 4 . 8 ( q , j = 6 . 8 hz , 1h ), 6 . 92 and 7 . 93 ( dd , j = 9 . 0 hz , 4h ). a solution of 2 -( 4 - acetylphenoxy ) propionic acid ( 1 . 5 g , 7 . 2 mmol ), hydroxylamine sulfate ( 0 . 72 g , 4 . 4 mmol ), and concentrated sulfuric acid ( 2 drops ) in acetic acid ( 30 ml ) is refluxed for 4 . 25 hours . the reaction is quenched with sodium carbonate ( 0 . 25 g , 2 . 4 mmol ) and concentrated to give a residue . the reaction residue is dissolved in water ( 50 ml ) and extracted with ethyl acetate ( 2 × 100 ml ). the ethyl acetate extract is dried and concentrated to give 2 -( 4 - acetamidophenoxy ) propionic acid ( 1 . 53 g ) ( yield 95 %): m . p . 170 °- 172 ° c . ; ir ( kbr ) 3400 ( vs ), 2900 ( s ) 1730 ( vs ), 1630 ( vs ), and 1603 ( vs ); 1 h nmr ( dmso - d 6 ) delta 1 . 47 ( d , j = 6 . 8 hz , 3h ), 1 . 87 ( s , 3h ), 2 . 06 ( s , 3h ), 4 . 65 ( q , j = 6 . 8 hz , 1h ), 6 . 73 and 7 . 42 ( dd , j = 9 . 0 hz , 4h ). to a solution of 2 -( 4 - acetamidophenoxy ) propionic acid ( 0 . 5 g , 2 . 2 mmol ) in ethanol ( 10 ml ) is added a drop of concentrated sulfuric acid and refluxed for 4 hours . the reaction is concentrated to dryness to give a residue . the residue is partitioned between water and ethyl acetate . the ethyl acetate layer is collected , dried ( mgso 4 ), and concentrated to give ethyl 2 -( 4 - acetamidophenoxy ) propanoate ( 0 . 44 g ) ( yield 80 %): 1 h nmr ( cdcl 3 ) delta 1 . 27 ( t , j = 7 . 0 hz , 3h ), 1 . 60 ( d , j = 7 . 0 hz , 3h ), 4 . 25 ( q , j = 7 . 0 hz , 2h ), 4 . 76 ( q , j = 7 . 0 hz , 1h ), 6 . 84 and 7 . 46 ( dd , j = 9 . 0 hz , 4h ), and 8 . 02 ( s , 1h ). ethyl 2 -( 4 - acetamidophenoxy ) propanoate ( 5 . 0 g , 2 . 0 mmol ) is hydrolyzed by refluxing for 6 hours at 80 ° c . with ethanol ( 10 ml ) and 3 drops of concentrated hydrochloric acid . the reaction is concentrated under reduced pressure to obtain ethyl 2 -( 4 - aminophenoxy ) propanoate ( 0 . 4 g ) ( yield 95 %).
2
attention is first directed to fig1 and 2 a of the drawings illustrating the protective breathing hood generally designated 10 which in fig1 is in a flat position and in fig2 a is illustrated donned over an individual &# 39 ; s head 11 . the protective hood 10 comprises a hood 12 made of a stretchable fire resistant material , e . g . silicon rubber which may resist heat up to about 400 °- 600 ° c . and which is an extremely elastic material whilst being impermeable to gases and biologic material . the hood 12 has an opening 14 through which the head of an individual is introduced and a neck sealing portion 16 which as illustrated in the figures is plaited at 18 so as to allow good sealing engagement about the individual &# 39 ; s neck ( see fig2 a ) whilst not choking the individual or causing an uncomfortable feeling . the arrangement is such that when the hood is donned over a user &# 39 ; s head the sealing portion 16 sealingly engages about the user &# 39 ; s neck preventing ingress of obnoxious gases or biologic material therethrough . as can further be illustrated in fig1 and 2 a , the protective hood 10 further comprises a visor 20 which in the present example is a uniform translucent portion extending over both eyes made of a material which is also a heat resistant material . however , it is to be appreciated that the visor 20 may be formed in other shapes and forms , e . g . two eye pieces extending opposite the eye locations of the hood or , the arrangement may be such that the entire hood 12 may be transparent and accordingly no particular visor is provided . the protective hood 10 is formed with two respiratory units 26 disposed offset with respect to the nose / mouth location of the individual , indicated in the figures at 30 . the intersecting dashed lined marked f in fig1 indicate a fold line about which the hood may be folded and may be preserved in a sealed , pocket - sized package other folding patterns are possible as well . one other important character of the invention noticed in fig1 a and 2 b is the deformation of the hood at the nose / mouth location giving rise to forming an internal chamber c ( see fig2 b ) between the nose / mouth location 30 and the individual &# 39 ; s face , the purpose of which will become apparent hereinafter . however , it is noticed that the chamber c renders respiratory units 26 to be is in flow communication with the nose and mouth of the individual . turning now to fig3 a and 3b , there are illustrated a pair of respiratory units 26 articulated to one another by a supporting member 38 . the particular structure of the respiratory units 26 is disclosed hereinafter in detail with reference to fig4 - 6 . in the particular embodiment ( fig3 a and 3b ), deforming member 38 is made of a rigid plastic material formed with two ring - like portions 40 clampingly secured to each of a pair of respiratory units 26 , with an intermediate bridging portion consisting of two members 42 a and 42 b , though other constructions are possible as well and which at the assembled position , while donned over an individual &# 39 ; s head , extend at the nose / mouth location to thereby deform the hood 12 giving rise to forming chamber c ( see also dashed lines in fig1 and 2 a ). bridging portions 42 a and 42 b are interconnected to the circular portions by integral hinges at 44 . for the sake of clarity , the supporting member 38 is illustrated also in fig1 and 2 a , by dashed lines . whilst in fig1 to 3 the deforming member 38 is in the form of a rigid member extending between the two respiratory units , other arrangements for deformation of the mask may be employed as well , for the sake of forming a chamber c . for example , the respective nose / mouth portion 30 may be provided with deforming ribs . such ribs ( not shown ) may be integrally molded during the process of molding the hood , e . g . made of silicon , or may be attached thereto by other means , e . g . adhering or welding ( e . g . heat or sonic , etc ) the ribs may be made of a rigid material other than that of the hood or may constitute an integral part thereof . further attention is now directed to fig4 - 6 for understanding the assembly and mode of operation of the respiratory units 26 . in the present embodiment , each of the respiratory units comprises a multi - receptacle member 48 facing the inside of the protective hood and a cover member 50 facing the outside of the hood . multi - receptacle member 48 is formed with a plurality of receptacles 54 which in the present example have the shape of a honeycomb and a hexagonal section , though other shapes are possible as well , e . g . circular , etc . each of the receptacles 54 has an outlet opening 56 which is covered by a fine grid 58 , so as to prevent outflow of the activated charcoal particles recovered within the receptacles 54 . cover member 50 is similarly formed with a plurality of inlet openings , each such openings fitted with a fine grid 66 also serving to prevent outflow of the activated charcoal particles 59 ( seen in fig6 ) received within the receptacles 54 . co - axially received within each respiratory unit 26 there is a one - way exhaling valve 70 which is in the form of a mushroom - type membrane valve with a stem member 72 snapingly received within a central opening formed at the multi - receptacle member 48 . a plurality of exhaling apertures 74 are formed in the multi - receptacle member 48 to facilitate flow of exhaled gases from the chamber c of the protective hood to the surrounding environment , after deforming the mushroom - type valve and then via the outlet apertures 78 formed in the cover member 50 . typically , the respiratory units 26 are also fitted with a biologic - material barrier in the form of filtering paper 84 ( which for the sake of convenience and practicality is in the form of a single sheet though other arrangements are available as well , e . g . individual pieces received in each of the receptacles 54 ). whilst in the present example , the receptacles 54 are stuffed with particulated activated charcoal 59 ( fig6 ), it is to be appreciated other forms of gas treating media is possible as well , e . g . uniform or layers of impregnated charcoal cloth or other charcoal carrying media , e . g . particulated charcoal embedded within non woven material , e . g . in the form of pellets , etc . as can best be seen in fig4 and 6 , the size of inlet opening 62 and outlet openings 56 is smaller than the actual size of the receptacles 54 . this arrangement ensures that inflow through the respiratory units is continuously treated and obnoxious material is absorbed by the activated charcoal particles 59 obviating the need for thick filtration material on the one hand and on the other hand , providing extended effective use / filtration . as can further be seen in fig4 and 6 , the receptacle member 92 is formed with an annular rim 90 and the cover member 50 is formed with a corresponding annular rim 94 , the latter provided with gripping teeth 96 at a outward facing portion thereof . the arrangement is such that at the assembled position the circular portion 40 of the deforming member 38 is clampingly received between rim portions 92 and 94 . a retaining ring 100 has a plurality of annular teeth 102 corresponding with teeth 96 of the rim 94 and is adapted for clampingly receiving therebetween respective portions of the hood 12 ( fig6 ) wherein the ring 100 is snapingly secured over the periphery of the cover member 50 . reverting now to the issue of chamber c formed in the protective hood in accordance with the present invention , as illustrated , for example in fig1 and 2 , it is to be appreciated that such a chamber is advantageous as it minimizes the feeling of suffocation in case such a protective hood is stretched over an individual &# 39 ; s breathing organisms ( nose and mouth ). furthermore , the construction of a chamber ( at times referred to as a breathing chamber , mixing chamber , speaking chamber , and other similar terms ) enables an individual wearing the protective hood to speak clearly . this is not facilitated in case of a hood which is stretched over the individual &# 39 ; s mouth . still another advantage of the chamber resides in that the individual may breathe freely without having to direct the exhaled gases through an particular outlet opening in which case speech becomes complicated or impossible .
0
[ 0013 ] fig1 illustrates a system 10 having low latency buffer control , according to one embodiment of the present invention . in particular , this embodiment of system 10 includes a processor 11 , a memory controller 12 and a memory 13 . memory 13 is a dram memory in the illustrated embodiment , but can be any type of memory used with a memory bus for which power dissipation is reduced when buffers driving the memory bus are disabled . in addition , this embodiment of memory controller 12 includes a buffer control circuit 14 and a set of n buffers 16 . fig1 shows a buffer 16 1 of the n buffers , with the remaining buffers being omitted for clarity . buffer control circuit 14 typically includes circuitry ( e . g ., combinatorial logic circuits ) to provide enable signals to buffers 16 , timed to reduce latency in memory accesses . the elements of this embodiment of system 10 are interconnected as follows . memory controller 12 is connected to memory 13 and processor 11 via system bus 18 and memory bus 17 , respectively . more particularly , buffer 16 of memory controller 12 are connected to memory bus 17 . in this embodiment , memory bus 17 has n bus lines , each being resistively terminated to a mid - range voltage , and system bus 18 has m bus lines . in this embodiment of memory controller 12 , buffer control circuit 14 is connected to buffers 16 . in particular , buffer control circuit 14 is connected to the enable input terminals of buffers 16 . further , in some embodiments , buffer control circuit 14 is connected to detect transactions being communicated on system bus 18 . [ 0017 ] fig2 illustrates the operational flow of system 10 ( fig1 ) in selectively enabling buffers 16 to reduce latency , according to one embodiment of the present invention . referring to fig1 and 2 , system 10 operates as follows . the system bus is monitored for transactions . in one embodiment , memory controller 12 monitors system bus 18 for transactions . more particularly , buffer control circuit 14 of memory controller 12 monitors system bus 18 to detect transactions . this operation is represented by blocks 21 and 22 . if a transaction is detected in block 22 , the operational flow proceeds to a block 24 ; however , if no transaction is detected in block 22 , the operational flow returns to block 21 . as shown in block 24 , buffers 16 are enabled . in one embodiment , buffer control circuit 14 provides enable signals to the n buffers of buffers 16 . in this embodiment , buffers 16 are conventional three - state buffers that present a high impedance to memory bus 17 when disabled , and either pull up or pull down the voltages of the bus lines of memory bus 17 when enabled . thus , in this embodiment , buffers 16 are enabled before the transaction is decoded ; thereby ensuring the buffers are enabled before they are needed to drive signals on memory bus 17 . in this way , the latency effects of the aforementioned “ buffer enable ” delay can be significantly reduced or even eliminated for memory accesses . the detected transaction is then decoded . in one embodiment , decode circuitry in memory controller 12 decodes the transaction . one function of the decode circuitry is to determine the “ target agent ” of the transaction . for example , for memory transactions , the targeted agent would be memory 13 . other types of transactions ( e . g ., pci transactions ), the targeted agent would be a different element ( e . g ., a pci card ). in one embodiment , the “ buffer enable ” delay transpires concurrently with the delay of the decode process , which , as described above , reduces or eliminates the impact of the “ buffer enable ” delay on memory access latency . a block 25 represents this operation . the decoded transaction is then evaluated to determine whether the transaction is a memory transaction . in one embodiment , buffer control circuit 14 determines whether the transaction is a memory transaction by determining whether the decoded address is within an address range allocated to memory . a block 26 represents this operation . if the transaction is a memory transaction , memory controller 12 performs the memory transaction as represented by a block 27 . buffers 16 are then disabled . in one embodiment , buffer controller circuit 14 disables the buffers by de - asserting the aforementioned enable signals . a block 28 represents this operation . however , if in block 26 the transaction is determined to be a non - memory transaction ( e . g ., a pci transaction ), the transaction is handled by the targeted agent as represented by a block 29 . for example , memory controller 12 can ignore the transaction , which will also be received by the targeted agent , thereby allowing the target agent to perform the transaction . the operational flow then returns to block 21 , with buffers 16 being disabled . [ 0025 ] fig3 illustrates a portion of memory controller 12 ( fig1 ), according to one embodiment of the present invention . in this embodiment , memory controller 12 includes a transaction store 31 and a decoder 32 . in addition , buffer control circuit 14 ( fig1 ) includes a logic circuit 33 . in this embodiment , transaction store 31 stores transactions received from system bus 18 . in one embodiment , transaction store 31 is implemented with a register . decoder 32 determines , as one of its functions , the targeted agent of a received transaction . in one embodiment , decoder 32 is substantially similar to transaction decoders used in existing memory controllers . in this embodiment , logic circuit 33 includes standard logic gates to generate the enable signals provided to buffers 16 with the desired timing . transaction store 31 is connected to receive transactions from system bus 18 . decoder 32 is connected to the output port of transaction store 31 . in addition to buffers 16 , logic circuit 33 is connected to an output port of decoder 32 . further , in this embodiment , logic circuit 33 is connected to monitor transactions received by transaction store 31 . as previously described , buffers 16 have output leads connected to memory bus 17 . the operation of this embodiment of memory controller 12 in enabling buffers 16 is described below in conjunction with fig4 . [ 0028 ] fig4 illustrates the operational flow of memory controller 12 ( fig3 ) in enabling its memory interface buffers , according to one embodiment of the present invention . referring to fig3 and 4 , this embodiment of memory controller 12 operates as follows . this embodiment of memory controller 12 operates in general as described above in conjunction with fig2 with block 24 being described in more detail . although previously described , blocks 21 , 22 and 24 - 29 are described again to include the interactions with the elements of fig3 . memory controller 12 performs blocks 21 and 22 to monitor and detect transactions being sent over the system bus . in this embodiment , logic circuit 33 of memory controller 12 monitors system bus 18 to detect transactions . if logic circuit 33 does not detect a transaction in block 22 , the operational flow returns to block 21 . however in this embodiment , if logic circuit 33 does detect a transaction , logic circuit 33 asserts enable signals provided to buffers 16 . the asserted enable signals enables the buffers as described above for block 24 . a block 41 represents this operation . in addition , the transaction is received by the memory controller . in this embodiment , transaction store 31 receives and stores the transaction . a block 42 represents this operation . blocks 41 and 42 of this embodiment are operations of block 24 ( fig1 ). although block 42 is shown in fig4 as being performed after block 41 , in practice block 42 may be performed before or concurrently with block 41 . as previously described , because buffers 16 are enabled before the transaction is decoded ; the buffers are enabled before they are needed to drive signals on memory bus 17 . thus , the latency effects of the aforementioned “ buffer enable ” delay can be significantly reduced or even eliminated for memory accesses . memory controller 12 then performs block 25 to decode the received transaction . in this embodiment , decoder 32 of memory controller 12 decodes the transaction , which includes determining the “ target agent ” of the transaction . memory controller 12 then performs block 26 to determine whether the transaction is a memory transaction . in this embodiment , decoder 32 determines the targeted agent of the transaction . if the transaction is a memory transaction , memory controller 12 performs block 27 . in one embodiment , memory controller 12 performs the memory transaction using circuitry ( not shown ) similar to that in existing memory controllers . then memory controller 12 performs block 28 to disable buffers 16 . in this embodiment , logic circuit 33 disables the buffers by de - asserting the aforementioned enable signals . however , if in block 26 the transaction is not a memory transaction , memory controller 12 performs block 29 , allowing the targeted agent to handle the transaction . in one embodiment , memory controller 12 simply ignores the non - memory transaction . the operational flow then proceeds to block 21 , with buffers 16 remaining disabled . although block 28 is shown as being performed after block 29 under these circumstances , in some embodiments block 28 is performed before or concurrently with block 29 . [ 0038 ] fig5 illustrates a portion of memory controller 12 ( fig1 ), according to another embodiment of the present invention . this embodiment is similar to the embodiment of fig3 except that the transaction store is implemented as a queue or pipeline and the buffer control circuit includes a memory transaction detector connected to monitor transaction via the transaction store instead of directly . more particularly , in this embodiment , memory controller 12 includes a transaction queue 31 a and decoder 32 . in addition , buffer control circuit 14 ( fig1 ) includes a logic circuit 33 a and a memory transaction detector 51 . in one embodiment , memory transaction detector 51 is implemented as a decoder configured to decode only the address signals needed determine whether the transaction is a memory transaction . in this embodiment , transaction queue 31 a stores multiple transactions received from system bus 18 . in one embodiment , transaction queue 31 a is implemented with a fifo ( first in first out ) buffer . decoder 32 operates as described above in conjunction with fig3 . logic circuit 33 a is used in generating the enable signals provided to buffers 16 , responsive to the output signal of memory transaction detector 51 . transaction queue 31 a is connected to receive transactions from system bus 18 . in addition , transaction queue 31 a is connected to decoder 32 and to memory transaction detector 51 . memory transaction detector 51 is connected to logic circuit 33 a , which in turn is connected to buffers 16 . the operation of this embodiment of memory controller 12 in enabling buffers 16 is described below in conjunction with fig6 . [ 0041 ] fig6 illustrates the operation of memory controller 12 ( fig5 ) in enabling its memory interface buffers , according to one embodiment of the present invention . referring to fig5 and 6 , this embodiment of memory controller 12 operates as follows . memory controller 12 performs blocks 21 and 22 to monitor and detect transactions being sent over the system bus . in this embodiment , transaction queue 31 a of memory controller 12 monitors system bus 18 to detect transactions . if transaction queue 31 a does not detect a transaction in block 22 , the operational flow returns to block 21 . however in this embodiment , if transaction queue 31 a does detect a transaction , transaction queue 31 a receives and stores the transaction . transaction queue 31 a can store more than one transaction . a block 61 represents this operation . memory controller 12 then performs block 25 to decode a transaction stored in transaction queue 31 a . more particularly , decoder 32 receives the “ oldest ” transaction stored in the transaction queue and decodes it as previously described . memory controller 12 then performs block 26 to determine whether the transaction is a memory transaction . in this embodiment , decoder 32 determines the targeted agent of the transaction . in the transaction is not a memory transaction , memory controller performs block 29 ( as described above ) and the operational flow returns to block 21 . however , if the transaction is a memory transaction , memory controller 12 determines whether buffers 16 are enabled . in this embodiment , logic circuit 33 a determines whether these buffers are enabled . a block 62 represents this operation . if the buffers are not enabled , memory controller 12 performs block 41 ( described above ) to enable the buffers . in this embodiment , logic circuit 33 a asserts the enable signals to enable buffers 16 . in one embodiment , memory controller 12 enables the buffers as previously described in conjunction with fig4 by monitoring transaction queue 31 a . after the buffers are enabled ( either after performing block 41 or if the buffers were already enabled as found in block 62 ), memory controller 12 then receives the memory transaction from transaction queue 31 a , as represented by a block 63 . in this embodiment , decoder 32 receives the memory transaction from transaction queue 31 a . then memory controller 12 performs block 27 ( as described previously ) to execute the memory transaction . memory controller 12 then checks the contents of transaction queue 31 a and determines whether it contains any unexecuted memory transactions . in this embodiment , memory transaction detector 51 checks each transaction stored in transaction queue 31 a to determine whether the transaction is a memory transaction . in one embodiment , memory transaction detector 51 provides a signal to logic circuit 33 a that indicates whether transaction queue 31 a contains a memory transaction . blocks 64 and 65 represent these operations . in some embodiments , memory transaction detector 51 can be configured to check a subset of the transactions stored in transaction queue 31 a rather than all of the transactions . for example , only the next transaction ( or some small number of transactions ) to be performed is checked in one embodiment . this embodiment may be advantageous for relatively large transaction queues by allowing the buffers to be disabled if the next few transactions in the queue are non - memory transactions . if transaction queue 31 a does not contain a memory transaction , memory controller 12 performs block 28 to disable buffers 16 . in this embodiment , logic circuit 33 a receives the output signal from memory transaction detector 51 and if the signal indicates that there are no pending memory transaction , logic circuit 33 a de - asserts the enable signals . however , if transaction queue 31 a does contain a memory transaction , the operational flow returns to block 63 to receive the next transaction ( which need not be a memory transaction ) from transaction queue 31 a , leaving buffers 16 enabled . [ 0052 ] fig7 illustrates the operation of memory controller 12 ( fig5 ), according to another embodiment of the present invention . referring to fig5 and 7 , memory controller 12 operates as follows to enable buffers 16 . the transactions received and stored by memory controller 12 are monitored for memory transactions . in one embodiment , memory transaction detector 51 monitors the contents of transaction queue 31 a for transactions . a block 71 represents this operation . the stored transactions are then checked to determine whether any are memory transactions . in one embodiment , memory transaction detector 51 decodes a stored transaction to determine whether it is a memory transaction . for example , memory transaction detector 51 may be configured to determine whether the transaction to be outputted by transaction queue 31 a during the next cycle is a memory transaction . a block 72 represents this operation . if the transaction checked in block 72 is not a memory transaction , the operational flow returns to block 71 . however , if the transaction is a memory transaction , block 41 is performed as described above to enable the buffers . in this embodiment , memory transaction detector 51 provides a signal to logic circuit 33 a to assert the enable signals provided to buffers 16 . memory controller 12 then performs block 25 to decode a transaction stored in transaction queue 31 a . more particularly , decoder 32 receives the “ oldest ” transaction stored in the transaction queue and decodes it as previously described . memory controller 12 then performs block 26 to determine whether this transaction is a memory transaction . in this embodiment , decoder 32 determines this targeted agent of the transaction to determine whether the transaction is a memory transaction . if this transaction is a memory transaction , memory controller 12 performs block 27 as previously described to execute the memory transaction and then block 28 to disable buffers 16 . in this embodiment , logic circuit 33 a de - asserts the enable signals to disable buffers 16 . however , if the transaction is not a memory transaction , memory controller 12 performs block 29 as previously described , allowing the targeted agent to perform the transaction . 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 , the 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 in one or more embodiments . in addition , embodiments of the present description may be implemented not only within a semiconductor chip but also within machine - readable media . for example , the designs described above may be stored upon and / or embedded within machine readable media associated with a design tool used for designing semiconductor devices . examples include a netlist formatted in the vhsic hardware description language ( vhdl ) language , verilog language or spice language . some netlist examples include : a behavioral level netlist , a register transfer level ( rtl ) netlist , a gate level netlist and a transistor level netlist . machine - readable media also include media having layout information such as a gds - ii file . furthermore , netlist files or other machine - readable media for semiconductor chip design may be used in a simulation environment to perform the methods of the teachings described above . thus , embodiments of this invention may be used as or to support a software program executed upon some form of processing core ( such as the cpu of a computer ) or otherwise implemented or realized upon or within a machine - readable medium . a machine - readable medium includes any mechanism for storing or transmitting information in a form readable by a machine ( e . g ., a computer ). for example , a machine - readable medium can include such as a read only memory ( rom ); a random access memory ( ram ); a magnetic disk storage media ; an optical storage media ; and a flash memory device , etc . in addition , a machine - readable medium can include propagated signals such as electrical , optical , acoustical or other form of propagated signals ( e . g ., carrier waves , infrared signals , digital signals , etc .). although the present invention has been described in connection with a preferred form of practicing it and modifications thereto , those of ordinary skill in the art will understand that many other modifications can be made to the invention within the scope of the claims that follow . accordingly , it is not intended that the scope of the invention in any way be limited by the above description , but instead be determined entirely by reference to the claims that follow .
6
as required , detailed embodiments of the present invention are disclosed herein ; however , it is to be understood that the disclosed embodiments are merely exemplary of the invention , which may be embodied in various forms . therefore , specific structural and functional details disclosed herein are not to be interpreted as limiting , but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed structure . referring to the drawings in more detail , the reference numeral 1 generally designates a reminder device which embodies the present invention . the apparatus 1 generally includes a housing 2 including a logo plate or lens 3 overlaid on an electronic display device or light source 4 ( fig4 ) and a timer or timer circuit 5 . the timer circuit 5 is adapted to provide a display activation signal to the light source 4 after a set interval to illuminate or call attention to the logo plate 3 , to thereby provide a reminder to use a product of a brand associated with the logo plate 3 or otherwise engage in some activity associated with a brand or entity identified on the logo plate 3 . the housing 2 may be formed of a plastic and of a size to contain circuitry 8 of the apparatus 1 . in the embodiment shown , the logo plate 3 forms a front wall of the housing 2 . preferably , the logo plate 3 has logo indicia 10 ( fig1 ) formed thereon which is of such a nature as to have a different appearance when the display device 4 is activated . for example , the logo indicia 10 could be transparent regions of the logo plate 3 . alternatively , the logo indicia 10 may simply be imprinted on the plate 3 with portions of the plate 3 being either transparent or translucent , such that light emitted from the light source 4 is visible through the logo plate 3 . the logo indicia 10 may be an actual trademark design or logo 11 or may be text letters forming a brand name of the product or service associated with the apparatus 1 . in addition to a trademark , the logo indicia could be a trade name , service mark , collective membership mark , or the name of an entity such as a corporation , association or club relative to which some activity is to be performed or taken at a preset time period or interval . it is also forseen that a generic name for the product could be used in association with the logo . referring to fig4 the timer circuit 5 may be any of a number of digital counter / timer circuits which may be programmed to count a selected number of clocked cycles and to output a signal state when the target count is reached . the signal state persists until a reset switch 12 is operated , which re - initiates the timer circuit 5 . the output signal state can be used to activate the display device 4 , either directly or through an external driver ( not shown ). the timer circuit 5 may be preprogrammed for a timer cycle which is appropriate for the activity associated with the logo indicia 10 . alternatively , the timer circuit 5 may by adapted to be user programmable , with the provision of appropriate programming switches ( not shown ). the circuitry 8 may incorporate a test switch 14 which causes the timer circuit 5 to activate the display device 4 ( i . e . activate the light source ) until the reset switch 12 is operated or until a test interval times out . the circuitry 8 may also incorporate a sounder device 18 which is activated when the timer circuit 5 activates the display device 4 . the sounder 18 may be a very low power type of sounder which produces chirping or clicking type sounds , such as are used on some types of personal digital assistants , pda &# 39 ; s . the logo display device 4 may be one or more light emitting diodes ( led &# 39 ; s ), a plasma display , a liquid crystal display ( lcd ) or the like . preferably , the display device 4 is a low power consumption device to preserve the life of a battery 16 which powers the timer circuit 5 , the sounder 18 if present , and the display device 4 . although the display device 4 is shown as positioned behind the lens 3 and visible through the logo indicia 10 , alternatively , it may be positioned adjacent the logo indicia 10 . either way , activation of the display device 4 calls visual attention to the logo indicia 10 , to thereby remind the owner to utilize a product of a brand associated with the logo indicia 10 . preferably , the battery 16 is a small , but efficient type of battery , such as certain types of lithium - ion batteries which are available in “ button ” sizes . referring to fig2 the circuitry 8 is positioned within the housing 2 . the reset switch 12 and the test switch 14 are accessible on a rear wall 20 of the housing 2 . a battery access panel 22 may also be provided on the rear wall , to replace the battery 16 as necessary . the apparatus 1 includes a mechanism for positioning it in a conspicuous location . the illustrated apparatus 1 includes one or more magnets 24 for magnetically securing the housing 2 in a convenient location , such as on a refrigerator 26 ( fig3 ) or other appliance , a metal cabinet of a kitchen , a computer case , or the like which is conspicuous to the user . alternatively , the magnets 24 could be replaced by some other securing mechanism , such as a strip of hook and loop fastener , a double sided adhesive strip , a key ring , or the like . the apparatus 1 is preferrably provided by the manufacturer of the product with which the logo 11 is associated with the timer circuit 5 preprogrammed for a timer cycle appropriate for the associated product . when the product is used for the first time , the reset switch 12 is operated to initiate operation of the timer circuit 5 . the apparatus 1 is placed in a conspicuous location , such as on a refrigerator 26 , using the magnets 24 . the timer circuit 5 may be programmed so that the test switch 14 can be operated at any time without interrupting a timer cycle in progress . when the time cycle completes , the timer circuit 5 applies a display or illumination enable signal to the display device 4 to activate it and illuminate or otherwise call visual attention to the logo 11 . a sounder 18 may also be activated . the display enable signal preferably persists until the reset switch 12 is again operated , at which time , the timer circuit 5 re - initiates the timer cycle . although the reminder apparatus 1 has been described with reference to administration of medications , it is not intended to be limited to such activity . the apparatus 1 may also be applied to any other activity which is associated with a manufacturer , organization , or other entity having a known brand or name . for example , an organization can have the apparatus 1 manufactured with their organization name applied as the logo 11 to remind a member of the organization to attend a bi - weekly or monthly meeting , or to pay their dues , or the like . further , the reminder could be supplied by an entity which performs routine maintenance services , to remind the user when to contact the service provider the next time the service should be performed . for example , a business which performs automobile oil changes could provide a reminder device 1 with its logo 10 wherein the timer was programmed to activate the display device or light source 4 at the recommended interval for having an oil change ( such as every three months ). it is also foreseen that the apparatus could be constructed without the timer or timer circuit , to instead provide a device which can be selectively activated to light up a logo and activate a sounder in response to pressing a button or upon detection of motion in past the apparatus or by other activation means now known or later developed . it is to be understood that while certain forms of the present invention have been illustrated and described herein , it is not to be limited to the specific forms or arrangement of parts described and shown .
6
referring now to the drawings in detail , and first to fig1 thereof , it may be seen that the reference numeral 1 has been used to designate a hollow axially elongated and cylindrical housing . a ram 3 is received in the interior of the housing component 1 and can slide up and down therein , being movable by conventional reciprocating means ( not shown ). the interior of the housing 1 is filled with a gas , such as air . the gas which is displaced during movement of ram 3 can flow through axially elongated channels 5 which are provided in the walls of the housing 1 . the housing 1 is affixed , on its non - illustrated upper end , to a carrier rope or the like so as to be suspended therefrom and to be able to follow the downward movement of a pile 6 . in this embodiment of the invention , the pile 6 is of a tubular configuration . an impact - transmitting ram follower 7 is arranged between the pile 6 and the impacting body 3 . the upper portion of the ram follower 7 is surrounded by the lower portion of the housing 1 . an annular striking surface 8 of the ram follower 7 abuts the upper end face of the free uppermost end of the tubular pile 6 . the ram follower 7 is of a unitary construction , and has a plurality of cylindrical sections of different diameters . the ram follower 7 also has an annular horizontal ledge surface 9 intermediate its top and bottom , on the top of one of the cylindrical sections . the cylindrical housing 1 carries on , on its inner surface , and below the path of reciprocation of ram 3 relative to the housing 1 , a radially inwardly projecting annular flange 53 . furthermore , the housing 1 includes two cylindrical surfaces 11 and 12 which are arranged underneath annular flange 53 and are separated from one another by annular shoulder 13 . the lower cylindrical surface 12 has a diameter which exceeds that of the upper cylindrical surface 11 . a hollow , generally cylindrical piston 16 is guided along the cylindrical surfaces 11 and 12 for limited displacement along the axis of housing 1 . piston 16 has an upwardly facing annular shoulder 17 located at its bottom , and is displaceable between a lower abutment projection 15 provided at the inner surface of the housing component 1 , an an upper abutment projection 14 which cooperates with the top of piston 16 . an annular hollow space or compartment 20 is bounded between piston 16 and the lower cylindrical surface 12 , the height of the compartment 20 being determined by the distance between the annular shoulders 13 and 17 . in this first embodiment illustrated in fig1 the compartment 20 continues upwardly into the annular flange 53 of the housing 1 from shoulder 17 of piston 16 . the upper end of compartment 20 jogs outwardly above shoulder 13 and communicates with a pressure medium channel 29 which incorporates a closing valve 30 . the pressure medium channel 29 communicates , through a conduit 48 and a switching valve 49 , with a pressure medium pump 50 . liquid and gas are introduced within compartment 20 to form a liquid cushion 28 at the bottom and gas cushion 27 located above the liquid cushion . the pressure in compartment 20 can be controlled by the controlled admission of fluid and / or gas into compartment 20 , under such conditions of pressure and volume as will adapt the properties of the gas and liquid to the particular requirements of any specific application . toroidal seals 18 and 19 are arranged between cylindrical surfaces 11 and 12 and those outer surfaces of the piston 16 which cooperate therewith , to seal the liquid and gas within compartment 20 . the piston 16 is normally pressed by the superatmospheric pressure prevailing in the compartment 20 against support surface 9 . when the circular ramming surface 4 at the bottom of the ram 3 strikes a corresponding circular struck surface 36 located at the top of ram follower 7 during operation , the energy of the impact is transmitted directly to the pile 6 by the annular striking surface 8 which is provided on the bottom of ram follower 7 . the recoil ( which may be very pronounced , especially when the pile 6 has a substantial length ) is transmitted from the pile 6 via striking surface 8 to the ram follower 7 . the support surface 9 of ram follower 7 , which abuts the radially outermost surface of shoulder 17 on the annular piston 16 , forces the piston upwardly against the superatmospheric pressure of the gas cushion 27 inside compartment 20 . inasmuch as the liquid cushion 28 also contained in the compartment 20 is as a practical matter , incompressible , the volume reduction of the compartment 20 which results from lifting of the piston 16 proportionally increases the pressure of the gas cushion 27 as a function of the displacement of piston 16 . thus , piston 16 can be moved upwardly by the energy of the recoil only until equilibrium between the upwardly directed recoil force and the downwardly directed force exerted by the gas cushion has been established . by adjusting the initial superatmospheric pressure in the compartment 20 to correspond to the recoil forces which are to be expected ( based , inter alia , on the dimensions of pile 6 , the characteristics of the pile driver , and the resistance of the earth strata into which the pile 6 is to be driven ) it is possible to protect the housing from destruction caused by recoil by absorbing recoil energy in the gas cushion . in this manner , an increased lifespan of the pile driver is obtained and the wall thickness and thus the transverse dimensions of the housing 1 can be reduced , which further results in reduction of cost , material consumption , and weight . inasmuch as the piston 16 need have only small radial thickness , and inasmuch as compartment 20 is situated at that inner circumferential region of housing 1 which corresponds to the annular shoulder 17 of the piston 16 , and inasmuch as compartment 20 may be vertically elongated as needed , it is not necessary to increase the exterior diameter of the housing 1 beyond those dimensions which are required in order to accommodate the ram 3 . the housing 1 is preferably cylindrical and the diameter thereof need be only slightly larger than the diameter of the ram 3 and , most advantageously , it may correspond to the exterior diameter of the tubular pile 6 to be driven . fig2 shows a second embodiment of the present invention which in principle corresponds to the first embodiment disclosed . however , in this second embodiment , bores 21 are used instead of surfaces 11 and 12 . the bores are located in an annular flange 51 which projects radially inwardly from the cylindrical internal surface of housing 1 , and are uniformly spaced along the circumference of flange 51 and are oriented parallel to the longitudinal axis of the housing 1 . a vertically elongated piston 23 with an enlarged head at its top is received in each of the bores 21 for limited vertical movement therein and bounds the bottom of a compartment 26 in each bore . each bore 21 is formed with an annular step 22 which cooperates with an annular collar 24 of the piston 23 to limit the downward movement of the piston 23 within the bore . furthermore , a toroidal seal 25 is so provided on the head of piston 23 as to press against the surface which bounds the bore 21 . the lower end face of each of the pistons 23 cooperates with the annular support surface 9 of ram follower 7 . again , liquid and gas are contained in compartment 26 to form an upper gas cushion 27 and a lower cushion 28 . the top of compartment 26 communicates with a pressure - medium channel 29 which is equipped with a closing valve 30 . thus , as before the liquid cushion 28 and the gas cushion 27 can be brought to that superatmospheric pressure which is proper , considering the particular pile 6 to be driven and the strata resistance encountered , by introducing liquid and / or gas under pressure into the compartment 26 through the pressurized medium channel 29 . inasmuch as the bores 21 which accommodate the pistons 23 are spaced uniformly around the periphery of the housing 1 , and inasmuch as the lower end faces of the pistons 23 are likewise pressed uniformly against the support surface 9 of the ram follower 7 , the pistons 23 will be substantially uniformly forced upwardly against the pressurized contents of compartments 26 during the resilient recoil of the pile 6 which occurs immediately after the pile 6 has been driven downwardly by ram follower 7 . as before , upward movement of the pistons 23 reduces the volumes of compartments 26 and causes the pressure within the compartments 26 to rise , until equilibrium is established and the recoil shock is absorbed by the gas . in this second embodiment , the compartments 26 can communicate with one another through conventional passageways ( not shown ), equalizing the pressure in all the compartments . since flange 51 extends radially inwardly from the cylindrical internal surface of the housing 1 , below ram 3 and above ram follower 7 to the periphery of ram follower 7 , no increase in internal diameter of housing 1 is necessary , and housing 1 can again have an external diameter which is only slightly larger than ram 3 and ram follower 7 . thus , the outer diameter of the housing 1 only slighly exceeds the diameter of the tubular pile 6 , so that the housing 1 of the pile drive can follow the top end of the pile 6 through any pile guides which may surround the pile 6 during driving . a third embodiment of the invention is illustrated in fig3 of the drawing , wherein the ram follower 7 ( which is arranged between the top end of the pile 6 and the ram 3 ) is received in a hollow cylindrical housing 1 for reciprocation , is provided with a well 31 which has an annular step 32 and is coaxially with the axes of ram follower 7 and housing 1 . an impact piston 33 provided with a corresponding annular collar is slidable within well 31 along a limited vertical distance . the circular ramming surface 4 which is located at the lower end of ram 3 will , during ramming , strike the circular end face 34 of the impact piston 33 and the annular top surface of ram follower 7 which surrounds the piston . a toroidal seal 35 is arranged between the impact piston 33 and the surface bounding the well 31 . the impact piston 33 partially bounds a chamber which is coaxially arranged within the ram follower 7 . as before , a lower liquid cushion 38 and an upper gas cushion 37 are accommodated within the chamber and the well 31 . an upwardly extending pressure medium channel 39 is provided , which is closed by a closing valve 40 . the ram follower 7 again has an annular support surface 9 which is formed by an annular shoulder provided near upper end of the ram follower 7 . the ram follower 7 is further provided , in that outer peripheral region which is bounded by the support surface 9 , with a plurality of vertically elongated bores 41 which are spaced uniformly around the circumference of support surface 9 . each of the bores 41 has a radially extending annular step 42 intermediate its top and bottom . a substantially cylindrical piston 43 is accommodated in each of the bores 41 for limited vertical movement therein and is provided at its lower end with an annular collar 44 to limit such motion . a toroidal seal 45 is arranged between the piston 43 and the surface bounding the bore 41 . the piston 43 partially bounds a compartment 46 , each of the compartments 46 being in communication , through a connecting channel 47 , with the chamber and the well 31 . as a result of the superatmospheric pressure within the bore 31 , the chamber , the connecting channels 47 and the compartments 46 , all the pistons 43 are pressed upwardly . an annular flange 52 extends radially inwardly from the cylindrical interior surface of housing 1 between ram 3 and support surface 9 of ram follower 7 . the annular flange 52 is provided , at its lower face , with an annular support surface 10 which is abutted by the upper end faces at the tops of pistons 43 . the impact piston 33 is urged by the superatmospheric pressure of the gas cushion 37 into its extended position in which the annular collar 44 abuts the annular step 32 . in this extended position , the upper end face 34 of the impact piston 33 is located approximately 3 to 30 millimeters above the impact surface 36 of ram follower 7 . during its downward movement , the ram 3 first hits the upper end face 34 of the impact piston 33 and shifts the impact piston 33 downwardly so that the volume of the gas cushion 37 contained in the chamber of the bore 31 is reduced . subsequently , the ramming surface 4 of the ram 3 hits the annular impact surface 36 of the follower 7 , and the resulting hard metal - to - metal impact is directly transmitted to the pile 6 via the annular striking surface 8 located at the lower end of the ram follower 7 . the pile 6 which is set in motion by this impact will be kept in motion by additional increased pressure obtained during the pushing of the impact piston 33 into the well 31 , so that the impact piston 33 reassumes its extended position relative to the ram follower 7 in which it abuts the annular step 32 . the recoil which originates in the pile 6 and which is transmitted via the annular striking surface 8 to the ram follower 7 , causes the ram follower 7 to move upwardly with respect to the pistons 43 which press against the support surface 10 of the housing component 1 . thus , liquid is expelled from compartments 46 into the chamber and the well 31 , which results in a reduction in the volume of , and a corresponding increase in the pressure in , the gas cushion 37 . in this manner , the recoil is absorbed without subjecting the housing component 1 to recoil shock . when the number of pistons 43 , individual cross - sectional areas of the pistons 43 relative to the cross - sectional area of the impact piston 33 , and the adjusted superatmospheric pressure of the gas cushion 37 , are properly selected , two desirable results can be achieved . first , the recoil is absorbed and the housing thereby protected . next , the great impact of the ram 3 on the impact surface 36 of ram follower 7 loosens the pile 6 , and the prolonged force applied to the pile thereafter increases the actual movement of the pile . in all embodiments , the exterior diameter of the housing 1 will not exceed the exterior diameter of the pile by more than 10 %. it will be understood that each of the elements described above , or two or more together , may also find a useful application in other types of constructions differing from the types described above . while the invention has been illustrated and described as embodied in an arrangement for driving large - diameter , tubular piles , it is not intended to be limited to the details shown , since various modifications and structural changes may be made without departing in any way from the spirit of the present invention . so , for instance , the pressure of the respective gas cushion can be adjusted to the respective pile - driving conditions even during the operation of the arrangement by a corresponding control of the respective closing valve and of the pressure of the fluid admitted therethrough . without further analysis , the foregoing will so fully reveal the gist of the present invention that others can by applying current knowledge readily adapt it for various applications without omitting features that , from the standpoint of prior art , fairly constitute essential characteristics of the generic or specific aspects of this invention .
4
with reference now to the accompanying figures and the following detailed description , an apparatus and method for uniformly heating an aircraft structure 10 to provide a uniform temperature in this structure for repairing the structure is disclosed . in fig1 and 2 , the aircraft structure 10 includes a left hand composite laminate 12 and a right hand composite laminate 14 separated by an aluminum heat sink 16 . the laminates 12 and 14 and heat sink 16 rest on a composite base panel 18 . however , it will be understood that the present invention need not use a heat sink 16 and the laminate or laminates being repaired can be of any configuration . lying atop the laminates 12 and 14 and heat sink 16 is a graphite fiber blanket 20 having highly conductive pitch graphite fibers . lying atop the blanket 20 is a silicone rubber heat blanket 22 . blanket 22 is of the type commonly known in the industry that contains heater wires therein through which current can pass to provide heat to perform a repair on the laminates 12 and 14 . in the absence of the graphite fiber blanket 20 , as the laminates 12 and 14 are heated by the heat blanket 22 , the temperature distribution in the laminates and aluminum heat sink will vary considerably with time , as seen in fig3 . however , by use of the graphite fiber blanket 20 , the temperature distribution between the aluminum bar heat sink 16 and the laminates 12 and 14 and within the laminates is much more uniform , as seen in fig4 providing a much more uniform temperature throughout the laminates . in addition , the temperature rise of the entire aircraft structure is much quicker , providing for a faster and more uniform bonding of the repair material to the aircraft structure . the graphite fiber blanket transfers heat from hot spots to cold spots and assists in maintaining uniform temperature with resulting improved repair patch integrity . of course , after the repair is completed , the blanket 20 and silicone rubber heat blanket 22 are removed . the graphite fiber blanket 20 utilized is formed of the type of material discussed in u . s . pat . no . 5 , 316 , 080 , which patent is incorporated herein by reference in its entirety , which has a very high thermal conductivity , exceeding even that of copper . the thermal conductivity of the fibers can be , for example , about three times that of copper . one graphite fiber blanket 20 found usable in the process of the present invention is manufactured by amoco performance products , inc . as thermalgraph ™ fabric under the trademark thornel ®. both the thermalgraph ™ fabric ewc - 300x and the thermalgraph ™ fabric ewc - 500x have been found suitable . the test illustrated in fig4 was with ewc - 300x fabric . these materials are pitch fiber based high thermal conductivity woven fabrics . due to the orthotopic nature of the weave and the high longitudinal thermal conductivity of the fibers , biaxial thermal conductivity is achieved . the ewc - 300x is a plain weave fabric constructed from four - thousand filament continuous pitch tows . ewc - 500x is available as an eight harness satin weave fabric constructed from two - thousand filament continuous pitch tows . the ewc - 300x material has a count ( warp and fill ) of 11 × 10 tows per inch and a weight of 599 g per square meter . the fabric electrical resistivity ( warp and fill ) is 0 . 05 ω / sq . the density is 2 . 1 g per cubic centimeter and the yam electrical resistivity is 4 . 0 - 5 . 0 micro ohm meters . the estimated thermal conductivity is 200 - 300 w / m ° k . the ewc - 500x material has a count ( warp and fill ) of 20 × 20 tows per inch and a weight of 485 g per square meter . the thickness is 0 . 61 mm and the resistivity is 0 . 03 ω / sq . the density is 2 . 15 g per cubic centimeter and the yarn electrical resistivity is 2 . 3 to 2 . 8 micro ohm meters . the estimated thermal conductivity is 400 - 500 w / m ° k . in the preferred embodiment , a three - ply graphite fiber blanket 20 is formed composed of three plies of the ewc - 300x material stitched together . in the assembly illustrated in fig1 and 2 , the silicone rubber heat blanket 22 is a rectangle of 12 inches by 18 inches . the aluminum heat sink is a bar 5 / 16 inch thick by 21 / 2 inches wide by 18 inches long . with reference to fig1 - 5 , a modified blanket 50 will be described which incorporates graphite fiber such as used in blanket 20 and metal sheet . the blanket 50 is used in the same manner as blanket 20 , as illustrated in fig1 and 2 and is a substitute for blanket 20 . the blanket 50 can be used in the repair of aircraft structures of composites or metals . the metal sheet can be copper , silver , platinum or other high thermal density materials . with reference to fig5 one blanket 50 constructed in accordance with the teachings of the present invention is shown with the blanket 50 constructed with two sheets 52 and 54 of copper 0 . 016 inches thick ( 16 mils ), a single - ply sheet 56 of graphite fiber of thickness about 0 . 010 inches ( 10 mils ), two sheets 58 and 60 of copper 0 . 016 inches thick , a three - ply sheet 62 of graphite fiber of thickness about 0 . 030 inches ( 30 mils ), two sheets 64 and 66 of copper sheet 0 . 016 inches thick , a three - ply sheet 68 of graphite fiber of thickness about 0 . 030 inches ( 30 mils ), a single sheet 70 of copper sheet 0 . 016 inches thick , a three - ply sheet 72 of graphite fiber of thickness about 0 . 030 inches ( 30 mils ), and two sheets 74 and 76 of copper sheet 0 . 016 inches thick . the blanket is encased within a teflon ( polytetrafluoroethylene ) cover 78 having a thickness of 5 mils ( 0 . 005 inches ). the use of a metal in sheet form , such as copper , silver , platinum or other high thermal density material , provides the advantage of combining a relatively high thermal mass that , in conjunction with the high conductivity graphite fiber , provides uniform temperature in the aircraft structure for repair . the metal , such as copper , can have various forms . for example , it can be sheet ( generally considered to be of thickness 0 . 010 inches or more ), foil ( generally considered to be of thickness less than 0 . 010 inches ), braid , or mesh . for purposes of the application , including the claims , sheet will refer collectively to sheet , foil , braid or mesh . the metal , such as copper , not only acts to distribute thermal energy , but also as a thermal storage medium as a reservoir of thermal energy . the metal sheet will preferably have sufficient thickness to add to the performance of the blanket 50 , but will not be so thick as to be too heavy or inflexible as many of the structures to be repaired have a curvature and it is desirable for the blanket 50 to conform to the surface of the structure being repaired . for copper , it is expected that a range of thickness between about 0 . 008 inches ( 8 mils ) and about 0 . 020 inches ( 20 mils ) would be satisfactory . of course , if the surface of the structure to be repaired is flat , flexibility of blanket 50 is not critical and the thickness of the metal sheets can be any thickness desired . it is preferable to encase the modified blanket 50 within a teflon ( polytetrafluoroethylene ) cover 78 . the teflon ( polytetrafluoroethylene ) does not bond to the resins used in the repair and is capable of withstanding the temperature of repair , typically 350 to 500 ° f . if a kapton ( polyimide resin in the form of a film ) cover is used in substitution for teflon ( polytetrafluoroethylene ) cover 78 , repair temperatures up to about 700 ° can be employed . the three - ply graphite fiber material is preferably stitched together in the z ( thickness ) direction . any number of layers of graphite fiber and metal sheet can be used . the sheets of the blanket 50 , such as sheets 52 - 78 , can be secured together at a single center tie point for ease of handling but are preferably not otherwise secured together . although a single embodiment of the invention has been illustrated and described with numerous specific details in the forgoing description and accompanying drawings , it will be understood that the invention is not limited to the embodiment disclosed , but is capable of numerous rearrangements , modifications and substitutions of parts and elements without department from the spirit and scope of the invention .
1
referring to fig1 and fig2 , fig1 illustrates the structure of a light source system according to a first embodiment of the present invention , and fig2 is a front view of the wavelength conversion device and the color filter device in the light source system shown in fig1 . as show in fig1 , the light source system in this embodiment mainly includes an excitation light source 101 , a dichroic mirror 102 , a minor 104 , lenses 103 and 105 , a wavelength conversion device 106 , a color filter device 107 , a driving device 108 and a light homogenization device 109 . the excitation light source 101 is for generating an excitation light . in this embodiment , the excitation light source 101 is ultraviolet or near - ultraviolet laser diode or ultraviolet or near - ultraviolet light emitting diode , in order to generate ultraviolet or near - ultraviolet excitation light . as show in fig2 , the wavelength conversion device 106 has a ring structure , including at least one wavelength conversion area . in the present embodiment , the wavelength conversion device 106 includes a red wavelength conversion area , a green wavelength conversion area , a blue wavelength conversion area and a yellow wavelength conversion area , which are provided in circumferential subsections of the ring structure . different wavelength conversion materials are coated on the wavelength conversion areas respectively ( for example , phosphor materials or nanomaterials ). the wavelength conversion materials can convert the ultraviolet or near - ultraviolet excitation light that illuminate them into the converted light of corresponding color . specifically , the red wavelength conversion area converts the ultraviolet or near - ultraviolet excitation light incident to it into red converted light , the green wavelength conversion area converts the ultraviolet or near - ultraviolet excitation light incident to it into green converted light , the blue wavelength conversion area converts the ultraviolet or near - ultraviolet excitation light incident to it into blue converted light , and the yellow wavelength conversion area converts the ultraviolet or near - ultraviolet excitation light incident to it into yellow converted light . in the present embodiment , a reflective substrate is provided under the wavelength conversion materials in order to reflect the converted light generated by the wavelength conversion materials , so that the exit direction of the converted light output from the wavelength conversion area is opposite to the incident direction of the excitation light incident to the wavelength conversion area . as show in fig2 , the color filter device 107 has a ring structure , coaxially fixed with the wavelength conversion device 106 , and disposed outside the ring of the wavelength conversion device 106 . in other embodiments , the color filter device 107 can also be disposed inside the ring of the wavelength conversion device 106 . the color filter device 107 includes at least one color filter area . in the present embodiment , the color filter device 107 includes a red filter area , a green filter area , a blue filter area and a yellow filter area , which are provided in circumferential subsections of the ring structure . each color filter area corresponds to a wavelength conversion area of the wavelength conversion device 106 . in the present embodiment , the color filter area and the wavelength conversion area of the same color are set at a 180 - degree angle from each other with respect to the center of the ring structures of the wavelength conversion device 106 and the color filter device 107 . the different color filter areas have different spectral responses , and filter the converted light of corresponding colors , in order to improve the color purity of the converted lights . of course , the color filter area and the wavelength conversion area of the same color can be set at angles with respect to the center of the ring structures of the wavelength conversion device 106 and the color filter device 107 . as show in fig1 , the driving device 108 is a rotary device which has a rotary shaft 1081 , for example , a rotary motor . the wavelength conversion device 106 and the color filter device 107 are coaxially fixed on the rotary shaft 1081 , and rotate synchronously under the driving of the rotary shaft 1081 . in the working process of the light source system 100 shown in fig1 , the ultraviolet or near - ultraviolet excitation light generated by the excitation light source 101 is transmitted through the dichroic mirror 102 , converged by the lens 103 , incident on the wavelength conversion device 106 , to form a light spot 101 a on the wavelength conversion device 106 as shown in fig2 . the wavelength conversion device 106 and the color filter device 107 rotate synchronously under the driving of the driving device 108 , so that the wavelength conversion areas of the wavelength conversion device 106 and the color filter areas of the color filter device 107 can rotate synchronously . when the wavelength conversion device 106 and the color filter device 107 rotate , the wavelength conversion areas of the wavelength conversion device 106 are disposed in the propagation path of the ultraviolet or near - ultraviolet excitation light generated by the excitation light source 101 sequentially and periodically , so that the ultraviolet or near - ultraviolet excitation light can be converted into the converted light of different colors sequentially by the respective wavelength conversion areas . the converted lights of different colors are further reflected by the wavelength conversion areas respectively , guided by the first optical assembly which is composed of lenses 103 and 105 , dichroic minor 102 , and reflecting minor 104 , then incident on the light filer device 107 and form a light spot 101 b as shown in fig2 . in the first optical assembly , the lenses 103 and 105 are used for collecting and condensing the converted light respectively , so that the divergence angle of the converted light can be decreased . the dichroic minor 102 and the reflecting minor 104 are used for reflecting the converted light , so that the propagation direction of the converted light can be changed . in the present embodiment , the dichroic mirror 102 and the reflecting mirror 104 are set at a 90 - degree angle to each other and 45 - degree angle to the incident direction of the converted light . in the present embodiment , because of the reflection of the dichroic minor 102 and the reflecting minor 104 , the propagation direction of the converted light is shifted by a predetermined distance and inverted by 180 - degree angle , and the light spot 101 a is set at 180 - degree angle to the light spot 101 b with respect to the center of the ring structures of the wavelength conversion device 106 and the color filter device 107 . in this case , the wavelength conversion device 106 is fixed with respect to the color filter device 107 , and the wavelength conversion areas of the wavelength conversion device 106 and the color filter areas of the color filter device 107 with the same colors are set at 180 - degree angle from each other with respect to the center of the ring structures of the wavelength conversion device 106 and the color filter device 107 and rotate synchronously , so that the converted light of different colors generated by the wavelength conversion areas of the wavelength conversion device 106 are incident on the color filter areas of the color filter device 107 with the same colors after they pass through the dichroic minor 102 and the reflecting mirror 104 , and the color purity is improved by the color filter area with the same color filtering the light . after filtering by the color filter area of the color filter device 107 , the converted light then is incident on the light homogenization device 109 to be made uniform . in the light source system 100 of the present embodiment , the wavelength conversion device 106 and the color filter device 107 are fixed with respect to each other and driven synchronously by the same driving device . at the same time , the wavelength conversion area and the color filter area of the same color are synchronized by the first optical assembly . it has the advantages that : the structure is simple , it is easy to implement and the synchronization effect is excellent . in addition , each element of the first optical assembly is stationary with respect to the excitation light source , and do not rotate with the rotation of the wavelength conversion device 106 and the color filter device 107 , so the optical stability is improved . further , since the converted light generated through wavelength conversion generally has an approximately lambertian distribution , if the converted light is directly incident on the color filter area , the incident angle will be distributed in the range of 0 degree to 90 degrees . however , the transmittance of the color filter area will shift with the increase of the incident angle , so in the present embodiment , the first optical assembly further includes a light convergence device ( for example , a lens 105 ) to converge the converted light , which can decrease the incident angle of the converted light incidence on the color filter area and further improve the color filter effect . in a preferred embodiment , by adjusting the first optical assembly , the energy of the converted light that is incident on the light filter 107 with incident angles less than or equal to 60 degrees can be more than 90 % of the total energy of the converted light . in the present embodiment , the dichroic mirror 102 and the reflecting mirror 104 can be replaced by other forms of planar reflecting device , and the lenses 103 and 105 can be replaced by other forms of optical devices . for example , the lens 105 may be replaced by various forms of light convergence devices like a solid or hollow tapered light guide , a lens or lens group , a hollow or solid composite light condenser , or a curved reflecting mirror , etc . in addition , in the present embodiment , the wavelength conversion areas of the wavelength conversion device 106 can be a combination of one or more of the red wavelength conversion area , the green wavelength conversion area , the blue wavelength conversion area and the yellow wavelength conversion area , and the excitation light source can be another suitable light source . alternatively , those skilled in the art can select the wavelength conversion area and the excitation light source with other colors as desired . in this case , the color filter areas of the color filter device 107 are configured according to the colors of the converted light generated by the wavelength conversion areas of the wavelength conversion device 106 , and the present invention shall not be limited to any specific arrangement . referring to in fig3 and fig4 , fig3 is a schematic structural view of the second embodiment of the light source system of the present invention , and fig4 is a front view of the wavelength conversion device and the color filter device of the light source system shown in fig3 . the light source system 200 of the present embodiment and the light source system 100 as shown in fig1 and fig2 differ in that : the excitation light source 201 is a blue laser or blue light - emitting diode in order to generate a blue excitation light . as show in fig4 , in the present embodiment , besides of a red wavelength conversion area , a yellow wavelength conversion area and a green wavelength conversion area , the wavelength conversion device 206 further includes a blue light transmission area . the color filter device 207 includes a red color filter area , a yellow color filter area and a green color filter area . in the present embodiment , the area of the color filter device 207 which is corresponding to the blue light transmission area of the wavelength conversion device 206 is not required to have a particular optical property , and it can be provided as a counterweight balance area for rotation balance , so it should have the same or similar weight as the other color filter areas . in the present embodiment , the wavelength conversion device 206 and the color filter device 207 rotate synchronously under the driving of the driving device 208 , so that the wavelength conversion areas and the blue light transmission area of the wavelength conversion device 206 are sequentially and periodically disposed in the propagation path of the blue excitation light generated by the excitation light source 201 . the wavelength conversion areas convert the blue excitation light incident on them into the converted light of corresponding colors and reflect them , and the blue light transmission area transmits the blue excitation light incident on it . the blue light transmission area can be provided with appropriate scattering materials to destroy the collimation of the blue excitation light . the converted light reflected by the wavelength conversion device 206 is guided by the first optical assembly comprised of lenses 203 and 205 , dichroic mirror 202 and reflecting mirror 204 and incident on the color filter area of corresponding color on the color filter device 207 , so that it is filtered by the color filter area to improve its color purity . the blue excitation light transmitted by the wavelength conversion device 206 is guided by the second optical assembly comprised of lenses 210 and 213 , reflecting mirror 211 and dichroic mirror 212 , and is combined with the converted light filtered by the color filter device 207 into one light beam , which is incident on the light homogenization device 209 to be made uniform . of the second optical assembly , the lenses 210 and 213 are used for collecting and converging the blue excitation light transmitted by the wavelength conversion device 206 , and the reflecting minor 211 and the dichroic mirror 212 are used to reflect the blue excitation light transmitted by the wavelength conversion device 206 to change its propagation path . in the present embodiment , the reflecting minor 211 and the dichroic mirror 212 are arranged in parallel with each other and they are set at 45 degrees to the incident direction of the blue excitation light so that the propagation direction of the blue excitation light is shifted by a predetermined distance but its propagation direction remains the same . in the present embodiment , the blue excitation light generated by the excitation light source 201 is directly outputted as the blue light through transmission . in the present embodiment , the reflecting minor 211 and the dichroic mirror 212 can be replaced by other forms of planar reflecting devices , and the lenses 210 and 213 can be replaced by other forms of optical devices . in addition , the above - described structure is also applicable to the light source system in which excitation light sources of other colors are used . referring to fig5 and fig6 , fig5 is a schematic structural view of the light source system according to the third embodiment of the present invention , fig6 is a front view of the wavelength conversion device and the color filter device of the light source system shown in fig5 . the light source system 300 of the present embodiment and the light source system 200 shown in fig3 and fig4 differ in that : the light source 300 further includes . in addition to the excitation light source 301 , a red illumination light source 315 ( for example , a red laser or a red light emitting diode ) in order to generate a red illumination light . the red illumination light source 315 and the excitation light source 301 are respectively provided on the opposite sides of the wavelength conversion device 306 and the color filter device 307 . the red illumination light generated by the red illumination light source 315 passes through the lens 314 , the dichroic mirror 311 , the lens 310 to be incident on the wavelength conversion device 306 ; its incident direction is opposite to that of the excitation light generated by the excitation light source 301 . in the present embodiment , the wavelength conversion device 306 includes a red light transmission area , a yellow wavelength conversion area , a green wavelength conversion area and a blue light transmission area . the color filter device 307 includes a red light transmission area , a yellow color filter area , a green color filter area and a counterweight balance area . in the present embodiment , under the driving of the driving device 308 , the wavelength conversion device 306 and the color filter device 307 rotate synchronously , so that the wavelength conversion areas , the red light transmission area and the blue light transmission area of the wavelength conversion device 306 are disposed in the propagation path of the blue excitation light generated by the excitation light source 301 and the red illumination light generated by the red illumination light source 315 sequentially and periodically . the various wavelength conversion areas convert the blue excitation light incident on them into the converted light of corresponding color and reflect it , the blue light transmission area transmits the blue excitation light incident on it , and the red light transmission area transmits the red illumination light incident on it . the blue light transmission area and the red light transmission area can be provided with appropriate scattering materials to destroy the collimation of the blue excitation light and the red illumination light . the converted light reflected by the wavelength conversion device 306 is guided by the first optical assembly comprised of lenses 303 and 305 , dichroic minor 302 and reflecting mirror 304 and incident on the color filter area of corresponding color on the color filter device 307 , so that it is filtered by the color filter area to improve its color purity . the red illumination light transmitted by the wavelength conversion device 306 is guided by the first optical assembly comprised of lens 303 and 305 , dichroic mirror 302 and reflecting mirror 304 and incident to the red light transmission area of the color filter device 307 along the same propagation path of the converted light , then transmitted by the red light transmission area . the blue excitation light transmitted by the wavelength conversion device 306 is guided by the second optical assembly comprised of lenses 310 and 313 , dichroic minors 311 and 312 , and combined with the converted light filtered by the color filter device 307 and the red illumination light transmitted by the color filter device 307 into one light beam , which is incident on the light homogenization device 309 to be made uniform . in a preferred embodiment , in order to ensure that the light homogenization device 309 receives only one color light at any time , the rotation position of the wavelength conversion device 306 is detected , and a synchronization signal is generated based on the detection . the excitation light source 301 and the red illumination light source 315 are turned on and off in a time - division manner according to the synchronization signal . specifically , the red illumination light source 315 is turned on only when the red light transmission area is in the propagation path of the red illumination light generated by the red illumination light source 315 , and is turned off when the yellow wavelength conversion area , the green wavelength conversion area and the blue light transmission area are in the propagation path of the red illumination light . the excitation light source 301 is turned on only when the yellow wavelength conversion area , the green wavelength conversion area and the blue light transmission area are in the propagation path of the blue excitation light generated by the blue excitation light source , and is turned off when the red light transmission area is in the propagation path of the blue excitation light . in addition , in another preferred embodiment , a dichroic filter which transmits the red illumination light and reflects the blue excitation light can be provided in the red light transmission area , a reflecting minor which reflects the red illumination light can be provided for the yellow wavelength conversion area and the green wavelength conversion area on the side facing the red illumination light source 315 , and a dichroic filter that transmits the blue excitation light and reflects the red illumination light can be provided in the blue light transmission area . in the present embodiment , the red light outputted from the light source system 300 is supplied directly by the red illumination light source 315 , which can avoid the problem of low conversion efficiency of the red wavelength conversion material . of course , when it needs to improve the color purity , the red light transmission area can be replaced by a red color filter area . in the present embodiment , those skilled in the art can use other illumination light source to generate the illumination light of other colors . referring to fig7 , fig7 is a schematic structural view of the light source system according to the fourth embodiment of the present invention . the light source system 400 of the present embodiment and the light source system 300 shown in fig5 and fig6 differ in that : the excitation light source 401 of the present embodiment is an ultraviolet or blue excitation light source . at the same time , the wavelength conversion device 406 in the present embodiment is provided with a yellow wavelength conversion area , a green wavelength conversion area and a red light transmission area . so the excitation light source 401 is only used to excite the yellow wavelength conversion area and the green wavelength conversion area to generate yellow converted light and green converted light . the light source system 400 in the present embodiment further includes a blue illumination light source 416 in addition to the excitation light source 401 and the red illumination light source 415 . the blue illumination light generated by the blue illumination light source 416 passes through the second optical assembly comprised of lenses 417 and 418 and dichroic mirror 419 , is combined with the converted light filtered by the color filter device 407 and the red illumination light transmitted or filtered by the color filter device 407 into one light beam , which is incident on the light homogenization device 409 to be made uniform . in the present embodiment , the excitation light source 401 , the red illumination light source 415 and the blue illumination light source 416 can also be turned on and off in a time - division manner similar to the third embodiment . in the present embodiment , the red light outputted from the light source system 400 is supplied directly by the red illumination light source 415 and the blue light outputted from the light source system 400 is supplied directly by the blue illumination light source 416 , which can avoid the problem of low conversion efficiency of the wavelength conversion materials , and is more suitable for the display field . referring to fig8 , fig8 is a schematic structural view of the light source system according to the fifth embodiment of the present invention . the light source system 500 of the present embodiment and the light source system 100 shown in fig1 and fig2 differ in that : the wavelength conversion device 506 converts the excitation light generated by the excitation light source 501 into the converted light and transmits it . the converted light transmitted by the wavelength conversion device 506 is guided by the first optical assembly comprised of lenses 503 and 505 and reflecting minor 502 and 504 and incident on the color filter area of the same color on the color filter device 507 . after filtering by the color filter area it is incident on the light homogenization device 509 . in addition , the excitation light source 501 can also be a blue light source . a light transmission area can be further provided on the wavelength conversion device 506 . the light transmission area is provided in the propagation path of the excitation light generated by the excitation light source 501 periodically and transmits it . after being transmitted by the light transmission area , the excitation light passes through the first optical assembly comprised of lenses 503 and 505 and reflecting minor 502 and 504 , and is guided to another light transmission area or color filter area on the color filter device 507 along the same propagation path as the converted light , to be is transmitted or filtered . referring to fig9 , fig9 is a schematic structural view of the light source system according to the sixth embodiment of the present invention . the light source system 600 of the present embodiment and the light source system 500 shown in fig8 differ in that : the light source system 600 of the present embodiment further includes , in addition to the excitation light source 601 , a red illumination light source 615 in order to generate a red illumination light . the red illumination light source 615 and the excitation light source 601 are provided on the same side of the wavelength conversion device 606 and the color filter device 607 . the red illumination light generated by the red light illumination light source 615 is reflected by the dichroic minor 613 , converged by the lens 611 , then incident on the wavelength conversion device 606 along the same direction as the excitation light generated by the excitation light source 601 . the excitation light generated by the excitation light source 601 is converted into the converted light by the wavelength conversion area of the wavelength conversion device 606 , and is transmitted by the wavelength conversion device 606 . the red illumination light generated by the red illumination light source 615 is transmitted directly by the red light transmission area of the wavelength conversion device 606 . the converted light transmitted by the wavelength conversion device 606 and the red illumination light is guided by the first optical assembly comprised of reflecting minor 602 and 604 and lenses 603 and 605 , and incident on the color filter area and the red light transmission area of the color filter device 607 . the converted light filtered by the color filter area and the red illumination light transmitted by the red light transmission area are further incident on the light homogenization device 609 . in addition , the red light transmission area can be replaced by a red color filter area . in addition , the excitation light source 601 and the red illumination light source 615 in the present embodiment can also be turned on and off in a time - division manner similar to the third embodiment . referring to fig1 , fig1 is a schematic structural view of the light source system according to the seventh embodiment of the present invention . the light source system 700 of the present embodiment and the light source system 600 shown in fig9 differ in that : the light source system 700 of the present embodiment further includes a blue illumination light source 716 in addition to the excitation light source 701 and the red illumination light source 715 . the blue illumination light generated by the blue illumination light source 716 passes through the second optical assembly comprised of lens 717 and dichroic minor 718 , and is combined with the converted light filtered by the color filter device 707 and the red illumination light filtered or transmitted by the color filter device 707 into one light beam , which is incident on the light homogenization device 709 to be made uniform . in the present embodiment , the excitation light source 701 , the red illumination light source 715 and the blue illumination light source 716 can be turned on and off in a time - division manner similar to the third embodiment . referring to fig1 , fig1 is a schematic structural view of the light source system according to the eighth embodiment of the present invention . the light source system 800 of the present embodiment and the light source system 100 shown in fig1 and fig2 differ in that : in the present embodiment the excitation light generated by the excitation light source 801 is converged by the fly eye lenses 803 and 804 and converging lens 805 , then incident on the wavelength conversion device 806 through the light entrance port on the reflecting device 802 . the converted light reflected by the wavelength conversion device 806 is then reflected by the reflecting device 802 and incident on the color filter device 807 . the reflecting device 802 is semi - ellipsoidal or hemispherical and its reflecting surface faces inside . the converted light filtered by the color filter device 807 is further incident to the tapered light guide rod 809 . when the reflecting device 802 is semi - ellipsoidal , the converted light from the vicinity of one focus point of the reflecting device 802 can be reflected to the vicinity of the other focus point ; when the reflecting device 802 is hemispherical , if two points are located near the center of the sphere and symmetrical with respect to the center of the sphere , then the reflecting device 802 can approximately reflect the converted light from one symmetrical point to the other . in addition , in other embodiments , the reflecting device 802 can be provided without a light entrance port , and the excitation light source 801 and the reflecting device 802 are provided on the opposite sides of the wavelength conversion device 806 . the excitation light generated by the excitation light source 801 is incident on the wavelength conversion device 806 and the converted light is then transmitted through the wavelength conversion device to the reflecting device 802 . it &# 39 ; s worth noting that , under the reflection of the reflecting device 802 , the light spot formed by the excitation light generated by the excitation light source 801 incident on the wavelength conversion device 806 and the light spot formed by the converted light incident on the color filter device 807 are located at 0 degree from each other with respect to the center of the ring structure of the wavelength conversion device 806 and the color filter device 807 ; thus , the wavelength conversion area and color filter area of the same color on the wavelength conversion device 806 and color filter device 807 also need to be set at 0 degree from each other with respect to the center of the ring structure of the wavelength conversion device 806 and the color filter device 807 . of course , in other embodiments , through appropriate optical arrangement , the light spot formed by the excitation light incident to the wavelength conversion device 806 and the light spot formed by the converted light incident to the color filter device 807 can be set at any angle from each other with respect to the center of the ring structure of the wavelength conversion device 806 and the color filter device 807 , so the wavelength conversion area and the color filter area of the same color on the wavelength conversion device 806 and color filter device 807 can be set at any angle with respect to the center of the ring structure of the wavelength conversion device 806 and the color filter device 807 . referring to fig1 , fig1 is a schematic structural view of the light source system according to the ninth embodiment of the present invention . the light source system 900 of the present embodiment and the light source system 800 shown in fig1 differ in that : the wavelength conversion device 906 and the color filter device 907 are fixed coaxially by the bracket 908 , and are spaced apart along the axial direction . a tapered light guide rod 909 is provided between the wavelength conversion device 906 and the color filter device 907 . the excitation light generated by the excitation light source 901 is converged by the fly eye lens 903 and 904 and the converging lens 905 , then incident on the wavelength conversion device 906 through the light entrance port on the reflecting device 902 . the converted light reflected by the wavelength conversion device 906 is incident on the reflecting device 902 and reflected . the converted light reflected by the reflecting device 902 is first incident to the light guide rod 909 . the light guide rod 909 collects the converted light in order to reduce the divergence angle of the converted light . after guided by the light guide rod 909 , the converted light is incident on the color filter device 907 , so that the incident angle on the color filter device 907 is smaller , and the filtering effect is improved . in the present embodiment , the light guide rod 909 can also be replaced by other optical device that is able to achieve the functions described above . further , in the present embodiment , if the wavelength conversion device 906 is a transmission type , the reflecting device 902 can be omitted , and then the converted light is transmitted by the wavelength conversion device 906 and incident on the light guide rod 909 directly . as described above , in the embodiment shown in fig1 and fig1 , an illumination light source can be further provided in addition to the excitation light sources 801 and 901 , such as a red illumination light source or a blue illumination light source . referring to fig1 , fig1 is a schematic structural view of the light source system according to the tenth embodiment of the present invention . the light source system 1000 of the present embodiment and the light source system 100 shown in fig1 and fig2 differ in that : the wavelength conversion device 1006 of the present embodiment is a cylindrical structure , and the wavelength conversion areas are provided on the outside surface of the sidewall of the cylindrical structure . the color filter device 1007 has a ring structure . the wavelength conversion device 1006 and the color filter device 1007 are further coaxially fixed on the rotating shaft of the driving device 1008 , and rotate coaxially and synchronously under the driving of the driving device 1008 . in the working process of the light source system 1000 according to the present embodiment , the excitation light generated by the excitation light source 1001 is transmitted by the dichroic mirror 1002 , converged by the lens 1003 , then incident on the outside surface of the sidewall of the wavelength conversion device 1006 . the wavelength conversion areas on the outside surface of the sidewall of the wavelength conversion device 1006 convert the excitation light into the converted light and reflect it . after reflected by the wavelength conversion device 1006 , the converted light is guided by the first optical assembly which is comprised of lens 1003 and 1004 and the dichroic mirror 1002 , and incident on the color filter device 1007 . the color filter areas on the color filter device 1007 are provided outside of the cylindrical structure of the wavelength conversion device 1006 , so that the converted light can be incident on them and filtered to improve the color purity . after filtered by the color filter areas of the color filter device 1007 , the converted light is further incident on the light homogenization device 1009 to be made uniform . in other embodiments , the wavelength conversion device 1006 can also transmit the converted light to the color filter device 1007 . referring to fig1 , fig1 is a schematic structural view of the light source system according to the eleventh embodiment of the present invention . the light source system 1100 of the present embodiment and the light source system 100 shown in fig1 and fig2 differ in that : in the present embodiment the wavelength conversion device 1106 and the color filter device 1107 are two cylindrical structures which are fixed coaxially and nested within each other , and the wavelength conversion areas and the first color filter areas are provided on the sidewalls of the two cylindrical structures respectively . the color filter device 1107 is located outside of the wavelength conversion device 1106 . the wavelength conversion device 1106 and the color filter device 1107 are further coaxially fixed on the rotating shaft of the driving device 1108 , and rotate coaxially and synchronously under the driving of the driving device 1108 . in the working process of the light source system 1100 according to the present embodiment , the excitation light generated by the excitation light source 1101 is reflected by the reflecting mirror 1102 , converged by the lens 1103 , then incident on the wavelength conversion device 1106 . the wavelength conversion areas of the wavelength conversion device 1106 convert the excitation light into the converted light and transmit it . after being transmitted by the wavelength conversion device 1106 , the converted light is guided by the first optical assembly comprised of lens 1104 and incident on the color filter device 1107 . the color filter areas of the color filter device 1107 filter the converted light to improve its color purity . after filtering by the color filter areas of the color filter device 1107 , the converted light is further incident on the light homogenization device 1109 to be made uniform . referring to in fig1 and fig1 , fig1 is a schematic structural view of the light source system according to the twelfth embodiment of the present invention , and fig1 is the front view of the wavelength conversion device and the color filter device of the light source system shown in fig1 . the light source system 1200 of the present embodiment and the light source system 200 shown in fig3 and fig4 differ in that : in the present embodiment , the wavelength conversion device 1206 and the color filter device 1207 are two strip structures adjoined side by side , where the wavelength conversion areas and the first color filter areas are arranged side by side in the two strip structures . in the present embodiment , the wavelength conversion device 1206 includes a red wavelength conversion area , a green wavelength conversion area , a blue light transmission area and a yellow wavelength conversion area which are arranged side by side sequentially from top to bottom . the color filter device 1207 includes a red color filter area , a green color filter area , a blank area and a yellow color filter area which are arranged side by side sequentially from top to bottom . the wavelength conversion device 1206 and the color filter device 1207 move in an oscillating linear translational motion under the driving of a suitable driving device ( e . g . a linear motor ), so that the red wavelength conversion area , the green wavelength conversion area , the blue light transmission area and the yellow wavelength conversion area of the wavelength conversion device 1206 are periodically provided in the propagation path of the blue excitation light generated by the excitation light source 1201 . the wavelength conversion areas convert the blue excitation light incident on them into converted light of corresponding colors and reflect them , and the blue light transmission area transmits the blue excitation light incident on it . the blue light transmission area can be provided with an appropriate scattering material to destroy the collimation of the blue excitation light . the converted light reflected by the wavelength conversion device 1206 is guided by the first optical assembly comprised of lenses 1203 and 1205 , dichroic minor 1202 and reflecting mirror 1204 , then incident on the color filter area of corresponding color on the color filter device 1207 , so that it is filtered by the color filter area to improve its color purity . the blue excitation light transmitted by the wavelength conversion device 1206 is guided by the second optical assembly comprised of lens 1210 and 1213 , reflecting mirror 1211 and dichroic mirror 1212 , and combined with the converted light filtered by the color filter device 1207 into one beam of light , which is incident to the light homogenization device 1209 to be made uniform . in the present embodiment , the structure of the wavelength conversion device 1206 and the color filter device 1207 can also be applied to the other embodiments described above , which is not described . the present invention further provides a light source assembly constituted by the wavelength conversion device and the color filter device which are described in the above embodiments . in summary , in the light source system and the light source assembly of the present invention , the color filter device and the wavelength conversion device are fixed with respect to each other , and they are driven by a same driving device , which can bring the advantages that : the structure is simple , it is easy to implement , and the synchronization effect is excellent . the invention is not limited to the above described embodiments . various modification and variations can be made in the light source device and system of the present invention based on the above descriptions . thus , it is intended that the present invention cover modifications and variations that come within the scope of the appended claims and their equivalents , as well as the direct or indirect application of the embodiment in other related technical fields .
5
the following embodiments further illustrate the contents of the present invention , but they should not be understood to limit the present invention . modifications or substitutions made to the method , process or condition of the present invention , when not deviating from the spirit and essence of the present invention , all are within the scope of the present invention . if not specifically indicated , the technical means used in the embodiments are routine means well known to the skilled person in the art . the brown planthopper resistant rice material ri35 ( hao p y , liu c x , wang y y , chen r z , tang m , du b , zhu l l , he g c ( 2008 ) herbivore - induced callose deposition in the sieve plates of rice : an important mechanism for host resistance . plant physiology 146 : 1810 - 1820 ) was crossed with a rice variety sensitive to brown planthopper ( taichung native 1 , tn1 , bought from national rice seed resource library ) to establish the f2 population containing bph14 . in order to evaluate the brown planthopper resistance phenotype of each single plant in the f2 mapping population , the seedling bulk screening test was used to examine the resistance of each single plant in the population . the pest resistance level of single f2 plant is calculated according to the pest resistance level of all single plants of the corresponding f 2 - 3 family . using the methods of pcr ( polymerase chain reaction ), polyacrylamide gel electrophoresis , rflp probe and southern blotting ( sambrook , et al .) the separation state of ssr and rflp molecular probes was detected of each single f2 plant . based on the subtype of f2 molecular marker , joinmap3 . 0 software ( kyazma b . v ., po box 182 , 6700 a { dot over ( d )}{ dot over ( )} wageningen , netherlands ) was used to establish the molecular marker genetic linkage map of the rice chromosome . with the assistance of the quantitative character analyzing software mapqtl5 . 0 ( kyazma b . v ., po box 182 , 6700 ad wageningen , netherlands ), interval mapping analysis was combined with the quantitative data of brown planthopper resistance phenotype collected in the seedling bulk screening test . the results indicate : a qtl peak value exists between the 3 rd chromosome molecular markers r1925 and g1318 , the lod value reaches 49 . 3 and the contribution rate to the phenotypic variance is 90 . 6 %. based on earlier results , the methods of pcr ( polymerase chain reaction ) and polyacrylamide gel electrophoresis are used to screen the f2 population with two ssr markers rm514 , located outside of r1925 and g1318 , and sm1 , located within r1925 and g1318 , to get 54 recombined single plants . integrating the molecular markers of recombinant single plants , the single plants having identical molecular markers and the same level of pest resistance were pooled ( table 1 ). except from the single plant sa69 , the 12 single plants rt25 - rt15 have identical phenotype with the molecular marker sm1 , but in sa69 , the phenotype is identical with g1318 . thus , bph14 is located between sm1 and g1318 . for the preparation of plant high molecular weight genomic dna , see the methods of zhang hongbin et al . ( zhang et al ., preparation of megabase dna from plant nuclei . plant j 1995 , 7 , 175 - 184 ). nuclei from the young leaves of brown planthopper resistance rice b5 ( wang b n , huang z , shui l h , ren x , li x h , he g c ( 2001 ) mapping of two new brown planthopper resistance genes from wild rice . chinese science bulletin 46 : 1092 - 1095 ) was extracted and embedded in low - melting point agarose . an appropriate amount of restriction enzyme bamhi was added to the embedded nuclei for partial digestion . pulsed field gel electrophoresis was performed with the chef mapper pulsed field electrophoresis system to isolate the needed fragment . the strongest gel band from the region containing the 50 - 250 kb fragment was cut out and placed into the dialysis bag . the dna fragment was recovered using electroelution ( strong et al ., marked improvement of pac and bac cloning is achieved using electroelution of pulsed - field gel - separated partial digests of genomic dna . nucleic acids res . 1997 , 25 , 3969 - 3961 ). the large fragment dna isolated with electroelution was collected and put into a 1 . 5 ml centrifuge tube , 600 ng recovered dna fragment ( 50 - 250 kb ) was mixed with 200 ng dephosphorylated vector bibac2 , incubated at 60 ° c . for 10 min and cooled to room temperature . t4 dna ligase was added and the mixture was incubated at 16 ° c . for 16 h . taking 2 μl ligation product and 40 μl dh10b competent cells , the gene pulser system was used to perform electrotransformation . the transformed cells were plated onto agarose containing 50 mg / l kanamycin and incubated at 37 ° c . overnight . positive clones were picked from the plate and inoculated into a 384 well cell culture plate containing 70 μl medium , and incubated at 37 ° c . for 30 h . after the construction of the library , two copies were made with genetix q - pix and one perserved at − 80 ° c . in order to estimate the distribution of the length of the inserted fragment and the volume of the clones , 30 bibac clones were randomly picked from the library , and their plasmids extracted by alkaline lysis . after digesting with appropriate amount of noti , the length of the inserted fragment was confirmed with pulsed field gel electrophoresis ( shi z y , ren x , weng q m , li x h , he g c ( 2003 ) construction of genomic library of a bph - resistant rice line with binary vector and physical map of qbp1 locus . plant science 1165 : 879 - 885 ). all the bac clones were screened for the r1925 - g1318 region . after double digestion with bamhi and ecori , electrophoresis was performed and the nucleic acid fragments were transferred to a membrane . then , the end of the digested clone was labeled with radioactive α - 32 p - dctp . southern blotting with the bac clones was performed as before , and the bac clones which have overlaps and the length of the overlapped fragment based on the hybridization signal were identified . based on the results , the physical map was constructed ( fig3 c ). for the terminal isolation of bac positive clones , see the tail - pcr method invented by liu yaoguang et al . ( liu and whittier , thermal asymmetric interlaced pcr : automatable amplification and sequencing of insert end fragments from p1 and yac clones for chromosomewalking . genomics 25 : 674 - 681 ). the results of the screen and tail - pcr show that the bac clone 76b10 contains the complete bph14 gene ( fig3 c ). sequence analysis for the entire sequence of the bph14 gene containing clone was performed ; the ncbi database was searched using this sequence as the target sequence to identify the homologous sequence of the nipponbare genome in this region . ricegaas online software ( sakata , k ., nagamura , y ., numa , h ., antonio , b . a ., nagasaki , h ., idonuma , a ., watanabe , w ., shimizu , y ., horiuchi , i ., matsumoto , t ., sasaki , t . & amp ; higo , k . : “ ricegaas : an automated annotation system and database for rice genome sequence ”, 2002 . nucleic acids res ., 30 : 98 - 102 ) was used to perform gene prediction and annotation , also clustalw was used for comparative analysis ( table 2 ). by comparing the predicted genes of the two , it was found that the disease resistant protein encoded by the 4 th gene of the pest resistance rice is quite different from that of nipponbare . now , it is commonly considered that the sucking and eating of rice by piercing - sucking insects is similar to the process of rice infection by pathogenic bacteria , therefore , the mechanism of rice to resist piercing - sucking insects might be the same as that of resisting pathogenic bacteria . thus , this gene can be determined to be bph14 . using the predicted gene corresponding to the est as a probe , phage in situ hybridization with the cdna library of brown planthopper induced pest - resistant rice b5 was performed ( wang x l , weng q m , you a q , zhu l l , he g c ( 2003 ) cloning and characterization of rice rh3 gene induced by brown planthopper . chinese science bulletin 48 : 1976 - 1981 ). after three rounds of in situ hybridization , two chosen phage clones with pcr were examined , and afterwards the length of the inserted fragment was determined with enzyme digestion . full length cdna was sequenced . its nucleotide sequence is as shown in sequence listing , seq id no : 2 . however , the skilled person in the art will understand that according to the nucleotide sequence disclosed in the present invention , by designing appropriate primers , the bph14 gene can be amplified and obtained from the genome of brown planthopper resistance rice . for example , primers : 5 ′ ctccctgactgaagaagagaagag3 ′ ( seq id no : 4 ) and 5 ′ tgctagagtgattacttatgatg3 ′ ( seq id no : 5 ), the sequence can be obtained by using long fragment pcr amplification kit and amplifying the genome of brown planthopper resistance rice or wild rice ( 94 ° c . for 2 minutes ; 30 cycles of 94 ° c . for 15 seconds , 58 ° c . for 30 seconds , 72 ° c . for 7 minutes ; 72 ° c . for 2 minutes ). the vector used is pcambia1301 ( bought from australia center for the application of molecular biology to international agriculture ). based on the result of genome sequencing , primers were designed ( 5 ′ cgg aattc ctccctgactgaagaagagaagag3 ′ ( seq id no : 6 ), 5 ′ cgg aattc tgctagctgtgattctcttatgatg3 ′ ( seq id no : 7 ) that contain an ecori linker . using these primers , the genome of pest - resistant rice b5 was amplified as described below ( z . huang et al ., identification and mapping of two brown planthopper resistance genes in rice . theor appl genet , 2001 , 102 : 929 - 934 ). the total volume of pcr reaction is 50 μl , 1 μl dna , 10 × buffer 5 μl , 10 mm dntp 1 μl , 10 mm primers each 3 μl , high - fidelity taq enzyme 1 u ; reaction program : 94 ° c . 2 min , 94 ° c . 15 s , 58 ° c . 30 s , 72 ° c . 7 min 30 s , totaling 30 cycles . the product was purified by adding 1 / 10 volume 3 mm naac and 2 × volume absolute alcohol . the obtained sequence contains a 1960 bp promoter and 4997 bp genomic sequence upstream of bph14 , and downstream 436 bp 3 ′ non - translational region , which was digested with ecori , where the total volume the digestion system was 20 μl : about 5 μl ( 1 μg ) pcr product , 1 × reaction buffer , ecori 1 u , mixed well and incubated at 37 ° c . overnight . the product was precipitated with 1 / 10 volume 3 mm naac and 2 × volume absolute alcohol , recovering the needed fragment . the digestion system of pcambia1301 vector is as stated before , purified with the purification kit . the ligation reaction used is as follows : genomic fragment 1 μl , vector 0 . 5 μl , 2 u t4 ligase , 5 × buffer 2 μl , total volume 10 μl , ligate at 4 ° c . overnight . the ligation product was transformed into e . coli dh10b by heat shocking at 42 ° c . for 90 s , adding in 400 μl lb , recovering for 45 minutes , transferring 200 μl of the culture onto la plate containing kanamycin , and incubating at 37 ° c . overnight . single clones were picked , amplified , and plasmid extracted and tested by enzyme digestion . a positive clone was picked and electro - porated into argobacterium eha 105 . cloning was confirmed by extracting the plasmid and verified with pcr . the argobacterium culture containing the constructed vector was preserved by taking 750 μl and adding 50 % glycerol of the same volume , mixing well . the culture was stored at − 70 ° c . primers were designed based on full length cdna sequence , containing xmai and xbai linker ( 5 ′ tccccccgggatggcggagctaatggccac3 ′( seq id no : 8 ), 5 ′ gctctagactacttcaagcacatcagccta3 ′ ( seq id no : 9 )). total rna was extracted from b5 leaf sheath using trizol of invitrogen ( invitrogen corporation , 5791 van allen way , po box 6482 , carlsbad , calif . 92008 ), then , the cdna of b5 was obtained by using the reverse transcription kit of fermentas ( fermentas international inc , 830 harrington court , burlington ontario l7n 3n4 canada ); reaction system : total rna 1 μg , oligo ( dt ) 1 μl , 5 × buffer 4 μl , inhibitor 1 μl , 10 mmdntp 2 μl , reverse transcriptase 1 μl , incubate at 42 ° c . for 1 hour . b5 cdna was amplified using the designed primers . the pcr reaction system is as described above , however , in the program , elongate at 72 ° c . for 4 min to get the cdna sequence of bph14 . meanwhile , the promoter required for cdna transcription can be obtained from pcr amplification of the 35s promoter present in pcambia1301 . using the designed primers containing ecori and xmai linker ( 5 ′ cggaattcatggtggagcacgacactct3 ′ ( seq id no : 10 ), 5 ′ tccccccgggatctcattgccccccgggat3 ′ ( seq id no : 11 )), the 35s promoter sequence was amplified from pcambia1301 . the pcr reaction system used is as described above , however the elongation time is 1 min . the 35s promoter and the pcambia1301 vector were digested with ecori and xmai each . the 35s fragment and the linearized vector were ligated and transformed into e . coli after recovery . the obtained positive clone and the bph14 cdna sequence was digested with xmai and xbai each , the products were recovered , ligated and transformed . a 35s : bph14 vector was constructed and electro - porated into argobacterium eha 105 , the detailed process is described above . the above mentioned bph14 genomic transformation vector and cdna transformation vector were separately introduced into the ordinary rice variety kasalath ( bought from national rice seed resource library or national rice research institute ) sensitive to brown planthopper using the genetic transformation method mediated by argobacterium eha 105 ( hiei et al ., 1994 , efficient transformation of rice ( oryza sativa l .) mediated by argobacterium and sequence analysis of the boundaries of the t - dna . plant journal 6 : 271 - 282 ). at the same time , a blank vector ( pcambia1301 ) was used as a negative control . 14 cultured seedlings , obtained from each of the two transformed lines above , and 4 control seedlings , were planted in the field . after harvesting the t1 generation separately , homozygous plants ( 14 plants each ) were selected for the pest resistance test . after the pest resistance test at the seedling stage and at mature stage , in both cases , the brown planthopper resistance of transgenic plants is evidently increased , while the control plants have no resistance against brown planthopper . all the pest resistance level of transgenic rice at seedling stage is between grade 3 - 5 , as determined by the process set forth in huang , et al . ( huang z et al , 2001 identification and mapping of two brown planthopper resistance genes in rice . theor . appl . genet . 102 , 929 - 934 ). the transgenic plants at mature stage are in good condition after the addition of pests and they can set seeds normally . at the same time , epg ( peiying hao et al , herbivore - induced callose deposition on the sieve plates of rice : an important mechanism for host resistance . plantphysiol , 2008 , 146 : 1810 - 1820 ) showed that when brown planthoppers feed on transgenic plants , evidently less time is spent on phloem . the test of honeydew method ( p . paguia , honeydew excretion measurement techniques for determining differential feeding activity of biotype of nilaparvata lugens on rice varieties . j . econ . entomol , 1980 , 73 : 35 - 40 ) proved that the amount of excretion egested by brown planthopper fed on transgenic plants decreased . thus , the cloned bph14 can cause resistance of the rice against the feeding of brown planthoppper on rice . molecular marker assists the selection of bph14 carrying brown planthopper resistance rice 3 . 1 based on the genomic sequence and cdna sequence of bph14 gene , multiple pairs of primers of ssr marker or sts marker can be designed . in the present embodiment , the pair of primers 5 ′ ctgctgctgctctcgtattg3 ′ ( seq id no : 12 ), 5 ′ cagggaagctccaagaacag3 ′ ( seq id no : 13 ) is used as labeling primers for the selection of rice with pest resistance . the length of the amplified fragment is 172 bp . by performing pcr amplification , using primers designed on the bph14 gene sequence , one can test for the presence of the molecular marker by polyacrylamide gel electrophoresis . the cross - breeding offspring plants showing the same pcr bands as pest - resistant rice ( amplification product contains a 172 bp fragment ) are the selected plants containing bph14 gene ( fig2 ). the pest resistance of these plants is confirmed with seedling bulk screening test and test at mature stage . brown planthopper resistance rice is bred through self cross and economical character selection of these plants . 3 . 2 one can evaluate brown planthopper resistance of the mapping population by using the seedling bulk screening test : f3 seeds were harvested from the f2 plants , and approximately 20 seedlings ( called one family ) were grown in a tray . resistant control variety ri35 and sensitive control variety tn1 were grown together . once the plants developed approximately 2 - 3 leaves , the plants were inoculated with 2nd - 4th instar brown planthopper nympha ( 10 nympha / plant ) and the state of damage was recorded in each of the families when all sensitive control tn1 plants were dead . the experiment was repeated for 3 times with each material . according to the results of pest resistance evaluation , the families of the mapping population were classified as to their pest resistance level . 4 . 1 . the construction of ri35 / tn1 f 2 population and phenotype evaluation using art recognized methods ( wang b n et al , 2001 mapping of two new brown planthopper resistance genes from wild rice . chinese . sci . bull . 46 , 1092 - 1095 , huang z et al , 2001 identification and mapping of two brown planthopper resistance genes in rice . theor . appl . genet . 102 , 929 - 934 ), the dominant brown planthopper resistance gene bph14 was found to be located at the end of the long arm of the rice 3 rd chromosome , and its rflp marker is between r1925 and g1318 . due to the high difficulty of the rflp technique , a huge amount of work is required in large - scale breeding and screening . in order to search for simple and efficient molecular markers that had tighter link with bph14 , we chose the brown planthopper resistant variety ri35 which originated from the 7 th generation of recombinant inbred line between b5 and minghui 63 , only carrying brown planthopper resistance major gene bph14 ( ren x et al , 2004 dynamic mapping of quantitative trait loci for brown planthopper resistance in rice . cereal . res . commun . 32 , 31 - 38 ). hybrids were produced using ri35 as the female parent and brown planthopper susceptible rice variety . tn1 as the male parent . ri35 / tn1 f 2 segregation population was constructed . ri35 / tn1 f 2 : 3 lines were respectively obtained from each f 2 single strain by inbreeding . resistance evaluation of parent plants and f 2 : 3 lines was conducted with introduction during seedling stage . to ensure that the parent plants and each line from the f 2 : 3 population grow at the same rate , all experimental materials were respectively soaked and hastened to germinate before the seeding . 20 seeds from each line ( variety ) were seeded in a 54 cm long , 35 cm wide and 8 cm high bread box filled with nutrient soil . 40 materials were seeded in each box , including 2 resistant parent plants and 4 susceptible parent plants . thinning was conducted seven days after seeding . sick and weak seedlings were discarded , and at least 15 plants were kept in each cup . when the seedlings reached three - leaf stage , they were inoculated with 2 ˜ 3 instar brown planthopper larvae at the ratio of 8 per seedling , and were covered with nylon mesh . when the susceptible variant tn1 died out , each single strain was evaluated for resistance at grade 0 , 1 , 3 , 5 , 7 and 9 ( table 3 ) according to the method described by huang et al ( huang z et al , 2001 identification and mapping of two brown planthopper resistance genes in rice . theor . appl . genet . 102 , 929 - 934 ), and the resistance grade of each line from the parent plants and the population was calculated by weighted mean , and the single strain genotype was estimated from the resistance grade . dna of the parent plants and each line of f 2 population was extracted using ctab technique ( murray m g & amp ; thompson , 1980 rapid isolation of high - molecular - weight plant dna . nucleic acids res 8 : 4321 - 4325 ). since r1925 and g1318 locate respectively in 32g11 and 96m04 , bac clones of nipponbare rice genome , we conducted a search for ssr motifs in the sequences of these two bac clone using the search tool ssrit described by temnykh , et al . ( temnykh s , declerck g , lukashova a , lipovich , cartinhour s , mccouch s . computational and experimental analysis of microsatellites in rice ( oryza sativa l . ): frequency , length variation , transposon associations , and genetic marker potential . genome research . 2001 . 11 ( 8 ): 1441 - 1452 ) with the following parameters : maximum motif length was tetramer , the minimum repeat was 5 . all ssr motifs longer than 15 bases ( motif length × repeat times ) were selected and primers were designed based on their flanking sequences as candidate ssr markers . ssr markers were analyzed in accordance with temnykh &# 39 ; s method ( temnykh s et al , 2000 mapping and genome organization of microsatellite sequences in rice . theor appl genet . 100 : 697 - 712 ). the 10 μl reaction system included : 10 mm tris - hcl ph8 . 3 , 50 mm kcl , 1 . 5 mm mgcl 2 , 50 μm dntps , 0 . 2 μm primer , 0 . 5 u taq polymerase and 20 ng dna template . amplification is conducted using ptc - 100 pcr amplifier : 94 ° c . 2 min ; 94 ° c . 15 sec , 55 ° c . 30 sec , 72 ° c . 1 . 5 min , 35 cycles ; 72 ° c . 5 min . amplified products were separated using 6 % undenatured page gel , and visualized by silver staining ( zhu et al , 2004 identification and characterization of a new blast resistance gene located on rice chromosome 1 through linkage and differential analyses . phytipathology 94 : 515 - 519 ). amplified dna bands were observed using a transilluminator with a fluorescent lamp . the results were recorded . primers that had polymorphism between parent plants were analyzed in f 2 population and population genotype data were obtained . the genetic map of rice ssr markers was constructed with population genotype data based on the law of linkage and crossover . the software used was mapmaker / exp3 . 0 . a whole genome scan was conducted using composite interval mapping ( cim ) from windows qtl cartographer v2 . 0 software . a segregation analysis between the brown planthopper resistance and ssr markers was conducted using the analytical software mapmaker / exp3 . 0 , and kosambi functions were converted into genetic distances ( cm ). 4 . 3 screening of ri35 / tn1 f 2 and f 5 population using molecular markers and positioning of bph14 gene based on the positioning results of qtl , f 2 single plants were screened using the flanking ssr markers sg1 and sm4 to obtain the single plants which had recombination between the two markers . the genotype and phenotype of each single strain were checked as described above to explore which markers cosegregated with the resistance phenotype . using molecular marker - assisted selection , we selected f 2 single plants which were heterozygous in bph14 site and preferably derived from tn1 or heterozygous in other sites ; after inbreeding , single plants that were heterozygous in bph14 site and preferably derived from tn1 in other sites were obtained using molecular marker - assisted selection . eventually , f 5 inbred population was constructed , in which except for the bph14 site , all other regions were from the genome of tn1 . based on the results of ( 1 ), f 5 single plants were screened using the flanking ssr markers rm570 and sm4 to obtain the single plants which had recombination between the two markers . the genotype and phenotype of each single strain were checked as described above to explore which markers cosegregated with the resistance phenotype . based on the results of ( 2 ), gene library of b5 was screened , and bac clones of b5 gene library covering the two markers were obtained . after sequencing , the said sequence was compared for dna difference with the corresponding sequence of nipponbare . primers were designed based on the difference of sequences to amplify the dna sequence of ri35 and tn1 . primers that have polymorphism were used in the analysis of f 2 and f 5 recombinant single plants to explore whether they cosegregated with resistance phenotype . group introduction test in seedling stage showed that the resistance grade of ri35 and tn1 were 2 . 7 and 9 respectively , which indicated that ri35 was brown planthopper resistant while tn1 was susceptible . the resistance grade of f 1 plants was 3 . 4 , showing resistance against brown planthopper , indicating that the resistance of ri35 was controlled by dominant gene . the frequency distribution of the resistance grade of 100 f 2 : 3 lines against brown planthopper showed continuous distribution . the minimum value was 3 . 0 while the maximum value was 9 . 0 , and three obvious peaks were found at the three locations of 3 . 5 , 5 . 5 and 8 . 5 . based on the resistance grade f 2 : 3 lines were divided into three phenotypes : resistance , segregation of resistance and susceptibility , and susceptibility . the corresponding genotypes of the f 2 single plants were recorded as three types : rr ( homozygous resistance ), rr ( heterozygous resistance ) and rr ( homozygous susceptibility ). the segregation of resistance and susceptibility of f 2 population was in accordance with a 1 : 2 : 1 ratio ( χ 2 = 0 . 54 , χ 2 005 = 5 . 99 ) ( table 2 ). huang zhen and wang buna have identified two dominant brown planthopper resistance genes , bph1 and bph15 , from b5 , a fertility line of o . officinalis . ri35 comprises one brown planthopper resistance major gene bph14 . therefore , in this study , qtl of the f 2 population was positioned using the ssr markers from the 3 rd chromosome to determine whether it was in accordance with previous studies . based on the search results of ssrit , we selected all the ssr motifs longer than 15 bases ( motif length times × repeat times ), and designed primers based on their flanking sequences . depending on the different bac clones these motifs were situated , these ssr markers were named as sg1 , sg2 , etc . and sm1 , sm2 , etc . consecutively . we used these ssr markers to amplify the dna of the parent plants ri35 and tn1 . only sg1 , sg6 , sg9 and sm1 , sm4 showed polymorphism between parent plants in electrophoresis . whereafter we used ssr markers that had polymorphism between parent plants to locate the qtl of the f 2 population . the results showed that there was one qtl site between sg1 and sm4 at the end of the long arm of the 3 rd chromosome , whose lod value was 25 . 3 and the contribution rate was 67 . 5 %. molecular marker sg6 and sg9 cosegregated with bph14 . sg1 was 2 . 1 cm from bph14 ; rm570 and sm1 were 0 . 8 cm from bph14 ; sm4 was 1 . 5 cm from bph14 ( fig1 ). the accurate rate of sg1 , sg6 , sg9 , rm570 , sm1 and sm4 were 98 %, 100 %, 100 %, 99 %, 99 % and 98 %. the distance between sg1 and sm4 was large . in sequenced indica rice variety nipponbare , the distance was 270 kb . therefore , to search for markers more tightly linked to bph14 , we screened 3700 f 2 single plants using sg1 and sm4 . the results showed that , only 26 single plants had recombination between marker sg1 and sm4 . we used other ssr markers , as well as r1925 and g1318 to check the genotype of the recombinant single plants , and combined with the resistance evaluation results , we found that bph14 cosegregated with sm1 ( table 5 , fig1 ) we constructed the inbred f 5 population using the method of molecular marker - assisted selection in which other than bph14 site , all other regions were from the genome of tn1 . 5000 f 5 single plants were screened using the flanking ssr marker rm570 and sm4 , and 15 single plants that had recombination between the two markers were obtained . we checked the genotype of the recombinant single plants , and combined with the resistance evaluation results of recombinant single plants , we found bph14 located between sm1 and sm4 . g1318 was used to check the genotype of these recombinant single plants , and eventually bph14 was positioned between sm1 and g1318 ( table 6 , fig1 ). through screening the gene library of b5 , 76b10 , a bac clone covering both markers was obtained . after sequencing , the sequence was compared for dna difference with the corresponding nipponbare sequence , and primers named 76 - 1 , 76 - 2 etc . were designed based on the difference of sequence to amplify the dna sequence of ri35 and tn1 . eventually only 76 - 2 had polymorphism between ri35 and tn1 . the obtained single plants were analyzed by 76 - 2 , and it was found that 76 - 2 cosegregated with bph14 . the results showed that , the molecular markers described above have few recombinant single plants with bph14 , therefore they are useful to detect the existence of bph14 resistance major gene , and brown planthopper resistant rice varieties can be obtained using the method of molecular marker - assisted breeding so that the progression of breeding brown planthopper resistant rice varieties in china can be expedited . a from this table we can find that the molecular marker sm1 cosegregates with the resistance phenotype . this result shows that bph14 locates between molecular marker rm570 and g1318 and cosegregates with sm1 a numbers of the single plants indicate that f 5 populations eventually obtained from these f 2 single plants using molecular marker - assisted selection were used to accurately position bph14 . b from this table we can find that the molecular marker 76 - 2 cosegregates with resistance phenotype . the result shows that bph14 locates between molecular marker sm1 and g1318 and cosegregates with 76 - 2 . one embodiment of the present invention provides an isolated nucleic acid molecule comprising a nucleotide sequence that comprises a brown planthopper resistance gene bph14 selected from the group consisting of seq id no : 1 and seq id no : 2 . in another embodiment , the nucleotide sequence encodes a polypeptide molecule comprising the amino acid sequence seq id no : 3 . in yet another embodiment , the nucleotide sequence is operably linked to a heterologous promoter . another embodiment of the present invention provides an expression vector comprising the isolated nucleic acid molecule comprising a nucleotide sequence that comprises a brown planthopper resistance gene bph14 selected from the group consisting of seq id no : 1 and seq id no : 2 . in yet another embodiment , the present invention provides a transgenic plant , plant tissue , or plant cell comprising the expression vector . in still yet another embodiment , the transgenic plant , plant tissue , or plant cell is a monocot . in further yet another embodiment , the transgenic plant , plant tissue , or plant cell is rice . yet another embodiment of the present invention provides a method for producing a transgenic plant which expresses a bph14 gene , comprising the steps of : ( a ) stably transforming a cell of a plant with a nucleic acid molecule comprising a nucleic acid sequence selected from the group consisting of seq id no : 1 and seq id no : 2 to produce a transformed cell ; ( b ) regenerating a transgenic plant from the transformed cell ; and ( c ) growing the transgenic plant wherein the nucleic acid molecule is expressed . in another embodiment , the transgenic plant is a monocot . in still yet another embodiment , the transgenic plant is rice . further yet another embodiment of the present invention provides a molecular marker associated with brown planthopper resistance , wherein the molecular marker is selected from the group consisting of : sg1 , sg6 , sg9 , rm570 , sm1 , 76 - 2 , and sm4 . in one embodiment , sg1 is amplified by primers seq id nos : 14 and 15 . in another embodiment , sg6 is amplified by primers seq id nos : 16 and 17 . in yet another embodiment , sg9 is amplified by primers seq id nos : 18 and 19 . in still yet another embodiment , rm570 is amplified by primers seq id nos : 20 and 21 . in further yet another embodiment , sm1 is amplified by primers seq id nos : 22 and 23 . in another embodiment , 76 - 2 is amplified by primers seq id nos : 24 and 25 . in yet another embodiment , sm4 is amplified by primers seq id nos : 26 and 27 . still yet another embodiment of the present invention is a method for determining the presence or absence of brown planthopper resistance in a plant or seed , comprising analyzing genomic dna from the plant or seed for the presence of a molecular marker linked to a quantitative trait locus associated brown planthopper resistance , wherein the molecular marker is selected from the group consisting of : sg1 , sg6 , sg9 , rm570 , sm1 , 76 - 2 , and sm4 . in another embodiment , the method further comprises analyzing genomic dna from a plant or seed for the presence of a second molecular marker linked to a quantitative trait locus associated with brown planthopper resistance , wherein the second molecular marker is g1318 . in yet another embodiment , the plant or seed is a monocot . in still yet another embodiment , the plant or seed is rice . another embodiment of the present invention is a quantitative trait locus associated with brown planthopper resistance , wherein the quantitative trait locus is located in a 34 kb region between a first molecular marker and a second molecular marker on chromosome 3 of rice . in another embodiment , the quantitative trait locus comprises bph14 .
8
according to fig1 , a first example of insulator 1 design is given according to the invention , and obtained by stacking metallic foils 2 as the reflectors . these foils are separated by a thin layer of insert powder 3 making up the insert material . each foil 2 is a reflective foil 4 of large size , previously covered with powder 3 . insert powder 3 can be placed on reflective foil 2 by putting it in a recipient containing said powder 3 . the reflective foil 2 is advantageously a metallic foil , for example an aluminum foil . an aluminum foil between 5 and 100 microns thick , commercially available in widths of about 1 m , is advantageously used . powder 3 has the advantage of being of a particle size less than 1 μm and particularly between 5 to 20 nm and of a density between 10 and 250 kg / m 3 . this powder 3 is placed on each foil 2 , with a thickness approximatively of 10 to 300 microns . it is clear that various thicknesses of the foil 2 may be used , or that the thickness may be varied in decreasing or increasing order . this is also valid for the layers of powder 3 . insert material 3 can for instance be alumina , calcium silicate , and precipitated silica or titanium dioxide . the material used is advantageously presented in the form of a powdered pyrogenic silica . the pivotal quality of this powder 3 is that it presents a low solid conduction , and that its pore size is less than 1 micron . this allows to offer good insulating properties without limits in temperature of use (& lt ; 1000 ° c .) and at various pressures of use . for example , the following results are obtained at a temperature of 50 ° c . : pressure ( mbar ) heat conductivity ( mw /( m . k ) 0 . 05 1 100 14 1000 19 thus , for temperatures less than 100 ° c . on the hot side and a pressure of around 0 . 05 mbar , a thermal conductivity of 0 . 5 to 1 . 5 mw /( m . k ) is obtained . it can be observed that the insulator according to the invention can accomplish performances well above those of a classic insulator of micro - porous type , and this at pressures similar to those obtained on an industrial scale , for example by on - site pumping . in addition , the insulating material according to the invention shows great flexibility , allowing coiling around tubes of any diameter , but especially small diameter in the order of 1 cm . the insulating material can be used in a classical manner in any application requiring advanced insulation and upon which a force is applied . this is the case for instance of a tube , a container , etc . the material thus built shows great flexibility . in fig2 , a section view of a specific application of insulator 1 is shown , used to protect a closed curved surface of cylindrical shape , such as a tube for instance . insulator 1 is built by continuous spiral loops of a reflective foil 4 trapping insert powder 3 in successive layers . by operating radially outward from tube 7 , it is possible to protect a succession of insulating elements . reflective foil 4 prevents heat radiation in a known manner , and powder 3 prevents in an also known manner convection and conduction . conduction is mainly avoided by preventing any contact between the various loops of reflective foil 4 . this function is ensured by insert powder 3 , which serves as a spacer between the successive loops of foil 4 . the last loop of insulator 1 is protected by a suitable device 6 , a rim or a thin metal foil . the insulator is coiled around tube 7 as follows . tube 7 is for instance rotated upon its axis using a device not shown , so that reflective foil 4 and powder 3 can be coiled around it . reflective foil 4 then takes up the shape of a spiral between which loops an approximately constant thickness of powder 5 is trapped . powder 3 is placed on the foil as previously indicated . it is clear that this setup can be applied to any closed curved surface . in fig3 , another embodiment of the insulator 2 is shown , using a unique foil 9 folded in zigzag , with each fold 11 separated by a coat of powder 10 . foil 9 and powder 10 are of the same material as foil 4 and powder 3 . it is obvious that insulating material obtained this way may be used in pipes , containers or any other application . fig4 shows a longitudinal view of tube 7 protected by the insulator according to fig2 . after coiling foil 4 , coated with powder 3 around tube 7 . it is advantageous to band the coiled insulator made up of reflective foil 4 by using a cylindrical splint rim 6 , which can be easily manufactured by those skilled in the art . the splint rim 6 ensures better cohesion of the insulating assembly around tube 7 and limits any possible shift of powder 3 on curved surfaces . such an embodiment only makes use of silica and alumina for the insulating parts . this allows the whole unit to increase in temperature . the fact that the tube can be coiled and that only materials withstanding high temperature are used , makes the baking of such a tube practically possible . in the previous figures , the various sectional views show clearly the position of the various loops or folds delimited by foil 4 , separated by powder film 3 or 10 . it stands to reason that the spacing between loops or folds is enlarged for the sake of the drawing . it is also obvious that foil and powder are in intimate contact , as previously explained . fig5 illustrates an embodiment of the insulator 1 , of sizable width to protect a very long tube . foils 11 , 12 and 13 , commercially easily available are used in this aim and placed side by side according to the desired width , the desired length of each foil being by definition adjustable according to the user &# 39 ; s requirements . in order to ensure reflection continuity of the reflective foils , each foil is placed with a partial overlap strip . shown in the figure are overlap strip 14 between foils 11 and 12 and overlap strip 15 between foils 12 and 13 . this method makes it possible to fabricate an insulator of a large size by using spiral coiling around a tube or enclosure , or by using zigzag folding as shown in fig3 .
1
the compression of the outer surfaces is generally effected by calandaring , and more closely - or widely - spaced embossed patterns can also be selected as needed . depending on the material , the calandaring is generally peformed preferably at 100 ° to 200 ° c . at a pressure of up to 0 . 5 kg / cm 2 , with a roller speed of 5 - 25 m / min . if up to 10 % of the surface area is embossed , the result is an absorbent material that is suitable for absorbing fluids . with an increasing proportion of embossed surface area , the surface becomes less and less absorbent ; the recessed portions of the embossed pattern can additionally serve as a kind of reservoir , while the raised areas can serve as the absorbent cushion . the compression can also be accomplished with the aid of chemical substances , such as physiologically unobjectionable air - and moisture - permeable synthetic resins that do not irritate the skin , with which the outer surface is treated to a variable extent as needed . such resins are known to one skilled in the art for producing various articles of batting of wadding suitable fiber materials include cotton , viscose , synthetic fibers , or mixtures of these . for producing the cotton pads according to the present invention , the procedure is , for example , as follows : preparation of the fibers to make the card web is done in the usual manner , for example on carding , card brushing or similar suitable machines . next , the card web is combined into at least three continuous card web faces having the desired total weight , and then the embossing of the first and second card web face with the patterns that are desired and are needed for the particular intended use is performed in a known manner . the three ( or more ) card web faces are then put together to form a structure of alternating embossed and uncompressed layers - the web - like structure thus obtained is now stamped or cut into the desired shape and packed in a suitable manner . depending on the intended use , a further treatment , such as sterilization , impregnation with active ingredients , and so forth , can also be performed before or after the web is cut to size . this process makes it possible to use conventional equipment , and products having a smooth , fiber - free , non - powdering yet still soft outer surface and an absorbent closed - edge seam are produced . however , production can also be done with known machines by aerodynamic or hydrodynamic methods . if desired , the compressed outer surface layers can have further slightly compressed layers placed in between them , to increase the absorbency of the products . a round pad for cosmetic purposes , having a thickness of approximately 3 . 7 mm , for instance , comprises an uncompressed middle part approximately 1 . 5 mm in thickness and one compressed upper and lower surface layer each , each of which is approximately 0 . 8 mm thick . these outer surfaces are both provided with a waffle pattern , one with a very close pattern and the other with a widely spaced pattern of this kind . the product feels very soft and fluffy , but does not become linty or dusty and has excellent absorbency on the coarsely - patterned , less - compressed side . production is done in the following manner , by way of example : 100 % cotton combings , pure and bleached white , are prepared on a carding machine into a carb web . this card web is combineed into three continuous card web faces having a total weight of approximately 350 g / m 2 . two of these card web faces are separately compressed in an embossing calender and provided with a waffle pattern , which is done at a roller temperature of 150 ° c ., a passage speed of 12 m / min , and a pressure of 1100 kg / 20 cm linearly . the three card web faces are then combined into a sandwich - like structure in such a way that the two compressed , embossed faces form the outer surfaces and the third , practically uncompressed face , comes to rest in between these two surfaces . this web of material now travels beneath a stamp , and the desired circles are stamped out , and then stacked into a roll and packed in plastic bags . the foregoing description of the specific embodiments will so fully reveal the general nature of the invention that others can , by applying current knowledge , readily modify and / or adapt for various applications such specific embodiments without departing from the generic concept , and therefore such adaptations and modifications are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments . it is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation .
8
the present invention provides monosaccharides derivatives , which can be used for the inhibition and prevention of cell adhesion and cell adhesion mediated pathologies , including , for example , inflammatory and autoimmune diseases , for example , bronchial asthma , rheumatoid arthritis , type i diabetes , multiple sclerosis , allograft rejection or psoriasis . pharmaceutically acceptable salts , pharmaceutically acceptable solvates , enantiomers , diastereomers or n - oxides of these compounds having the same type of activity also are provided . the present invention also provides for pharmaceutical compositions containing the monosaccharide derivatives of the present invention , which also may contain pharmaceutically acceptable carriers or diluents . such pharmaceutical compositions can be used for the treatment of inflammatory and autoimmune diseases , for example , bronchial asthma , rheumatoid arthritis , type i diabetes , multiple sclerosis , allograft rejection or psoriasis . while the present invention has been described in terms of its specific embodiments , certain modifications and equivalents will be apparent to those skilled in the art and are included within the scope of the present invention . in accordance with one aspect , there is provided compounds having a structure of formula i , r 1 can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , heterocyclyl , heteroaryl , heterocyclylalkyl , heteroarylalkyl , aralkyl or —( ch 2 ) n o ( c ═ o ) nhr x , wherein n can be an integer 2 - 10 , and r x can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl or heteroarylalkyl ; r 2 and r 3 together can form a five membered acetal wherein the carbon joining the two oxygen atoms is substituted with r l and r m , wherein r l and r m can be hydrogen , alkyl , alkenyl , alkynyl , cycloalkyl , aryl or aralkyl ; r l and r m together can join to form a cyclic ring ( e . g ., a ( 3 - 8 )- membered cyclic ring ); or r l and r m together can join to form an oxo , wherein the ring optionally can contain one or more heteroatoms selected from o , n or s , and the ring optionally can be substituted with one or more of alkyl , alkenyl , alkynyl , acyl , substituted amino , cycloalkyl , carboxy , oxo , hydroxy , alkoxy , aryloxy , halogen ( e . g ., f , cl , br or i ), aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl , heterocyclylalkyl , or — c (═ o ) qr 7 , wherein q can be o or nh , and r 7 can be alkyl , alkenyl , alkynyl , aryl , aralkyl , cycloalkyl , or heteroarylalkyl ; or when q is nh , r 7 also can be heteroaryl , heterocyclyl or heterocyclylalkyl ; r 2 and r 3 , instead of forming an acetal , optionally and independently can be lower ( c 1 - c 4 )- alkyl , ( ch 2 ) k - aryl , — c (═ r y ) nhr x or acyl , wherein k can be an integer from 1 - 4 , r y can be o or s , and r x can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl or heteroarylalkyl ; and r 5 can be hydrogen , alkyl , cycloalkyl , heteroaryl , heterocyclyl , — nr p r j , or or z ; or when r 4 is oh , or c or h , then r 5 can be — nhc (═ o ) or s , — nhyr d , — nhc (= t ) nr t r x or —( ch 2 ) w ( c ═ o ) nr a r b , wherein r p and r j independently can be hydrogen , alkyl , cycloalkyl , aryl , heteroaryl , heterocyclyl , heteroarylalkyl , heterocyclylalkyl , or aralkyl , or r p and r j may together join to form a cyclic ring ( 5 - 8 membered ), which optionally may be benzofused , containing 0 - 4 heteroatom selected from 0 - 4 heteroatoms selected from o , s , or n wherein the ring may be substituted with one or more of alkyl , alkenyl , alkynyl , amino , substituted amino , cycloalkyl , carboxy , oxo , hydroxy , alkoxy , aryloxy , halogen , aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl or heterocyclylalkyl ; wherein r z can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl , heterocyclylalkyl , acyl or — c (═ o ) nr f r q , wherein r f and r q independently can be hydrogen , alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heterocyclyl , heteroaryl , heteroarylalkyl , heterocyclylalkyl or s ( o ) 2 r 6 ; or r f and r q can together form a ring , wherein r 6 can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl , heteroarylalkyl or substituted amino ; r s can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heterocyclylalkyl or heteroarylalkyl , y can be — c (═ o ), — c (═ s ) or so 2 ), r d can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl or heterocyclylalkyl , t can be o , s , — n ( cn ), — n ( no 2 ), or — ch ( no 2 ), r t can be h , oh or r x , r x can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl or heteroarylalkyl , w can be 1 - 4 , and r a and r b independently can be hydrogen or r d , or r a and r b , together with the nitrogen atom carrying them , can be the n - terminus of an amino acid or di - tetrapeptide , wherein r f and r q independently can be hydrogen , alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heterocyclyl , heteroaryl , heteroarylalkyl , heterocyclylalkyl or s ( o ) 2 r 6 ; or r f and r q can together form a ring , wherein r 6 can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl , heteroarylalkyl or substituted amino ; and wherein when w is hydrogen , then r 4 can be hydrogen , or c , — nhc (═ o ) or s , — nhyr d , — nhc (= t ) nr t r x , or —( ch 2 ) w ( c ═ o ) nr a r b , wherein r c can be hydrogen , alkyl , cycloalkyl , aryl , heteroaryl , heterocyclyl , acyl or — c (═ o ) nr f r q , r s can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heterocyclylalkyl or heteroarylalkyl , y can be — c (═ o ), — c (═ s ) or so 2 ), r d can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl or heterocyclylalkyl , t can be o , s , — n ( cn ), — n ( no 2 ), or — ch ( no 2 ), r t can be h , oh or r x , r x can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl or heteroarylalkyl , w can be 1 - 4 , and r a and r b independently can be hydrogen or r d , or r a and r b , together with the nitrogen atom carrying them , can be the n - terminus of an amino acid or di - tetrapeptide , wherein r f and r q independently can be hydrogen , alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heterocyclyl , heteroaryl , heteroarylalkyl , heterocyclylalkyl or s ( o ) 2 r 6 ; or r f and r q can together form a ring , wherein r 6 can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl , heteroarylalkyl or substituted amino ; or when w is alkyl , then r 4 can be — or z , wherein r z can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl , heterocyclylalkyl , acyl or — c (═ o ) nr f r q , wherein r f and r q independently can be hydrogen , alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heterocyclyl , heteroaryl , heteroarylalkyl , heterocyclylalkyl or s ( o ) 2 r 6 ; or r f and r q can together form a ring , wherein r 6 can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl , heteroarylalkyl or substituted amino . in one embodiment , when r 5 is or z and r 4 is or c , then r c and r z can be joined together to form a six - membered acetal , wherein the carbon joining the oxygens is substituted with r l and r m wherein r l and r m can be hydrogen , alkyl , alkenyl , alkynyl , cycloalkyl , aryl or aralkyl ; r l and r m together can join to form a cyclic ring ( e . g ., a ( 3 - 8 )- membered cyclic ring ); or r l and r m together can join to form an oxo , wherein the ring optionally can contain one or more heteroatoms selected from o , n or s , and the ring optionally can be substituted with one or more of alkyl , alkenyl , alkynyl , acyl , substituted amino , cycloalkyl , carboxy , oxo , hydroxy , alkoxy , aryloxy , halogen ( e . g ., f , cl , br or i ), aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl , heterocyclylalkyl , — c (═ o ) qr 7 , wherein q can be o or nh , and r 7 can be alkyl , alkenyl , alkynyl , aryl , aralkyl , cycloalkyl , or heteroarylalkyl ; or when q is nh , r 7 also can be heteroaryl , heterocyclyl or heterocyclylalkyl . the term “ alkyl ,” unless otherwise specified , refers to a monoradical branched or unbranched saturated hydrocarbon chain having from 1 to 20 carbon atoms . this term can be exemplified by groups , for example , methyl , ethyl , n - propyl , iso - propyl , n - butyl , iso - butyl , sec - butyl , t - butyl , n - pentyl , isopentyl , neopentyl , n - hexyl , n - decyl , tetradecyl , and the like . alkyl groups may be substituted further with one or more substituents selected from alkenyl , alkynyl , alkoxy , cycloalkyl , cycloalkenyl , acyl , acylamino , acyloxy , alkoxycarbonylamino , azido , cyano , halogen , hydroxy , oxo , thiocarbonyl , carboxy , carboxyalkyl , aryl , heterocyclyl , heteroaryl , arylthio , thiol , alkylthio , aryloxy , nitro , aminosulfonyl , aminocarbonylamino , — nhc (═ o ) r x , — nr a r b , — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , — c (═ o ) heteroaryl , c (═ o ) heterocyclyl , — o — c (═ o ) nr a r b wherein r x , r t , r a and r b are the same as defined earlier , nitro , — s ( o ) m r 6 ( wherein m is an integer from 0 - 2 and r 6 can be alkyl , alkenyl , alkynyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heterocyclylalkyl , heteroarylalkyl or substituted amino ). unless otherwise constrained by the definition , alkyl substituents may be further substituted by 1 - 3 substituents selected from alkyl , carboxy , — nr a r b , — c (═ o ) nr a r b , — oc (═ o ) nr a r b , — nhc (═ o ) nr a r b ( wherein r a and r b are the same as defined earlier ), hydroxy , alkoxy , halogen , cf 3 , cyano , and — s ( o ) m r 6 , ( where r 6 and m are the same as defined earlier ); or an alkyl group as defined above may also be interrupted by 1 - 5 atoms of groups independently chosen from oxygen , sulfur and — nr a —, where r a is chosen from hydrogen , alkyl , cycloalkyl , alkenyl , cycloalkenyl , alkynyl , aryl , acyl , aralkyl , — c (═ o ) or s wherein r s is the same as defined earlier , s ( o ) 2 r 6 ( where r 6 is as defined earlier ), — c (═ o ) nr a r b ( wherein r a and r b are as defined earlier ). unless otherwise constrained by the definition , all substituents may be further substituted by 1 - 3 substituents chosen from alkyl , carboxy , — nr a r b , — c (═ o ) nr a r b , — o — c (═ o ) nr a r b wherein r a and r b are the same as defined earlier hydroxy , alkoxy , halogen , cf 3 , cyano , and — s ( o ) m r 6 , where m and r 6 are the same as defined earlier ; or an alkyl group as defined above that has both substituents as defined above and is also interrupted by 1 - 5 atoms or groups as defined above . the term “ alkenyl ,” unless otherwise specified , refers to a monoradical of a branched or unbranched unsaturated hydrocarbon group preferably having from 2 to 20 carbon atoms with cis or trans geometry . in the event that alkenyl is attached to the heteroatom , the double bond cannot be alpha to the heteroatom . alkenyl groups may further be substituted with one or more substituents selected from alkyl , alkynyl , alkoxy , cycloalkyl , cycloalkenyl , acyl , acylamino , acyloxy , — nhc (═ o ) r x , — nr a r b , — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , — o — c (═ o ) nr a r b ( wherein r a and r b are the same as defined earlier ), alkoxycarbonylamino , azido , cyano , halogen , hydroxy , oxo , thiocarbonyl , carboxy , arylthio , thiol , alkylthio , aryl , aralkyl , aryloxy , heterocyclyl , heteroaryl , heterocyclyl alkyl , heteroaryl alkyl , aminosulfonyl , aminocarbonylamino , alkoxyamino , nitro , or s ( o ) m r 6 ( wherein r 6 and m are the same as defined earlier ). unless otherwise constrained by the definition , all substituents may optionally be further substituted by 1 - 3 substituents selected from alkyl , carboxy , hydroxy , alkoxy , halogen , — cf 3 , cyano , — nr a r b , — c (═ o ) nr a r b , — o — c (═ o ) nr a r b ( wherein r a and r b are the same as defined earlier ) or — s ( o ) m r 6 ( wherein r 6 and m are the same as defined earlier ). the term “ alkynyl ,” unless specified refers to a monoradical of an unsaturated hydrocarbon , preferably having from 2 to 20 carbon atoms . in the event that alkynyl is attached to the heteroatom , the triple bond cannot be alpha to the heteroatom . alkynyl groups may further be substituted with one or more substituents selected from alkyl , alkenyl , alkoxy , cycloalkyl , cycloalkenyl , acyl , acylamino , acyloxy , alkoxycarbonylamino , azido , cyano , halogen , hydroxy , oxo , thiocarbonyl , carboxy , arylthio , thiol , alkylthio , aryl , aralkyl , aryloxy , aminosulfonyl , aminocarbonylamino , nitro , heterocyclyl , heteroaryl , heterocyclylalkyl , heteroarylalkyl , — nhc (═ o ) r x , — nr a r b , — nhc (═ o ) nr x r t , — c (═ o ) nr a r b , — o — c (═ o ) nr a r b ( wherein r x , r t , r a and r b are the same as defined earlier ), — s ( o ) m r 6 ( wherein r 6 and m are the same as defined earlier ). unless otherwise constrained by the definition , all substituents may optionally be further substituted by 1 - 3 substituents chosen from alkyl , carboxy , carboxyalkyl , hydroxy , alkoxy , halogen , cf 3 , — nr a r b , — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , — c (═ o ) nr a r b ( wherein r x , r t , r a and r b are the same as defined earlier ), cyano , and — s ( o ) m r 6 ( where r 6 and m are the same as defined earlier ). the term “ cycloalkyl ,” unless otherwise specified , refers to cyclic alkyl groups of from 3 to 20 carbon atoms having a single cyclic ring or multiple condensed rings , which optionally may contain one or more olefinic bonds . such cycloalkyl groups include , by way of example , single ring structures , for example , cyclopropyl , cyclobutyl , cyclooctyl , cyclopentenyl , and the like , or multiple ring structures , for example , adamantanyl , and bicyclo [ 2 . 2 . 1 ] heptane , or cyclic alkyl groups to which is fused an aryl group , for example , indane , and the like . cycloalkyl groups may further be substituted with one or more substituents selected from alkyl , alkenyl , alkynyl , alkoxy , cycloalkyl , cycloalkenyl , acyl , acylamino , acyloxy , alkoxycarbonylamino , azido , cyano , halogen , hydroxy , oxo , thiocarbonyl , carboxy , carboxyalkyl , arylthio , thiol , alkylthio , aryl , aralkyl , aryloxy , aminosulfonyl , aminocarbonylamino , — nr a r b , — nhc (═ o ) nr x r t , — nhc (═ o ) r x , — c (═ o ) nr a r b , — o — c (═ o ) nr a r b ( wherein r x , r t , r a and r b are the same as defined earlier ), nitro , heterocyclyl , heteroaryl , heterocyclylalkyl , heteroarylalkyl , s ( o ) m — r 6 ( wherein r 6 and m are the same as defined earlier ). unless otherwise constrained by the definition , all substituents may optionally be further substituted by 1 - 3 substituents chosen from alkyl , carboxy , hydroxy , alkoxy , halogen , cf 3 , — nr a r b , — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , — o — c (═ o ) nr a r b ( wherein r x , r y , r a , and r b are the same as defined earlier ), cyano , and — s ( o ) m r 6 ( wherein r 6 and m are the same as defined earlier ). the term “ alkoxy ,” unless otherwise specified , refers to the group o - alkyl , wherein alkyl is the same as defined above . the term “ aralkyl ,” unless otherwise specified , refers to alkyl - aryl linked through alkyl ( wherein alkyl is the same as defined above ) portion and the alkyl portion contains carbon atoms from 1 - 6 and aryl is as defined below . the examples of aralkyl groups include benzyl , ethylphenyl and the like . the term “ aryl ,” unless otherwise specified , refers to a carbocyclic aromatic group , for example phenyl , anthryl , biphenyl or naphthyl ring and the like , optionally substituted with 1 to 3 substituents selected from halogen ( e . g ., f , cl , br , i ), hydroxy , alkyl , alkenyl , alkynyl , cycloalkyl , alkoxy , acyl , aryl , aryloxy , cyano , nitro , cf 3 , ocf 3 , coor e ( wherein r e can be hydrogen , alkyl , alkenyl , cycloalkyl , aralkyl , heterocyclylalkyl , heteroarylalkyl ), nhc (═ o ) r x , — nr a r b , — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , — o — c (═ o ) nr a r b ( wherein r a and r b are the same as defined earlier ), —( so 2 ) m r 6 ( wherein r 6 and m are the same as defined earlier ), carboxy , heterocyclyl , heteroaryl , heterocyclylalkyl , heteroarylalkyl or amino carbonyl amino . the aryl group may optionally be fused with cycloalkyl group , wherein the cycloalkyl group may optionally contain heteroatoms selected from o , n or s . the term “ aryloxy ” denotes the group o - aryl wherein aryl is the same as defined above . the term “ heteroaryl ,” unless otherwise specified , refers to an aromatic ring structure containing 5 or 6 carbon atoms , or a bicyclic aromatic group having 8 to 10 carbon atoms , with one or more heteroatom ( s ) independently selected from n , o or s , optionally substituted with 1 to 4 substituent ( s ) selected from halogen ( e . g ., f , cl , br , i ), hydroxy , alkyl , alkenyl , alkynyl , cycloalkyl , acyl , carboxy , aryl , alkoxy , aralkyl , cyano , nitro , — nr a r b , —( ch 2 ) w c (═ o ) r g ( wherein w is an integer from 1 - 4 and r 9 is hydroxy , or z , nr a r b , — nhor z or — nhoh ), — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , — s ( o ) m r 6 , or — o — c (═ o ) nr a r b ( wherein m , r 6 , r z , r t , r x , r a and r b are the same as defined earlier ). unless or otherwise constrained by the definition , of the substituents are attached to the ring atom , be it carbon or heteroatom . examples of heteroaryl groups are pyridinyl , pyridazinyl , pyrimidinyl , pyrrolyl , oxazolyl , thiazolyl , thienyl , isoxazolyl , triazinyl , furanyl , benzofuranyl , indolyl , benzothiazolyl , benzoxazolyl , and the like . the term “ heterocyclyl ,” unless otherwise specified , refers to a non aromatic monocyclic or bicyclic cycloalkyl group having 5 to 10 atoms in which 1 to 4 carbon atoms in a ring are replaced by heteroatoms selected from o , s or n , and are optionally benzofused or fused heteroaryl of 5 - 6 ring members and / or are optionally substituted with one or more of halogen ( e . g ., f , cl , br , i ), hydroxy , alkyl , alkenyl , alkynyl , cycloalkyl , acyl , aryl , alkoxy , alkaryl , cyano , nitro , oxo , carboxy , — c (═ o ) nr a r b , so 2 r 6 , — o — c (═ o ) nr a r b , — nhc (═ o ) nr x r t , or — nr a r b ( wherein r 6 , r x , r t , r a and r b are the same as defined earlier ). unless or otherwise constrained by the definition , the substituents are attached to the ring atom , be it carbon or heteroatom . also unless or otherwise constrained by the definition the heterocyclyl ring may optionally contain one or more olefinic bond ( s ). examples of heterocyclyl groups include oxazolidinyl , tetrahydrofuranyl , dihydrofuranyl , benzoxazinyl , benzthiazinyl , benzimidazolyl , carbaxolyl , indolyl , phenoxazinyl , phenothiazinyl , dihydropyridinyl , dihydroisoxazolyl , dihydrobenzofuryl , azabicyclohexyl , dihydroindolyl , pyridinyl , isoindole 1 , 3 - dione , piperidinyl or piperazinyl . “ heteroarylalkyl ,” unless otherwise specified , refers to alkyl - heteroaryl group linked through alkyl portion , wherein the alkyl and heteroaryl are the same as defined earlier . “ heterocyclylalkyl ,” unless otherwise specified , refers to alkyl - heterocyclyl group linked through alkyl portion , wherein the alkyl and heterocyclyl are the same as defined earlier . “ acyl ,” unless otherwise specified , refers to — c (═ o ) r ″ wherein r ″ is selected from alkyl , cycloalkyl , aryl , aralkyl , heteroaryl , heterocyclyl , heteroarylalkyl or heterocyclylalkyl . “ substituted amino ,” unless otherwise specified , refers to a group — n ( r k ) 2 , wherein each r k is independently selected from hydrogen ( provided that both r k groups are not hydrogen ( defined as “ amino ”)), alkyl , alkenyl , alkynyl , aralkyl , cycloalkyl , aryl , heteroaryl , heterocyclyl , heterocyclylalkyl , heteroarylalkyl , acyl , s ( o ) m r 6 ( wherein m and r 6 is the same as defined above ), — c (═ r y ) nr a r b ( wherein r y , r a and r b are the same as defined earlier ) or nhc (═ r y ) nr t r x ( wherein r y , r t and r x are the same as defined earlier ). unless otherwise constrained by the definition , all substituents may optionally be further substituted by 1 - 3 substituents chosen from alkyl , aralkyl , cycloalkyl , aryl , heteroaryl , heterocyclyl , carboxy , carboxyalkyl , hydroxy , alkoxy , halogen , cf 3 , cyano , — c (═ r y ) nr a r b , — o ( c ═ o ) nr a r b ( wherein r a , r b and r y are the same as defined earlier ) and — oc (═ r y ) nr a r b , — s ( o ) m r 6 ( where r 6 is the same as defined above and m is 0 - 2 ). the term “ leaving group ,” unless otherwise specified , generally refers to groups that exhibit the desirable properties of being labile under the defined synthetic conditions and also , of being easily separated from synthetic products under defined conditions . examples of such leaving groups include , but are not limited to , halogen ( e . g ., f , cl , br , i ), triflates , tosylate , mesylates , alkoxy , thioalkoxy , hydroxy radicals and the like . the term “ activated derivative of a carboxylic acid ,” for example , that of a suitable protected amino acid , aliphatic acid or an aromatic acid , refer to the corresponding acyl halide ( e . g ., acid fluoride , acid chloride or acid bromide ), corresponding activated esters ( e . g ., nitro phenyl ester , the ester of 1 - hydroxybenzotriazole or the ester of hydroxysuccinimide , hosu ) or a mixed anhydride for example anhydride with ethyl chloroformate and other conventional derivatives within the skill of the art . the term “ protecting groups ,” unless otherwise specified , refers to moieties that prevent chemical reaction at a location of a molecule intended to be left unaffected during chemical modification of such molecule . unless otherwise specified , protecting groups may be used on groups , such as hydroxy , amino , or carboxy . examples of protecting groups are found in t . w . greene and p . g . m . wuts , “ protective groups in organic synthesis ”, 2 nd ed ., john wiley and sons , new york , n . y ., which is incorporated herein by reference . the species of the carboxylic protecting groups , amino protecting groups or hydroxy protecting groups employed are not critical , as long as the derivatised moieties / moiety is / are stable to conditions of subsequent reactions and can be removed without disrupting the remainder of the molecule . the terms “ pharmaceutically acceptable salts ” or “ pharmacologically acceptable salts ,” unless otherwise specified , refer to derivatives of compounds that can be modified by forming their corresponding acid or base salts . examples of pharmaceutically acceptable salts include , but are not limited to , mineral or organic acids salts of basic residues ( such as amines ), or alkali or organic salts of acidic residues ( such as carboxylic acids ), and the like . the term “ amino acid ,” unless otherwise specified , refers to both natural and unnatural amino acids . the term “ natural amino acid ,” unless otherwise specified , refers to the twenty two naturally occurring amino acids glycine , alanine , valine , leucine , isoleucine , serine , methionine , threonine , phenylalanine , tyrosine , trytophan , cysteine , proline , proline , histidine , aspartic acid , asparagines , glutamic acid , glutamine , γ - carboxyglutamic acid , arginine , ornithine and lysine in their l form . the term “ unnatural amino acid ,” unless otherwise specified , refers to the ‘ d ’ form of the twenty two naturally occurring amino acids described above . it is further understood that the term unnatural amino acid includes homologues of the natural amino acids , and synthetically modified form of the natural amino acids commonly utilized by those in the peptide chemistry arts when preparing synthetic analogues of naturally occurring peptides , including d and l forms . the synthetically modified forms include amino acids having alkylene chains shortened or lengthened by up to two carbon atoms , amino acids comprising optionally substituted aryl groups , and amino acids comprised halogenated groups preferably halogenated alkyl and aryl groups . the term “ unnatural amino acids ,” unless otherwise specified , also refers to beta amino acids . the term “ peptide ,” unless otherwise specified , refers to a molecule comprising a series of amino acids linked through amide linkages . a dipeptide refers to a peptide having 2 amino acids , a tripeptide refers to a peptide having 3 amino acids and tetrapeptide refers to a peptide having four amino acids , wherein the term amino acid is as defined earlier . the compounds of this invention contain one or more asymmetric carbon atoms and thus , can exist as racemates and racemic mixtures , single enantiomers , diastereomeric mixtures or individual diastereomers . all such isomeric forms of these compounds are expressly encompassed by the present invention . each stereogenic carbon can have an r or s configuration . although the specific compounds exemplified in this application may be depicted in a particular stereochemical configuration , compounds having either the opposite stereochemistry at each chiral center , or mixtures thereof , are contemplated in the invention . although amino acids and amino acid side chains may be depicted in a particular configuration , both natural and unnatural forms are contemplated in the invention . also , geometric isomers of olefins , c ═ n double bonds and the like , can be present in the compounds of this invention , and all such stable isomers are contemplated in the present invention . the compounds of the present invention can be prepared by techniques well known in the art and familiar to skilled synthetic organic chemist . in addition , the compounds of the present invention can be prepared , for example , by following the reaction schemes as depicted . a compound of formula iv can be prepared following scheme i . accordingly , a compound of formula ii ( wherein r 1 , r 2 , r 3 and r 5 are as described earlier ) reacts with a compound of formula iii ( wherein x is o , s and r f is same as described earlier ) to form a compound of formula iv . this reaction can be carried out in an organic solvent , for example , dichloromethane , dichloroethane , chloroform or carbon tetrachloride . 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[( phenyl - sulfonyl )- amino ]- carbonyl }- 6 - deoxy - α - l - sorbofuranoside ( compound no . 1 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - chloro - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 2 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ phenyl - sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 3 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 4 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 5 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - chloro - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 6 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( phenyl - sulfonyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 7 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( phenylsulfonyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 8 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - α - l - sorbofuranoside ( compound no . 9 ); hydrochloride salt of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 10 ); hydrochloride salt of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - chloro - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 11 ); 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 12 ); 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 13 ); hydrochloride salt of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 14 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 15 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 16 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 17 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - piperidinyl )- α - l - sorbofuranoside ( compound no . 18 ); 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 19 ); 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 -[ 2 - hydroxy - 2 - oxo - ethyl ]- phenyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 20 ); tris salt of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 21 ); tris salt of - 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 22 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - piperidinyl )- α - l - sorbofuranoside ( compound no . 23 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 24 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 25 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 26 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -[ 4 -( 2 - hydroxy - 2 - oxo - phenyl )- amino ]- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 27 ); tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -[( 4 -{ 2 - hydroxy - 2 - oxo - ethyl }- phenyl )- amino ]- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - pyrrolidinyl )- ethyl ]- amino - α - l - sorbofuranoside ( compound no . 28 ); tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -[{ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl }- amino ]- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - piperidinyl )- ethyl ] amino - α - l - sorbofuranoside . ( compound no . 29 ); tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -[ 2 -( 4 - morpholinyl )- ethyl ]- amino - α - l - sorbofuranoside ( compound no . 30 ); tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - cycloheptyl - amino )- ethyl ]- amino - α - l - sorbofaranoside ( compound no . 31 ). a compound of formula x and xii can be prepared , for example , following scheme ii . accordingly , a compound of formula v ( wherein r 1 , r 2 and r 3 are same as defined earlier ) can oxidize to form a compound of formula vi . this reaction can be carried out in an organic solvent , for example , dichloromethane , diethyl ether , tetrahydrofuran in the presence of oxidizing agents , for example , pyridinium dichromate ; pyridinium chlorochromate ; dimethylsulfoxide in combination with acetic anhydride , oxalyl chloride , or trifluoroacetic anhydride ; periodinane , or mixtures thereof . the compound of formula vi can react with hydroxylamine hydrochloride to form a compound of formula vii . this reaction can be carried out in an organic solvent , for example , ethanol , methanol , propanol or isopropyl alcohol in the presence of a base , for example pyridine , diisopropylethylamine , triethylamine , or mixtures thereof . the compound of formula vii can be reduced to a compound of formula viii . this reaction can be carried out in an organic solvent , for example , tetrahydrofuran , dimethylformamide , diethylether , dioxane , or a mixture thereof in the presence of at least one reducing agent , for example , lithium aluminum hydride , sodium borohydride , or a mixture thereof . the compound of formula viii can be reacted via path a to form a compound of formula x . accordingly in path a , the compound of formula viii can be reacted with a compound of formula ix ( wherein r d is same as defined earlier , l is a leaving group , for example , oh ( activated in - situ , as known to a skilled practitioner ) or halogen ( e . g ., cl , br or i ) and y is c ═ o or so 2 ) to give the compound of formula x . the reaction of a compound of formula viii with a compound of formula ix ( wherein y is c (═ o ) and l is oh ) to give a compound of formula x ( path a ) through the intermediacy of an activated derivative of a carboxylic acid can be carried out in an organic solvent , as well as in the presence of at least one condensing agent and / or an base . examples of the organic solvent include dimethylformamide , dioxane , tetrahydrofuran , or a mixture thereof . examples of the at least one condensing agent include 1 -( 3 - dimethylaminopropyl )- 3 - ethyl carbodiimide hydrochloride , dicyclohexylcarbodiimide , or a mixture thereof . examples of a base include n - methylmorpholine , diisopropylamine , triethylamine , or a mixture thereof . alternatively , this reaction can be carried out through a mixed anhydride by reacting the compound of formula ix with a chloroformate , for example , ethyl chloroformate or isobutylchloroformate . the reaction of a compound of formula viii with a compound of formula ix ( wherein y is c ═ o or so 2 and l is cl ) to give a compound of formula x ( path a ) can be carried out in an organic solvent and in the presence of a base . examples of organic solvents include dichloromethane , dichloroethane , chloroform carbon tetrachloride , tetrahydrofuran , dimethylformamide , or mixtures thereof . examples of bases include pyridine , triethylamine , diisopropylethylamine or mixtures thereof . the compound of formula viii also can be reacted via path b to form a compound of formula xii . accordingly in path b , the compound of formula viii is reacted with a compound of formula iii or with a compound of formula xi ( wherein ar is aryl , r f is same as defined earlier ) to form a compound of formula xii . the reaction of a compound of formula viii with a compound of formula iii or a compound of formula xi to give a compound of formula xii ( path b ) can be carried out in an organic solvent and in the presence of a base . examples of organic solvents include dichloromethane , dichloroethane , dimethylsulfoxide , tetrahydrofuran , dimethylformamide , or mixtures thereof . examples of bases include triethylamine , diisopropylethylamine , pyridine , or mixtures thereof . ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -[{[( 4 - fluoro - phenyl )- amino ]- carbonyl }- amino ]- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 32 ); ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -{[( butyl - amino )- carbonyl ]- amino }- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 33 ); ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -{[( 4 - fluoro - phenyl )- sulfonyl ]- amino }- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 34 ); ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -{[( 4 - fluoro - phenyl )- carbonyl ]- amino }- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 35 ); ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -[{[( 2 - phenylethyl )- amino ]- thiocarbonyl }- amino ]- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 36 ); ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -[ f {[( 4 -[ 2 - hydroxy - 2 - oxo - ethyl ]- phenyl )- amino ]- carbonyl }- amino ]- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 37 ); ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 -{[ 3 -( 1 , 3 - benzodionol - 5 - yl )- propanoyl ]- amino }- α - l - erythro - hex - 2 - ulofuranoside ( compound no . 38 ). compounds of formula xvii and xviii can be prepared following scheme iii . accordingly , path a : a compound of formula xiii can be reacted with a compound of formula xiv ( wherein p is a protecting group , for example , aralkyl or acyl ) to form a compound of formula xv . the compound of formula xiv can be deprotected to form a compound of formula xvi under deprotection conditions . this reaction can be carried in an organic solvent , for example , methanol , ethanol , propanol , isopropylalcohol , tetrahydrofuran or ethyl acetate . examples of deprotection conditions include hydrogenation utilizing palladium on carbon or under catalytic transfer hydrogenation condition of ammonium formate and palladium on carbon . alternatively , the tosylate can be displaced with an azido group , reduction of which would yield a compound of formula xvi . path b : a compound of formula xiii can be reacted with sodium azide to form a compound of formula xiiia . this reaction can be carried out in an organic solvent , for example , tetrahydrofuran , dimethylformamide , diethylether , dioxane , or a mixture thereof . a compound of formula xiiia can be reacted with compound of formula xiiib ( wherein r 8 is alkyl ) to form a compound of formula xiiic . this reaction can be carried out in an organic solvent and a base . examples of organic solvents include , for example , tetrahydrofuran , dimethylformamide , diethyl ether , dioxane , or a mixture thereof . examples of bases include sodium hydride or potassium tert - butoxide . a compound of formula xiiic can be reduced to form a compound of formula xvi . this reaction can be carried in an organic solvent , for example , methanol , ethanol , propanol , isopropylalcohol , tetrahydrofuran or ethyl acetate using catalysts for example palladium on carbon or platinum on carbon in the presence of hydrogen . the compound of formula xvi ( wherein r 9 is hydrogen or alkyl ) can be reacted with a compound of formula ix via path a to form a compound of formula xvii . the reaction of a compound of formula xvi with a compound of formula ix ( when y is c (═ o ) and l is oh ) to give a compound of formula xvii ( path a ) through the intermediacy of an activated derivative of a carboxylic acid , can be carried out in an organic solvent , in the presence of condensing agents and in the presence of a base . examples of organic solvents include dichloromethane , dioxane or tetrahydrofuran . examples of condensing agents include 1 -( 3 - dimethylaminopropyl )- 3 - ethyl carbodiimide hydrochloride or dicyclohexylcarbodiimide . examples of bases include n - methylmorpholine , diisopropylethylamine or triethylamine . alternatively , this reaction can be carried out through mixed anhydride by reacting compound of formula ix with a chloroformate , for example , ethyl chloroformate or isobutylchloroformate . the reaction of a compound of formula xvi with a compound of formula ix ( when y is c ═ o or so 2 and l is cl ) to give a compound of formula xvii ( path a ) can be carried out in an organic solvent and in the presence of a base . examples of organic solvents include dichloromethane , dichloroethane , chloroform , carbon tetrachloride , tetrahydrofuran or dimethylformamide . examples of bases include pyridine , triethylamine or diisopropylethylamine . the compound of formula xvi can be reacted with a compound of formula iii or with a compound of formula xi via path b to give a compound of formula xviii . this reaction can be carried out in an organic solvent and optionally in the presence of a base . examples of organic solvents include dichloromethane , dichloroethane , dimethylsulfoxide , tetrahydrofuran or dimethylformamide . examples of bases include triethylamine , diisopropylethylamine or pyridine . 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - fluorophenyl )- amino ]- carbonyl }- amino - α - l - sorbofuranoside ( compound no . 39 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -[( 4 - fluorophenyl )- sulfonyl ]- amino - α - l - sorbofuranoside ( compound no . 40 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -( ethylsulfonyl )- amino - α - l - sorbofuranoside ( compound no . 41 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 4 - fluoro - phenyl )- carbonyl }- amino - α - l - sorbofuranoside ( compound no . 42 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[ 3 -( 1 , 3 - benzodioxol - 5 - yl )- propanoyl ]- amino }- α - l - sorbofuranoside ( compound no . 43 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[{( 4 -[ 2 - hydroxy - 2 - oxo - ethyl ]- phenyl )- amino }- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 44 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( butyl - amino )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 45 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -({[( 4 - fluoro - phenyl )- amino ]- thiocarbonyl }- amino )- α - l - sorbofuranoside ( compound no . 46 ). 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -[({[ 2 -( carboxymethyl ) phenyl ] amino }- carbonyl ) amino ]- α - l - sorbofuranoside ( compound no . 66 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -[({[ 3 -( carboxymethyl ) phenyl ] amino }- carbonyl ) amino ]- α - l - sorbofuranoside ( compound no . 67 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - trifluoromethyl ) benzoyl ] amino }- α - l - sorbofuranoside ( compound no . 68 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - fluorophenyl ) acetyl } amino ]- α - l - sorbofuranoside ( compound no . 69 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 3 - fluorobenzoyl ) amino }- α - l - sorbofuranoside ( compound no . 70 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( quinolin - 2 - ylcarbonyl ) amino }- α - l - sorbofuranoside ( compound no . 71 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 2 - thienylacetyl ) amino }- α - l - sorbofuranoside ( compound no . 72 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 73 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 74 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 3 , 4 - dimethoxybenzoyl ) amino }- α - l - sorbofuranoside ( compound no . 75 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( isoquinolin - 1 - ylcarbonyl ) amino }- α - l - sorbofuranoside ( compound no . 76 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[ 4 -( acetylamino ) benzoyl ] amino }- α - l - sorbofuranoside ( compound no . 77 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( pyridin - 4 - yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 78 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 6 - dichloropyridin - 4 - yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 79 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( quinolin - 3yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 80 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 5 - methyl - 3 - phenylisoxazol - 4 - yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 81 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( phenyl ) acetyl }- amino - α - l - sorbofuranoside ( compound no . 82 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - chlorophenyl ) acetyl ] amino - α - l - sorbofuranoside ( compound no . 83 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 5 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 84 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 85 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 86 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 87 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 4 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 88 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 6 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 89 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - methylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 90 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 91 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 5 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 92 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 4 , 5 - trifluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 93 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 - dichlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 94 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - hydroxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 95 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - methylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 96 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 97 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -[( 1 , 3 - benzodioxol - 5 - ylacetyl ) amino ]- l - sorbofuranoside ( compound no . 98 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - hydroxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 99 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - hydroxy - 3 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 100 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - isopropylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 101 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[ biphenyl - 4 - ylacetyl ] amino }- α - l - sorbofuranoside ( compound no . 102 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - methylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 103 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - fluoro - 6 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 104 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - chloro - 4 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 105 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - trifluoromethoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 106 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - trifluoromethoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 107 ); 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o - methyl - 6 - deoxy - 6 -{[( 4 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 108 ); 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 109 ); 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 dichlorophenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 110 ); 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 111 ); 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 112 ); or 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 113 ). a compound of formula xxiii can be prepared by scheme iv . thus , a compound of formula xiii can be reacted with a compound of formula xix ( wherein p is a protecting group , for example , aralkyl or acyl ) to form a compound of formula xx ( wherein r 1 , r 2 and r 3 is same as defined earlier ). the compound of formula xx can be deprotected to form a compound of formula xxi . the deprotection can be carried out in an organic solvent and under conditions of deprotection . examples of organic solvents include methanol , ethanol , propanol , isopropylalcohol , tetrahydrofuran or ethyl acetate . examples of conditions of deprotection include hydrogenatically utilizing palladium on carbon or under catalytic transfer hydrogenation conditions of ammonium formate and palladium on carbon . the compound of formula xxi can be reacted with a compound of formula xxii ( wherein hal is halogen , and r x is same as defined earlier ) to yield a compound of formula xxiii . this reaction can be carried out in an organic solvent and in the presence of a base . examples of organic solvents include dichloromethane , dichloroethane , chloroform , carbon tetrachloride , tetrahydrofuran or dimethylformamide . examples of bases include pyridine , triethylamine or diisopropylethylamine . a compound of formula xxix can be prepared following scheme v . thus , a compound of formula xxv can be reacted with a compound of formula xxvi to form a compound of formula xxvii . the reaction can be carried out in an organic solvent and a base in the presence of a phase transfer catalyst . examples of organic solvents include , for example , dimethylsulfoxide or n , n - dimethylformamide . examples of bases include , for example , potassium hydroxide or sodium hydroxide . examples of phase transfer catalysts include , for example , tetrabutylammonium iodide or tetrabutylammonium bromide . the compound of formula xxvii can be reacted with a compound of formula xxviii ( wherein r f is same as described earlier ) to yield a compound of formula xxix . the reaction can be carried out in an organic solvent , for example , dichloromethane , dichloroethane , chloroform or carbon tetrachloride . compounds prepared using scheme v include , but are not limited to : 1 - o -[ 6 -{( 4 - nitro - phenyl )- amino - carbonyloxy }- hexyl ]- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( compound no . 48 ); 1 - o -[ 6 -{( 4 - chloro - phenyl )- amino - carbonyloxy }- hexyl ]- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( compound no . 49 ); 1 - o -[ 6 -{( 4 - methoxy - phenyl - amino - carbonyloxy )- hexyl ]- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( compound no . 50 ); or 1 - o -{ 6 -[( 4 - methyl - phenyl )- amino - carbonyloxy }- hexyl ]- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( compound no . 51 ). a compound of formula xxxi can be prepared by following scheme vi . thus , the compound of formula v ( wherein r 1 , r 2 and r 3 are same as defined earlier ) can be oxidized to the compound of formula vi . the compound of formula vi can be reacted with a grignard reagent to form a compound of formula xxx . this reaction can be carried out in an organic solvent , for example , dry tetrahydrofuran or diethylether . examples of grignard reagents include , for example , alkyl magnesium chloride , for example , methyl magnesium chloride . the compound of formula xxx can be reacted with a compound of formula xxviii ( wherein r f is same as described earlier ) to form a compound of formula xxxi . this reaction can be carried out in an organic solvent and in the presence of a base . examples of organic solvents include , for example , dichloromethane , dichloroethane , dimethylsulfoxide , tetrahydrofuran or dimethylformamide . examples of bases include , for example , triethylamine , diisopropylethylamine or pyridine . ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 52 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -{[( phenylsulfonyl )- amino ]- carbonyl }- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 53 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - methyl - phenyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 54 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - chloro - phenyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 55 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -{[{ 2 , 5 - dichloro - phenyl )- sulfonyl }- amino ]- carbonyl }- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 56 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 2 - methyl - phenyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 57 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - piperidinyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 58 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - azepanyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 59 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - morpholinyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 60 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - pyrrolidinyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 61 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o - heptyl - 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 62 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - dimethylamino )- propyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 63 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 2 - azepanyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 64 ) ( 4ξ )- 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - methylphenyl ) sulphonyl ] amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 114 ), ( 4ξ )- 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 2 - methylphenyl ) sulphonyl ] amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 115 ), ( 4ξ )- 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - chlorophenyl ) sulphonyl ] amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 116 ), ( 4ξ )- 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[ phenylsulphonyl ] amino } carbonyl ]- 6 - deoxy - α - l erythro - hex - 2 - ulofuranoside ( compound no . 117 ), or ( 4ξ )- 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - fluorophenyl ) sulphonyl ] amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 118 ). a compound of formula xxxiii can be prepared following scheme vii . thus , a compound of formula xxxii ( wherein r 1 , r 2 and r 3 are as described earlier ) can be reacted with the compound of formula xxviii ( wherein r f is same as described earlier ) to form the compound of formula xxxiii . this reaction can be carried out in an organic solvent and optionally in the presence of a base . examples of organic solvents include , for example , dichloromethane , dichloroethane , tetrahydrofuran or dioxane . examples of bases include , for example , triethylamine , diisopropylethylamine or pyridine . a particular illustrative compound prepared through scheme vii is , for example : wherever esters are specified in the compounds disclosed above , one of ordinary skill in the art optionally could hydrolyze them to their respective acids . for example , hydrolysis of alkyl esters ( for example , ethyl , methyl or benzyl ester ) to their corresponding acids can be carried out in the presence of a base ( for example , lithium hydroxide , sodium hydroxide or potassium hydroxide ). alternatively , hydrolysis of benzyl esters can be carried out hydrogenatically using catalysts ( for example , palladium on carbon or platinum on carbon ). esters , for example , tert - butyl , can be hydrolyzed to their corresponding acids in the presence of acid ( for example , trifluoroacetic acid or hydrochloric acid ). where specific bases , acids , solvents , condensing agents , hydrolyzing agents and other reagents are mentioned in the above schemes , it is understood that other acids , bases , solvents , condensing agents , hydrolyzing agents and other reagents known to those skilled in the art also may be used . similarly , reaction temperatures and duration of reactions may be adjusted according to the desired needs . suitable salts of the compounds represented by formula i are pharmacologically acceptable salts and can be prepared so as to solubilize the compound in aqueous medium for biological evaluations , as well as to be compatible with various dosage formulations and to aid in the bioavailability of the compounds . examples of such salts include inorganic acid salts ( e . g ., hydrochloride , hydrobromide , sulfate , nitrate or phosphate ), organic acid salts ( e . g ., acetate , tartrate , citrate , fumarate , maleate , toluenesulfonate or methanesulfonate ). when free carboxylic acid groups are included in the formula i as substituents , they may form organic and inorganic base salts ( for example , tris ( hydroxymethyl ) aminomethane , sodium , potassium , calcium , magnesium , or ammonium and the like ). these salts may be prepared by prior art techniques known to one of ordinary skill in the art , for example , treating the compound with an equivalent amount of inorganic or organic base in water . while the present invention has been described in terms of its specific embodiments , certain modifications and equivalents will be apparent to those skilled in the art and are included within the scope of the present invention . wherein w is h and r 2 & amp ; r 3 together form isopropylidene radical wherein w is h and r 2 & amp ; r 3 and r c ( when r 4 is or c ) and r z ( when r 5 is or z ) together form isopropylidene radical the examples mentioned below demonstrate the general synthetic procedure as well as the specific preparation for the preparation for the preferred compound . the examples are given to illustrate particular aspects of the invention and do not limit the scope of the present invention . the compound 1 - methyl - 5 -( 2 - methoxy - phenyl )- 3 - propyl - 1 , 6 - dihydro - pyrazolo [ 4 , 3 - d ] pyrimidin - 7 - one was added in small portions to a cooled solution of chlorosulfonic acid . the temperature of the reaction mixture was maintained at about 10 - 15 ° c . and stirred for 5 - 6 hours . thionyl chloride was slowly added and the reaction mixture was stirred for an additional 20 hours . reaction mixture was poured onto crushed ice followed by the addition of dichloromethane and stirred for 15 minutes . the reaction mixture was filtered through celite pad . the organic layer was collected and the solvent was evaporated off . the solvent was dried over anhydrous sodium sulfate . the residue thus obtained was triturated with hexane and filtered to obtain the title compound . triethylamine ( 3 . 5 ml ) and methanesulphonylchloride ( 1 . 4 ml ) were added to a solution of 2 - butoxyethanol ( 2 gm ) in dichloromethane ( 40 ml ) at 0 ° c . and stirred for 1 hour at the same temperature . the reaction mixture was taken in water and extracted with dichloromethane , the combined organic layers were dried over anhydrous sodium sulfate . the dichloromethane was evaporated under the reduced pressure to get the desired crude title compound ( 3 . 8 gm ). sodium hydride ( 406 mg ) was added to a solution of 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( 4 gm ) in dimethylformamide ( 50 ml ) at 0 ° c . and stirred for about 10 mins . to the reaction mixture was added methanesulphonic acid 2 - butoxy - ethyl ester ( 3 gm ) obtained from step a above at the same temperature and further stirred for 2 hrs at room temperature . the reaction mixture was taken in water and extracted with ethyl acetate , the combined organic layers were dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield crude product , which was purified by column chromatography , using 20 % ethylacetate - hexane as eluant to yield the title compound ( 3 gm ). hclo 4 ( 1 . 7 gm ) was added to a solution of 1 - o -( 2 - butoxyethyl )- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( 3 gm ) obtained from step b above in tetrahydrofuran ( 20 ml ) at 0 ° c ., and stirred for 4 hrs at the same temperature . excess hclo 4 was neutralized by addition of dilute sodium hydroxide solution . the reaction mixture was extracted with ethyl acetate and the combined organic layers were dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield crude product , which was purified by column chromatography , using 30 % ethyl acetate - hexane as eluant to yield the title compound ( 2 . 6 gm ). triethylamine ( 1 . 7 ml ) and p - toluenesulfonylchloride ( 1 . 7 gm ) were added to a solution of 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - α - l - sorbofuranoside ( 2 . 6 gm ) obtained from step c above in dichloromethane ( 60 ml ) at room temperature and stirred for 12 hrs . then reaction mixture was taken in water and extracted with dichloromethane . the combined organic layers were dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield crude product , which was purified by column chromatography , using 30 % ethyl acetate - hexane as eluant to yield the title compound ( 2 . 0 gm ). nmr . ( 400 mhz , cdcl 3 ): δ 7 . 82 ( d , 2h , 8 hz ), 7 . 33 ( d , 2h , 8 hz ), 4 . 41 ( s , 1h ), 4 . 35 ( s , 1h ), 4 . 32 - 4 . 33 ( m , 1h ), 4 . 21 - 4 . 22 ( m , 2h ), 3 . 65 - 3 . 75 ( m , 5h ), 3 . 37 - 3 . 39 ( m , 4h ), 2 . 44 ( s , 3h ), 1 . 50 - 1 . 54 ( m , 2h ), 1 . 46 ( s , 3h ), 1 . 35 ( s , 3h ), 0 . 88 - 0 . 99 ( m , 3h ) benzenesulfonyl isocyanate ( 0 . 057 ml ) was added to a solution of 1 - o - decyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l sorbofuranoside ( 150 mg ) in dichloromethane ( 10 ml ) at 0 ° c ., stirred for 1 hour at this temperature and followed by stirring at room temperature for 3 hours . the solvent was evaporated under reduced pressure and the residue was purified over silica gel column using 30 % ethyl acetate - hexane as eluent to yield the title compound ( 210 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 8 . 04 ( 2h , d , j = 9 hz ), 7 . 61 ( 3h , m ), 4 . 98 ( 1h , s ), 4 . 45 ( 2h , s ), 3 . 62 - 3 . 46 ( 5h , m ), 1 . 59 ( 2h , m ), 1 . 48 ( 3h , s ), 1 . 36 ( 3h , s ), 1 . 27 ( 14h , m ), 1 . 06 ( 3h , d , j = 6 hz ), 0 . 87 ( 3h , d , j = 6 hz ) analogs of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[( phenyl - sulfonyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 1 ) listed below can be prepared by replacing benzene sulfonyl isocyanate with the appropriate isocyanate , as applicable in each case : 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - chloro - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 2 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ phenyl - sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 3 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 4 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- o - l - sorbofuranoside ( compound no . 5 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - chloro - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 6 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( phenyl - sulfonyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 7 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( phenylsulfonyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 8 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - α - l - sorbofuranoside ( compound no . 9 ), hydrochloride salt of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - methyl - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside . ( compound no . 10 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 - chloro - phenyl )- sulfonylamino ]- carbonyl }- 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside . ( compound no . 11 ). methyl 4 - isocyanatophenyl acetate ( 0 . 57 g ) was added dropwise with continuous stirring to a solution of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( 1 . 0 g ) ( prepared as described in u . s . pat . no . 5 , 637 , 570 ) in dichloromethane ( 20 ml ) at 0 - 5 ° c . the reaction mixture was allowed to warm to room temperature and after 24 hours , dichloromethane was removed under reduced pressure to obtain crude product . the crude residue thus obtained was purified by column chromatography using 30 % ethyl acetate - hexane as eluent to yield the title compound ( 1 . 40 g ). 1 hnmr ( cdcl 3 , 300 mhz ): δ 7 . 32 - 7 . 35 ( 2h , m ), 7 . 26 - 7 . 12 ( 2h , m ), 6 . 78 ( 1h , bs , nh ), 5 . 23 ( 1h , bs ), 4 . 55 - 4 . 50 ( 2h , m ), 3 . 67 - 3 . 62 ( 4h , m ), 3 . 57 - 3 . 47 ( 5h , m ), 2 . 80 ( 2h , d , 5 . 9 hz ), 2 . 72 - 2 . 67 ( 4h , m ), 1 . 77 ( 1h , bs ), 1 . 591 . 48 ( 10h , m ), 1 . 38 ( 3h , s ), 1 . 24 ( 10h , bs ), 0 . 84 ( 3h , t , 6 . 3 hz ). analogs of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - ethoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 12 ) described below can be prepared by replacing methyl 4 - isocyanatophenylacetate with the appropriate isocyanate , as applicable in each case . 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 13 ), hydrochloride salt of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 14 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 15 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 16 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 17 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - methoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - piperidinyl )- α - l - sorbofuranoside ( compound no . 18 ). 1n sodium hydroxide ( 50 ml ) was added to a solution of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - ethoxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( 1 . 20 g ) ( obtained from example 2 ) in methanol ( 20 ml ), and the reaction mixture was stirred at 50 ° c . after 5 hours , methanol was removed under reduced pressure and the reaction mixture was treated with dilute hcl until ˜ ph 5 was obtained . the solid thus separated was extracted with ethyl acetate . the organic extracts were washed with water and brine and dried over anhydrous sodium sulfate . the residue thus obtained was purified by column chromatography using 30 % ethyl acetate - hexane as eluent to furnish the title compound ( 0 . 95 g ). 1 hnmr ( cdcl 3 , 300 mhz ): δ 7 . 26 - 7 . 00 ( 4h , m ), 6 . 5 ( 1h , bs ), 5 . 15 ( 1h , bs ), 4 . 60 ( 1h , bs ), 3 . 69 - 3 . 63 ( 1h , m ), 3 . 58 ( 3h , m ), 3 . 26 - 3 . 21 ( 1h , m ), 3 . 10 - 3 . 04 ( 3h , bs ), 2 . 89 ( 3h , m ), 2 . 78 ( 3h , m ), 1 . 76 ( 4h , bs ), 1 . 62 - 1 . 52 ( 4h , m ), 1 . 48 - 1 . 38 ( 95h , m ), 1 . 38 - 1 . 35 ( 3h , m ), 1 . 31 - 1 . 25 ( 8h , bs ), 0 . 86 ( 3h , t , 7 . 7 hz ). analogs of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 19 ) described below can be prepared by hydrolyzing the respective esters to their corresponding acids . 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[( 4 -[ 2 - hydroxy - 2 - oxo - ethyl ]- phenyl )- amino ]- carbonyl }- 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 20 ), tris salt of 1 - o - heptyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 21 ), tris salt of - 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 22 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - piperidinyl )- α - l - sorbofuranoside ( compound no . 23 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 4 - morpholinyl )- α - l - sorbofuranoside ( compound no . 24 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 25 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -( 1 - pyrrolidinyl )- α - l - sorbofuranoside ( compound no . 26 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o -[{ 4 -( 2 - hydroxy - 2 - oxy - ethyl )- phenyl }- amino ]- carbonyl - 6 - deoxy - 6 -( 1 - azepanyl )- α - l - sorbofuranoside ( compound no . 27 ). methyl 4 - isocyanatophenyl acetate ( 0 . 50 g ) was added to a solution of 1 - o - decyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -[ 2 -( 1 - pyrrolidinyl )- ethyl ]- amino - α - l - sorbofuranoside ( 1 . 0 g ) ( prepared as described in u . s . pat . no . 5 , 637 , 570 ) in dichloromethane ( 20 ml ) at 0 - 5 ° c ., with continuous stirring . the reaction mixture was allowed to warm to room temperature . after 6 hours , dichloromethane ( 30 ml ) was added to the reaction mixture and organic layer was washed with water and brine , and then dried over anhydrous sodium sulfate . the solvent was removed under reduced pressure and the residue thus obtained was purified by column chromatography using 50 % ethyl acetate - methanol as eluent to yield the title compound ( 1 . 16 g ). 0 . 5 n aqueous sodium hydroxide solution ( 30 ml ) was added to a solution of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -[( 4 -{ 2 - methoxy - 2 - oxo - ethyl }- phenyl )- amino ]- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - pyrrolidinyl )- ethyl ]- amino - α - l - sorbofuranoside ( 0 . 6 g ) ( obtained from step a above ) in methanol ( 5 ml ), and the reaction mixture was stirred at 50 ° c . after 3 hours , the solvent was evaporated and residue was dissolved in water . the aqueous solution was acidified to ˜ ph 5 with concentrated hcl and extracted with ethylacetate . the organic extracts were washed with water and brine , and dried over anhydrous sodium sulfate . the solvent was removed at reduced pressure to yield the title compound ( 0 . 34 g ). tris ( hydroxymethyl ) aminomethane ( 0 . 057 g ) was added to a solution of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -[( 4 -{ 2 - hydroxy - 2 - oxo - ethyl }- phenyl )- amino ]- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - pyrrolidinyl )- ethyl ] amino - α - l - sorbofaranoside ( 0 . 3 g ) ( obtained from step b above ) in ethanol ( 20 ml ) at room temperature and the reaction mixture was stirred for one hour . ethanol was removed at reduced pressure to yield the title compound as a hygroscopic solid ( 34 mg ). 1 h nmr ( dmso , 300 mhz ): δ 7 . 34 ( 2h , d , 8 . 2 hz ), 7 . 13 ( 2h , d , 8 . 2 hz ), 4 . 35 ( 1h , s ), 4 . 31 ( 1h , bs ), 4 . 06 ( 1h , bs ), 3 . 73 - 3 . 12 ( 16h , m ), 1 . 87 ( 4h , bs ), 1 . 50 - 1 . 03 ( 22h , m ), 0 . 85 ( 3h , bs ) analogs of tris salt of - 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -[( 4 -{ 2 - hydroxy - 2 - oxo - ethyl }- phenyl )- amino ]- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - pyrrolidinyl )- ethyl ] amino - α - l - sorbofuranoside ( compound no . 28 ) described below can be prepared by replacing 2 -( 1 - pyrrolidinyl )- ethylamine in step a with the appropriate amine , as applicable in each case . tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -[{ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl }- amino ]- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - piperidinyl )- ethyl ] amino - α - l - sorbofuranoside ( compound no . 29 ), tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -[ 2 -( 4 - morpholinyl )- ethyl ]- amino - α - l - sorbofuranoside ( compound no . 30 ), tris salt of 1 - o - decyl - 2 , 3 - o - isopropylidene - 4 - o -{[ 4 -( 2 - hydroxy - 2 - oxo - ethyl )- phenyl ]- amino }- carbonyl - 6 - deoxy - 6 -[ 2 -( 1 - cycloheptyl - amino )- ethyl ]- amino - α - l - sorbofuranoside ( compound no . 31 ). pyridinium dichromate ( 1 . 52 g ) and acetic anhydride ( 1 . 15 ml ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - α - l - sorbofuranoside ( 1 . 5 g ) ( prepared as described in u . s . pat . no . 5 , 637 , 570 ) in dichloromethane ( 10 ml ) at room temperature . the reaction mixture then was refluxed for 2 - 3 hours . the solvent was evaporated under reduced pressure and the resulting residue was dissolved in ethyl acetate and filtered over silica gel . the filtrate was evaporated under reduced pressure to yield the title compound as yellow oil ( 1 . 3 g ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 4 . 59 ( 1h , q , 6 hz ), 4 . 32 ( 1h , s ), 3 . 53 - 3 . 48 ( 4h , m ), 1 . 59 - 1 . 52 ( 5h , m ), 1 . 43 ( 3h , s ), 1 . 38 - 1 . 26 ( 21h , m ), 0 . 90 - 0 . 86 ( 3h , m ). hydroxylamine hydrochloride ( 0 . 74 g ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - oxo - 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( 1 . 3 g ) ( obtained from step a above ) in pyridine - ethanol ( 1 : 1 , 3 ml ) at room temperature . the reaction mixture was refluxed at about 75 ° c . for 3 hours , after which the solvent was evaporated under reduced pressure and the residue was dissolved in water and extracted with ethyl acetate . the combined organic extracts were washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield crude oil , and purified by column chromatography , using 10 % ethyl acetate - hexane as eluent to yield the title compound ( 1 g ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 41 ( 1h , d , 16 hz ), 5 . 29 - 5 . 14 ( 1h , m ), 5 . 01 - 4 . 90 ( 1h , m ), 3 . 58 - 3 . 49 ( 4h , m ), 1 . 56 - 1 . 38 ( 13h , m ), 1 . 26 ( 16h , m ), 0 . 88 - 0 . 86 ( 3h , m ). lithium aluminum hydride ( 0 . 29 g ) was added portion - wise to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - hydroxy - imino - α - l - sorbofuranoside ( 1 g ) ( obtained from step b above ) in dry tetrahydrofuran with vigorous stirring at room temperature and further stirred overnight at room temperature . the reaction mixture then was quenched with a few drops of 10 % aqueous sodium hydroxide solution , diluted with ethyl acetate , and the resulting residue was filtered over celite . the filtrate was evaporated under reduced pressure to yield the title compound as yellow oil ( 800 mg ). 4 - fluorophenyl isocyanate ( 0 . 03 ml ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ( 100 mg ) ( obtained from step c above ) in dichloromethane ( 3 ml ) at 0 ° c . and stirred for 2 hours . the reaction mixture then was concentrated and the resulting crude oil was purified by column chromatography using 15 % ethyl acetate - hexane as eluent to yield the title compound ( 90 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ7 . 31 - 7 . 28 ( 2h , m ), 7 . 00 ( 2h , t , 8 . 5 hz ), 6 . 39 ( 1h , s ), 5 . 04 ( 1h , d , 9 hz ), 4 . 55 ( 1h , d , 4 . 5 hz ), 4 . 02 - 3 . 88 ( 2h , m ), 3 . 60 - 3 . 47 ( 4h , m ), 1 . 62 - 1 . 50 ( 5h , m ), 1 . 44 - 1 . 25 ( 27h , m ), 0 . 89 - 0 . 85 ( 3h , m ). 4 - fluoro - benzoyl chloride was added to a solution having 100 mg of a compound obtained from step c of example 6 ( i . e ., ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ), in dichloromethane ( 3 ml ) at 0 ° c . the reaction mixture was stirred for 2 - 3 hours and then taken into water and extracted with dichloromethane . the combined organic extracts were washed with aqueous sodium bicarbonate , water and brine and dried over anhydrous sodium sulfate . solvent was evaporated under reduced pressure to obtain crude yellow oil , which was purified by column chromatography using 15 % ethyl acetate - hexane as eluent to furnish the title compound ( 75 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 83 - 7 . 79 ( 2h , m ), 7 . 14 ( 2h , t , 9 hz ), 6 . 37 ( 1h , d , 9 hz ), 4 . 60 ( 1h , d , 3 hz ), 4 . 30 ( 1h , m ), 4 . 06 ( 1h , m ), 3 . 61 - 3 . 50 ( 4h , m ), 1 . 59 - 1 . 49 ( 5h , m ), 1 . 41 - 1 . 36 ( 6h , m ), 1 . 26 ( 18h , m ), 0 . 90 - 0 . 85 ( 3h , m ). n - butyl isocyanate ( 0 . 03 ml ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ( 100 mg ) ( obtained from step c of example 6 ) in dichloromethane ( 3 ml ) at 0 ° c . the reaction mixture was stirred for 3 hours and solvent was evaporated under reduced pressure . the crude residue thus obtained was purified by column chromatography using 20 % ethyl acetate - hexane as eluent to yield the title compound ( 85 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 4 . 56 - 4 . 51 ( 2h , m ), 4 . 25 ( 1h , bs ), 3 . 91 ( 2h , m ), 3 . 60 - 3 . 47 ( 4h , m ), 3 . 19 - 3 . 15 ( 2h , m ), 1 . 58 - 1 . 46 ( 8h , m ), 1 . 38 - 1 . 30 ( 4h , m ), 1 . 26 ( 21h , m ), 0 . 95 - 0 . 86 ( 6h , m ). triethylamine ( 0 . 04 ml ) and 4 - fluorobenzene sulfonyl chloride ( 53 mg ) were added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ( 100 mg ) ( obtained from step c of example 6 ) in dichloromethane ( 3 ml ) at 0 ° c . and stirred for 3 hours . the reaction mixture was taken into water and extracted with ethyl acetate . the organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the resulting crude oil was purified by column chromatography using 15 % ethyl acetate - hexane as eluent to yield the title compound ( 80 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 94 - 7 . 90 ( 2h , m ), 7 . 18 ( 2h , t , 9 hz ), 5 . 07 ( 1h , d , 9 hz ), 4 . 02 ( 1h , d , 6 hz ), 3 . 89 ( 1h , m ), 3 . 48 - 3 . 40 ( 4h , m ), 3 . 22 ( 1h , m ), 1 . 56 - 1 . 49 ( 5h , m ), 1 . 27 - 1 . 22 ( 24h , m ), 0 . 90 - 0 . 86 ( 3h , m ). n - methylmorpholine ( 0 . 03 ml , 0 . 29 mmol ) and 1 - hydroxy benzotriazole ( 40 mg , 0 . 29 mmol ) were added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ( 100 mg ) ( obtained from step c of example 6 ) and 3 - benzo [ 1 , 3 ]- dioxol - 5 - yl - propionic acid ( 52 mg , 0 . 26 mmol ) in dimethylformamide ( 3 ml ) at 0 ° c . after 0 . 5 hours , n -( dimethylaminopropyl )- n - ethyl carbodiimide hydrochloride ( 132 mg , 0 . 67 mmol ) was added to the reaction mixture and stirred overnight at room temperature . the reaction mixture was quenched with water , extracted with ethyl acetate , and the combined organic extracts were washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield crude yellow oil which was purified by column chromatography using 20 % ethyl acetate - hexane as eluent to furnish the title compound ( 80 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 6 . 71 - 6 . 64 ( 3h , m ), 5 . 92 ( 2h , s ), 5 . 62 ( 1h , d , 9 hz ), 4 . 45 ( 1h , d , 4 . 5 hz ), 4 . 09 ( 1h , m ), 3 . 90 ( 1h , m ), 3 . 58 - 3 . 46 ( 4h , m ), 2 . 91 - 2 . 86 ( 2h , m ), 2 . 51 - 2 . 46 ( 2h , m ), 1 . 57 - 1 . 50 ( 5h , m ), 1 . 25 - 1 . 10 ( 24h , m ), 0 . 89 - 0 . 85 ( 3h , m ). ( 4 - phenoxycarbonylamino - phenyl )- acetic acid methyl ester ( 77 mg ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ( 100 mg ) ( obtained from step c of example 6 ) in dimethyl sulfoxide ( 3 ml ) and triethylamine ( 0 . 04 ml ) at 0 ° c . the reaction mixture was stirred at room temperature for 2 hrs , taken into water and extracted with ethyl acetate . the combined organic extracts were washed with water and brine and dried over anhydrous sodium sulfate . solvent was evaporated under reduced pressure and the residue thus obtained was purified by column chromatography using 15 % ethyl acetate - hexane as eluent to yield the title compound ( 95 mg ). 1 hnmr ( 300 mhz , cdcl 3 ): δ 7 . 28 - 7 . 19 ( 4h , m ), 6 . 40 ( 1h , bs ), 5 . 08 ( 1h , d , 9 hz ), 4 . 56 ( 1h , d , 6 hz ), 4 . 02 - 3 . 92 ( 2h , m ), 3 . 68 ( 3h , s ), 3 . 61 - 3 . 49 ( 6h , m ), 1 . 59 ( 2h , m ), 1 . 51 ( 3h , s ), 1 . 38 - 1 . 25 ( 24h , m ), 0 . 88 - 0 . 85 ( 3h , m ). lithium hydroxide monohydrate ( 7 mg , 0 . 17 mmol ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - di - deoxy - 4 -[{[( 4 -[ 2 - methoxy - 2 - oxo - ethyl ]- phenyl )- amino ]- carbonyl }- amino ]- α - l - erythro - hex - 2 - ulofuranoside ( 95 mg , 0 . 17 mmol ) ( obtained from step a above ) in tetrahydrofuran : methanol : water ( 3 : 1 : 1 , 5 ml ) at 0 ° c . the reaction mixture was stirred for 2 hours . the solvent was evaporated under reduced pressure and the resulting crude mass was taken into water and extracted with ethyl acetate . the aqueous layer was acidified with aqueous sodium hydrogen sulfate and then extracted with ethyl acetate . the combined organic extracts were washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield the title compound ( 65 mg ). 1 hnmr ( 300 mhz , cdcl 3 ): δ 8 . 67 ( 1h , s ), 7 . 30 ( 2h , d , 9 hz ), 7 . 10 ( 2h , d , 9 hz ), 6 . 17 ( 1h , d , 9 hz ), 4 . 44 ( 1h , s ), 3 . 88 - 3 . 80 ( 2h , m ), 3 . 53 - 3 . 45 ( 6h , m ), 1 . 48 - 1 . 32 ( 5h , m ), 1 . 23 - 1 . 16 ( 24h , m ), 0 . 86 - 0 . 82 ( 3h , m ). triethylamine ( 0 . 04 ml ) and 2 - phenylethylisothiocyanate ( 0 . 04 ml ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 , 6 - dideoxy - 4 - amino - α - l - erythro - hex - 2 - ulofuranoside ( 100 mg ) ( obtained from step c of example 6 ) in dichloromethane ( 3 ml ) at room temperature and then the reaction mixture was refluxed for 3 hours . the solvent was evaporated under reduced pressure and the resulting crude oil was purified by column chromatography using 20 % ethyl acetate - hexane as eluent to yield the title compound ( 95 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 36 - 7 . 21 ( 5h , m ), 5 . 74 ( 1h , d , 9 hz ), 4 . 56 ( 2h , m ), 3 . 94 - 3 . 89 ( 1h , m ), 3 . 69 - 3 . 48 ( 6h , m ), 2 . 95 - 2 . 90 ( 2h , m ), 1 . 54 ( 5h , m ), 1 . 38 - 1 . 26 ( 21h , m ), 0 . 90 - 0 . 85 ( 3h , m ). benzylamine ( 3 ml ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - tosyl - α - l - sorbofuranoside ( 5 g ) and the reaction mixture was heated for about 2 hours at 110 ° c . the benzylamine was distilled out under reduced pressure and the residue thus obtained was purified over a silica gel column using 25 % ethyl acetate - hexane as a eluent to yield the title compound ( 4 . 17 g ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 20 - 7 . 35 ( 5h , m , aromatic ), 4 . 42 ( 1h , s ), 4 . 33 ( 1h , q , j = 6 hz ), 4 . 22 ( 1h , d , j = 3 hz ), 3 . 79 ( 2h , abq ), 3 . 64 ( 2h , dd ), 3 . 45 - 3 . 52 ( 2h , m ), 3 . 22 ( 1h , dd ), 2 . 99 ( 1h , dd ), 1 . 51 - 1 . 55 ( 5h , m ), 1 . 37 ( 3h , s ), 1 . 29 ( 18h , bs ), 0 . 87 ( 3h , t , j = 3 hz ). 10 % pd / c ( 2 g ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene6 - deoxy - 6 - benzylamino - α - l - sorbofuranoside ( 4 . 1 g ) ( obtained from step a above ) in methanol ( 20 ml ). the reaction mixture was shaken using a parr apparatus at 60 psi for 12 hours at room temperature . the reaction mixture was filtered over celite and the filtrate was concentrated under reduced pressure to yield the title compound ( 2 . 5 g ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 4 . 42 ( 1h , s ), 4 . 20 - 4 . 24 ( 2h , m ), 3 . 60 - 3 . 71 ( 4h , m ), 3 . 21 - 3 . 22 ( 1h , dd , 15 hz , 3 hz ), 3 . 08 - 3 . 10 ( 1h , dd , 15 hz , 6 hz ), 1 . 57 - 1 . 61 ( 5h , m ), 1 . 36 ( 3h , s ), 1 . 25 ( 18h , bs ), 0 . 87 ( 3h , t , 6 hz ). 4 - fluorophenyl isocyanate ( 35 . 4 mg ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) ( obtained from step b above ) in dichloromethane ( 10 ml ) at 0 ° c . and the reaction mixture was allowed to warm to room temperature and stirred for 2 hours . the reaction mixture was concentrated under reduced pressure and the residue was purified over silica gel ( 100 - 200 mesh ) column using 40 % ethyl acetate - hexane as eluent to yield the title compound ( 130 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 2 ( 2h , m ), 6 . 99 ( 2h , t , 9 hz ), 4 . 49 ( 1h , bs ), 4 . 46 ( 1h , s ), 4 . 11 - 4 . 33 ( 3h , m ), 3 . 44 - 3 . 74 ( 9h , m ), 1 . 41 - 1 . 55 ( 5h , m ), 1 . 35 ( 3h , s ), 1 . 25 ( 18h , bs ), 0 . 85 ( 3h , t , 6 hz ). 4 - fluorophenyl isothiocyanate ( 39 . 5 mg ) and triethylamine ( 0 . 01 ml ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b of example 13 in dichloromethane ( 5 ml ). the reaction mixture was stirred at room temperature for one hour . the reaction mixture was concentrated under reduced pressure and the residue was purified over a silica gel column using 15 % ethyl acetate - hexane as eluent to yield the title compound ( 130 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 26 - 7 . 08 ( 4h , m ), 4 . 77 ( 2h , m ), 4 . 47 - 4 . 42 ( 1h , m ), 4 . 06 ( 1h , s ), 3 . 72 - 3 . 69 ( 1h , m ), 3 . 54 - 3 . 46 ( 4h , m ), 1 . 55 - 1 . 11 ( 26h , m ), 0 . 88 ( 3h , t , 6 hz ). triethylamine ( 0 . 036 ml ) and 4 - fluorobenzene sulfonylchloride ( 50 mg ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b of example 13 in dichloromethane ( 5 ml ) at 0 ° c . the reaction mixture was stirred for 3 hours at room temperature . the reaction mixture then was taken into distilled water and extracted with dichloromethane . the combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over a silica gel column using 10 % ethyl acetate - hexane as eluent to yield the title compound ( 75 mg ). 1 h nmr ( 300 mhz , cdcl 3 ) δ : 7 . 87 - 7 . 92 ( 2h , m ), 7 . 16 - 7 . 26 ( 2h , m ), 4 . 37 ( 1h , s ), 4 . 24 - 4 . 28 ( 1h , m ), 3 . 99 - 4 . 04 ( 1h , dd , 8 hz , 3z ), 3 . 65 - 3 . 70 ( 2h , m ), 3 . 48 - 3 . 53 ( 2h , d , 6 hz ), 3 . 23 - 3 . 28 ( 2h , t , 6 hz ), 1 . 45 - 1 . 58 ( 5h , m ), 1 . 31 ( 3h , s ), 1 . 25 ( 18h , bs ), 0 . 88 ( 3h , t , 6 hz ). 4 - fluorobenzoyl chloride ( 0 . 03 ml ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b of example 13 in dichloromethane ( 2 ml ) at 0 ° c . the reaction mixture was stirred for one hour at room temperature . the reaction mixture then was concentrated under reduced pressure and the residue was purified over a silica gel ( 100 - 200 mesh ) column using 15 % ethyl acetate - hexane as eluent to yield the title compound ( 58 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 77 - 7 . 81 ( 2h , m ), 7 . 08 - 7 . 26 ( 2h , t , 9 hz ), 6 . 47 ( 1h , bs ), 4 . 40 - 4 . 46 ( 2h , m ), 4 . 03 - 4 . 09 ( 2h , m ), 3 . 88 - 3 . 90 ( 1h , m ), 3 . 74 - 3 . 77 ( 1h , d , 9 hz ), 3 . 53 - 3 . 62 ( 4h , m ), 1 . 50 - 1 . 58 ( 5h , m ), 1 . 35 ( 3h , s ), 1 . 25 ( 18h , bs ), 0 . 88 ( 3h , t , 6 hz ). analogs of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 4 - fluoro - phenyl )- carbonyl }- amino - α - l - sorbofuranoside ( compound no . 42 ) described below can be prepared by replacing 4 - fluorobenzoyl chloride with the appropriate chlorides , as applicable in each case . 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - trifluoromethyl ) benzoyl ] amino }- α - l - sorbofuranoside ( compound no . 68 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - fluorophenyl ) acetyl } amino ]- α - l - sorbofuranoside ( compound no . 69 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 3 - fluorobenzoyl ) amino }- α - l - sorbofuranoside ( compound no . 70 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( quinolin - 2 - ylcarbonyl ) amino }- α - l - sorbofuranoside ( compound no . 71 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 2 - thienylacetyl ) amino }- α - l - sorbofuranoside ( compound no . 72 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 73 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 74 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( 3 , 4 - dimethoxybenzoyl ) amino }- α - l - sorbofuranoside ( compound no . 75 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( isoquinolin - 1 - ylcarbonyl ) amino }- α - l - sorbofuranoside ( compound no . 76 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[ 4 -( acetylamino ) benzoyl ] amino }- α - l - sorbofuranoside ( compound no . 77 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( pyridin - 4 - yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 78 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 6 - dichloropyridin - 4 - yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 79 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( quinolin - 3yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 80 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 5 - methyl - 3 - phenylisoxazol - 4 - yl )- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 81 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{( phenyl ) acetyl }- amino - α - l - sorbofuranoside ( compound no . 82 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - chlorophenyl ) acetyl ] amino - α - l - sorbofuranoside ( compound no . 83 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 5 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 84 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 85 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 86 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 87 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 4 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 88 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[ 2 , 6 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 89 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - methylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 90 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 91 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 5 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 92 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 , 4 , 5 - trifluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 93 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 - dichlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 94 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - hydroxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 95 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - methylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 96 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 97 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -[( 1 , 3 - benzodioxol - 5 - ylacetyl ) amino ]- l - sorbofuranoside ( compound no . 98 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - hydroxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 99 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - hydroxy - 3 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 100 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - isopropylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 101 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[ biphenyl - 4 - ylacetyl ]- amino }- α - l - sorbofuranoside ( compound no . 102 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - methylphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 103 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - fluoro - 6 - chlorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 104 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - chloro - 4 - fluorophenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 105 ), 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - trifluoromethoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 106 ), or 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 2 - trifluoromethoxyphenyl ) acetyl ] amino }- α - l - sorbofuranoside ( compound no . 107 ). 3 -( 3 , 4 - methylenedioxyphenyl )- propionic acid ( 50 mg ), followed by n - methylmorpholine ( 62 mg ) and 1 - hydroxybenzotriazole ( 38 mg ) were added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b of example 13 in n , n - dimethylformamide ( 3 ml ) at 0 ° c . the reaction mixture was stirred for 30 min at 0 ° c . n -( dimethylaminopropyl )- n - ethyl carbodiimide hydrochloride ( 56 mg ) was added to the reaction mixture and the reaction mixture was stirred for 24 hours at room temperature . the reaction mixture was taken in distilled water and extracted with ethyl acetate . the combined organic layer was washed with distilled water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over silica gel column using 30 % ethyl acetate - hexane as eluent to yield the title compound ( 87 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 6 . 62 - 6 . 74 ( 3h , m ), 5 . 92 ( 2h , s ), 4 . 43 ( 2h , s ), 4 . 20 ( 1h , m ), 3 . 95 - 4 . 06 ( 2h , m ), 3 . 51 - 3 . 71 ( 5h , m ), 2 . 88 ( 2h , 2h , 6 hz ), 2 . 43 ( 2h , t , 6 hz ), 1 . 58 ( 2h , m ), 1 . 50 ( 3h , s ), 1 . 35 ( 3h , s ), 1 . 25 ( 18h , bs ), 0 . 88 ( 3h , t , 6 hz ). n - butyl isocyanate ( 0 . 03 ml ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b of example 13 in dichloromethane ( 5 ml ) at 0 ° c . the reaction mixture was warmed to room temperature stirred for one hour . the reaction mixture was concentrated under reduced pressure and the residue was purified over silica gel column using 15 % ethyl acetate - hexane as eluent to yield the title compound ( 80 mg ). 1 hnmr ( 300 mhz , cdcl 3 ): δ 4 . 45 ( 1h , s ), 4 . 25 ( 1h , m ), 4 . 06 - 4 . 05 ( 1h , d , 3 hz ), 3 . 71 - 3 . 51 ( 5h , m ), 3 . 25 ( 1h , m ), 3 . 14 ( 2h , t , 6 hz ), 1 . 57 - 1 . 55 ( 2h , m ), 1 . 51 - 1 . 24 ( 28h , m ), 0 . 94 - 0 . 84 ( 6h , m ). triethylamine ( 0 . 071 ml ) and ( 4 - phenoxycarbonylamino - phenyl )- acetic acid methyl ester ( 147 mg ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 200 mg ) obtained from step b of example 13 in dry tetrahydrofuran ( 5 ml ) at room temperature . the reaction mixture was stirred for 3 hours at room temperature and then heated to and maintained at 50 ° c . overnight . the reaction mixture was taken into distilled water and extracted with ethyl acetate . combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over a silica gel column using 20 % ethyl acetate - hexane as eluent to yield the title compound ( 270 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 18 - 7 . 26 ( 4h , m ), 5 . 21 ( 1h , bs ), 4 . 46 ( 1h , s ), 4 . 30 ( 2h , bs ), 4 . 09 - 4 . 12 ( 1h , d , 6 hz ), 3 . 69 - 3 . 73 ( 4h , m ), 3 . 53 - 3 . 63 ( 6h , m ), 3 . 42 ( 1h , bs ), 1 . 48 - 1 . 66 ( 5h , m ), 1 . 35 ( 3h , s ), 1 . 25 ( 18h , bs ), 0 . 86 ( 3h , m ). lithium hydroxide monohydrate ( 30 mg ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[{( 4 -[ 2 - methoxy - 2 - oxo - ethyl ]- phenyl )- amino }- carbonyl ]- amino }- α - l - sorbofuranoside ( 270 mg ) obtained from step a of example 19 , in tetrahydrofuran ( 6 ml ), methanol ( 2 ml ) and distilled water ( 2 ml ) at room temperature and stirred overnight . the reaction mixture was concentrated under reduced pressure , the residue was taken in distilled water and acidified with dilute aqueous sodium hydrogen solution . the aqueous layer was extracted with ethyl acetate and the combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield the title compound ( 200 mg ). 1 h nmr ( 300 mhz , d 2 o ): δ 7 . 28 - 7 . 31 ( 2h , d , 9 hz ), 7 . 11 - 7 . 13 ( 2h , d , 6 hz ), 4 . 32 ( 1h , s ), 4 . 14 ( 1h , m ), 3 . 99 ( 1h , s ), 3 . 18 - 3 . 56 ( 8h , m ), 1 . 47 - 1 . 49 ( 2h , m ), 1 . 39 ( 3h , s ), 1 . 29 ( 1h , s ), 1 . 24 ( 18h , bs ), 0 . 85 ( 3h , t , 6 hz ). analogs of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[{( 4 -[ 2 - hydroxy - 2 - oxo - ethyl ]- phenyl )- amino }- carbonyl ]- amino }- α - l - sorbofuranoside ( compound no . 44 ) described below can be prepared by replacing ( 4 - phenoxycarbonylamino - phenyl )- acetic acid methyl ester with the appropriate esters , as applicable in each case . triethylamine ( 0 . 036 ml , 0 . 258 mmol ) and ethanesulfonyl chloride ( 0 . 032 mg , 0 . 258 mmol ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b of example 13 in dichloromethane ( 5 ml ) at 0 ° c . the reaction mixture was stirred for 3 hours at room temperature and then taken into distilled water and extracted with dichloromethane . the combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over silica gel column using 25 % ethyl acetate - hexane as eluent to yield title compound ( 100 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 4 . 54 ( 1h , bs ), 4 . 42 - 4 . 37 ( 2h , m ), 4 . 12 - 4 . 09 ( 1h , d , 9 hz ), 3 . 80 - 3 . 72 ( 1h , m ), 3 . 57 - 3 . 39 ( 6h , m ), 3 . 11 - 3 . 03 ( 2h , q , 9 hz ), 1 . 57 - 1 . 26 ( 26h , m ), 0 . 88 ( 3h , t , 6 hz ). sodium azide ( 2 . 6 gm ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - tosyl - α - l - sorbofuranoside ( 4 . 4 gm ) in dimethylformamide ( 30 ml ) at room temperature and the reaction mixture was heated for about 10 hours at 110 ° c . the dimethylformamide was distilled out under reduced pressure , the residue was taken in distilled water and extracted with ethyl acetate . the combined organic layer was dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield the title compound ( 4 g ). sodium hydride ( 9 mg ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - aza - α - l - sorbofuranoside ( 130 mg ) obtained from step a above in tetrahydrofuran ( 5 ml ) at 0 ° c . and stirred for 20 mins . at the same temperature methyliodide ( 0 . 1 ml ) was added and further stirred for about 1 hr at room temperature . the tetrahydrofuran was distilled out under reduced pressure ; the residue was taken in distilled water and extracted with ethyl acetate . the combined organic layers was dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure to yield the title compound ( 100 mg ) 20 % pd / c ( 20 mg ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o - methoxy - 6 - deoxy - 6 - aza - α - l - sorbofuranoside ( 100 mg ) obtained from step b above in methanol ( 10 ml ). the reaction mixture was shaken under hydrogen atmosphere , using a parr apparatus at 60 psi for 2 hours at room temperature . the reaction mixture was filtered over celite and the filtrate was concentrated under reduced pressure and the residue was purified over a silica gel column using 10 % methanol - dichloromethane as eluent to yield the title compound ( 55 mg ). 4 - fluorophenylaceticacid ( 21 mg ), 1 - hydroxybezotriazole ( 20 mg ) and n - methylmorpholine ( 0 . 1 ml ) was added to a solution of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - o - methyl - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 55 mg ) obtained from step c above in dimethylformamide ( 5 ml ) at 0 ° c . and after 20 minutes at the same temperature was added edci . hcl ( 28 mg ). the reaction mixture was allowed to warm to room temperature and stirred for 12 hours . the reaction mixture was concentrated under reduced pressure the residue was taken in distilled water and extracted with ethyl acetate . the combined organic layers were dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over preparative tlc ( thickness 2 mm ) using 40 % ethylacetate - hexane as eluant to yield the title compound ( 35 mg ). 1 h nmr ( 400 mhz , cdcl 3 ): δ 7 . 21 - 7 . 26 ( m , 2h ), 7 . 00 - 7 . 05 ( m , 2h ), 5 . 84 ( bs , 1h , nh ), 4 . 49 ( s , 1h ), 4 . 31 - 4 . 33 ( m , 1h ) 3 . 63 - 3 . 65 ( m , 1h ), 3 . 43 - 3 . 59 ( m , 8h ), 3 . 44 ( s , 3h ), 1 . 55 - 1 . 58 ( m , 2h ), 1 . 26 - 1 . 48 ( m , 24h ), 0 . 86 - 0 . 89 ( m , 3h ). sodium azide ( 1 . 4 gm ) was added to a solution of 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - tosyl - α - l - sorbofuranoside ( 2 . 0 gm ) in dimethylformamide ( 20 ml ) at room temperature and the reaction mixture was heated for about 12 hours at 110 ° c . the dimethylformamide was distilled out under reduced pressure , the residue was taken in distilled water and extracted with ethyl acetate . the combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure the residue thus obtained was purified over a silica gel column using 20 % ethyl acetate - hexane as a eluant to yield the title compound ( 1 . 1 g ) 10 % pd / c ( 100 mg ) was added to a solution of 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene6 - deoxy - 6 - benzylamino - α - l - sorbofuranoside ( 1 g ) obtained from step a above , in methanol ( 30 ml ). the reaction mixture was shaken under hydrogen atmosphere using a parr apparatus at 60 psi for 2 hours at room temperature . the reaction mixture was filtered over celite and the filtrate was concentrated under reduced pressure and purified over a silica gel column using 20 % ethyl acetate - hexane as eluent to yield the title compound ( 800 mg ). 4 - fluorophenylaceticacid ( 48 mg ), 1 - hydroxybezotriazole ( 47 mg ) and n - methylmorpholine ( 0 . 05 ml ) was added to a solution of 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 - amino - α - l - sorbofuranoside ( 100 mg ) obtained from step b above in dimethylformamide ( 5 ml ) at 0 ° c . and after 20 minutes at the same temperature was added edci . hcl ( 66 mg ). the reaction mixture was allowed to warm to room temperature and stirred for 12 hours . the reaction mixture was concentrated under reduced pressure the residue was taken in distilled water and extracted with ethyl acetate . the combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over preparative tlc ( thickness 2 mm ) using 50 % ethyl acetate - hexane as eluant to yield the title compound ( 125 mg ). 1 h nmr ( 400 mhz , cdcl 3 ): m , 2h ), 7 . 01 - 7 . 05 ( m , 2h ), 5 . 82 ( bs , 1h , nh ), 5 . 45 ( s , 1h ), 4 . 20 - 4 . 27 ( m , 1h ), 3 . 95 - 3 . 97 ( m , 2h ), 3 . 65 - 3 . 73 ( m , 11h ), 1 . 25 - 1 . 61 ( m , 10h ), 0 . 87 - 0 . 91 ( m , 3h ). analogs of 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - fluorophenyl ) acetyl ]- amino }- α - l - sorbofuranoside ( compound no . 113 ) described below can be prepared by replacing 4 - fluorophenylacetic acid with the appropriate acids , as applicable in each case . 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 - difluorophenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 109 ), 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 , 4 dichlorophenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 110 ), 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 4 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 111 ), or 1 - o -( 2 - butoxyethyl )- 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{[( 3 - methoxyphenyl ) acetyl ] amino }- α - l - sorbofuranose ( compound no . 112 ). a mixture of 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - tosyl - α - l - sorbofuranoside ( prepared as described in u . s . pat . no . 5 , 637 , 570 ) ( 500 mg ) and 1 - benzylpiperazine ( 206 mg ) was heated with stirring for 7 - 8 hours . the reaction mixture was cooled and triturated with ether . a white solid precipitated , which was filtered and the filtrate was washed with water , saturated aqueous sodium bicarbonate solution and brine . the organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo . the residue was purified over a silica gel column using 30 % ethyl acetate - hexane as eluent to yield the title compound ( 550 mg ). 10 % palladium / carbon ( 275 mg ) and ammonium formate ( 1 . 0 g ) was added with stirring to solution of the 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -( 4 - benzylpiperazin - 1 - yl )- α - l - sorbofuranoside ( 550 mg ) obtained from step a above in methanol ( 20 ml ) and the reaction mixture was refluxed . after 1 hour , the reaction mixture was cooled and filtered through a bed of celite . it was repeatedly washed with hot dichloromethane and then washed with water . the organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo . the residue thus obtained was purified using column chromatography using 2 . 5 % methanol - dichloromethane as eluent to furnish the title compound ( 450 mg ). 4 - methoxy - 3 -( 1 - methyl - 7 - oxo - 3 - propyl - 6 , 7 - dihydro - 1h - pyrazolo [ 4 , 3 - d ] pyrimidin - 5 - yl )- benzenesulfonyl chloride was mixed with 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -( piperazin - 1 - yl )- α - l - sorbofuranoside ( 488 mg ) obtained in step b above and dissolved in a dichloromethane : pyridine ( 5 : 1 ml ) mixture at 0 ° c . after 1 hour , the solvent mixture was removed under reduced pressure and the residue was taken in dichloromethane . the organic layer was washed with saturated aqueous sodium bicarbonate solution and water and then dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over a silica gel column using 2 % methanol - dichloromethane as eluent to yield the title compound ( 350 mg ). 1 h nmr ( cdcl 3 , 300 mhz ): δ 8 . 82 ( 1h , d , 2 hz ), 7 . 81 ( 1h , dd , 2 & amp ; 6 . 6 hz ), 7 . 15 ( 1h , d , 8 . 7 hz ), 4 . 78 ( 1h , bs ), 4 . 37 ( 4h , m ), 4 . 27 ( 5h , s ), 4 . 1 ( 1h , s ), 3 . 61 ( 1h , m ), 3 . 55 - 3 . 48 ( 3h , m ), 3 . 08 ( 4h , bs ), 2 . 92 ( 2h , t , 7 . 4 hz ), 2 . 85 ( 2h , m ), 2 . 8 - 2 . 1 ( 7h , m ), 1 . 85 ( 2h , q , 7 . 4 hz ), 1 . 68 ( 3h , m ), 1 . 44 ( 3h , s ), 1 . 31 - 1 . 24 ( 2 . 4h , m ), 1 . 02 ( 3h , m ), 0 . 87 ( 3h , t , 5 . 8 hz ). ethereal hcl was added to 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 6 - deoxy - 6 -{ 1 -[ 4 -({ 4 - methoxy - 3 -[ 5 -{ 1 - methyl - 3 - propyl - 7 - oxo - 1 , 6 - dihydro - pyrazolo [ 4 , 3 - d ]- pyrimidinyl }]- phenyl }- sulfonyl )- piperazinyl ]}- α - l - sorbofuranoside ( 100 mg ) obtained from step c above , dissolved in minimum amount of ether ( 5 ml ) at 0 ° c . and stirred for about 40 minutes . the volatiles were removed under reduced pressure and the residue triturated with hexane to yield a white solid that was filtered and dried in vacuo to produce the title compound ( 100 mg ). potassium hydroxide ( 12 . 9 g ), followed by 6 - chloro - 1 - hexanol ( 11 . 56 g ) and a pinch of tetrabutylammonium iodide was added to a solution of a 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( 20 g )( prepared as described in u . s . pat . no . 6 , 329 , 344 ) in dimethylsulfoxide ( 80 ml ) at room temperature . the reaction mixture was stirred at 50 ° c . and after 5 hours , the reaction mixture was cooled and water was added . the aqueous layer was extracted with ethyl acetate and the organic extract was washed with water and brine , and dried over anhydrous sodium sulfate . the solvent was removed under reduced pressure and product was purified over a silica gel column using 10 % ethyl acetate - hexane as eluent to yield the title compound ( 22 . 5 g ). p - nitrophenyl isocyanate ( 0 . 51 g ) was added to a solution of 1 - o -[( 6 - hydroxyhexyl ]- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside obtained from step a of example 22 ( 1 . 0 g ) in dichloromethane ( 3 ml ) at 0 ° c . with continuous stirring . the reaction mixture was warmed to room temperature and stirred for 24 hours . the solvent was removed at reduced pressure and the residue was purified by column chromatography using 20 % ethyl acetate - hexane as eluent to furnish the title compound ( 1 . 24 g ) 1 hnmr ( cdcl 3 , 300 mhz ): δ 8 . 20 ( 2h , d , 8 . 9 hz ), 7 . 57 ( 2h , d , 8 . 9 hz ), 4 . 46 ( 1h , s ), 4 . 30 ( 1h , s ), 4 . 20 ( 2h , t , 6 . 2 hz ), 4 . 09 - 4 . 02 ( 3h , m ), 3 . 77 - 3 . 39 ( 4h , m ), 1 . 69 - 1 . 23 ( 20h , m ) analogs of 1 - o -[( 4 - nitro - phenyl - amino - carbonyloxy )- hexyl ]- 2 , 3 ; 4 , 6 - di - o - isopropylidene - α - l - sorbofuranoside ( compound no . 48 ) described below can be prepared by replacing p - nitrophenyl isocyanate with the appropriate isocyanate , as applicable in each case . methyl magnesium chloride in tetrahydrofuran ( 100 ml ) was added to a solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - oxo - 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( 2 . 60 g ) prepared in step a of example 6 at 0 ° c . in tetrahydrofuran ( 100 ml ). the reaction mixture was warmed to room temperature and stirred for 2 hrs . the reaction mixture then was quenched with water ( 5 ml ) and concentrated . the reaction mixture was extracted with ethyl acetate and the organic extracts were washed with water , brine and dried over sodium sulfate . the solvent was evaporated and the residue purified over a silica gel column using 5 % ethyl acetate - hexane as eluent to yield the title compound as viscous oil ( 1 . 93 g ). 1 h nmr ( cdcl 3 ): δ 4 . 12 ( s , 1h ), 3 . 91 ( q , j = 6 . 0 hz , 1h ), 3 . 57 - 3 . 46 ( m , 4h ), 2 . 64 ( s , 1h , — oh ), 1 . 57 ( s , 6h ), 1 . 41 ( s , 3h ), 1 . 26 - 1 . 15 ( m , 2h ), 0 . 88 ( t , j = 6 . 0 hz , 3h ). benzenesulfonyl isocyanate ( 0 . 13 ml ) was added slowly to a stirred solution of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( 0 . 12 g ) obtained from step a above in dichloromethane ( 2 ml ) and refluxed for 12 hours . the reaction mixture was concentrated and residue purified over a silica gel column to yield the title compound as pale brown solid ( 0 . 17 g ). 1 h nmr ( cdcl 3 ) δ : 8 . 00 ( d , j = 6 . 0 hz , 2h ), 7 . 62 ( m , 1h ), 7 . 54 ( m , 2h ), 4 . 57 ( s , 1h ), 4 . 00 ( q , j = 6 . 0 hz , 1h ), 3 . 50 - 3 . 39 ( m , 4h ), 1 . 52 ( d , j = 6 . 0 hz , 3h ), 1 . 34 - 1 . 17 ( m , 29h ), 0 . 88 ( t , j = 6 . 0 hz , 3h ); analogs of ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -{[( phenyl sulfonyl )- amino ]- carbonyl }- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 53 ) described below can be prepared by replacing sulfonyl isocyanate with the appropriate isocyanate , as applicable in each case . ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - methyl - phenyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 54 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 4 - chloro - phenyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranose ( compound no . 55 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -{[{ 2 , 5 - dichloro - phenyl )- sulfonyl }- amino ]- carbonyl }- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranose ( compound no . 56 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 -[{[( 2 - methyl - phenyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranose ( compound no . 57 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - piperidinyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 58 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - azepanyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 59 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - morpholinyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 60 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - pyrrolidinyl )- ethyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 61 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o - heptyl - 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 62 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - heptyl - 4 - o -[ 2 -( 1 - dimethylamino )- propyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 63 ), ( 4ξ )- 1 - o - dodecyl - 2 , 3 - o - isopropylidene - 4 - c - methyl - 4 - o -[{[( 2 - azepanyl )- sulfonyl ]- amino }- carbonyl ]- 6 - deoxy - α - l - erythro - hex - 2 - ulofuranoside ( compound no . 64 ). p - methylphenyl isocyanate ( 0 . 08 ml ) was added to a solution of 1 - o - heptyl - 2 , 3 - o - isopropylidene - α - l - sorbofuranoside ( 100 mg ) in dichloromethane ( 10 ml ) at room temperature and stirred overnight at room temperature . the reaction mixture was quenched with water and extracted with dichloromethane . the combined organic layer was washed with water and brine and dried over anhydrous sodium sulfate . the solvent was evaporated under reduced pressure and the residue was purified over silica gel column using 30 % ethyl acetate - hexane as eluent to yield the title compound ( 130 mg ). 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 26 - 7 . 09 ( 4h , m ), 6 . 64 ( 1h , s ), 4 . 51 ( 2h , m ), 4 . 44 ( 1h , s ), 4 . 13 - 4 . 12 ( 2h , m ), 3 . 85 - 3 . 76 ( 2h , dd , j = 15 hz ), 3 . 60 - 3 . 53 ( 3h , m ), 2 . 31 ( 3h , s ), 1 . 58 ( 3h , s ), 1 . 52 ( 3h , s ), 1 . 34 - 1 . 25 ( 10h , m ), 0 . 86 ( 3h , s ). the compounds of the present invention are tested in one or more of the assays described herein . standard assays are used to evaluate activity of compounds in present invention on inflammatory cells . attenuation of agonist - induced release of lipid mediator of neutrophil chemotaxis , leukotriene b4 ( ltb4 ), is used to evaluate inhibitory effect on neutrophils . venous blood was collected from healthy human donors using heparin as an anti - coagulant . neutrophils were isolated from freshly drawn blood after dextran sedimentation and ficoll separation ( eur j . biochem . 169 , 175 , 1987 ). 180 μl of the of neutrophil suspension ( 0 . 2 × 10 6 cells / ml ) was taken and added 19 μl of hank &# 39 ; s buffer salt solution along with 1 μl of the test drug ( 200 times concentrated ) in a 24 well plate and incubated at 37 ° c . for 1 hour . 3 minutes before the end of test compound incubation , 0 . 25 mm ca ++ / mg ++ were added . then , 0 . 3 μg / ml a23187 ( sigma chem , usa ) was added and incubated for further 10 min at 37 ° c . the reaction was stopped by adding 80 μl of cold methanol and centrifuged to remove cell debris ( j pharmacol exp ther . 297 : 267 , 2001 ). the samples were analysed for ltb 4 release using ltb 4 elisa kits ( assay design inc ., usa ). the amount of ltb 4 released was quantified and percent inhibition of ltb 4 release was calculated with respect to the difference between the a23187 stimulated and negative control cells , to compute ic 50 values . in vitro data obtained on the compounds 1 , 22 - 25 , 28 - 46 , 52 - 57 , and 65 - 118 showed ic 50 values of from & gt ; 30 μm to about 1 . 3 μm , for example , from about 25 μm to about 1 . 3 μm , for example , from about 10 μm to about 1 . 3 μm , for example , from about 3 μm to about 1 . 3 μm . in a 96 well uv - plate , 100 μl of phosphate buffer saline ( pbs ) containing dtt ( 200 μm ), atp ( 100 μm ) and calcium chloride ( 100 μm ) was added . to each well 0 . 5 μl of test drug ( 200 times concentrated ) or vehicle was added , followed by 4 μl of recombinant 5 - lox ( 3 units / μl ) and was incubated at 37 ° c . for 5 min . the reaction was initiated by adding 1 μl of 1 mm freshly prepared arachidonic acid and increase in absorbance was monitored at 236 nm for 10 min . ( j . biol . chem . 261 : 11512 , 1986 ). a plot of absorbance verses time curve was prepared and area under curve ( auc ) was computed for each well . percent inhibition of auc for different treatments was calculated with respect to the difference between the arachidonic acid stimulated and negative control values , to compute ic 50 values . compounds 69 , 70 , 78 , 94 , 106 and 116 - 118 were examined , giving ic 50 values of from about 5 . 4 μm to about 0 . 10 μm , for example , from about 1 . 7 μm to about 0 . 10 μm , for example , from about 0 . 75 μm to about 0 . 10 μm , for example , from about 0 . 30 to about 0 . 10 μm .
2
with reference now to the drawings , a device , controlling the flow of fluid is shown generally in fig1 and particularly in fig3 as a housing 1 to which a cover 3 is attached by any suitable means , such as by body screws 4 , to form a substantially water - tight chamber 5 having an inlet 7 and an outlet 9 . a single knob 11 is provided to operate the device in both its automatic and manual modes . the cover 3 has holes , generally indicated by 13 , through which the body screws 4 may pass to attach the cover 3 to the housing 1 . an impeller shaft boss 15 , a counter shaft lower boss 17 , and an eccentric shaft boss 19 are each formed in the cover 3 , into which the lower ends of the impeller shaft 21 , the counter shaft 23 , and the eccentric shaft 25 , respectively , are loosely fit to permit rotation of the shafts . gear cover bosses 27 are formed in the cover over which the corresponding cover bosses 29 of the gear cover 31 fit snugly to hold the gear cover 31 in place on the cover 3 . the upper end 35 of the impeller shaft 21 is adapted to accept the mounting of the impeller 37 thereon in a fixed relationship to the impeller shaft 21 . an impeller pinion 39 is formed intergral with the impeller shaft 21 . an impeller shaft bearing 41 is provided at the impeller shaft hole 45 in the gear cover 31 through which the upper end 35 of the impeller shaft 21 passes . the upper end 49 of the counter shaft 23 is made to fit loosely in the counter shaft upper boss 51 ( see fig4 ) which is formed in the gear cover 31 , thereby permitting the counter shaft 23 to rotate freely , however , such free rotation is not necessary for the proper operation of the device . a first gear / pinion 53 , second gear / pinion 55 , third gear / pinion 57 , and fourth gear / pinion 59 are stacked on the counter shaft 23 such that they may each rotate freely about the counter shaft 23 . the upper end 63 of the eccentric shaft 25 is adapted to have the pawl spring 65 mounted thereon . the longitudinal center line of the upper end 63 of the eccentric shaft 25 is offset from and parallel to the longitudinal center line of the eccentric shaft 25 itself . the pawl spring 65 fits loosely on the upper end 63 of the eccentric shaft 25 , so that the rotational motion of the eccentric shaft 25 is translated into translational motion of the pawl portion 97 of the pawl spring 65 . fifth gear / pinion 71 , sixth gear / pinion 73 , seventh gear / pinion 75 , and eighth gear 77 are mounted on the eccentric shaft 25 so that each , except the eighth gear 77 , are free to rotate about the eccentric shaft 25 . the eighth gear 77 is keyed to the eccentric shaft 25 so that rotation of the eighth gear 77 causes equal rotation of eccentric shaft 25 . each of the first through seventh gear / pinions 53 , 55 , 57 , 59 , 71 , 73 , and 75 , have a large diameter common gear portion , shown in fig4 for example by reference numeral 79 , and a small diameter pinion portion shown by reference numeral 81 . the impeller pinion 39 engages the large diameter common gear portion of the first gear / pinion 53 . the small diameter pinion portion of the first gear / pinion 53 engages the large diameter common gear portion of the fifth gear / pinion 71 . in like manner , the fifth gear / pinion 71 engages the second gear / pinion 55 , which in turn engages the sixth gear / pinion 73 , which in turn engages the third gear / pinion 57 , which in turn engages the seventh gear / pinion 75 , which in turn engages the fourth gear / pinion 59 , which in turn engages the eighth gear 77 , which is keyed to the eccentric shaft 25 . any suitable combination of numbers of gears and teeth on each gear is a selected to result in any desired relationship between the rotation of the impeller 37 , which is measuring the flow of the fluid through the device , and the rotation of the eccentric shaft 25 . the upper end 63 of the eccentric shaft 25 passes through an eccentric shaft hole 83 that is formed in the gear cover 31 . a deflection wall 85 is formed in the gear cover 31 to direct the fluid flow into the vanes 87 of impeller 37 . the deflection wall 85 is contoured smoothly to minimize turbulence during this change of direction of the fluid flow . a pawl spring tab 89 , seen most clearly in fig8 is formed in the gear cover 31 as an extension of the deflection wall 85 , which is a bearing surface for the spring portion 91 of the pawl spring 65 , and in conjunction with the pawl spring foot &# 39 ; s 93 bearing against the opposite side of the deflection wall 85 at the point indicated by reference numeral 95 , positions the pawl portion 97 of the pawl spring 65 properly to engage the ratchet portion 99 of the cam and ratchet wheel 101 during assembly of the device . the impeller 37 is fixed to the upper end 35 of the impeller shaft 21 such that rotation of the impeller 37 causes equal rotation of the impeller shaft 21 . the pawl spring 65 has a pawl spring foot 93 which , prior to completion of assembly of the device , bears against the deflection wall 85 as described above . the pawl portion 97 of the pawl spring 65 engages the ratchet portion 99 of the cam and ratchet wheel 101 . the spring portion 91 of the pawl spring 65 , by bearing against the deflection wall 85 , urges the pawl portion 97 of the pawl spring 65 against the teeth of the ratchet portion 99 of the cam and ratchet wheel 101 . the end of pawl 97 contains an incline 187 , which is best seen in fig1 and 3 . during assembly , the pawl spring foot 93 and spring portion 91 bear against the deflection wall 85 and pawl spring tab 89 , thereby positioning the pawl 97 to be slightly beneath the cam and ratchet wheel 101 , as best seen in fig1 . when the housing 1 , and hence the cam and ratchet wheel 101 , are lowered over the spring pawl 65 and other assembled components , the cam and ratchet wheel 101 engages the incline 187 , moving the pawl 97 to the periphery of the cam and ratchet wheel 101 , where the pawl 97 properly engages the ratchet teeth of the ratchet portion 99 . the foot 105 of the valve stem 107 is adapted to engage the cam portion 109 of the cam and ratchet wheel 101 . the central area of the valve stem 107 , shown generally by reference numeral 111 , is sufficiently uniform in cross section to permit smooth motion through the valve stem guides 113 formed in the housing 1 , as best seen in fig4 . the upper end 115 of the valve stem 107 is formed into a circular cup shaped member 117 having a slightly smaller outside diameter than the diameter of the throat 119 of the inlet 7 which is formed in the housing 1 , which throat 119 is also circular . the cup shaped member 117 has inside of it a stud 121 . the stem end 125 of the valve stem spring 127 is captured between the stud 121 and the cup shaped member 117 . the cup shaped member 117 has a grove 129 formed in its exterior periphery into which an elastic o - ring 131 fits snuggly such that the outside diameter of the o - ring 131 is slightly larger than the diameter of the throat 119 and such that when the valve stem 107 is in a closed position , the throat 119 is completely sealed against fluid flow . the hose nut ferrule 133 has a shoulder 135 which is large enough to trap the shoulder 137 of the coupling nut 139 between the hose nut ferrule 133 and the body of the inlet 7 , thereby permitting the coupling nut 139 to rotate freely . the hose nut ferrule is threaded externally to screw into complimentary internal threads of the inlet 7 of the housing 1 , thereby trapping the hose coupling 139 as described . the ferrule cup portion 141 of the hose nut ferrule 133 is supported along the longitudinal access of the hose nut ferrule 133 by three ribs 143 of the hose nut ferrule 133 . the ferrule end 145 of the valve stem spring 127 is captured in the ferrule cup 141 , thereby urging the valve stem 107 against the cam surface 109 of the cam and ratchet wheel 101 . the coupling nut 139 is adapted to accept connection to a hose as a supply of water under pressure . the filter washer 147 is pressed into place , being of such dimension and elasticity to assure a snug fit . in the chamber 5 is contained a gear train ( generally consisting of the impeller shaft 21 , the counter shaft 23 , eccentric shaft 25 , and the first gear / pinion 53 , second gear / pinion 55 , third gear / pinion 57 , fourth gear / pinion 59 , fifth gear / pinion 71 , sixth gear / pinion 73 , seventh gear / pinion 75 , and eighth gear 77 ), which gear train is denoted generally by the numeral 149 , the impeller 37 , the pawl spring 65 , the gear cover 31 , and the cam and ratchet wheel 101 . the inlet 7 and outlet 9 are formed in the housing 1 , the outlet 9 being adapted to connect with a hose or sprinkler . the inlet 7 is tapered to form the throat 119 , which is engaged by the o - ring 131 of the valve stem 107 when in the closed position . the fluid passageway inside the of the housing 1 beyond the throat 119 is contoured to deflect the fluid flow to the top of the gear cover 31 and against the deflector wall 85 , which in turn deflects the fluid flow into the vanes 87 of the impeller 37 , after which the fluid flow passes to the outlet 9 . a hole 155 is formed in the top of the housing 1 through which the stem 157 of the knob 11 passes . turning to the outside of the housing 1 , a large circular boss 161 , of smaller diameter than the knob 11 is formed in the housing 1 . a knob stopper ratchet 195 ( see fig6 ) is formed around the inside surface of the large circular boss 161 , having ratchet teeth which extend around about three - fourths of the circumference of the large circular boss 161 , and non - ratchet teeth detents around the balance of the circumference ( although this could be left smooth ), all corresponding to the ratchet portion 99 of the cam and ratchet wheel . the knob 11 is generally circular shaped and large enough to be conveniently handled manually . it contains markings to indicate various stages of the automatic mode of operation as well as the manual mode of operation . the stem 157 passes through the hole 155 , and on the opposite side of the housing 1 , is keyed to match the key 159 of the cam and ratchet wheel 101 and is fixed thereto by suitable means , such as a screw 163 . a suitable gasket or o - ring 165 is provided to seal the hole 155 around the stem 157 . a pivot boss 167 is provided on which the knob stopper 169 is mounted , as best seen in fig6 . a stop boss 171 is provided against which the spring portion 173 of the knob stopper bears . the pawl end 175 of the knob stopper 169 engages the ratchet teeth of the knob stopper ratchet 195 to permit rotation of the knob 11 in only one direction so long as the pawl end 175 engages said ratchet teeth . the cam and ratchet wheel 101 is a generally circular shape . the cam portion 109 has an increasing radius over about one - fourth of the circumference thereof , and has a fairly constant radius about the balance of the circumference . as seen best in fig4 when the valve stem 107 is in the closed position , the cam portion 109 bears against the inside of the housing 1 at a point opposite where the foot 105 of the valve stem 107 engages the cam portion 109 , generally indicated by reference numeral 110 . this arrangement supports the stem 157 against stress caused by water pressure on the valve stem 107 being transmitted to the stem 157 . the ratchet portion 99 has ratchet teeth about the outer circumference thereof , corresponding generally to that part of the cam portion 109 which has a constant radius . the ratchet portion 99 has no ratchet teeth on the circumference corresponding to that area of the cam portion 109 which has an increasing radius . the pawl 97 bears against the ratchet teeth of the cam and ratchet wheel 101 , thereby driving the cam and ratchet wheel 101 , while the valve stem 107 bears against that part of the cam portion 109 which has a constant radius ( which would correspond to a fully opened valve ). the pawl 97 bears against the toothless part of the ratchet portion 109 while the valve stem 107 bears against that part of the cam portion 109 which has an increasing radius , thereby permitting manual regulation of the rate of fluid flow without engagement of the automtic mechanism . part of the constant radius part of the cam portion 109 also corresponds to some of the toothless portion of the ratchet portion 99 , to permit full rate of fluid flow during the manual operating mode . the knob stopper 169 is so positioned within the knob 11 as to permit engagement of the pawl end 175 with the ratchet teeth of the large circular boss 161 only when the device is in the automatic mode ( i . e ., when the pawl 97 is engaging ratchet teeth of the ratchet portion 99 ). this prevents rotation of the cam and ratchet wheel 101 against the pawl 97 , in order to prevent damage to the internal mechanism of the device . the pawl end 175 bears against the non ratchet tooth portion of the large circular boss 161 during the manual operating mode ( i . e ., when the pawl 97 does not bear against ratchet teeth ). this corresponds to the valve stem 107 bearing against that part of the cam portion 109 which has an increasing radius , ( i . e . manual operation ). the outlet 9 can be adapted to accept sprinkler heads directly as shown in fig1 , and a base 181 can be attached to , or be made integral with , the cover 3 to support the combination of the sprinkler and the device together . in operation , a source of fluid , such as water , under pressure is attached , preferably through flexible hose , to the inlet 7 of the device , and a sprinkling device is attached directly , or through a hose , to the outlet 9 of the device . alternatively , a sprinkler is mounted directly on one orifice of the outlet , as shown in fig1 , and the second orifice of the outlet 9 is stopped with a cap 183 , or is connected in parallel to another sprinkler . in the automatic mode , as shown in fig9 the knob is turned clockwise to a position indicating the volume of water desired before automatic shutoff . this rotates the cam and ratchet wheel 101 , which forces the valve stem 107 against the valve stem spring 127 , and thereby opens the passageway at the throat 119 to permit water to flow through the device . the water flow is deflected across the vanes 87 of the impeller 37 , causing the impeller 37 and the impeller shaft 21 , to rotate . the impeller shaft 21 , being the input to the gear train 149 , causes the eccentric shaft 25 to rotate . as the eccentric shaft 25 rotates , a reciprocating transverse motion is imparted to the pawl 97 . this in turn engages the ratchet portion 99 , causing the cam and ratchet wheel 101 to rotate until the preselected volume of water has passed the impeller . at this point , the cam and ratchet wheel 101 moves from the position shown in fig1 to the position shown in fig7 wherein the valve stem 107 bearing against the cam portion 109 moves to the closed position , sealing the throat 119 against further flow . without having to remove the device , a manual mode of operation can be used , simply by rotating the knob 11 only during the first 90 degrees or so of operation , to the extent necessary to adjust the rate of flow to that which is desired . during the manual operation of the device , as shown in fig8 the pawl 97 will continue to reciprocate . a nub 185 is formed in the cam and ratchet wheel 101 , which lifts the end of the pawl 97 off of the cam portion 109 , as shown in fig8 to avoid unnecessary wear of the end of pawl 97 . this occurs generally in the high fluid flow area of manual operation , which would be expected to produce the fastest rate of wear otherwise . while there has been illustrated and described a preferred embodiment of the present invention , it will be understood that numerous changes or modifications will occur to those skilled in the art which still would embody the present invention . it is intended in the appended claims to cover all such changes and modifications as fall within the true spirit and scope of the present invention .
6
a frequency modulation oscillator 10 ( fig1 ) generates a carrier wave having a mean frequency fo which is linearly modulated with a sawtooth modulation signal from a generator 19 , producing a frequency deviation δf . this modulated wave is emitted towards the ground by an emission aerial 11 . after reflection by the ground , this wave is intercepted by a receiver signal aerial 12 . a mixer 13 forms the product of the signal received and a part of the signal emitted . it supplies a beat signal of the frequency fb according to the expression : where : τ is the delay of the wave between the emission and reception , the beat frequency fb is maintained constant by a control loop . because the maximum frequency deviation δf is also constant , the modulation period t is varied as a function of the delay τ . the delay τ depends on the altitude of the aircraft . for the values δf = 123 mhz and fb = 25 khz , t is varied by ten microseconds when the altitude is varied by one foot . the control loop maintains the parameter fb constant . a tracking discriminator 15 supplies a positive or a negative error voltage , depending on whether the beat frequency fb is too high or too low . this error voltage is integrated ( 17 ), amplified ( 18 ) and applied to the generator 19 for sawtooth signals of constant amplitude and variable slope . the generator 19 ultimately controls the frequency of the signal of oscillator 10 . when the apparatus is switched on , the slope of the sawtooth may be incorrect and the beat frequency fb may deviate too much from its nominal value for the beat signal to be accepted by a beat signal amplifier 14 which has a narrow frequency band . the absence of a correct signal on the output of the amplifier 14 is detected by a control discriminator 16 . the circuits for calibrating the parameters δf and fo and for controlling the precision of the control loop comprise two resonant cavities , operating at the frequencies f1 and f2 , which are represented by the block 20 . they are coupled to the output of the oscillator 10 as well as to a circuit 21 . the circuit 21 comprises three programmable counters . the first counter provides the timing of the output information by division of the clock frequency of the system . the second counter is used for measuring the modulation period t and the various time intervals necessary for the calibration . the third counter is used for measuring the calibration beat frequency fbc . there are also provided a microprocessor 22 and an interface circuit 23 between the microprocessor 22 and the integrator 17 . this circuit enables control of the integrator 17 by the control discriminator 16 under the control of the microprocessor 22 . a calibration oscillator 24 is provided for applying a calibration beat signal having the frequency fbc . the amplifier 14 is connected to the oscillator 24 through an electronic switch 25 , controlled by the microprocessor 22 through the interface 23 , during a calibration phase . a digitally controllable amplifier 26 adjusts the maximum magnitude of the signal provided by the generator 19 during the calibration phase , under the control of the microprocessor 22 . the switch 27 interrupts the connection between the tracking discriminator 15 and the integrator 17 when the integrator is controlled by the control discriminator 16 . an input / output bus 28 of the microprocessor comprises data lines , address lines and control lines . the bus 28 connects the microprocessor to all elements controlled thereby . the block 20 ( fig2 ) comprises two microwave resonant cavities 31 and 32 , equivalent to series oscillator circuits , which are coupled to the output of the carrier wave oscillator 10 . the tuning frequencies f1 and f2 are 4260 mhz and 4342 mhz , respectively . the energy absorbed by the cavities when the frequency emitted passes their tuning frequencies is detected by an amplitude detector 33 and from these signals two pulses are derived by means of a circuit 34 . these pulses , produced with respect to a threshold voltage v , are applied to the circuit 21 . the basic idea of this system is to centre the maximum frequency deviation δf and the mean frequency fo , emitted by the oscillator 10 , with respect to the tuning frequencies of the cavities 31 and 32 . this is shown in fig3 which illustrates the modulation signal . the frequency deviation δf &# 39 ; between the tuning frequencies of the two cavities 31 and 32 is 82 mhz , the lowest frequency f min = 4240 mhz and the maximum frequency deviation δf = 123 mhz . for the calibration of the oscillator 10 , the maximum frequency deviation δf emitted is controlled to the frequency deviation δf &# 39 ;, and the mean frequency fo to the tuning frequency f1 or f2 or ( f1 + f2 )/ 2 . where k = 123 / 82 = 3 / 2 for δf = 123 mhz . for a given sawtooth signal having the period t , ta represents the time interval separating the pulses applied to circuit 21 by the block 20 . for controlling the source 10 with respect to the maximum frequency deviation δf , the following conditions must be satisfied : the tuning frequencies of the two cavities are centered around 4300 mhz . in order to maintain the mean frequency fo at this value , the two intervals having the periods t and ta are centered with respect to each other . if tb is the period of time separating the start of the sawtooth from the pulse which is caused by the first cavity 31 , the following condition must be satisfied : in order to measure the period ta , it is necessary to take into account the width of the pulses produced by circuit 34 , because this width affects the period of time required by the calibration sawtooth to ensure that the frequency deviation δf has the correct value . the precision of the period tb used for calibrating the mean frequency fo is hardly affected by the width of the first pulse , because the mean frequency fo has a value of several thousands of mhz and an error of 2 or 3 mhz is not significant . the sawtooth signal is represented by the reference 40 ( fig4 ) and the pulses produced by amplitude detector 33 are represented by the references 41 and 42 . these pulses are shaped by the circuit 34 which produces the pulses 43 and 44 . the period of the sawtooth is denoted by the time t ; t1 is the period of time between the starts of the pulses 43 and 44 ; t2 is the period of time between the ends of the pulses 43 and 44 ; and t3 is the period of time between the starts of the sawtooth and the pulse 43 . these periods t , t1 , t2 and t3 take into account the widths of the pulses . after the measurement of these periods , the microprocessor 22 performs the following intermediate calculations : the latter term represents the period required by the calibration sawtooth in order to ensure that the frequency deviation δf is 123 mhz . the result is compared with t by forming the difference : a1 = 3ta / 2 - t and next information depending on a1 is applied by processor 22 to the digitally controllable amplifier 26 , which thereupon adjusts the amplitude of the sawtooth signal . the correct value of the frequency deviation δf will be obtained when ultimately a1 = 0 . the microprocessor subsequently determines tb = t3 and compares this result with ( t1 + t2 )/ 8 =( t - ta )/ 2 while forming the difference this term represents the correction to be applied to the oscillator 10 in order to ensure that the mean frequency fo has the correct value . the microprocessor sends information depending on a2 to the circuit 26 which thereupon shifts the level of the modulation signal . the correct mean frequency fo of 4300 mhz is obtained when ultimately a2 = 0 . the circuit 26 has a given transfer function for obtaining the gradients of 1 mhz / unit of the control signal for fo and 0 . 5 mhz / unit of the control signal for δf . in order to test the efficiency of the calibration it is sufficient to verify that the terms a1 and a2 are approximately zero at the end of each sequence . they are normally situated between + 1 and - 1 . under these circumstances the stability of the calibration is : ± 0 . 5 mhz for δf and ± 1 mhz for fo . the precision is only dependent on the precision of the tuning of the cavities ; it may be better than ± 0 . 5 mhz . the processing necessary for implementing the invention will be described hereinafter with reference to the charts shown in the fig5 a , 5b , 5c and the block diagram of fig1 . the first counter in the block 21 has a cycle of 40 ms which is used as a time base for the calibration sequence . the maximum duration of the calibration phase is 40 ms . this phase occurs every 400 ms . at the start of the calibration phase , the altimeter loop assumes the search mode . this state is triggered by the loss of control due to the disappearance of the ground signal ; this is detected by the control discriminator 16 . the ground signal is suppressed by the microprocessor 22 which sets the gain of the amplifier 14 to a minimum . the oscillator 24 is started , the control voltage of the generator 19 varies the frequency of the oscillator 24 from the high values to the low values and the calibration program is activated ( start ; fig5 a ). the microprocessor 22 reads a memory location mns ( block 50 ) which contains a value 10 at the start . a test ( block 51 ) is performed in order to determine whether the value mns is larger than or equal to 7 . if so , the microprocessor performs the operation mns - 1 ( block 52 ) and the program proceeds to a return instruction ( block 53 ). this provides time for the stabilization of control loop . the entering of the calibration program is repeatedly triggered by the interruptions of the sawtooth signal . when the value of mns is smaller than 7 ( block 51 ), the time base is changed from 200 khz to 1 mhz and mns is read again ( block 55 ). subsequently , the tests of the blocks 56 to 61 are performed on the value of mns . if mns = 6 during the test of the block 56 , the variable t is selected from the circuit 21 , the microprocessor performs the operation mns - 1 = 5 ( block 62 ) and the program enters the block 53 . at the next passage , if mns = 5 during the test of the block 57 , the value of t is measured , the variable t1 is selected , the operation mns - 1 = 4 is performed ( block 63 ) and the program enters the block 53 . similarly , if mns = 4 during the test of the block 58 , the value of t1 is determined , the variable t2 is selected and the operation mns - 1 = 3 is performed ( block 64 ). if mns = 3 in the test of the block 59 , the value of t2 is determined , the variable t3 is selected , and the operation mns - 1 = 2 ( block 65 ) is performed . if mns = 2 in the test of the block 60 , the value of the variable t3 is determined and the operation mns - 1 = 1 is performed ( block 66 ). the term 3ta / 2 represents the necessary period of the calibration sawtooth in order to ensure that the frequency deviation δf emitted is 123 mhz ; this condition is reached when a1 = 0 . a1 / 8 is the correction which is applied to the amplitude of the sawtooth in order to obtain the correct frequency deviation δf . the microprocessor performs the operation δf + a1 / 8 and loads the result at a memory address . subsequently , the value of δf is tested in the blocks 68 and 69 in order to determine whether it is within the specified limits , that is to say between 0 and 255 . if the conditions δf & gt ; 0 and δf & lt ; 255 are satisfied , δf has a correct value and is applied to the circuit 26 ( block 70 ) which adjusts the amplitude of the sawtooth . if δf & lt ; 0 in the test of the block 68 , 0 is applied to the circuit 26 and δf is set to 0 ( block 71 ). if δf & gt ; 255 in the test of the block 69 , the value 255 is applied to the circuit 26 and δf is set to 255 . subsequently , the microprocessor performs the calculations which are shown in the block 73 : ta / 2 ; ta / 4 ; a2 = t3 - ta / 4 ; a2 / 8 and fo + a2 / 8 . if the conditions fo & gt ; 0 and fo & lt ; 255 are satisfied , fo has a correct value and is applied to the circuit 26 in order to shift the level of the modulation signal ( block 76 ). if fo & lt ; 0 in the test of the block 74 , fo is set to 0 and 0 is applied to the circuit 26 ( block 77 ). if fo & gt ; 255 in the test of the block 75 , fo is set to 255 and the value 255 is applied to the circuit 26 ( block 78 ). in order to test the effectiveness of the calibration of the frequency deviation δf and the mean frequency fo , it suffices to verify that the terms a1 and a2 are approximately zero at the end of each calibration sequence . they are normally situated between + 1 and - 1 . in these circumstances , the calibration stability is : ± 0 . 5 mhz for the frequency deviation δf and ± 1 mhz for the mean frequency fo . the memory location which contains the calculated value a1 is read ( block 79 ). the condition a1 & gt ; 0 is tested ( block 80 ); if not , the test of the block 81 , a1 + 1 & gt ; 0 is performed . if the result of the test of the block 81 is larger than zero , the value of a1 is situated between the limits 0 and - 1 . if a1 is larger than 0 in the test of the block 80 , the test of the block 82 is performed for the condition a1 - 1 & lt ; 0 . if the result is smaller than zero , a1 is situated between the limits 0 and + 1 . if a1 is situated between + 1 and - 1 , a2 is tested ; if not , the operation mns - 1 = 0 is performed and the alarm code a is set to 32 ( block 83 ). if a1 is situated between + 1 and - 1 , a2 is subsequently tested in the same manner . a2 is read ( block 84 ) and the test a2 & gt ; 0 is performed ( block 85 ). if a2 ≦ 0 , the test of the block 86 verifies that a2 + 1 & gt ; 0 , which means that a2 is situated between 0 and - 1 . if a2 is larger than 0 in the test of the block 85 , the test of the block 87 verifies whether a2 - 1 & lt ; 0 , which determines whether a2 is situated between 0 and + 1 . in the case where a2 is situated between + 1 and - 1 , the program enters the block 88 ( fig5 c ). if a2 is situated beyond the limits + 1 and - 1 , the operation mns - 1 = 0 is performed and the alarm code a is set to 64 ( block 89 ). the alarm code a = 32 or a = 64 starts the reading of a memory location nmsq in which the number of the successive calibration sequences is stored ( block 90 ). nmsq is set to the value 10 at the end of the last successful calibration phase . thus , nmsq ≦ 0 is tested ( block 91 ). if nmsq & gt ; 0 , the operation nmsq - 1 is performed ( block 92 ) and the program enters the block 53 . thus , if the first attempt to calibrate the frequency deviation δf and the mean frequency fo is not successful , it is tried again , up to a maximum of 10 times . if the oscillator 10 is properly calibrated during a subsequent attempt , the program enters the block 88 to initiate the third counter in the circuit 21 , which is used in the measurement of fbc . if not , nmsq ≦ 0 is found in the test of the block 91 . in this case the failure code is loaded at an address fl and the radio altimeter is set to the alarm condition ( block 93 ). subsequently , the type of failure is tested during the tests 94 to 96 . the failure codes for the three types of failure are : ______________________________________fbc failure code = 128 ( 10000000 in binary form ), i . e . bit d7 activated in the 8 - bit word ( d7 to d0 ) fl ; fo failure code = 64 ( 01000000 ), i . e . bit d6 activated ; δ . sub . f failure code = 32 ( 00100000 ), i . e . bit d5 activated . ______________________________________ in this case , if d7 = 0 ( block 94 ) and d6 = 1 ( block 95 ), the mean frequency fo is incorrect and a lamp on the display panel lights up ( block 98 ). if d6 = 0 , d5 = 1 is tested in the block 96 and if the test is positive , the frequency deviation δf is incorrect and another lamp on the display panel lights up ( block 99 ). if the source is correctly calibrated , the program branches from the start and the condition mns = 1 is tested ( block 61 ), fig5 b . if mns = 1 , eight periods of the calibration beat signal are measured by the third counter of the circuit 21 . each period has a duration of 40 μs . so 8 periods have a duration of 320 μs . the operation mns - 1 = 0 is performed and subsequently the value of 8 / fbc is read by the microprocessor . the calibration beat frequency fbc has to be 25 khz ± 2 % in order to be correct so the inequalities 313 & lt ; 8 / fbc & lt ; 327 must be satisfied . if 8 / fbc & gt ; 327 in the test of the block 102 , fbc is not correct and the alarm code a is set to 128 . if 8 / fbc & gt ; 327 , the test 8 / fbc & gt ; 313 is performed ( block 103 ). if 8 / fbc is larger than 313 , the value of fbc is correct and the system is initiated again for the measuring phase and a given number of indicators and words are loaded with the reinitialization values which are : nmsq = 10 for the next calibration phase fl ( d5 )= 0 , fl ( d6 )= 0 , fl ( d7 )= 0 for indicating that there is no failure . crsn = 10 . the next calibration routine is started after ten normal height measurements when crsn = 0 . at the end of this operation , the calibration routine is terminated and the measuring phase is initiated . if 8 / fbc is greater than 327 or smaller than 313 in the tests of the blocks 102 and 103 respectively , the alarm code a is set to 128 ( block 104 ) and the program follows the sequence of the blocks 90 , 91 and 92 , i . e . it is attempted ten times to measure fbc within the specified limits . if this is found to be impossible after the tenth attempt , the sequences of the blocks 93 and 94 are performed and a lamp on the display panel lights up ( block 97 ).
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fig2 shows in simplified form the configuration of a rake receiver having a mixr ( multipath interference exchange reduction ) function according to one embodiment of the present invention . in fig2 , a path searcher 10 detects path timings from an a / d converted received signal . a mict generator 12 generates all possible multipath interference correlative timings ( micts ) in accordance with the equation ( 1 ) from the path timings detected by the path searcher 10 . a timing selector 14 , based on criteria to be described later , selects as many timings as there are fingers 16 from among the path timings detected by the path searcher 10 and the micts generated by the mict generator 12 , and supplies the selected timings to the respective fingers 16 . each of the fingers 16 despreads the received signal at the timing supplied from the timing selector 14 , and outputs the despread received signal . for any path for which the corresponding mict has been selected , a mixr combiner 18 applies an appropriate weight to the result of despreading at the mict and adds the weighted result to the result of the despreading performed at that path timing . a rake combiner 22 performs rake combining by multiplying the result of despreading each path by the complex conjugate of a channel estimate output from a channel estimator 20 ; here , for the paths on which the mixr combining is done , the rake combining is performed using the results of the mixr combining . as shown in fig3 , the timing selector 14 selects the path timings and micts based on the results of the snir ( signal to noise and interference ratio ) calculations performed by an snir calculator 17 for various combinations of path timings and micts . as shown in fig4 , for any path for which the corresponding mict has been selected , the snir calculator 17 calculates the snir ( snir mixr ) expected to be achieved by the mixr combining ( 18 ) and then , using the result , calculates the snir ( snir rake ) expected to be achieved by the rake combining ( 20 ). when the result of despreading at mict tij is appropriately weighted and mixr - combined with the result of despreading at the path timing t ii in fig1 , the snir improvement η ij is given as η ij = σ i 2 σ i 2 -  α i  2 ⁢  α j  2 ⁢ i 4 rssi ( 2 ) here , α i and α j are channel estimates for the paths i and j , respectively , | α i | 2 and | α j | 2 are signal powers for the paths i and j , respectively , i 2 is the transmitting power of the transmitter estimated at the receiving end , σ i 2 is the signal variance at the path i , and rssi is the received signal intensity . the snir improvement η i when mixr combining is performed for the path i by using an arbitrary number of micts is given by the following equation . η i = σ i 2 σ i 2 - ∑ k ≠ 1 ⁢  α i  2 ⁢  α k  2 ⁢ i 4 rssi · a ik ( 3 ) 0 ( when mict of timing t ik is not used ) for example , in the example of fig5 in which the number of detected paths is four , i . e ., t 11 , t 22 , t 33 , and t 44 , when mixr combining is performed for the path of t 11 by using only the mict of timing t 12 , a ik in the equation ( 3 ) is a 12 = 1 , a 13 = 0 , and a 14 = 0 . when t 14 is further used , then a 12 = 1 , a 13 = 0 , and a 14 = 1 . when mixr combining is performed between path timing t ii and mict tij , snir mixr ( i ) representing the snir of the path i after the mixr combining is calculated by the following equation using the improvement η ij given by the equation ( 2 ). here , snir ( i ) representing the snir of the path i before the mixr combining is obtained from snir mixr ( i ) when mixr combining is performed using an arbitrary number of micts is calculated by the following equation using η i given by the equation ( 3 ). when the paths i and j are rake - combined , snir rake representing the snir after the rake combining can be expressed as shown below by using the snir ( i ) and snir ( j ) of the respective paths i and j . snir rake = ( 1 2 +  α i  2 ⁢  α j  2  α i  4 +  α j  4 ) ⁢ · ( snir ⁡ ( i ) + snir ⁡ ( j ) ) ( 7 ) for any path for which mixr combining is performed before the rake combining , snir mixr ( i ) given by the equation ( 4 ) or ( 6 ) is used instead of snir ( i ) in the equation ( 7 ). the timing selector 14 can , for example , calculate the snir ( snir rake ) expected to be achieved by the rake combining by using the equations ( 3 ), ( 5 ), ( 6 ), and ( 7 ) for each of all possible combinations of path timings and micts , the total number of timings being equal to the number of fingers 16 , and can determine the most appropriate combination of the path timing and mict by selecting the combination that gives the largest snir rake . this method , however , requires an enormous computation time , but the computation time can be shortened by selecting the timings in accordance with the following procedure . fig6 is a flowchart illustrating one example of the timing selection process in the timing selector 14 . in fig6 , the timings are selected in the following sequence . snir of each path is calculated using the equation ( 5 ), and one path timing that gives the largest snir is selected ( step 1000 ). snir improvement η ij is calculated using the equation ( 2 ) for each mict for the selected path , and the mict that yields the largest η ij is determined as a candidate for selection ( step 1002 ). for the mict determined as the selection candidate ( if two or more micts have been determined as selection candidates , then for each of the candidates ), snir mixr expected to be achieved when the mict is additionally selected is calculated using the equations ( 3 ) and ( 6 ), and then snir rake is calculated ( step 1004 ). for each of unselected path timings , the snir rake expected to be achieved when the path timing is additionally selected is calculated ( step 1006 ). based on the results of steps 1004 and 1006 , the path timing or mict that gives the largest snir rake is selected ( step 1008 ). steps 1004 , 1006 , and 1008 are repeated until processing is completed for all the fingers . in this case , if path timing is selected in step 1008 , then the mict that yields the largest η ij in accordance with the equation ( 2 ) ( or η i in accordance with the equation ( 3 )) is selected from among the micts for the selected path , and added as a selection candidate ( step 1010 ); on the other hand , if mict is selected in step 1008 , then among the unselected micts for the path associated with the selected mict , the mict expected to yield the largest η i in accordance with the equation ( 3 ) when the mict is additionally selected is added as a selection candidate ( step 1012 ). in the equation ( 5 ), the signal variance σ i 2 may be assumed to be constant regardless of the path and , in step 1000 , the path that gives the largest signal power | α i | 2 may be selected , rather than selecting the path that gives the largest snir ( i ) by calculating the snir ( i ) in accordance with the equation ( 5 ). when determining the selection candidates in steps 1002 , 1010 , and 1012 , the mict where the signal power | α j | 2 or the snir ( j ) of the interference path j is the largest may be determine as the selection candidate , rather than determining as the selection candidate the mict that yields the largest η ij or η i . to explain this using the example of fig7 , when determining either t ik or t ij , both the micts for the path i , as the selection candidate , | α k | 2 and | α j | 2 ( the lengths of the arrows in fig7 ) or snir ( k ) and snir ( j ) are compared to determine the selection candidate , instead of calculating η ik and η ij and comparing them . in step 1004 , rather than calculating the equations ( 3 ) and ( 6 ) to obtain the snir mixr ( i ) expected to be achieved when the selected mict is added , the equation ( 3 ) may be approximated by the equation ( 2 ) by noting only the path i and the interference path j and the snir mixr ( i ) may be calculated by using the equation ( 2 ) and ( 4 ). by so doing , the effect of each of the plurality of micts for one path can be evaluated independently of whether any other mict is selected or not . further , the equation ( 2 ) can be approximated as shown below if it is assumed that the noise component is uncorrelated . η ij = 1 +  α i  2  α j  2 ( 8 ) if the smir ( i ) is obtained using the equation ( 8 ) instead of the equation ( 2 ), the calculation can be simplified . alternatively , the snir ( i ) may be obtained using the following equation instead of the equation ( 8 ). the effect of the mict selection for each different path timing can be evaluated independently without calculating snir rake . in this case , the increase smir ( ij ) in snir expected to be achieved when each mict is selected is calculated in advance by using η ij calculated by the equation ( 2 ), ( 8 ), or ( 9 ); then , the snir ( ii ) of each path timing and the snir ( ij ) of the mict calculated in advance are compared , and path timings and micts are selected in order of decreasing magnitude of snir ( ii ) or snir ( ij ). this serves to speed up the selection process . fig8 shows the case of three paths . in the example shown in fig8 , timings t 11 , t 22 , t 12 , t 33 , . . . are selected in this order in order of decreasing magnitude . fig9 shows another example of the selection performed in the timing selector 14 . in this example , all of the path timings detected by the path searcher 10 are selected and supplied to the fingers 16 , and as many micts as there are remaining fingers 16 are selected in the timing selector 14 from the micts generated by the mict generator 12 . fig1 shows a flowchart of the process performed in the timing selector 14 of the above example . in fig1 , first , all the path timings detected by the path searcher 10 are assigned to the fingers ( step 1100 ), and if there is any remaining finger , then for each mict generated by the mict generator 12 the snir mixr expected to be achieved when the mict is selected is calculated using the equations ( 2 ), ( 4 ), and ( 5 ) ( step 1102 ), and snir rake is calculated using the equation ( 7 ) ( step 1104 ). then , the micts are assigned to any remaining fingers in decreasing order of snir rake ( step 1106 ). transformations and simplifications similar to those in the selection process described with reference to fig6 can also be applied in the selection process shown in fig1 . that is , in the calculation of snir mixr in step 1102 , the signal power | α i | 2 may be used instead of the snir ( i ) in the equation ( 4 ) to calculate the snir mixr as snir mixr ( i )=| α i | 2 × η ij ( 11 ) alternatively , snir mixr ( i ) may be evaluated using the snir ( j ) or | α j | 2 of the interference path j . here , η ij in the equation ( 4 ) or ( 11 ) may be calculated using the equation ( 8 ) or ( 9 ) instead of using the equation ( 2 ). further , if the equation ( 7 ) is approximated as the equation ( 10 ), snir rake need not be calculated in step 1104 , but the micts can be selected by only comparing the snir mixr ( i ) evaluated in step 1102 as described above , that is , | α i | 2 × η ij or snir ( j ) or | α j | 2 . in the selection process of the timing selector 14 thus far described , there can occur cases where some of the path timings detected by the path searcher 10 and some of the micts generated by the mict generator 12 overlap each other on the time axis . fig1 shows the case where the path timing t ij of the path i and the timing t jk , the mict for the path j with respect to the path k , overlap each other , while the path timing t kk of the path k and the timing t ji , the mict for the path j with respect to the path i , overlap each other . in such cases , rather than selecting both of the two overlapping timings and supplying them to two fingers , either the timing that gives the larger snir is selected or the path timing rather than the mict is always selected . alternatively , the two overlapping timings may be jointly assigned to one finger , and the result of despreading there may be used as the result of despreading at the path timing as well as the result of despreading at the mict . there can also be cases where two mict timings overlap each other as shown in fig1 . in such cases , only the mict that gives the larger snir is selected . instead of comparing the snir , the selection may be made by comparing the | α j | 2 or snir ( j ) of the interference path . alternatively , the two mict timings may be jointly assigned to one finger , and the result of despreading there may be used as the result of despreading at the two micts . fig1 is a block diagram in which a configuration for obtaining data necessary for the selection in the timing selector 14 and data necessary for the calculation of mixr coefficients in the mixr combiner 18 is added to the configuration of fig2 . in fig1 , fingers 30 which perform despreading using despreading codes for channel estimation data are provided in addition to the fingers 16 which perform despreading using despreading codes for recovering user data , and the outputs of the fingers 30 are supplied to the channel estimators 20 where channel estimates α i are calculated . a level measurer 32 calculates rssi , σ i 2 , and i 2 from the a / d converted received data and the despreading results output from the fingers 30 . fig1 shows the detailed configuration of the level measurer 32 . as shown in fig1 , rssi is calculated by taking the average ( 36 ) of the received signal intensities ( 34 ). further , σ i 2 is obtained by calculating the variance ( 38 ) of the output of each finger 30 for each path , and i 2 is calculated by subtracting the long term average ( 42 ) of the sums ( 40 ) for all the paths from the long term average ( 44 ) of the received signal intensities .
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referring now to fig1 the vehicle tire 10 has a tread portion 12 sidewalls 11 and beads 13 . conventionally the bead 13 includes a rigid ring made of a number of coils of steel wire . the tread portion 12 comprises a reinforcement belt 15 normally composed of a woven fabric or metal fibres with a relatively thick outer layer of high quality tread rubber 14 . the sidewalls and the inner part of the tread portion being formed of a lower quality rubber with a fabric reinforcement therein . fig2 a and 2b is a flow chart of the complete recycling process for vehicle tires in which the proposed removal separation and collection of different quality rubbers is incorporated . tires are collected from a range of sources at a central receival facility 100 and placed into a store 101 . after receival the tires may be sorted in accordance with size , rubber quality , remaining tread thickness or other characteristics that can influence the extent and nature of subsequent processing . the tires pass from the store 101 to the first processing operation 102 wherein the tread portion 12 of the tire is separated from the two sidewall 11 and integral beads 13 . the tread portion and sidewall - bead portions are stored separately at store 103 for subsequent independent treatment . the respective portions of the tire may also be stored separately in accordance with quality and or size considerations . from the store 103 the tread portion and sidewall - bead portion travel separate paths 104 , 105 respectively to the mechanical tread rubber shredder 106 and sidewall disintegrator 111 . the tread portion 12 is fed in strip form through the mechanical shredder 106 , so the high quality tread rubber located outwardly of the reinforcement belt is removed . this can be effected by a rotary cutter or grinder , as hereinafter further described , which produces rubber particles of a selected size . as the tread rubber particles are removed independent of other components of the tire , such as reinforcement materials , and without addition of other materials such as water , the tread rubber particles can be immediately passed to storage bin 121 . subject to the nature of further use and sale of the reclaimed tread rubber it can conveniently be withdrawn from the bin in batch lots weighed at 122 , packaged at 123 and stored at 124 for subsequent sale . as will be referred to hereinafter , other reclaimed tire materials can also be weighed , packaged and stored at 122 , 123 and 124 by the latter being selectively operably coupled to storage bins 117 and 118 . after the high quality tread rubber has been removed by the shredder 106 the tread portion strip is passed through uhpl disintegrator 107 where it is subjected to ultra high pressure water jets that break the strip down to particulate form . the resulting particle mix of rubber and steel wire from the tread belt is subjected to a magnetic separator 108 to remove the steel wire from the rubber , the steel wire being passed to a steel scrap store 125 for subsequent sale . the rubber particle material passes from uhp disintegrator 107 to a dewatering station 109 from which the water is recycled to the uhp disintegrator and the rubber particle material passed via a surge bin 110 to a dryer 115 . after drying the rubber particle material is then passed through sizing screens 116 and rubber particles within selected size ranges are directed to respective storage bins 117 and 118 . subject to the extent of size variation in the rubber particle material produced , and market demands , the rubber particle material can be graded into more than two sizes . the graded rubber particles can be weighed packed and stored at 122 , 123 , and 124 as previously referred to . the individual sidewall and bead sections are passed from the store 103 to the further uhpl disintegrator 111 wherein they are subjected to ultra high pressure water jets that breakup the sidewalls into particular material of rubber and fibre , and also removes the rubber and fibre material from the bead , also in particulate form . the mixture of rubber and fibre material passes from the uhp disintegrator 111 to the dewatering station 112 from which the separated water is passed through the filter 119 and then recycled to the uhpl water supply . the rubber and fibre particle material is passed to the separator 113 which can be of a flotation or cyclonic type , whereafter the fibre is passed to store 126 , and the rubber particle material passes to the surge bin 114 . as the nature of the respective materials held in the surge bin 110 and surge bin 114 are substantially the same they are each processed together or sequenually through the same equipment down stream of the respective surge bin 110 , 114 . thus material from surge bin 114 is dried by the dryer 115 , graded by the screen 116 , and subsequently weighed , packed and stored as previously described in relation to material from surge bin 110 . it will be seen from the above description of the proposed recycling process that there is recovered in a usuable form substantially the whole material content of the tire in an integated process . the high grade tread rubber is completely separated from the other materials of the tire , the lower grade rubber in the sidewalls and tread are each recovered separated from the respective reinforcement materials , and the fibre and steel of reinforcement materials are individually recovered . as each of these components of a tire are usuable for differing purposes or in differing products , the maximum financial return is obtainable by processing used tires by the process above described . further details of one practical construction and arrangement of specific machines used in carrying out the proposed process will now be described . referring to fig3 there is shown in basic form a mechanism for initially separating the tire into three sections , a tread portion and two sidewall - bead portions , comprising a tire chuck assembly 20 and a cutter assembly 21 . the chuck assembly comprise a tire platform 23 mounted upon the base frame 24 to rotate about a vertical axis and driven by the motor 25 through the reduction gear train 26 . mounted on the tire platform 23 are four chuck fingers 27 equally spaced about the axis of the tire platform 23 to pass through a tire 10 positioned on the platform . the four fingers 27 are each mounted to be radially slidable in unison with respect to the tire platform 23 in order to accommodate a range of tire sizes , and to permit a tire to be received freely over the fingers and then gripped thereby by moving the fingers radially outward in unison . the radial movement of the fingers 27 is effected by the hydraulic motor 28 to retract and expand the finger as required during loading , driving and unloading of the tires from the chuck assembly . the cutter assembly 21 comprises a base frame 30 with a cutter column assembly 31 mounted thereon for linear movement relative thereto toward and away from the tyre chuck assembly 20 . the vertical cutter drive shaft 32 is rotatable supported at the upper and lower ends by bearing arms 33 and 34 projecting from the column 31 . the drive shaft 32 is coupled to the motor 35 . the lower saw blade 37 is mounted in a fixed location on the drive shaft 32 . the position of the saw blade 37 is selected so the blade is at a level to cut a tire mounted on the tire platform 23 of the chuck assembly in the area of the junction between the tire tread portion and lower sidewall as indicated at 16 in fig1 . the upper saw blade 36 is mounted on the splined upper portion 38 of the drive shaft 32 so it can be adjusted to the level of the junction of the tire tread portion and the upper sidewall of the tire on the chuck platform 23 . the arm 39 is vertically slidable in the track 42 provided on the column 31 under the control of the hydraulic cylinder 40 . the arm 39 carries the support 41 for the upper saw blade 36 whereby by operation of the hydraulic cylinder 40 the upper saw blade 36 can be positioned relative to the lower saw blade 37 to suit different width tires . the complete cutter column assembly 31 is slidably mounted on the base frame 30 and movable relative thereto under the control of the hydraulic cylinder 45 in order to move the saw blades 36 and 37 into and out of operational engagement with a tire mounted on the chuck platform 23 . when the saw blades are so engaged with the tire , and the tire is rotating , the two sidewalls and beads will be each separated from the tread portion of the tire . upon release of the fingers 27 of the chuck assembly 20 the three sections of tire , namely the tread portion and two sidewall and bead portions , can be removed from the chuck assembly for subsequent individual processing . the tread portion 12 of the tire as removed from the chuck platform 23 is in the form of an annulus and is subsequently guillotined or otherwise cut across the face of the tread portion so it may be either flattened or rolled for economic storage . if the tread portion is to be stored flat it is preferred to cut it into two or three sections . it is to be understood that the above described separation of the tread portion from the sidewalls may be effected at a location remote from the area where the tread portion and sidewalls are further processed . this initial separation assists in the economic transportation of the tire to the processing plant , as the space occupied by separated components of the tire is substantially less than that occupied by the tire when in one piece . suitable equipment to separate the tread portion from the sidewalls may be mounted on a trailer or vehicle so that the initial sectioning of the tire is carried out as part of the collection operation and would enable the tread portion to be rolled or stacked flat and the sidewalls stacked flat for subsequent transportation and / or storage before further processing . referring again to fig4 the tread rubber removal assembly 48 comprises conveyor 45 and feed rollers 49 , which receive the previously separated tread portion 12 , and withdrawal rollers 50 which feed the remainder of the tread portion , after the removal of the tread rubber , to the uhp treatment apparatus 53 . the tread rubber removal assembly 48 further includes back - up rollers 51 and a rotary cutting 52 , the latter having an appropriate cutting tooth formation on the upper surface thereof , and is driven at a speed relative to the feed rate of the tread portion to remove the tread rubber in an appropriate particle size . the position of the cutter 52 with respect to the back - up roller 51 is adjusted in accordance with sensed measurements of the tread portion , particularly the thickness thereof , so that the cutter 52 only removes that portion of the tread rubber below the level of the reinforcement belt in the tread portion of the tire . this tread rubber being of a higher quality than the remainder of the tire and is required to be kept separate therefrom . the high grade tread rubber is collected in the hopper 55 and withdrawn therefrom by the screw conveyor 56 and delivered to bin 121 ( fig2 b ). the remainder of the tread portion of the tire is then passed into the uhpl apparatus 53 by the conveyor 54 wherein two revolving heads 56 , each with an array of high pressure nozzles impinge jets of water onto the remainder of the tread portion to cut the rubber therein into small particles and strip it from reinforcement belt , which is normally , of a metal filaments construction . in order to separate the metal filaments , released as the rubber is removed by the uhp apparatus 53 , from the rubber a magnet structure 58 is provided adjacent the lower flight of the conveyor on the side thereof opposite the tread portion . the magnet structure is constructed to provide a magnetic field of sufficient strength to hold the metal filaments in contact with the conveyor and thereby separate the filaments from the rubber particles created by the uhpl jets . the influence of the magnetic field created by the magnet structure extends a short distance beyond the area where the tread rubber particles are collected in the hopper 59 so that beyond the magnetic influence the metal reinforcement belt fibres are discharged onto conveyor 54 . the rubber removed by the uhpl apparatus in particle form is collected in the hopper 59 and removed therefrom by the screw conveyor 57 with the water from the uhp apparatus being separated from the rubber particles . it will be appreciated that provision is made for the appropriate collection of the tread rubber removed by the cutter 52 independently of the rubber removed by the uhpl device , so the higher value tread rubber can be recycled separately . also the metal belt fibres can be recycled . the sidewalls with the beads integral therewith are processed independently as indicated in fig2 a by equipment as will now be described with reference to fig5 and 6 of the accompanying drawings . the sidewall and bead sections 11 are deposited on the conveyer 60 and passed sequentially beneath a series of three uhpl devices 61 positioned and operated to break up the rubber and fibre reinforcement of the sidewall and to remove rubber from the bead portion 13 . the sidewall and bead portion 11 of the tire as removed from the tread portion , is loaded onto the conveyor 60 in a row formation and are advanced through the treatment area 66 , wherein three uhpl devices 61 are arranged to operate simultaneously in breaking up the wall portion of the tire passing therethrough , and release the rubber attached to the bead wires . the three uphl devices are arranged so the full width of the side wall and bead portion is subjected to the action of the jets of the uph devices in a single pass . if desired the relative location of the uhpl devices may be adjusted for accommodating sidewall portions of differing diameters . it has been found that a small number , up to about four , of individual sidewall and bead portions can be stacked one on the other and subjected to the uhpl treatment in that stacked arrangement . it is to be appreciated that although the uhpl jets have a highly effective cutting action , they apply only minimum forces to the sidewall and bead portions and thus it is not required to hold down or otherwise secure the sidewall portions to the conveyor 60 . the rubber and fabric particle created in the breaking up of the sidewalls is collected in the hopper 62 from which it is passed by screw conveyor 67 to the dewater treaatment and then separation of the rubber from the fabric as referred to with respect to fig2 a and 2b . the steel wire of the bead is passed directly to storage or may be chopped to small lengths , or baked prior to storage . the equipment above described herin with reference to fig3 to 6 is intended to be only the currently best known equipment for carrying out the method claimed in this application . it is to be understood that other equipment may be used in the practice of the invention . also the individual processing of the respective sections of the tire are not necessarily carried out at the same time or at the same location . the uhpl cutting equipment as rererred in the description of the practical implementation of the present invention is not described herein in detail as the basic principles of operation of such equipment is well known and can be readily applied to provide cutting equipment suitable for use in carrying out the present invention .
8
in the drill rig 10 of fig1 a hook device 11 embodying the present invention is shown suspended from the usual travelling block 12 which is movable upwardly and downwardly relative to the crown block 13 by a suspending line 14 actuated by draw works 15 . hook 11 can support the drill string 16 during drilling , and through two links 17 can also support an elevator 18 for gripping and moving an upper section of the drill string during the process of adding a section of pipe to the string or removing a section from the drill string , or for other purposes . as seen in fig2 a and 3b , the present hook device includes a tubular outer body 19 centered about a vertical axis 20 and which has an outer cylindrical surface 21 and an inner cylindrical surface 22 . this body 19 is suspended by an upper connector structure 23 including a bail 24 by which the device is attached to the travelling block or other suspending element . a tubular inner body 25 is contained within outer body 19 and concentric therewith about axis 20 and is mounted for movement upwardly and downwardly along axis 20 relative to body 19 and for rotary movement about axis 20 relative to body 19 . body 25 is urged upwardly by yielding means preferably taking the form of a stack of belleville springs 26 . body 25 is connected at its lower end to a hook element 27 to which the drill string or other supported load can be connected , with that hook element having associated therewith a link supporting member 28 from which the links 17 are suspended . near its horizontal upper end surface 29 , body 19 contains an internal annular groove 30 centered about axis 20 and typically having the essentially rectangular configuration illustrated in fig3 a , with the downwardly facing upper wall 31 of the groove preferably being disposed directly horizontally to function as a load supporting shoulder . upper connector structure 23 includes two connector parts 32 which in the assembled condition of the device are spaced laterally apart and disposed parallel to one another , as seen in fig4 and 5 . opposite sides of these connector parts may be defined by parallel vertical surfaces 33 . at their opposite ends , the parts 32 have lugs 34 which are curved arcuately about axis 20 and project into groove 30 , with upper horizontal surfaces of the lugs engaging the downwardly facing groove walls 31 to support body 19 from parts 32 . in the assembled condition of the device , the parts 32 are held in their spaced condition of fig4 and 5 by a spacer 35 received therebetween , and having vertical parallel opposite side surfaces 36 engaging two of the surfaces 33 of parts 32 to hold them in positions in which their lugs 34 are received within groove 30 in supporting relation . the spacer has the vertical sectional configuration illustrated in fig3 a , to present arcuate end lugs 37 receivable within groove 30 . during assembly , these lugs 37 can be inserted downwardly through interruptions or notches 38 formed at diametrically opposite locations in the portion 39 of tubular body 19 above groove 30 . when spacer 35 is not in position between the two connector parts 32 , each of these connector parts can be moved to a position of vertical alignment with notches 38 , and is short enough horizontally to then be movable upwardly or downwardly past portion 39 at the location of notches 38 . thus , during assembly one of the connector parts can be inserted axially into body 19 through notches 38 and then be moved laterally to a position of extension into groove 30 , after which the other connector part can be inserted downwardly through notches 38 and then shifted laterally in the opposite direction to a spread condition in which the spacer 35 can be inserted downwardly between the parts to hold them in separated relation . the spacer may be moved into position by inserting its end lugs 37 through notches 38 as discussed . the parts may be disassembled in reverse manner , by first withdrawing spacer 35 upwardly through the notches , and then moving the two elements 32 sequentially to positions of alignment with notches 38 for withdrawal upwardly therethrough . the bail 24 also serves to hold parts 32 in spaced relation , by reception of each of the two connector eyes 40 of the bail between two upwardly projecting connector eyes or loops 41 of the two parts 32 ( fig4 ), with a pin 42 extending through the aligned openings in eyes 40 and 41 to interconnect the parts and effectively support parts 32 and body 19 from the bail . a horizontal plate 43 extends across the top of outer body 19 , and carries upwardly projecting plates 44 welded to plates 43 and received at the outer sides of eyes 41 , with plate 43 being secured to body 19 and to spacer 35 by screws 45 to hold the spacer in proper assembled position between parts 32 and thereby maintain the integrity of the entire supporting structure . at its lower end , body 19 may have a lower extension 19 &# 39 ; secured to the main section 19 of the body by screws 46 , and containing an annular bushing 149 engaging the outer cylindrical surface 150 of member 25 to center and guide that member for its rotary movement about and vertical movement along axis 20 relative to body 19 . a support ring 47 is confined between parts 19 and 19 &# 39 ; ( fig3 a ), to form an upwardly facing support shoulder on which an annular thrust bearing 48 ( typically a roller bearing as shown ) is supported . ring 47 may be formed of a number of arcuate segments having a combined circular extent slightly less than the annular extent of the space within which they are received , to facilitate their insertion into an inner groove 49 in body 19 during assembly of the parts , with a portion 50 of body extension 19 &# 39 ; engaging the radially inner surfaces of ring segments 47 to hold them in position . a ring 51 extending about tubular inner body 25 is supported on the upper race of bearing 48 for rotation about axis 20 , and has inner vertically extending keys 52 secured to the ring by screws 53 and projecting into vertical spline grooves 54 in the outer surface of body 25 in a relation retaining that body against rotation relative to ring 51 while permitting upward and downward movement of body 25 relative to the ring . downward movement of inner body 25 relative to outer body 19 is limited by engagement of a downwardly facing annular stop shoulder surface 147 formed on an annular flange 84 of body 25 with an upper annular stop shoulder surface 148 on ring 51 , in which condition downward load forces are transmitted directly from body 25 to body 19 independently of springs 26 . at its radially outer side , adjacent outer body 19 , ring 51 contains a series of circularly spaced notches 55 ( fig8 ) into which a locking pin 56 of a locking device 57 is projectable to releasably retain ring 51 and body 25 in any of a number of different rotary settings relative to body 19 . as seen in fig3 a , 8 and 9 , the locking device 57 includes an actuating member 58 which is accessible from the outside of outer body 19 and may take the form of a disc received within a tubular element 59 welded to the outside of body 19 , with member 58 being mounted to turn about an axis 60 extending perpendicular to and intersecting main axis 20 of the device . disc 58 is secured by screws 61 to a camming part 62 which is journalled for rotation within a bore 63 in a part 64 secured rigidly by screws 65 to body 19 . camming part 62 is retained against axial movement by an annular element 66 attached to part 64 by screws 67 and acting to confine an annular rib 68 on part 62 between the elements 64 and 66 while permitting rotation of part 62 . the locking pin 56 has a cylindrical enlargement 69 received slidably within a cylindrical inner bore or recess 70 in part 62 , and urged axially inwardly ( rightwardly in fig8 ) by a coil spring 71 , to yieldingly urge pin 56 to its fig8 active position of reception within one of the notches 55 in the outer surface of ring 51 . a pin 72 is connected rigidly to pin 56 and projects laterally therebeyond in opposite directions for reception within camming openings 73 ( fig9 ) in the tubular side wall of part 62 , so that upon rotation of member 58 and camming part 62 , the engagement of the pin 72 with camming edge 74 of part 62 will act to forcibly retract pin 56 radially outwardly away from axis 20 and against the tendency of spring 71 and to an inactive position out of notches 55 in ring 51 , thereby permitting rotation of the ring . reverse rotation of actuating member 58 and camming part 62 permits pin 56 to return radially inwardly toward axis 20 under the influence of spring 71 and to an active locking position retaining ring 51 against rotation about axis 20 from any of a series of different rotary settings of ring 51 and the tubular inner body 25 . above ring 51 , outer body 19 contains a camming ring 75 which is confined vertically between ring 51 and a top wall assembly 76 in a relation preventing vertical movement of the camming ring 51 while permitting its rotation about axis 20 . ring 75 has an outer cylindrical surface 77 engaging the inner cylindrical surface 22 of tubular outer body 19 , and has upper and lower horizontal surfaces 78 and 79 engaging top wall assembly 76 and ring 51 to locate ring 75 against vertical movement . extending upwardly from its bottom surface 79 , cam ring 75 has a series of circularly spaced notches 80 coacting with a locking device 57 &# 39 ; which is identical with the locking device 57 illustrated in fig3 a , 8 and 9 and is carried by the side wall of tubular outer body 19 at a location offset 90 ° ( ninety degrees ) about axis 20 from locking device 57 . the locking pin 56 &# 39 ; of device 57 &# 39 ;, corresponding to pin 56 of the previously described locking device 57 , is actuable radially inwardly and outwardly relative to axis 20 between a locking position of reception within one of the notches 80 in cam ring 75 and a radially outwardly retracted inactive position withdrawn from the notch , to thus releasably lock cam ring 75 in any of a series of different rotary settings relative to outer body 19 . as will be understood , the second locking device 57 &# 39 ; of course has an actuating member corresponding to member 58 of fig8 which is accessible from the outside of body 19 and is adapted to be rotated about an axis extending radially of main vertical axis 20 , and functions upon such rotation to move pin 56 &# 39 ; between its active and released positions through the action of a camming element corresponding to that represented at 62 in fig8 . in view of the identity of structure between the two locking devices 57 and 57 &# 39 ;, only one has been shown in detail in the drawings . for coaction with the camming ring 75 , the tubular inner body member 25 carries a cam follower roller 81 , mounted by a shaft 82 for rotation relative to the shaft about an axis 85 extending perpendicular to and intersecting axis 20 . shaft 82 may be attached to member 19 by extension through an opening 83 in an increased thickness upper flange portion of member 19 , with a nut 86 retaining the shaft against disassembly from member 19 . roller 81 is engageable with a downwardly facing inclined ramp surface 87 formed on a radially inner portion of camming ring 75 . as seen in fig1 , this ramp surface has a lowermost portion 88 at one location about axis 20 , and in extending circularly in both directions from that point is inclined upwardly through 180 ° ( one hundred and eighty degrees ) to a diametrically opposite location at which the ramp surfaces lead to a notch or interruption 89 at which the roller 81 does not engage the ramp surface ( see fig3 a ). the engagement of roller 81 with camming ramp surface 87 causes inner body 25 to be automatically rotated to a predetermined rotary position relative to cam ring 75 upon spring induced upward movement of the inner body , with that rotary setting being the position at which roller 81 is received within the interruption 89 at the highest point of ramp surface 87 . cam ring 75 can be locked in any desired rotary position relative to outer body 19 , so that the position to which the inner body is automatically turned upon upward movement is in a desired orientation with respect to outer body 19 . top wall assembly 76 is supported on an annular shoulder 90 in outer body 19 , and may be formed sectionally of a number of parts , as illustrated . more particularly , assembly 76 may include two rings 91 and 92 welded together at 93 and insertable downwardly into outer body 19 to the position of fig3 a , and an inner circular top wall element 94 secured to ring 92 by screws 95 . a central post structure 96 is carried by top wall 94 and projects downwardly therefrom along axis 20 to support the belleville springs 26 . this post structure 96 includes a part 97 extending upwardly through an opening 98 in top wall 94 , and suspended therefrom by connection of a nut 991 to the threaded upper end of part 97 . beneath part 97 , the post structure 96 includes a downardly projecting tube 99 secured in appropriate manner to part 97 as by welding a flange 100 to the upper end of tube 99 and then securing that flange to a flange 101 on part 97 by screws 102 . an annular flange 103 is welded to the lower end of tube 99 and projects radially outwardly therefrom to apply upward force to the belleville springs . a tubular roller bearing 104 projects upwardly into the lower end of tube 99 , with the outer race of the bearing being secured to flange 103 by screws 105 , and with the inner race engaging an externally cylindrical centering post carried by and projecting upwardly from a circular bottom wall 106 . the upper end of the stack of belleville springs 26 engages an annular horizontal top plate 107 , which transmits the upward force of the springs to member 25 by essentially annular engagement with a ring 108 secured rigidly to body 25 by a series of circularly spaced screws 109 . this ring 108 may extend through almost 360 ° ( three hundred and sixty degrees ) about axis 20 , being interrupted only at the location of the previously mentioned cam follower roller 81 . upward movement of plate 107 is limited by its contact with flange 100 of tube 99 . each of the belleville springs 26 is an annular element formed of spring steel centered about axis 20 and having an inner circular opening slightly greater in diameter than tube 99 to be located thereby without binding contact therewith . the outer circular edge 117 of each of the belleville springs is of a diameter slightly less than the internal diameter of tubular inner body 25 , to avoid binding contact with that body . each spring may be of essentially uniform thickness through its entire radial extent , and be defined by parallel upper and lower frustoconical surfaces 118 . the springs are arranged in a series of successive pairs , as illustrated , with the two springs of each pair facing oppositely , so that upon downward movement of the tubular inner body 25 relative to outer body 19 , the springs are deformed from their normal frustoconical shape toward flattened conditions , against the tendency of the resilient spring metal of which the elements 26 are formed , to yieldingly resist the downward movement of the inner body . these belleville springs are designed and selected to have a substantially constant spring rate through the entire range of downward movement of inner body 25 relative to the outer body 19 , i . e . the stack of belleville springs apply a substantially uniform upward force to the inner body throughout its range of vertical movement . this is desirable in order to avoid the development of excessive upward force in the spring assembly . if a coil spring having a non - uniform spring rate were utilized in lieu of the stack of belleville springs , the upward shock forces which would be applied by the inner body to the outer body upon upward movement of the inner body by the springs would be excessive and tend to degrade the overall assembly more rapidly than would be desired . to assist in dampening the upward and downward movements of inner body 25 relative to outer body 19 , the chamber in the inner body within which the springs are contained may be filled with an appropriate oil or other liquid , retained at the bottom of the chamber by seals 119 , with openings 120 allowing restricted flow of fluid through flange 103 , and with slits 121 in tube 99 allowing flow of the liquid radially between the interior and exterior of the tube . referring now to fig3 b , the lower connecting assembly or structure 123 by which tubular inner body 25 is attached to a suspended load includes , in addition to hook 27 and link supporting member 28 , two connector parts 124 and a spacer 125 therebetween , corresponding in certain respects to connector parts 32 and spacer 35 at the upper end of the device . parts 124 may be identical with one another and each have two parallel vertical opposite side surfaces 126 , with the inner of these surfaces of each member 124 being engageable with corresponding vertical opposite side surfaces 127 of spacer 125 in the fig3 b assembled condition of the parts . each part 124 has two arcuate flanges 128 at its opposite ends , which in the assembled condition project into an annular groove 129 formed in the lower end of tubular body 25 to support parts 124 and the rest of the lower connector structure from that inner body 25 . when spacer 125 is not in place between the two connector parts 124 , each of those parts may be moved laterally toward axis 20 relative to inner body 25 , and to a position in which the flanges 128 are aligned with notches 130 formed in member 25 beneath groove 129 , allowing each part 124 to be moved upwardly into body 25 to the location of groove 129 or be withdrawn downwardly therefrom by movement of flanges 128 through notches 130 during assembly and disassembly of the parts in the same way that upper elements 32 can be inserted or removed through notches 38 as discussed . after the parts 124 have been located in their fig1 position , spacer 125 can be moved upwardly between these parts to the spacing condition of that figure , and be retained at that location by screws 131 attaching part 125 rigidly to the bottom of inner body 25 . the link supporting member 28 has a portion 133 received between connector members 124 at a location beneath spacer 125 , and typically slightly narrower than member 125 with the vertical opposite side surfaces 132 of portion 133 of member 28 being parallel to and closely proximate the vertical inner surfaces 126 of members 124 . link supporting member 28 is elongated as shown in fig3 b , with the central portion 133 of member 28 being secured to members 124 by a cylindrical connector pin 134 received within aligned cylindrical openings 135 in parts 124 and 28 . member 28 has end portions 136 projecting laterally beyond members 124 and beyond hook 27 in opposite directions and shaped to define recesses 137 within which the upper portions of links 17 are received in supporting relation , with the upper eyes of the links extending about end portions 136 of member 28 and being detachably retained therein by closure elements 138 extending across the recesses and secured detachably at their opposite ends to member 28 . hook 27 has an upper bifurcated portion 139 forming two arms 140 which are received at opposite sides of connector member 124 , with inner vertical parallel surfaces 141 of arms 140 engaging the outer side surfaces 226 of the two members 124 and being secured to parts 124 and 28 by extension of end portions of pin 134 into cylindrical openings 142 in arms 140 . the lower end of member 27 has the usual hook shaped configuration , defining an upwardly facing recess 144 within which a bail or other element to be suspended is receivable , with a gate element 145 being adapted to releasably close the open side of the hook , and for that purpose being pivotable between the full line and broken line positions of fig1 , and being retainable in the full line closed position by latching mechanism represented at 146 . the hook of the present invention is used in conventional manner , to support a load in some instances by engagement with hook 27 , and under other circumstances through an elevator 18 suspended by links 17 attached to member 28 of the device . in either case , the load forces are cushioned by springs 26 , which resist downward movement of inner body 25 of the device with the load relative to outer body 19 . when the entire weight of the string is supported by the device 11 , or another similarly very heavy load is suspended , inner body 25 will be pulled downwardly against the tendency of springs 26 to a position in which the annular downwardly facing shoulder surface 147 on inner body 25 engages upwardly facing annular shoulder surface 148 on ring 51 , to thereby transmit the downward load forces directly from inner body 25 to outer body 19 through ring 51 , bearing 48 and ring 47 . when the load is released , the springs return the inner body and carried parts upwardly to the fig3 a position . this upward movement is limited by engagement of ring 107 with flange 100 , with the shock forces accompanying such engagement being minimized by the constant spring rate characteristic of the belleville springs as discussed previously . the inner body 25 can be locked in any desired rotary position relative to outer body 19 by actuating locking device 57 to move its lock pin 56 into a corresponding one of the notches in the outer surface of ring 51 , to thus retain the ring in a fixed rotary setting , and through the keys 52 retain the inner body in a corresponding rotary setting . when this lock is in released condition , camming ring 75 acts upon upward movement of the inner body 25 to turn that inner body to a predetermined rotary setting relative to the outer body . the position to which the cam returns the inner body may be predetermined by setting cam ring 75 to a desired rotary setting in outer body 19 , and then locking it in that setting by actuation of the second locking device 57 &# 39 ;. if the link supporting member 28 becomes worn in use , it may be easily removed by merely driving pin 134 out of the aligned openings in the various parts connected thereby , after which a new link supporting member may be moved into position and the parts then be reconnected by pin 134 to return the device essentially to its original condition . in assembled condition , the link supporting member 28 may be retained in rigidly fixed position relative to hook element 27 by a rigid cylindrical vertical pin 150 received at its opposite ends within aligned cylindrical recesses 151 and 152 in parts 27 and 28 . if desired , the vertical movement of inner body 25 relative to outer body 19 may be resisted by a shock absorber 154 contained within tube 99 and including a liquid filled cylinder 155 threadedly connected at its upper end to part 97 , and a piston 156 in the cylinder containing fluid passing apertures . the rod of piston 156 may have an enlargement 157 at its lower end engaging a rod 158 projecting upwardly from and fixed relative to bottom wall 106 to actuate the piston upwardly when the parts are returned by belleville springs 26 to their fig3 a positions . a spring 159 may urge the piston downwardly upon downward movement of inner body 25 relative to outer body 19 . as will be understood , the small apertures provided in the piston permit a predetermined restricted flow of liquid vertically past the piston to attain the desired shock absorbing effect preventing too abrupt spring urged upward movement of body 19 . while a certain specific embodiment of the present invention has been disclosed as typical , the invention is of course not limited to this particular form , but rather is applicable broadly to all such variations as fall within the scope of the appended claims .
4
fig1 shows a longitudinal section through a rock anchor with a tension member 1 , which is inserted into a borehole 2 . the borehole 2 is filled along its entire length with hardening material 3 , for instance synthetic resin adhesive , with the tension member 1 being embedded and anchored over a specific distance in the lower region of the borehole . the tension member 1 is freely extensible over the remaining portion of its overall length , for instance by being guided within a jacket tube 4 . an anchoring device a is arranged at the downstream ( or air ) side for securing the excavation face 5 . the anchoring device is supported by an anchor plate 6 against the excavation face 5 . a first embodiment of an anchoring device a is shown in elongated longitudinal - and cross - section and in fig2 to 4 . according to fig2 a the anchoring device consists of a support element 10 and an anchoring element 11 . this anchoring element 11 is designed as an anchor nut with a hexagonal cross - section ( fig4 ) which is threaded with its inside thread 7a upon the external thread 7b of a tension member provided as an anchor rod 1 &# 39 ;. the support element 10 includes a hollow body 12 which in the depicted embodiment consists of a cylindrical jacket with a hexagonal horizontal projection corresponding to the anchor nut ( fig3 ). the hollow body 12 is connected to form one piece with a base part 13 and have a central bore 14 for passage of the anchor rod 1 &# 39 ;. the bottom side of the base part 13 is hemispherical , in order to be able to execute angular rotations to a certain extent with respect to the anchor plate 6 . inside of the hollow body 12 in the region of a top surface 15 of the base part 13 , there are located projections 17 which adjacently protrude over the inside wall 16 of the hollow body 12 and form a shoulder 18 at their upper end . it is discernible from fig3 which shows a cross - section through the hollow body 12 without the anchor nut 11 , that the shoulder 18 forms a circular inner edge , whose diameter d corresponds to the diameter of the circle tangential to the hexagonal cross - section of the hollow body 12 . the shoulder 18 thus consists of individual partial faces 19 between the inscribed tangential circle and the inner face 16 of the hollow body 12 . the anchor nut 11 corresponds in its horizontal projectional shape to the inside cross - section of the hollow body 12 , so that it is retained non - rotatably therein , however it is longitudinally displaceable . fig2 a shows the anchor nut 11 shortly before contact with the shoulder 18 of the support element 10 . when the entire load is carried , the anchor nut 11 rests against the shoulder 18 of the support element 10 and thus transmits the anchoring force in the partial faces 19 ( fig4 ). the anchor nut 11 is turned on a lathe to be circularly shaped at its bottom end , so that it finds guidance is in the lower narrower region of the inside space of the hollow body 12 . the shoulder 18 itself is beveled at the surface , in order to make the application or engagement of the force more uniform . the strength of the material of the anchor nut 11 and the size of the partial faces 19 are chosen or tuned to each other in such a way that only an anchoring force up to a predetermined magnitude can be transmitted . when this force is exceeded the anchor nut 11 is plastically deformed in the region of the partial faces 19 . because of this deformation , a relative displacement between the support element 10 and the anchor nut 11 through a distance s is caused . fig2 b shows the condition after an accomplished displacement s &# 39 ;. the magnitude of the displacement travel s , which permits judgment of a specific amount by which the anchoring force has been exceeded , can be indicated in a simple manner by adapting the length of the anchor nut 11 to the length of the hollow body 12 so that the anchor nut 11 completely disappears in the hollow body 12 when a specific anchoring force is reached . the surface 20 of the anchor nut 11 and the surface 21 of the hollow body 12 then lie in one and the same plane . this means a change of the shape of the anchoring device which can also be perceived in an explicit manner from a certain distance . fig2 a and b however also show another more comfortable possibility for indicating the displacement travel s which basically permits also the indication of several force stages . here a head plate 22 , for instance of plastic material , is placed for , instance threaded , upon the outer end of the anchor rod 1 &# 39 ;. the head plate 22 is to be threaded on to a point where its bottom face 23 rests upon the top face 20 of the anchor nut 11 . it then has the spacing s to the surface 21 of the hollow body 12 . spacer pins 24 , 25 of different lengths are inserted in a clamped manner into the head plate 22 , and penetrate through the head plate 22 upwardly and are visually perceivable from the outside if the spacing s is reduced because a deformation has occurred . in the condition in fig2 a , the longest pin 24 is not yet in contact with the surface 21 of the hollow body 12 . in the condition in fig2 b , the pin 24 already protrudes upward , while the shorter pin 25 just contacts the surface 21 . any other indication devices can be utilized in place of these distance or spacer pins 24 , 25 . another embodiment will be described below with the help of fig1 a and b . it can also be described with the help of the embodiment depicted in fig1 to 4 how an overload can be indicated gradually in stages . for this purpose the edges at the bottom side of the anchor nut 11 are razed to different levels . the anchor nut 11 then comes to rest with only several of these partial faces 19 , mainly the lowermost ones , against the shoulder 18 of the support element 10 . it is depicted in the diagram shown in fig5 how a first longitudinal displacement through a travel s 1 occurs when the first stage of the tensile force p 1 is reached , until the next following partial faces of the anchor element 11 rest against the shoulder 18 . only when the second stage of the tensile force p 2 s reached does a displacement through the travel s 2 occur . further stages can possibly follow upon this displacement . these different load stages can be indicated by the different length pins 24 , 25 which emerge successively from the head plate 22 . the highest load stage is attained when all pins have emerged . a second embodiment of an anchoring device in the invention is depicted in fig6 and 7 . this embodiment can be used for instance if angular rotations of the anchor rod with respect to the anchor plate are not anticipated . the hollow body 32 of the support element 30 is in this case placed directly , meaning without a base part , upon a simple flat anchor plate 6 &# 39 ;. the anchor plate 6 &# 39 ; abuts on its part directly against the excavation face 5 . in this embodiment , the hollow body 32 is also provided with projections 34 in its lower region protruding inwardly beyond its inner wall 33 , which projections can , but are not required to , have an oblique surface . as is shown in fig7 a total of four such projections 34 are distributed across the inner periphery of the hollow body 32 . the anchoring element 31 consists of a simple circularly cylindrical member , which is insertable into and guided by the circularly cylindrical cavity of the hollow body 32 . in order to be able to thread the anchoring element 31 which is again provided with an inside thread 7a upon the external thread 7b of the anchor rod 1 &# 39 ;, the anchoring element can be provided with a hexagon 35 at its upper end . in this embodiment of the anchoring device , the projections 34 are worn off or razed when the tensile force is exceeded . the displacement travel arising therefrom is indicated on the outside to be visually recognizable in that the anchor nut 31 disappears inside of the hollow body 32 . a third embodiment of the anchoring device is depicted in fig8 and 9 . in this embodiment , the tension member of the anchor is a strand 1 &# 34 ; of steel wires , upon which a sleeve by way of an anchoring element 41 is undisplaceably pressed by radial clamping pressure . since this pressed - on sleeve 41 as a rule must consist of a comparatively soft material in order to be able to deform , an anchor ring 44 is arranged upstream of it in the force direction , which can be placed loosely upon the strand 1 &# 34 ;. the anchor ring 45 is provided with projections 45 extending in a helical screw manner at its outer circumference . the hollow body 42 of the support element 40 comprises here at its inner side 43 an internal thread 46 matching the projections 45 . the hollow body 42 consists expediently of a softer material than the anchor ring 44 . the hollow body 42 in this case abuts again upon the base part 47 , which in turn rests with its hemispherically - shaped bottom surface against the anchor plate 6 thus enabling angular rotations . with this embodiment of the anchoring element 41 , especially of the anchoring 44 and hollow body 42 , one also achieves to a certain extent a prestraining and bracing of the strand 1 &# 34 ;, since the hollow body 42 can be turned with respect to the bottom part 47 in a manner similar to a nut . in case of an overload , deformation occurs here in the threaded region between the anchor ring 44 and the hollow body 42 . the indication of the longitudinal displacement occurring herein is performed herein again by means of a head plate 48 which can be placed upon the strand 1 &# 34 ; or the anchoring element 41 from above . the head plate is here designed to form a cover hood 50 by molding a cylindrical wall 49 upon it , which hood reaches up to the region of the hollow body 42 and thus terminates the anchoring device so as to be protected from corrosion , to the extent that it includes the part for indicating the relative displacement . the pin 51 passes through the head plate 48 , which abuts against the upper end face 52 of the hollow body 42 , and exits upward from the head plate in case of a longitudinal displacement of this head plate connected with the strand 1 &# 34 ;. a last embodiment for an anchoring device pursuant to the invention , proceeding from the illustration in fig6 and 7 , is depicted in fig1 a and 10b . while the anchoring device as such corresponds in its essential characteristic , namely the support element 60 designed as a hollow body 62 and the anchoring element 61 designed as a nut , to that in fig6 and 7 , a particularly simple and economical embodiment of the indication device for the displacement travel s is shown here . a cover hood 65 is placed upon the upper end of the anchor rod 1 &# 39 ; equipped with an external thread 7b . the cover hood 65 consists of a head plate 66 which includes an extension 67 with an internal thread 7a at the inner side , which fits upon the external thread 7b of the anchor rod 1 &# 39 ;. this cover hood 65 itself is formed by molding a cylindrical wall 68 at the external circumference of the head plate 66 . the hood 65 can be screwed so far upon the anchor rod 1 &# 39 ; until its lower end comes to sit upon the surface of the anchor plate 6 &# 39 ;. thus a closed - off cavity inside of the cover hood 65 is formed , which cavity can also be filled with corrosion protection material . the cylindrical wall 68 of cover hood 65 is provided in the course of its length at the inside with a circumferential annular groove 69 , forming a rated break point in compression . if , when the anchoring force is exceeded , the projections 64 protruding beyond the inner face 63 of the hollow body 62 are worn off by the anchoring element 61 , if such a longitudinal displacement occurs , then the cylindrical wall 68 of the cover hood 65 is stressed in compression . this compressive stress results in rupture at the weakest point , in the region of the annular groove 69 , which then deforms outwardly into a bead 70 ( fig1 b . ). in this way the encapsulation of the anchoring device for protection against corrosion can be combined in a particularly simple and economical manner with an indication of having exceeded the anchoring force which is clearly recognizable visually on the outside . while the invention has been illustrated and described as embodied in an anchoring device for a rod - shaped tension member of an anchor , it is not intended to be limited to the details shown , since various modifications and structural changes may be made without departing in any way from the spirit of the present invention . without further analysis , the foregoing will so fully reveal the gist of the present invention that others can , by applying current knowledge , readily adapt it for various applications without omitting features that , from the standpoint of prior art , fairly constitute essential characteristics of the generic or specific aspects of this invention .
4
fig1 shows an element 100 , which in this case is a tapered body sinker of heavy metal . the element could be a bobber , a weight holder ( a / k / a drop shot rig ) or an element unrelated to the fishing arts , such as a connector or flag on a line or filament . note that line or filament is meant in its most generic sense , such as from a micro - thin optical fiber to a large diameter steel cable . this invention is not limited to the type of line . the term filament is only used for convenience and is not a limitation . through the core of the element is a passage 102 with openings 104 and 106 at its ends . the passage is shown as linear / straight , but can be serpentine , spiral or other path , though straight is preferred . openings 104 / 106 can be circular , but the preferred structure is a non - round shape as it aids in its other function as a stop , as will be explained later . therefore , other shapes are shown in fig2 - 5 , such as round with ears ( points of engagement ) 108 , star shaped 106 c , hex or octagon 106 a and cross / star / phillips 106 b . many other shapes are acceptable and are incorporated herewith . such shapes have some element which would prevent the rotation of a stop element ( discussed below ). thus the importance of the shape selection is its ability to mate with the stop element and prevent counter - rotation . fig6 illustrates another feature of the invention . in addition to the passage 102 in the body 100 , a second cut into the body can be made from the outside . this access cut or slit 110 , permits the filament ( any kind of line ) to reach the passage 102 without the need to thread the filament through the passage end to end . this would require either cutting the line or having a free end to the line , something which is often impossible . instead , the access cut , whether straight ( not shown ) or other pattern , provides a way to slide the line into the passage without having a free end . thus the cut must be at least large enough to accommodate the filament ( directly or under compression ) and small enough that a portion of the stop element 114 can be inserted therein , preferably under compression or distention by stretching ( elongating ). the use of a serpentine cut 110 makes it more difficult for the line to slide free on its own without manual assistance . a notched cut ( having a jog offset portion ) 112 in fig1 is an alternative . it has a sharp right angle which accomplishes the same effect as the serpentine cut , but is even more reliable in preventing separation of the element ; however , it is much more difficult to insert the line therein . to make the invention have the slideable feature , a stop ( or stopper ) element 114 is inserted into the opening 102 and it is friction created by twisting of the stop element which locks the filament to the element 100 , such as a sinker or bobber , in the fishing arts . in this embodiment , the stop element is shown as a sleeve that separates the line 140 from the inner surface of the passageway 102 . stop element 114 , has an elongated body / twistable sleeve 116 , preferably made of an elastomeric material . the body is preferably sized to extend to and preferably beyond the length of passage 102 so that it extends beyond the opening 104 and 106 . at the end of the body are preferably anti - rotation elements ( ears ) 118 on either or both ends . these anti - rotation elements / features are shown with ears 120 which correspond to notches / recesses 108 in or associated with ( i . e . in some way mechanically linked with ) element 100 in fig2 . it can be appreciated , that when the ears and notches mate , the body is secured against rotation on both ends . it is possible to create this securing feature with other shapes as shown both in fig2 - 5 and 8 - 10 ( oval , rectangular , hex or non circular cross section , etc ), so long as an interlocking engagement is achieved to prevent relative rotation . entirely different anti - rotation elements or means are contemplated within the scope of this term . it is only required that the counter rotation be prevented when the element is twisted to the desired degree . fig1 illustrates the concept of how the stop 114 engages the filament 130 ( shown in broken lines as it passes through the element 100 and passage 102 ). the stop is first inserted into the element 100 in one of two ways . either by forcing it through one opening 104 / 106 to the other , or by forcing it through the cut 110 ( not shown in fig1 ). it may be preferable to stretch the stop lengthwise to make it thinner for purposes of getting into the cut 110 since it will generally be preferred to make it wider than the cut , so that it cannot fall out . with the stop in place , and the filament threaded therethrough , it is now possible to lock the element ( such as a bobber , sinker or some other element ) to the line / filament . in the preferred embodiment , the user twists either ( bulbous ) end 122 of the stop 114 . the shape of the end 122 should be large enough so as not to be drawn into the passage 104 . it may help to pull end 122 upwardly away from the element 100 for ease of twisting . this will cause the body 116 to engage the filament 130 and prevent it from slipping . this twisting is schematically suggested by line 140 in fig1 ( 140 is not a serpentine cut ). it is possible that the stop could become untwisted ; thereby allowing the filament to be released , but the addition of engagement elements will prevent this . the preferred engagement element are the anti - rotation elements 118 which engage recesses 108 ( fig2 ) but as shown in fig2 - 5 and 8 - 10 , there are a multiplicity of ways to prevent counter rotation of the twisted body 116 . fundamentally , it is necessary to engage both ends of the stop element with the main element 100 to prevent counter rotation . shaping the elements 118 to mate with like recesses 108 ( of any shape ) will accomplish this . note that it would be possible to fix one end 122 and twist the other . fixing could be accomplished by gluing or swedging ( or like means for fixing ) the end against counter - rotation . it would be possible to eliminate one of the bulbus ends 122 by gluing or otherwise fixing the body 116 to the element 100 near one end ( it must be however free to twist at least a portion of the body to insure engagement with the line ). fig1 shows a cut 112 in element 100 which is not serpentine but has at least one shoulder ( though it may be curved and not at right angles as shown ) to prevent the stop body from sliding out of the element 100 . fig1 illustrates another advantage of the present invention . in this configuration the element 100 has a stop and the ends of the stop 130 are shown . the line 130 has a knot 150 ( or other fixed stop on the line ) and when the stop 114 is in its released / relaxed position , the element is free to slide along the line 130 . this might be a common occurrence in any use of this device . a common problem with heavy objects which are slideable is that they encounter fixed stops and with the stop the impact can damage the line . in the case known , the impact of a heavy sinker could snap the line or gradually weaken it . thus it would be desireable to prevent hard impacts . the ends 122 of the stop element provide the additional advantage that they cushion the impact of a slideable object against the shock of a fixed stop on the line . it is appreciated that this shock absorbing / protecting feature can be provided to any slideable element without the need for the stop / locking engagement feature of twisting the body 114 around the line 130 . in such case , the anti - rotation features of this device are not required . rather , only an elastomeric or other cushioning material extending from at least one end of the slideable element 100 . it will be appreciated that this detailed description of the invention and preferred embodiments is not all encompassing . to cover every possible variation would make this text impossibly long . instead , the inventive concepts and some preferred embodiments were explained in detail but deviation from the preferred embodiments to other structures within the scope of the inventive concepts is to be considered part of this invention .
0
the system of the present invention comprises two main components : an illuminator , and a level display . these two main components interact with a conventional water level gauge 22 as can be seen in fig1 a . a conventional water level gauge 22 is made up of a series of ports 3 , arranged vertically along a column 2 , each comprising an opening 4 protected by glass , though which light may pass . when installed on a water boiler , or similar device , water or steam or a combination of the two will pass from the boiler , through the pipe 1 , and into the column 2 . an operator , who wishes to inspect the column 2 may peer through the series of ports 3 , and determine the level of water within the gauge , and correspondingly , the boiler . as can be seen in fig2 a , 2 b , and 2 c , an illuminator 14 and level display 23 interact with a level gauge 22 by an interface that is formed between hooks 18 on the outer housings of the illuminator and the level display and a bolt 17 on the column 2 of the level gauge . referring to fig3 a - 3 e , the illuminator may comprise an electronic printed circuit board ( pcb ) 10 containing an array of red and green light emitting diodes ( leds ) 19 , an array of piano - convex lenses 13 , equal in number to the number of leds 19 , and an external housing 20 , made up of a first portion 8 and a second portion 9 , adapted for attachment to a conventional water level gauge . the light emitting diodes may be configured in a paired linear array mounted along the longitudinal axis of the electronic pcb as shown in fig3 a , with one first color and one second color light emitting diode in each pair being mounted adjacent to each other along the lateral axis of the electronic pcb 10 . further , the first and second color light emitting diodes are preferably configured with at least two lights emitting diodes of the first color in parallel for independent operation , and at least two light emitting diodes of the second color in parallel for independent operation . the pcb 10 utilizes precision resistors to regulate the current supplied to each led 19 . the pcb further utilizes a terminal block corresponding to each led 19 that provides a connection point for the input power and allows for jumpering between individual pcbs 10 . the pcb 10 is mounted on an electronics divider 11 which is , in turn , attached to the first portion 8 and second portion 9 of the external housing 20 . a lens divider board 12 is positioned adjacent to the array of leds 19 , and is attached to the first and second portions 8 , 9 of the outer housing . this lens divider board 12 , has a number of plano - convex lenses 13 , equal to the number of leds 19 present on the pcb 10 . these lenses 13 focus light through an equal number of holes 21 in a heat divider 26 mounted on the first portion 8 of the external housing 20 so as to provide light to be passed through a level gauge . the first and second portions 8 , 9 of the illuminator housing 20 further include an array of offset slots 24 extending substantially completely from top to bottom . these slots 24 are designed and offset to limit the transmission of heat originating in the level gauge . the typical operating environment of a level gauge for a steam boiler is very high , typically in the range of 696 degrees f . ( 369 degrees celsius ). by introducing these slots to the design , heat transmission by conduction from the level gauge to the pcb board assembly and the leds is reduced , and the leds are isolated from these high operating temperatures . referring now to fig4 a , 4 b , and 4 c , the level display 23 may comprise a viewing screen 15 for viewing the light transmitted from the leds , having passed through a conventional water level gauge , an adjustable end plate 5 for blocking the unused red and green images , and a first portion 16 and second portion 7 of an external housing adapted for attachment to a conventional water level gauge . an adjustable end plate 5 provides openings 6 at the levels of concern and blocks the display of unwanted red and green light . the adjustable end plate 5 ensures that the operator can clearly distinguish between the levels and reduces error . referring now to fig5 and 6 , a second heat divider 25 is provided for reducing the transmission of heat from the level gauge 22 to the view screen 15 . additionally , an array of offset slots 24 extends substantially completely from top to bottom of the level display 23 . these slots 24 are designed and offset to limit the transmission of excess heat originating in the level gauge 22 , which may impair the functionality of the display . the bi - color water level gauge and illuminator device taught herein generally provides an improved means for determining the water level in a boiler steam drum , heater , or similar water / steam device .
6
fig1 shows the major components of the fill bonding apparatus . two different sheet types , type a and type b , are loaded onto feeder trays 1 and 2 , respectively . gantry 3 moves horizontally to pick and place sheets type a and b , alternately , on the fill stack 4 . vacuum chucks 5 and 6 remove the sheets from the stacks 1 and 2 . arrays of thermal bonding tips 7 weld the sheets together when they are placed on the fill stack 4 . fig2 illustrates the main parts of the thermal bonding device . hemispherical tip 10 extends through insulator and holding bushing 20 . heater block 30 provides heat to the tip 10 . air passage 40 extends through heater block 30 and rod 50 to provide a conduit for pressurized air to the tip 10 . rod 50 extends vertically through slide bushing 60 to allow vertical movement of the heater block , tip , and rod . spring 70 provides vertical force resistance to movement of tip 10 . collar 80 is fixed to tip 10 and provides a positive vertical stop to the motion of the tip . heat sensing device 90 provides feedback to control the temperature of the tip 10 . fig3 illustrates an isometric view of the thermal bonding apparatus . fig4 a is an elevation view of the fill bonding apparatus illustrating the starting position in the sequence of operation with parts labeled as in fig1 . fig4 b illustrates simultaneously raising the stacking tray 4 and the sheet type a feeder tray 1 . sheet type a is loaded into the gantry 3 and held in place by the vacuum chuck 5 . fig4 c illustrates simultaneously lowering the sheet type a feeder tray 1 and stacking tray 4 while sheet type a is in the loaded position . fig4 d illustrates moving the gantry 3 to the sheet type b loading position and sheet type a stack placing position . fig4 e illustrates simultaneously raising the stacking tray 4 and sheet type b feeder tray 2 . sheet type b is loaded into the gantry 3 and held in place by the vacuum chuck 5 . sheet type a is released by the vacuum chuck and placed on the stacking tray 4 . fig4 f illustrates simultaneously lowering the sheet type b feeder tray 2 and stacking tray 4 while sheet type b is in the loaded position . fig4 g illustrates moving the gantry 3 to the sheet type a bonding position and sheet type b stack placing position fig4 h illustrates simultaneously raising the stacking tray 4 and sheet type a feeder tray 1 . sheet type a is loaded into the gantry 3 and held in place by the vacuum chuck 5 . sheet type a and sheet type b are bonded together on the stacking tray 4 . this is the same position shown in fig4 b except bonding is being performed . fig4 i illustrates returning the sheet type a feeder and stacking tray to the start position as illustrated in fig4 c which shows the gantry 3 loaded with sheet type a . fig5 a illustrates the bonding tip just contacting the fill stack as the fill stack moves up . the bond tip heated . this occurs in position 8 of the machine . fig5 b illustrates the bonding tip being pushed up as the fill stack continues to move up . this compresses the spring and puts downward pressure on the bonding tip fig5 c illustrates the heated bonding tip extending down into the fill stack bond point as the sheets are heated . the spring decompresses partially during this step as the tip “ melts ” down into the bond site , still keeping pressure on the bond . the holding bushing 20 prevents the bonding tip from pushing too far into the fill stack . fig5 d illustrates the end of the bond heating cycle . at this point , the bond is melted together . as the fill stack is lowered , a burst of air is injected through the tip which pushes the sheets together and improves the bond strength . this air burst also helps eject the tip from the bond site without sticking a “ bubbled - out ” joint can also be provided to enhance the bond , in which the melted bond site is blown into a partial bubble shape as air is injected . the bubble is a larger on the bottom of the joint , which keeps it from pulling out . some instantaneous cooling may also occur , solidifying the joint . fig5 e is the last step and corresponds to position 1 of the machine cycle . the tip has been completely removed from the bond site , and the site is allowed to cool .
1
referring to fig1 , 2 and 3 , embodiments of a system , method and apparatus of strain - assisted recording for controlling reversal mechanism and tightening switching field distribution in bit patterned media are disclosed . fig1 depicts schematic side views of patterned media stacks , that may be used for bit patterned strain - assisted recording , under no excitation ( fig1 a ) and under excitation ( fig1 b ), i . e ., as the sil lattice 11 is at rest or distorted respectively . fig1 is a representative of a strain - induced rotation of the ml anisotropy . in one embodiment , the simplest structure of the multilayer used as media for bit patterned media in the invention may comprise a seed layer 13 , a buffer layer 15 , the magnetic media layer ( ml ) 17 , the strain - inducing layer ( sil ) 11 , and a cap layer 19 . the ml may be a multilayer or alloy , amorphous , crystalline or polycrystalline , with an out - of - plane , in - plane , or another direction of magnetic anisotropy with respect to the film plane . magnetic or non - magnetic film materials may be deposited on an object as , e . g ., either a large substrate ( disk ) or on some dot already formed on the disk . in either case , the top of the object is supposed to be flat . this flat top surface defines the direction of growth of the magnetic or non - magnetic film ( perpendicular to the flat top surface ). the “ plane ” of deposited layers ( films ) is therefore parallel to the flat top surface . the “ film plane ” indicates the two - dimensional direction of the substrate surface in space . it can contain transition metals ( e . g ., co , fe , ni ) and / or 5d metals ( e . g ., pt , pd ) and / or rare earth metals ( e . g ., tb , dy , sm ) and / or segregant ( e . g . b , cr , sio x , tao x ). the ml may be engineered as a combination of alloys and multilayers . the sil dimension variation can originate from different effects . in one case , the sil can be a magnetostrictive material ( e . g . smdyfe , tb 1 - x fe x , fe 3 pt , fe / pt , etc .) whose lattice is distorted when the writing field is applied . during a write cycle , the disk drive head applies a magnetic field on a given pre - patterned bit / dot . the magnetostrictive sil overcomes a lattice distortion and therefore induces a strain on the ml . the structural change applied to the ml generates a rotation or an amplitude variation of the ml total anisotropy . the sil may be engineered as a combination of alloys and multilayers , and the invention is compatible with having a soft underlayer ( sul ) below the patterned dots . the sul may be located below or included in the seed layer . in another case , the sil can be magnetic or nonmagnetic and overcome a large structural change at temperatures between 350 and 700 kelvin ( e . g . shape memory alloy , etc .). for certain non - magnetic or magnetic materials , the stable crystalline phase ( i . e ., the organization of the atoms inside the material ) is changing from one temperature to another . analogously , water is liquid for temperatures higher than 0 ° c . and solid for temperatures lower than 0 ° c . during a write cycle , the disk drive head initially heats up a given pre - patterned bit / dot to a transition temperature . the sil changes its structure thus inducing a strain on the ml . the structural change applied to the ml generates a rotation or an amplitude variation of the ml anisotropy . again , the sil may be engineered as a combination of alloys and multilayers , and the invention is compatible with having an sul below the patterned dots . in another case , the transition layer can be a piezoelectric layer ( magnetic or non - magnetic ) whose lattice parameters change with an applied voltage . see , e . g ., h . boukari , et al ., j . appl . phys . 101 , 054903 ( 2007 ); and j . w . lee , et al ., appl . phys . lett . 82 , 2458 ( 2003 ). during a write cycle , the disk drive head induces a difference of electrical potential between the disk and the head , strong enough to polarize the piezoelectric sil of a given pre - patterned bit / dot . the electrical polarization induces a sil structure distortion thus inducing a strain on the ml . the structural change applied to the ml generates a rotation or an amplitude variation of the ml anisotropy . the sil may be engineered as a combination of alloys and multilayers , and the invention is compatible with having an sul below the patterned dots . the variation direction or amplitude of the ml anisotropy due to transferred stress from the sil can be calculated as following . at rest , the direction of the ml magnetization orientation is ruled , within the stoner - wohlfarth assumptions , by the intrinsic magnetocrystalline anisotropies . in the case of a ml for bit patterned recording , the ml may be tuned to have a uniaxial anisotropy . the energy related to this uniaxial magnetocrystalline anisotropy is e 1 = k 1 sin 2 θ where k is the magnetocrystalline anisotropy constant , i . e . the anisotropy amplitude , and θ the angle between the magnetization and the magnetocrystalline anisotropy direction . the transferred strain from the sil to the ml generates an additional magnetic uniaxial anisotropy inside the ml . the energy related to the strain - induced anisotropy is e 2 = k 2 sin 2 ( α − θ ) where α is the angle between the magnetocrystalline anisotropy and the strain - induced anisotropy directions . as an example , in the case of a linear strain , k 2 is the strain induced anisotropy amplitude and would be calculated as gλσ where g is numerical constant depending on the lattice distortion , λ the ml magnetostriction coefficient and σ the strain amplitude . fig2 shows the magnetocrystalline anisotropy and the strain - induced anisotropy inside the ml as well as the magnetic field 21 at an angle β from the magnetization direction 23 . the most energetically stable position of the magnetization at remanence as a function of k 1 , k 2 and α can be calculated as the θ value which minimizes the anisotropy energy e tot = e 1 + e 2 . various cases have to be differentiated . in the case where α = 0 deg , the total anisotropy energy is e tot =( k 1 + k 2 ) sin 2 θ . therefore , the strain does not affect the overall anisotropy direction but the amplitude of the anisotropy along the magnetocrystalline anisotropy direction . as a function of the sign of the magnetostriction constant λ and the sign of the strain σ ( i . e . elongation or compression of the ml lattice ), the anisotropy amplitude can be increased or decreased due to the strain compared with k 1 . in the case where α = 90 deg , the total anisotropy energy is e tot = k 1 sin 2 θ + k 2 sin 2 ( 90 − θ ). therefore if k 1 = k 2 , the total anisotropy energy , e tot = 2k 1 = 2k 2 , does not depend on the magnetization orientation . in that case , the strain induces the suppression of the ml magnetocrystalline anisotropy . if k 1 ≠ k 2 , the anisotropy energy has two minima corresponding to the case where the magnetization is along the ml magnetocrystalline anisotropy axis and the case where the magnetization is along the strain - induced anisotropy axis . in the case where a α ≠ 0 deg and α ≠ 90 deg , the total anisotropy energy is e tot = k 1 sin 2 + k 2 sin 2 ( α − θ ). then , the most energetically stable magnetization position is given by θ min = tan − 1 [( k 1 sin 2α )/( k 2 + k 1 sin 2α )] fig3 is a diagram of θ min as a function of α , for different values of k 2 . applied to bit patterned media , the strain - induced rotation or amplitude decrease of the ml anisotropy has three main effects . the first one is to decrease the switching field during the writing . indeed , within the stoner - wohlfart model , the switching field can be reduced by 50 % when the angle β between magnetization and magnetic field direction is reduced from 0 deg to 45 deg . see , e . g ., j . p . wang , nature , mater . 4 , 191 ( 2005 ); and m . yamada and s . nakagawa , ieee trans . mag . 43 , 2346 ( 2007 ). the second effect is to decrease the switching field distribution , i . e ., the dot - dot variation of switching field . indeed , in the case of a strain - assisted writing process , the switching field value is no longer defined by the intrinsic properties of the ml . as an example , a strain - assisted rotation of the ml anisotropy , i . e . of the ml magnetization , from β = 180 deg to 135 deg relative to the field direction decreases the switching field distribution originating from the intrinsic distribution of anisotropy direction in the ml ( see fig2 ). indeed , within the stoner - wohlfarth assumptions , the evolution of switching field due to a δβ variation for β = 135 deg is very small compared with the switching field variation due to the same δβ around β180 deg . the third effect is to increase the addressability of single bits during the write process . using the activation of the sil in combination with a write field pulse increases the selectivity for the bit that has to be written , since both sil activation and magnetic field directly acting on the ml are to first order independent processes . therefore their distributions add independently , thus yielding a narrower total switching field distribution . in still other embodiments , depending on how fast the strain can be released from the dot , strain - assisted recording can be used to increase the write process speed . in a sub - ns range , as the strain is transferred from the sil to the ml , the ml magnetization is not instantaneously re - oriented or relaxed along the new anisotropy axis direction , but starts processing around the new anisotropy axis . this effect is described by the landau - lifshitz - gilbert ( llg ) equation . the magnetization precession can be large enough to bring the magnetization further than 90 deg away from its remanent position . if the strain is removed at the time where the magnetization is further than 90 deg away from its remanent position , the magnetization is forced onto a new trajectory towards the remanent anisotropy direction at 180 degrees from its original orientation . therefore , depending on how fast the strain can be released from the dot , the magnetization switching can be operated using only one magnetization precession around the strain - induced anisotropy axis , i . e ., on a sub - nanosecond scale . in still other embodiments , if the excitation pulse and anisotropy change is controlled well enough ( primarily with respect to timing ), and if the bit is read before being written , a magnetic field may not be necessary to switch the magnetization and it could solely be controlled via the sil and the correct timing of switching it on and off ( of activating and de - activating it ). other examples of the invention may include a system for strain - assisted recording for controlling reversal mechanism and tightening switching field distribution in bit patterned media , comprising : a seed layer ; a buffer layer on the seed layer ; a strain - inducing layer ( sil ) on the buffer layer ; a magnetic media layer ( ml ) on the sil ; a cap layer on the ml ; and the sil induces a strain on the ml , such that a structural change applied to the ml generates a rotation or an amplitude variation of the total anisotropy of the ml . the ml may comprise at least one of a multilayer , alloy , amorphous , crystalline and polycrystalline material , and the sil is above the ml . the ml also may comprise a uniaxial anisotropy that is one of out - of - plane , in - plane or any other direction with respect to a film plane , and the ml is sandwiched between a pair of sil layers . alternatively , the ml may comprise at least one transition metal selected from the group consisting of co , fe and ni , and / or at least one 5d metal selected from the group consisting of pt and pd , and / or at least one rare earth metal selected from the group consisting of tb , dy and sm , and / or at least one segregant selected from the group consisting of b , cr , sio x and tao x . the ml may further comprise a combination of alloys and multilayers . in some embodiments , the sil is a magnetostrictive material selected from the group consisting of : smdyfe , tb1 − xfex , fe3pt and fe / pt , whose lattice is distorted when a write field is applied . in another alternative , the sil is magnetic or nonmagnetic , and is characterized by a large structural change at temperatures between 350 and 700 kelvin . in addition , the sil may have a piezoelectric layer whose lattice parameters change with an applied voltage , and / or the sil may comprise one of an alloy or a multilayer , and combines the properties of magnetostriction , large structural change at temperatures between 350 and 700 kelvin , and a piezoelectricity . while the invention has been shown or described in only some of its forms , it should be apparent to those skilled in the art that it is not so limited , but is susceptible to various changes without departing from the scope of the invention .
1
referring first to fig1 and 2 , wherein are best shown the general features of the invention , the methane generator , indicated generally by the reference numeral 10 , is shown as including an open - topped tank 11 enclosed with an insulating jacket 33 . the tank is of fairly heavy construction and may be made of cement , metal or fiberglass - reinforced plastic . a gas collector 12 is vertically and rotatably slidable in the tank and is preferably made of relatively light - weight and leak - proof construction , so that it can float and move upwardly under gas pressure . a feed means 13 is provided centrally of the collector for introducing raw slurry through the collector deep into the tank . a conduit means 15 extends from the upper portion of the collector for removing methane from the gas collector , there being a double acting solenoid valve 20 to regulate the flow of product gas . solenoid valve 20 has two cores . energization of a first core shifts the valve to the closed position and energization of a second core shifts the valve to the open position . referring also to fig4 valve 20 is controlled by an upper level switch s1 and a lower level switch s2 . when upper level switch s1 is closed the second core is energized and the valve is shifted to the open position . when lower level switch s2 is closed , the first core is energized and valve 20 is shifted to the closed position . a dash - shaped retainer 16 is located in the upper portion of the tank and is provided with apertures 17 . a plurality of rods 18 extend downwardly from the collector and pass through the slots 17 in the retainer into a body 14 of slurry located in the tank . the slurry contains coarse solids which are held submerged in the slurry by the retainer 16 as shown in fig4 . solenoid valve 20 remains in the closed or open condition until one of the cores is energized to change its condition . the cores which control the opening and closing of the valve 20 are energized to perform their respective functions by the momentary closing of switches s1 and s2 . referring now to fig1 and 2 , it can be seen that the gas collector 12 is free to rotate ( as well as slide vertically ) in the interior of the tank 11 and that the apertures 17 in the retainer 16 are concentric slots . the tank 11 is provided with a sidewall 19 in the form of a circular tube whose inner surface is a circular cylinder . the collector 12 has an outer surface 21 that slides smoothly in the circular cylindrical surface of the tank . the retainer 16 rests on an annular ledge 22 which is fixed to the inner surface of the tank . the retainer is like a sewer cover and has sufficient weight , so that it is not easily moved from its position of rest on the ledge 22 by the coarse material beneath it . an overflow pipe 23 is located on the tank a substantial distance above the retainer 16 to regulate the slurry level 11 between the tank and jacket 33 to maintain the slurry at a predetermined temperature for digestion of slurry and solids . the feed means 13 that is provided for introducing raw coarse organic feed material into the tank consists of a feed tube 25 extending vertically downwardly from the top wall of the gas collector . the tube has a conical entrance portion 26 and the slurry or solid organic matter is introduced under pressure by a concentric feed screw 27 . the feed tube 25 extends through a central circular aperture 28 formed in the retainer 16 . the operation of the invention will now be readily understood in view of the above discussion . the raw stock is introduced into the apparatus by the rotation of the feed screw 27 in the tube 25 with its conical entrance 26 . raw organic matter or stock may be in the form of animal manure , industrial , agricultural , and domestic waste , garbage , and even normal trash which has been nominally masticated or chopped . water or liquid waste is added directly to the generator or added to the stock to give a thick slurry which is introduced into the generator . when the feed rate is regulated properly , a certain amount of spent slurry will pass outwardly through the overflow pipe 23 in direct proportion to the amount introduced . as methane gas is generated in the body 14 of slurry , the gas flows upwardly through the portions of the slots 17 in the retainer 16 that are not occupied by the rods 18 and accumulates in the collector 12 . eventually , this will cause the collector to move upwardly so that a finger 34 at the top of the collector 12 closes upper level switch s1 which causes the solenoid valve 20 to open and release the accumulated methane gas through the conduit 15 to a storage container or for immediate use as fuel in burning and like processes in home , farm or business . any excess can , of course , be sold . some of the gas necessarily must be used in producing the hot water for heater 30 used for heating the generator with the heat - exchanger 24 . as the gas is released from the collector 12 , the collector moves downwardly until finger 34 closes lower level switch s2 which energizes the first core and causes the solenoid valve 20 to close . solenoid valve 20 remains in the closed condition until the collector 12 again rises to the level where switch s1 closes to shift the solenoid valve 20 to the open condition . the collector 12 moves up and down as gas that is generated in the generator is accumulated in the collector and released from the collector . this causes the rods 18 to move up and down through the slots 17 and serve to open up the coarse solids submerged in the slurry , so that the suspended solids cannot form a hard mat on the upper surface of the slurry and prevent the release of gas . in addition to providing the vertical motion of the rods 18 , the collector is capable of rotating to and fro and , since the conduit 15 is flexible , this rotation causes the rods to further break up the solids submerged in the body 14 of slurry and held down by the retainer . the retainer holds down the solids immersed within the slurry and thereby facilitates the process of bioconversion . fig3 shows an arrangement in which three methane generators 11 , 29 , and 31 are enclosed in an insulated housing 32 and used to carry on the operation . in this case , the rate of feed of slurry brought about by the screw 27 is selected in an amount such that complete conversion to methane does not take place in only one generator , so that it is necessary to use a battery of generators . this results in an increase of generator capacity by adding generators as required . the rate of feed and operation is selected such that the spent effluent can be dried or directly used as fertilizer . properly operated , the spent slurry is odorless or has a mild marshy odor . based on the performance of a 20 gallon methane generator constructed in accordance with the basic principles of the present invention , it is possible to evaluate the feasibility of a small methane generator on a farm having one or two cows . the basic generator is generally similar to the construction shown in fig3 and consists of three 300 - gallon fiberglass tanks , each of which were 36 inches in diameter and 7 feet tall . they are provided with 30 - inch high floating gas collectors and nearly 3600 cubic feet of the gas was stored in inflatable vinyl bags protected by fencing . normally , 120 lbs . of manure are diluted with 40 lbs . of water to 160 lbs . ( that is to say , 12 % solids ) and the thick slurry is fed into the generator . the generator tanks are interconnected and the spent slurry left the third tank after nearly 45 days of retention time . this arrangement will produce 120 cubic feet of biogas per day . the loading rate could increase to almost 320 lbs . per day with 20 days retention time to obtain 240 cubic feet of gas daily . the three tanks are clustered together , wrapped with 180 feet of 1 / 2 inch diameter soft copper tubing , and provided with a heavily insulated enclosure . hot water is circulated through the copper tubing to maintain 104 ° f . ( 40 ° c .) throughout the year . it can be seen that the entire system is passive and requires little attention or repair . for proper operation of the unit , one must assume the following conditions : 1 . the installation is on a farm or a municipal waste dump area where there are no legal or social restrictions . 2 . all possible effort is made to minimize heat loss from the generators , so that it does not take more than 10 % of the gas produced per day to maintain the 104 ° f . temperature . 3 . the labor for the installation of the tank and the fabrication and installation of the gas collectors and the necessary alterations to accommodate the system are provided by the owner without charge . it is felt , therefore , that , if it is necessary to provide professional installation , spent slurry in the amount of about 2 tons can be sold as fertilizer for about $ 75 / ton in exchange for such labor . 4 . the evaluation assumes that fuel costs continue to rise at about 10 % per year . 6 . the services of a competent and enthusiastic consultant are available . it should be kept in mind that the coarse material is retained under the retainer 16 . the advantage of this is that it ( a ) need not be commuted to make a fine slurry , and ( b ) it is retained at the favorable micro - organism level or environment . it is always submerged in the active environment ( bathed from all sides by liquid ). the solids that are fed through the screw feed 27 into the depth of slurry in tank 11 float up but kept submerged in the slurry under the retainer 16 . these are acted upon by microbes and gas is released . the vertical and rotative action of the floating gas collector 12 and its rods give free mechanical action to keep the dense mass open for gas to escape . that is to say , no external energy need be provided for : ( a ) reducing the bulky solids into fine particles to be made into slurry , ( b ) keeping the particles in suspension by thorough and continuous agitation in the generator tank during microbiological bioconversion action on them , and ( c ) piercing open the mat that forms under the retainer in the slurry . all of these functions are accomplished by harnessing the mechanical advantages of natural forces of buoyancy , gas pressure , relative densities , gravitational flow , etc . the leakage of finer solids upwardly through slots and apertures in the retainer are small and immaterial . the material costs come to about $ 2 , 000 and , when this money is obtained in the form of a loan , the savings will pay off this loan in around 6 years . after the loan is repaid , the generator will continue to produce gas valued at no less than $ 550 per year . in addition , such a methane generator operating on a small farm will go far in reestablishing the symbiosis between the human being and the environment by making use of the &# 34 ; waste &# 34 ; to provide energy and fertilizer through a natural process of recycling . it is obvious that minor changes may be made in the form , construction and applications of the invention without departing from the material spirit thereof . it is not , however , desired to confine the invention to the exact form herein shown and described , but it is desired to include all such as properly come within the scope claimed .
8
in fig1 the numeral 10 generally designates a twin rotor screw compressor having a male rotor 20 and a female rotor ( not illustrated ). the rotors are located in rotor housing 12 . outlet casing 14 is secured to the discharge side of rotor casing 12 and bearing casing 16 is secured on the other side of outlet casing 14 . rotor casing 12 , outlet casing 14 , and bearing casing 16 are suitably secured together as by bolts 18 . compressor 10 has a suction plenum s and a discharge plenum d . normally communication between the suction plenum s and discharge plenum d is through the pump structure defined by the rotors and associated structure . the structure described to this point is generally conventional . the present invention adds threaded bore 12 - 1 in rotor casing 12 to connect suction chamber s with discharge chamber d . valve assembly 40 is secured in bore 12 - 1 and normally prevents flow between suction chamber s and discharge chamber d via bore 12 - 1 . referring to fig2 valve assembly 40 is illustrated in its normally closed position . hex head member 42 is threaded into bore 12 - 1 in rotor casing 12 and coacts with o - ring 44 to provide a seal . member 42 has a bore 42 - 1 , a bore 42 - 2 , an annular recess 42 - 3 and a flange portion 42 - 4 . the valve body is made up of members 50 , 52 and 54 . member 50 has a threaded bore 50 - 1 , a plurality of circumferentially spaced slots 50 - 2 and an annular flange 50 - 3 . member 54 has a threaded bore section 54 - 1 , a smooth bore section 54 - 2 , a valve seat 54 - 3 , a valve port 54 - 5 , flange portion 54 - 6 and annular groove 54 - 7 in flange portion 54 - 6 . o - ring 60 is located in groove 54 - 7 and normally seals against flange 42 - 4 . because neither flange 50 - 3 nor flange 54 - 6 can pass through bore 42 - 2 , they must be located on opposite sides of member 42 for assembly . connection of members 50 and 54 is through annular connector 52 which has a threaded portion 52 - 1 which is threadedly receivable in threaded bores 50 - 1 and 54 - 1 and has a central bore 52 - 2 . there are various sequences for assembling members 50 , 52 and 54 together . valve disk 56 and spring 57 must be in bores 54 - 1 / 54 - 2 before member 52 is threaded into bore 54 - 1 . spring 58 must be in bore 42 - 1 / annular recess 42 - 3 prior to member 52 being threaded into both of threaded bores 50 - 1 and 54 - 1 . member 52 serves four functions : ( 1 ) it serves to connect members 50 and 54 ; ( 2 ) it serves as a spring seat for spring 57 ; ( 3 ) it adjusts the bias of spring 57 ; and ( 4 ) forms a portion of the relief flow path when valve disk 56 is unseated . in the fig2 position of valve member 40 , all of the valves are closed , member 54 extends into the discharge chamber d and valve disk 56 is exposed to discharge chamber pressure over the area of port 54 - 5 . the other side of valve disk 56 is exposed to suction chamber pressure and the bias of stiff spring 57 which may exert a biasing force equivalent to several hundred psi on valve disk 56 tending to keep it closed . light spring 58 has a biasing force on the order of one to six psi and is located between flange 50 - 3 and annular recess 42 - 3 . spring 58 in conjunction with the discharge pressure acting on member 54 and valve disk 56 tends to keep the integral valve body made up of members 50 , 52 and 54 in place and is opposed by the net suction pressure acting on members 50 , 54 and valve disk 56 . when there is a higher pressure in the suction chamber than in the discharge chamber , as during reverse operation , the pressure differential acting across the valve body made up of members 50 , 52 , 54 and valve disk 56 will cause the unseating of flange 54 - 6 from flange 42 - 4 under a nominal pressure differential of a few psi . fig3 illustrates the position of valve member 40 when it is opened responsive to reverse operation . the fluid path from the higher pressure suction chamber to the lower pressure discharge chamber will serially be bore 42 - 1 , bore 50 - 1 and slots 50 - 2 . when the pressure in the discharge chamber exceeds the desired discharge pressure , this pressure acting on valve disk 56 will cause valve disk 56 to unseat against the stiff bias of spring 57 and the suction pressure acting on the opposing side of valve disk 56 . fig4 illustrates valve disk 56 unseated responsive to excess discharge pressure . when valve disk 56 is unseated a fluid path between the discharge and suction chambers will be established serially including valve port 54 - 5 , bore 54 - 2 , grooves 56 - 1 in valve disk 56 , bore 54 - 1 bore 52 - 2 , bore 50 - 1 and slots 50 - 2 . although a preferred embodiment of the present invention has been illustrated and described , other changes will occur to those skilled in the art . it is therefore intended that the present invention is to be limited only by the scope of the appended claims .
5
with reference to fig1 there is shown the general operation of a gyroscopic flying cylinder body 10 in accordance with the present invention when thrown by a hand 16 as an aerial sports toy . the body 10 includes a hollow cylindrical body 12 with a leading end 34 and a trailing end 36 . a dense and weighted rim 14 is shown attached to the interior of the cylinder 12 at the leading end 34 . the body 10 is shown being manually held by a hand 16 just prior to launch . when the body 10 is thrown by the hand 16 , gripping fingers 18 work in cooperation with a wrist 20 to impart axial spin to the device in the direction illustrated by arrow 22 . at the same time , the hand 16 provides an initial forward velocity along spin axis 24 . it is anticipated that manual usage will include games of catch or competition events in which throwers aim for maximum flight times , distance or accuracy . the forward rim 14 is preferably made of spring steel that allows for resiliency when gripped by hand 16 . the rim may be formed into a ring by bending the spring steel in a circular fashion and fastening it by a weld adhesive , or by mechanical means . the rim 14 may be heavily coated with any number of plastic coatings to avoid exposure of sharp edges and provide of safety . the cylinder 12 of the body 10 can be constructed by adhering materials such as plastic , rubber , cloth or thin metal around the outside , the inside , or both the inside and outside of the rim 14 . the body 10 is designed for manufacturability . the rim 14 can be fashioned from either a steel strap , wire coil or spring by using traditional rolling , welding , coiling or spin - making equipment . the material which makes up the cylinder 12 can simply be wrapped around the rim 14 by hand or by utilizing machines . adhesion of the material to the rim 14 can be achieved by utilizing either glue or transfer tapes . the use of tape has the advantage of enabling the product to be sold in a disassembled kit form , if so desired . a rim with a section of transfer tape wrapped around the rim may be sold in ring form . a protective layer on the tape may then be removed , and a strip of stiff but rollable material is wrapped around the rim , and held by the adhesive . injection molding and extrusion manufacturing processes also can be readily utilized . referring to fig4 the product can alternatively be sold with the rim 114 lying flat incorporating a buckling mechanism at opposite ends 115a and 115b and transfer tape 117 affixed to one side . the body 100 also would be sold flat . the product could be assembled by the end - user as follows : a protective layer 118 of the transfer tape 117 is removed from the flat rim 114 exposing the adhesive . the flat rim is taped to the leading edge of the body 100 . the flat rim and body are then formed into a cylinder as seen in fig5 whereby the rim is fastened into a circle by coupling the ends 115 of the rim . the rim is positioned on the inside of the cylinder and the spring tension of the rim naturally holds it and the body 10 in a circular fashion . a seam is formed with tape 119 along the cylinder &# 39 ; s length when the body is fastened together . in a preferred embodiment of the present invention , the cylinder 12 has a diameter of about 3 . 75 inches , a length of about 2 . 125 inches , and a wall thickness of about 0 . 010 inches , while the front rim portion 14 has a wall thickness of about 0 . 040 inches . the aft portion of the ring that abuts the cylinder wall forms a negligible differential of about 0 . 030 inches . as noted above it is desirable that this aft portion be thin so as to minimize turbulence introduced by that discontinuity . preferably the thickness is less than about 0 . 4 % of the external surface area of the body 10 . the length of the rim 14 is 0 . 5 inches , which accounts for 23 . 5 % of the body &# 39 ; s 10 total length . a range of about 18 % to 32 % is satisfactory . the cylinder 12 and the rim 14 combination weighs approximately 26 grams . these dimensions provide optimal characteristics for a game of catch because of the following results : a straight and stable flight can be achieved for both long and short distances ; the cylinder fits comfortably within the grip of an average sized man ; the diameter of the cylinder is large enough to reduce the possibility of someone being inadvertently struck in the eye ; and the cylinder &# 39 ; s lightweight construction prevents serious harm if someone is accidentally struck . it will be recognized that body 10 can be launched by various known mechanical or powered mechanisms means which can aim and impart the initial velocity and spin conditions . such means may be carried aboard a spinning device or may be externally separate . included in these means are springs , catapults and other leverage mechanisms , explosive or burning propellant system , as well as normal powered devices running on electricity or various fuel systems . referring again to fig1 it has been found that when properly thrown , the device will initially follow a substantially linear flight path from the initial direction 24 . rapid spinning imparts gyroscopic effects which tend to stabilize the flight path against the gravitational forces acting to rotate the heavy gyroscopic rim 14 downward about a horizontal axis 32 . toward the end of the flight , when the spinning and forward velocity diminish , the device will process from right to left about a vertical axis 26 . the flight then will veer to the left along path 30 . the end of flight is characterized by the rim nosing down accompanied by gyroscopic coring motions . fig2 shows a side view of the body 10 with the weighted , dense and balanced rim 14 oriented with its x axis along the direction of launch arrow 24 . the rim portion 14 is comprised of a thin annular metal band attached to the leading edge of the internal wall of the cylinder 12 . the body &# 39 ; s center of gravity is shown at point 42 . fig3 shows the front view of the body 10 corresponding to the line 3 -- 3 of fig2 with y and z axes exposed . leading edge 44 is comprised of the rim 14 and the cylinder 12 has a thickness of less than about 0 . 1 inch . the performance of the body 10 is heavily dependent upon the weight of the rim 14 . the weight of the rim 14 is preferably between 75 % and 90 % of the total weight of the body 10 . experiments have been performed to obtain these results . comparative performance tests have been made which show the importance of appropriate up - front weighting to obtain significant gyroscopic effects and enhanced flight performance . plastic models were used having body lengths of 2 inches and diameters of 3 . 75 inches . various weighted metal rims with densities of 7 . 85 g / cm3 have been added to the forward region along the leading edge . table 1 below presents &# 34 ; normal thrown &# 34 ; averages of approximate flight ranges of devices with different rim weight percentages obtained under wind still conditions and an observation appraisal of flight characteristics . table 1______________________________________ % of rim weight to average normalthe total device throw ( yards ) flight characteristics______________________________________51 % 15 yds very wobbly spin , poor lift , does not soar , no precession . 64 % 20 yds wobbly spin , poor lift , does not soar , no precession . 73 % 50 yds rough spin , exhibits lift and soars somewhat , some precession . 81 % 65 yds smooth spin , exhibits good lift and soars well , precession . 86 % 65 yds very smooth spin , exhibits good lift and soars well , much precession . 90 % 40 yds noses down , much precession . ______________________________________ to summarize , the table shows that performance unexpectedly and dramatically increases , as weighting increases to the range of 75 % to 90 % and then dramatically falls off above 90 %. not only is rim weight important to performance , but density of the rim in proportion to overall body weight is also a key factor . to demonstrate this point , comparative performance tests have been made , which show the importance of rim density to obtain significant gyroscopic spinning and enhanced flight performance . as with the previously described tests , plastic models were used , each having a body length of 2 inches and a diameter of 3 . 75 inches . in this case , the weights of the rims were held constant at 17 grams , but the materials used had different densities . the overall weight was kept the same as indicated above , 26 grams . while this is a desirable weight for long distance throws , different weights can be employed so long as the other parameters are met , such as the rim weight and location , and rim density . the table below presents &# 34 ; normal throw &# 34 ; averages of approximate flight ranges of devices with different rim densities obtained under wind - still conditions and observation appraisals of flight characteristics . table 2______________________________________ density to average normal flightmaterial total weight throw ( yards ) characteristics______________________________________polycarbonate 1 to 21 . 6 25 yds wobby spin , poor lift , unstable flight . aluminum 1 to 9 . 6 35 yds rough spin , some lift , unstable flight . tin 1 to 4 . 5 56 yds smoother spin , exhibits lift , more stable . steel 1 to 3 . 3 65 yds smooth spin , lifts very well , very stable flight . lead 1 to 2 . 3 74 yds smooth spin , very strong lift , very stable flight . ______________________________________ it should be noted that this gyroscopic data confirms the expectation of improved distances and flight characteristics with increased forward rim weight distributions and density to weight make - up . as can be seen , rims of polycarbonate , which has a density of 1 . 2 grams per cm 3 , or aluminum , having a density of 2 . 7 grams per cm 3 , gave unsatisfactory performance . by contrast , tin , 5 . 75 g / cm 3 ; steel , 7 . 84 gm / cm 3 ; and lead 11 . 34 gm / cm 3 gave good results . further experimentation has shown that a density to total weight ratio of less than about 1 to 8 is satisfactory . weight distributions of the present invention are determined without regard to aerodynamic modifications concerning the shape of the cylinder &# 39 ; s wall . in contrast , prior art weight distributions are cited in conjunction with a variety of specific aerodynamic shape modifications . nevertheless , weight distributions of previous designs are well below the criteria of having the rim account of 75 % of the total weight , as indicated above . furthermore , there is nothing in the prior art which reveals the importance of having high density material for making the rim . as indicated earlier , proper body trim factors must accompany the gyroscopic rim parameters to obtain the exceptional flight performance of the present invention . therefore , previous designs cannot achieve sufficient gyroscopic stabilization to reach the greater ranges or smoother flight characteristics exhibited by the present invention . the superior design of the present invention over the prior art is dramatically evidenced in drastic performance improvement . maximum ranges for &# 34 ; hard throws &# 34 ; of the present invention by a typical man can exceed 150 yards . by comparison , tests show that &# 34 ; hard throws &# 34 ; of hills &# 39 ; actual device ( which hill claimed a considerable improvement overall previous patents ) have rough flights and do not exceed 35 yards . also , hard throws of mcmahon &# 39 ; s device show rough flights and do not exceed 30 yards . although the present invention has been described in considerable detail with reference to certain preferred cylindrical aerial toy versions thereof , other versions and applications are possible . the present invention can be utilized in the defense industry as a bullet , projectile , mortar , target practice device , self - propelled aircraft , etc . also , it may be used in the medium of water as a torpedo or submarine . furthermore , various hollow body shapes and known aerodynamic modifications may also be spun and flown . therefore , the spirit and scope of the appended claims should not necessarily be limited to the description of the preferred version sand applications contained herein .
0
fig1 schematically illustrates a model seismic survey matrix according to the invention wherein geophones are distributed over the terrain of interest in an orderly manner of period and spacing . for this example , the geophones are aligned in four rows , t 1 , t 2 , t 3 and t 4 . row t 3 is extended discontinuously across a physical obstacle such as a river or highway . distributed along each of the geophone rows are three ( for example ) rams , 10 . construction of a ram 10 will be described more fully with respect to fig5 , 6 and 7 . the rams are connected by two receiver line cables 12 respective to an “ a ” side and a “ b ” side of each ram . see fig5 . as shown in cross - section by fig3 , a receiver line cable 12 comprises four pairs of geophone channel conduits 32 and two pairs of communication conduits 30 and 31 , surrounding a stress carrying core element 28 . the six pairs of receiver line conduit are aligned within an insulation annulus 24 and encased by a shield jacket 26 . the receiver line cable is terminated at both ends with a universal cable connector 39 . this cable connector allows connection of the receiver line cable to any ram 10 , ltu 14 , blu 38 or to the cru 18 as shown in fig1 . the connector pins include one pair 135 for communication conduit 30 , a second pair 136 for communication conduit 31 , four pairs 137 for geophone channel conduits , and two unused pairs 138 . the unused pairs are retained to allow use of a universal cable connector 39 for all types of cable in the system , including receiver line cable , base line cable and jumper cable types . referring to fig1 , the two receiver line cable sections respective to rams r - 1 / ram 1 and r - 1 / ram 2 in row t 1 are mutually joined by a back - to - back connection 36 . the same is true for the receiver line cables between r - 2 / ram 2 and r - 2 / ram 3 in row t 2 . row t 4 includes two back - to - back connectors 36 . the back - to - back connectors 36 provide continuity between communication conduits 30 and 31 of connected receiver line cables 12 but not for the geophone channel conduits 32 . each of the four geophone channel conduits 32 in a single cable section respectively connects to only one ram . hence , each ram receives up to eight geophone channels in this preferred embodiment example . it is common industry practice for each geophone channel 32 to be connected with a plurality of geophones . each of the geophones respective to a given channel 32 has a predetermined position relative to the seismic disturbance location whereby those commonly connected geophones all receive substantially the same subsurface reflection signal thereby ( through summation ) reinforcing the signal strength but receive substantially different seismic noise , thereby attenuating noise when summed . usually , not always , the geophone signals through the channels 32 are analog : analog - to - digital conversion being performed by the ram as will subsequently be described more fully . however , a / d conversion by dedicated circuitry in individual geophone units is possible and is advantageous under certain circumstances . again referring to fig1 , ltus 14 1 , 14 2 and 14 3 join the rows t 1 , t 2 and t 3 to a base line cable 16 . the ltus will be described more fully with respect to fig9 . the base line cable 16 shown in cross - section by fig4 comprises eight communication conduit pairs 34 1 - 8 within an insulation annulus 24 and shield jacket 26 . at the core of the assembly may be a stress carrying core 28 . a universal cable connector 39 terminates both ends of a section of base line cable , allowing connection to any module in the system . connector pins 147 for communication conduits 34 are shown . the universal connector 39 is physically identical to the connector used in the receiver line and jumper cable types allowing full inter - connectability of all equipment in the system . shown in fig1 is a section of base line cable 16 joining ltus 14 4 and 14 5 . the use of base line cable 16 instead of receiver line cable 12 to connect rams that are on the same logical receiver line , as in this example , illustrates one aspect of the inter - connectability and adaptability of the system . the eight communication conduits 34 1 - 8 ( fig4 ) connect the geophone field matrix to a cru 18 ( fig1 ) that is often carried in a vehicle for mobility . depending on the data processing capacity of the cru 18 , one or more base lines 16 may serve a cru 18 . there are eight communication conduits in the base line cable 16 and two communication conduits in each receiver line cable 12 . geophone data will be reported to the cru 18 along the four receiver lines r - 1 through r - 4 . two of the eight communication conduits of the base line are made available to each active receiver line ensuring a one - to - one correspondence between receiver line and base line conduits that are utilized . specifically , receiver line r - 1 serves rams r - 1 / ram 1 and r - 1 / ram 2 . data from geophone channels 1 - 8 connected to ram r - 1 / ram 1 is initially processed by that ram and transmitted along receiver line communication conduit 30 1 to base line communication conduit 34 5 . the data produced by geophone channels 9 - 16 of row t 1 is processed by ram r - 1 / ram 2 and transmitted along receiver line communication conduit 31 1 to base line communication conduit 34 1 . receiver line r - 2 serves r - 2 / ram 1 , r - 2 / ram 2 , r - 2 / ram 3 in row t 2 and r - 2 / ram 4 in row t 3 . the communication conduit 30 2 and 31 2 respective to the cable 12 end sections for rows t 2 and t 3 are linked by a jumper cable 17 . the jumper cable is a cable that may contain only two communication conduits and no geophone channel conduits . it may be used to connect the ends of two receiver lines to form a loop . the data of geophone channels 9 - 16 in row t 2 is transmitted by r - 2 / ram 2 and channels 17 - 24 in row t 3 is transmitted by r - 2 / ram 3 along receiver line communication conduit 30 2 to base line communication conduit 34 6 . the data of geophone channels 25 - 32 in row t 3 is transmitted by r - 2 / ram 4 along receiver line communication conduit 31 2 to base line communication conduit 34 2 . also , geophone data from channels 1 - 8 of row t 2 is transmitted by r - 2 / ram 1 along communication conduit 31 2 to base line communication conduit 34 2 . receiver line r - 3 serves only geophones 1 - 8 in row t 3 that are signal processed by r - 3 / ram 1 . the data is transmitted along receiver line communication conduit 30 3 to base line communication conduit 34 7 . receiver line r - 4 serves r - 4 / ram 1 in row t 1 and r - 4 / ram 2 in row t 3 . in row t 4 , receiver line r - 4 also serves r - 4 / ram 3 , r - 4 / ram 4 and r - 4 / ram 5 . geophone channels 25 - 32 in row t 4 are connected to r - 4 / ram 4 for data transmission along receiver line communication conduit 30 4 to base line communication conduit 34 8 . receiver line communication conduit 31 4 receives the data of geophone channels 1 - 8 in row t 1 , channels 17 - 24 in row t 4 and channels 33 - 40 in row t 4 for transmission to the cru along base line communication conduit 34 4 . receiver line communication conduit 30 4 receives the data of geophone channels 9 - 16 in row t 3 and channels 25 - 32 in row t 4 for transmission to the cru along base line communication conduit 34 8 . the invention embodiment of fig2 illustrates two receiver lines r - 1 and r - 2 connected to a base line 16 . the communication conduits 30 1 and 31 1 of receiver line r - 1 connect r - 1 / ram 1 , r - 1 / ram 2 and r - 1 / ram 3 to base line communication conduits 34 1 and 34 5 , respectively . the communication conduits 30 2 and 31 2 of receiver line r - 2 connect r - 2 / ram 1 , r - 2 / ram 2 and r - 2 / ram 3 to base line communication conduits 34 2 and 34 6 , respectively . the rams 10 , the ltus 14 , and the cru 18 communicate by several types of digital data packets . the cru 18 uses “ commands ” to communicate with the line equipment comprising the rams 10 , ltus 14 , blus 38 and repeaters . the line equipment sends line data back to the cru . each piece of equipment in the matrix system knows its orientation relative to the cru . rams and ltus recognize only commands on their cru side and line data on their line side . each ram and ltu inherently has a logical “ command side ” and a “ line side ”. there is no physical difference between the two sides , and either physical side may play either functional role . definitively , however , the command side is the side closer to the cru , normally , with a possible exception in the case where both physical sides are reachable by direct path from the cru ( requires looping of receiver lines by use of jumper cable 17 ). in the preferred embodiment , in a multipath environment as in fig2 , the command side of each device is determined by the cru under the control of the operator . the cru may switch the sides of a particular ram or ltu as the survey progresses . this would be desirable , for example , in response to a communication failure in a particular cable segment . another benefit of this ability to configure the directionality of the rams and ltus is that when the cru is moved to another location during the course of the survey , these modules are readily adapted to the new network configuration by the operator ( without the necessity of a physical visit to the site of every ram and ltu to be reconfigured , as in prior art ). in fig2 the jumper cable 17 allows rams to communicate with the cru from either side , and thus with a simple re - assignment of command side , an otherwise stranded ram can be accessed by the cru . the cru controls the assignment of command side at system initialization by sending a “ power - up ” voltage to the device . a digital data packet includes 204 bits per packet . of this total , 8 data bits are reserved for a packet identification header , 192 bits are available for data use , and 4 bits are reserved for a data integrity check ( checksum ). commands may comprise , for example , of 32 bits of data for instructing one ( or all ) line equipment module to perform a given task . for example , the software may instruct a particular ltu to “ power off ” all rams on its “ b ” side . in another case , the software program may instruct all rams to switch into a low - power mode . typically , the data bit structure of a command data packet devotes the first 5 bits in the sequence to identification of a packet type e . g . command , interrogate command or line data . the sixth and seventh bits in a command packet identify the type of device ( ram , ltu , etc .) to which the command is being sent . the eighth bit in the command preamble is a “ global ” bit that defines which devices are to act on the command . one setting of the global bit addresses all devices of the selected type . another setting incorporates the 16 following bits to specifically designate which devices are to act on the command ( addressed command ). the last 8 bits in a command packet define the command being sent . when an ltu receives a command from the truck , it forwards the command simultaneously in three directions : out the “ a ” side , the “ b ” side and the “ line side ” ( unless the command is the special case of an interrogate command , which is treated differently ). as each ram on the spread receives a command , it decides ( based on the preamble and address bits ) whether or not to act upon it , then sends it to the next device on the line . interrogate commands are a special type of command consisting of only 8 bits . the interrogate commands tell all devices to transmit line data back to the cru if primed to do so by previous commands . in identifying an interrogate command , a device looks at only the first five bits of data and ignores the rest . upon receiving an interrogate command , an ltu passes it to the rams on its “ a ” side and on its “ b ” side simultaneously , then begins transmitting toward the cru the prior time sample “ a ” and “ b ” data which it has stored in memory . when the prior sample data has been transmitted for the “ a ” and “ b ” sides , the ltu , having purposely delayed sending the interrogate command out the “ line ” side to minimize the gap in transmission of data towards the cru , begins transmitting newly received “ line ” side data ( from the current sample ) toward the cru . if an ltu does not receive enough responses within the programmed length of time , it inserts simulated data for the missing rams . if the ltu receives too many responses , it ignores those over the defined number . this method allows the cru to identify the origin of data packets without resorting to use of explicit identification bits within the data packet . once finished with the “ a ” side , the ltu repeats the process on the “ b ” side . thereafter , the ltu sends the interrogate command out the “ line side ” side . the ltu must transmit data toward the cru in this order “ a ”, “ b ” and “ line ” sides . the order transmitted is the same order as would have occurred if it had actually interrogated the “ a ” side , the “ b ” side and the “ line ” sides in turn . this strict adherence to the correct ordering of data packets for transmission toward the cru is necessary for reducing data packet size through omission of identifying information , which improves efficiency of the telemetry . a ram or ltu may be used in repeater mode . in this mode its function is merely to receive commands from the cru and transmit them on the “ line ” side to the next ram or ltu . in repeater mode the ram or ltu also receives data from the “ line ” side and decodes and re - transmits the data toward the cru . when an active ram ( activated by previous commands ) receives an interrogate command , it begins sending its data towards the cru . just before finishing transmitting its data packet , ( e . g . at a time calculated to minimize the time gap in transmission ) the ram passes the 8 - bit interrogate command to the next ram or ltu on the line . line data packets consist of 204 data bits , for example . these packets include either analog - to - digital ( e . g . geophone pulse or geophone noise ) or status ( e . g . battery voltage , serial number , etc .) information sent by line equipment to the recording system . the first 8 bits of a line data packet are the preamble . bits 1 - 5 identify the block of information as data from the line as described previously . the next 3 bits identify what type of information is contained in the packet and how it was originated . for example , information may be real or simulated shot data , or device status . the data word portion of a line data packet is 192 bits long and may include either shot data ( 24 bits from each of a ram &# 39 ; s eight channels ) or status information . the remaining four bits of a line data packet are the checksum count . before a ram sends data to the recording system , it counts the number of “ high ” bits ( or “ 1 s ”) in the data word and writes the total here in binary format . the ram counts in cycles of 16 ( from 0 to 15 ), repeating the cycle until it finishes counting all high bits in the data word . for example , if a total of 20 bits were set “ high ” in the data word , the ram would count to 15 then repeat the cycle , counting 16 as 0 , 17 as 1 , 18 as 2 , 19 as 3 and 20 as 4 . the checksum count in this case would be 4 ( written as “ 0 - 1 - 0 - 0 ” in binary format ). after a ram sends line data towards the cru , each device along the way verifies it . when a device receives line data , it counts the high bits in the data word and compares that number with the data packet &# 39 ; s checksum count . if these numbers do not match , the device notes the fact that it detected a transmission problem . the device then sends the data towards the cru and waits for more data from the line or the cru . after collecting data , the system polls all devices on the line in order to determine which devices detected transmission problems and where to place error flags on the cru monitor display , for example . the construction of a ram 10 , as is shown schematically by fig5 , comprises a communication module 40 and an analog - to - digital conversion module 42 . the communication module 40 is supported by a clock circuit 44 and a central processing unit ( cpu ) 46 . the cpu includes a random access memory circuit 48 . the communication module is energized by a power supply circuit 45 that manages the power demands upon an internal battery 47 and an external battery 49 . the schematic of analog - to - digital module 42 is shown more expansively by fig6 to include , for each analog signal channel 32 , a line surge isolator 50 for limiting stray voltage surges ; an analog signal amplifier 52 ; and an analog - to - digital converter 54 . each analog - to - digital converter 54 transmits , upon receipt of an interrogation signal ( called an interrogate command ) from the communication module 40 ( fig5 ), its current geophone signal value to the communication module 40 for integration into a respective data packet . the communication module 40 of a ram is schematically represented by fig7 to comprise a line surge isolator 56 to limit voltage surges carried by the communication conduits 30 and 31 . digital values of the geophone signals are received from the analog - to - digital converter 42 . the delivery of the digital signals is coordinated by the cpu 46 to encode a data packet onto one or the other of the communication conduits 30 or 31 . of the two communication conduits 30 and 31 in a receiver line 12 , one is selected to receive the data packet transmission . the other communication conduit is decoded and retransmitted by a repeater circuit in the controller 60 . generally , each communication conduit 30 or 31 is logically connected for data packet input from alternate ram units along a single receiver line . with respect to fig2 , for example , communication conduit 30 1 may be connected to receive data packets from r - 1 / ram 1 and r - 1 / ram 3 whereas r - 1 / ram 2 may report data packets along communication conduit 31 1 . under the software program control of the cpu 46 , fig5 , and paced by the clock circuit 44 , the controller 60 ( fig7 ) receives the digital signal values from the analog - to - digital conversion module 42 and combines that data with other header and with the checksum data to create a data packet . the seismic sampling rate is programmable from about 0 . 125 samples per ms to about 4 ms / sample , for example . amplitude data are stored in the ram &# 39 ; s memory until an interrogate command is received , after which it transmits the amplitude data in the form of data packets along the receiver line toward the cru . along the receiver lines 12 , signal streams comprising a series of data packets are redirected into base line 16 signal streams by either ltus 14 or blus 38 . the only difference between the two signal transmission units is an expanded data memory capacity for the blus 38 . both ltus and blus potentially have signal processing capability . with respect to the fig9 schematic of an ltu 14 , for example , the preferred embodiment of the invention comprises communication conduits for a pair of receiver lines 12 a and 12 b and communication conduits for a pair of base lines 16 a and 16 b . each of these ports is served by a remotely controlled line isolator circuit 64 . in the normal operational mode , communication conduits 30 a and 31 a respective to receiver line 12 a and communication conduits 30 b and 31 b respective to receiver line 12 b , are connected to the communication module 70 . similar to the ram 10 , the communication module 70 of ltu 14 is directed by a cpu 72 and paced by a clock circuit 74 . the cpu 72 memory capacity is expanded by random access memory 76 . a unit power distribution circuit 66 is supplied by internal batteries 68 and / or external batteries 67 . the blu 38 of fig8 is substantially the same as an ltu 14 of fig9 except for bulk data storage capacity 78 . a blu may be used in place of an ltu , but not necessarily vice versa . in instances where the bulk data storage of the blu is not required , the terms “ ltu ” 14 and “ blu ” 38 are used interchangeably in this description of the preferred embodiments and in the following claims . the preferred embodiment of the cru 18 is represented by fig1 to include communication conduits for two base lines 16 that are served by respective communication modules 80 . the communication modules 80 are paced by a clock 82 and externally powered by a source 84 such as a battery or generator . a power management circuit 86 includes both filtering and distribution . a cpu 88 controls the communication modules 80 . the cpu 88 is functionally supported by a random access memory 85 and a bulk data storage circuit 87 . the entire system is manually interfaced by a keyboard 90 , a monitor 92 , a mouse 94 , a plotter 96 and a printer 98 . the communication modules 80 for the cru 18 are illustrated schematically by fig1 to include line isolators 100 1 - 8 for each of the eight communication conduits 34 1 - 8 and a data controller 102 . there are several distinctive characteristics of the software programs that control the invention operation . these distinctive characteristics cooperate to overcome several obstacles or inefficiencies inherent in prior art systems . one of these inefficiencies is an occurrence of large time lapses between data packets resulting in a reduction in the amount of line equipment that can be accessed in a given time period . another inefficiency arises from the complex relationship between ( 1 ) data cable length , ( 2 ) data transmission bit rate and ( 3 ) data generation rate . to address the prior art inefficiency of data rate transmission and to reduce the interval between data packets , the operational procedure of the invention includes a signal protocol by which the digital data packets are assembled and queued for transmission from the numerous rams to the cru 18 . this procedure generally includes transmission of an interrogate command from the cru to the ltus 14 . the ltus relay the interrogate command on toward the ram units along each of the receiver line communication conduits 30 and 31 . respective to the pair of communication conduits 30 and 31 in a single receiver line 12 , the two interrogate commands are independently timed . they may or may not be simultaneously emitted . although both of the communication conduits 30 and 31 in a single receiver line 12 are connected to each ram in the respective receiver line , the response each ram will make to the connection is normally different . referring to fig2 , an interrogate command a 0 originates from the cru 18 and is carried along communication conduit 34 1 of base line 16 to ltu 14 1 , for example . the ltu 14 1 relays the interrogate command a 0 along conduit 30 1 to r - 1 / ram 1 upon receipt , the r - 1 / ram 1 begins immediately to sequentially transmit along the communication conduit 30 1 , back to the ltu 14 1 , the data packet containing the data of all geophone system channels 32 ( fig5 ) connected to r - 1 / ram 1 . significantly , the signal a 0 is not carried further along communication conduit 30 1 than r - 1 / ram 1 . when signal a 0 is received by r - 1 / ram 1 , a timing delay is initiated by the ram communication module 40 for the relay transmission of interrogate command a 1 along communication conduit 30 1 from r - 1 / ram 1 to r - 1 / ram 3 via the repeater circuitry in r - 1 / ram 2 . the length of this time delay is variable as a function of numerous system and project parameters . in particular , the time delay is most strongly influenced by the number of geophone system channels connected to a particular ram ( i . e . 4 , 6 or 8 ), the cable type and length , the number of repeater rams and the transmission bit rate between the rams . the design philosophy of the retransmission delay of interrogate command a 0 is to coordinate transmission of the last data packet from r - 1 / ram 1 with arrival of the first data packet from r - 1 / ram 3 at r - 1 / ram 1 and to minimize the inter - packet stream gap between the successive signal streams . although the interrogate command a 1 is received by r - 1 / ram 2 , the signal is merely repeated on to r - 1 / ram 3 . when the interrogate command a 0 is received by r - 1 / ram 1 , transmission of the data packets respective to the geophone system channels reporting to r - 1 / ram 1 ( up to 8 , for example ) begins immediately . however , execution of the data packet signal requires a finite time period . a portion of this finite time period is the delay interval for the relay transmission of interrogate command a 1 by r - 1 / ram 1 . while the data packet from r - 1 / ram 1 is being transmitted back to the ltu 14 1 , interrogate command a 1 advances to r - 1 / ram 3 to initiate a corresponding data packet transmission from that ram . immediately , transmission of the r - 1 / ram 3 data packets begins along the segment of communication conduit 30 1 between r - 1 / ram 3 and r - 1 / ram 1 that has carried interrogate command a 1 . the origination of interrogate command a 1 is timed to make the first elements of the data packet from r - 1 / ram 3 arrive at r - 1 / ram 1 just after the last of the r - 1 / ram 1 data packet is transmitted . an interrogate command b 0 transmitted from the cru 18 independently of interrogate command a 0 is relayed by ltu 14 along line communication conduit 31 1 to r - 1 / ram 1 . upon receipt of the interrogation command b 0 , r - 1 / ram 1 merely relays the signal on to r - 1 / ram 2 . r - 1 / ram 2 begins transmission of a respective data packet to the ltu 14 1 along the segment of communication conduit 31 1 between r - 1 / ram 2 and r - 1 / ram 1 . upon receipt of the data packet , r - 1 / ram 1 merely repeats the data packet signals to the ltu 14 1 . the interrogate command delay at each of the rams is not a fixed value but is potentially variable for each ram depending on the number of analog channels reporting to a respective ram , the number of repeater rams between the active rams and other factors affecting transmission time . although the preferred embodiment of the invention provides for 8 geophone system channels 32 to each ram , the respective cpu 46 may be programmed to accommodate any number of channels less than 8 , also . moreover , there is no rule of nature that sets the maximum number of analog channels at 8 . this is simply a matter of equipment design and engineering practicalities . it should also be noted that the communication conduit 30 or 31 for a particular ram may be changed from one to the other . such a step may be required in the event of a broken connection or continuity in an intended communication conduit . however , in the event of such a change , the interrogate command delay time at the affected ram may be altered . of especial note is a logical break capability of each ram to be programmed for the termination rather than re - transmission to the next ram of an interrogate command . this capability allows the receiver lines to be looped and thus have cable connections to two ltus 14 . functionally , however , in a given programmed configuration , each ram will operate with only one pair of communication conduits 30 / 31 respective to a single , designated , ltu 14 . in one example , as represented by fig1 , the continuity of geophone row t 3 is interrupted between rams r - 3 / ram 1 and r - 2 / ram 4 by an insurmountable obstacle such as a river or sheer cliff . consequently , the interrogate command from base line communication conduit 34 3 that would normally be transmitted to r - 2 / ram 4 from ltu 14 3 is , instead , terminated by the ltu . cooperatively , the interrogate command from ltu 14 2 that would normally be terminated at r - 2 / ram 3 is transmitted further via jumper cable 17 to r - 2 / ram 4 in geophone row t 3 . in the similar example shown in fig2 , the obstacle is represented by the logical break line p - p across conduits 30 2 and 31 2 between r - 2 / ram 2 and r - 2 / ram 3 . interrogate commands c 0 and d 0 from the cru 18 are relayed by ltu 14 2 . interrogate command c 0 is received by r - 2 / ram 1 and delayed for retransmission to r - 2 / ram 3 as interrogate command c 1 . because of a logical break command to r - 2 / ram 2 , interrogate command c 1 is not issued . meanwhile , interrogate command d 1 is relayed through r - 2 / ram 1 to r - 2 / ram 2 for the r - 2 / ram 2 geophone data . however , no retransmission signal d 1 is issued by r - 2 / ram 2 . the r - 2 / ram 3 geophone data is reported along conduit 30 1 via jumper cable 17 in response to a delay of interrogate command a 2 from r - 1 / ram 3 . although this result may obviously be accomplished by a physical disconnection of the communication conduits along the line p - p between r - 2 / ram 2 and r - 2 / ram 3 , the need for such reporting reassignment may not always be apparent at the time the rams are distributed . moreover , certain rams may fail after distribution and require replacement , repair or omission . with the present invention , the options of omissions and revised connections may be exercised from the cru 18 as compared to the prior art options of repair or replacement that require a physical return to the respective ram locations . the logical break capacity of the invention may be accomplished by direct commands ( originated by the cru ) to the cpus 46 respective to the rams . the cpus 46 program the respective rams to cause them to selectively prevent the retransmission of interrogate command by strictly defining the sequencing of data packets based on the network configuration , the position of any data packet within the sequence may be used to determine which ram created that data packet . and because the data packet sent in response to one interrogate command contains data samples that were created proximate the time of the interrogate command &# 39 ; s arrival at the creating ram , the time the data packet was created need not be explicitly stated within the data packet . the time of creation is implicitly knowable by its position within the overall data stream arising from the interrogate command thus , both the ram of origin and the time of creation of any data packet can be implicitly determined . this reduces the amount of data that must be explicitly written within the data packet . therefore the total amount of data that is transmitted is reduced accordingly . this aids in the optimization of seismic telemetry and makes the system more efficient and cost effective . the multiple base line communication conduits , e . g . conduits 34 1 through 34 8 and their respective receiver lines are each made to independently follow the methods as described above for sequencing data packets by the actions of the base line units and rams . thus multiple data trains , one per base line communication conduit , exist simultaneously and may be operated in parallel , optimizing total transmission capacity . data packet integrity along communication conduits is affected by transmission rate , transmission power , cable type and cable length . as cable length increases so does the attenuation . attenuation is greater as the transmission rate increases . to optimize the transmitted signal definition , the transmission bit rate and transmission power must be tuned for the length of the communication conduit . data bit definition relates to the ability of the receiving instrument to distinguish a data bit in the received signal continuum . due to transmission line losses , data bit definition will decay over the length of the transmission line . at some point along the line length , the data bit pulse that was transmitted has decayed beyond distinction from random noise anomalies . using a lower transmission bit rate , the distance may be extended over which reliable communication may occur . also , using greater power in transmission may extend this transmission distance . the ability to control the power of transmission is a feature of the preferred embodiment of this invention . the control is exercised from the cru and determines the power level of transmission used by the rams and ltus . the power level is increased as required for greater distances of transmission and decreased for lesser distances . as different cable lengths and types may be used on one project , there may be different transmission power settings invoked for different rams within the network , and the power level used by rams may differ from that used for ltus . power of signal transmission may be set differently for forward transmission toward the cru and reverse transmission ( away from the cru ). power settings depend on transmission characteristics of the communication conduits of the cables , length being a primary characteristic , but other characteristics such as nature of the conductors also influences the power required and hence the optimum setting . it is generally beneficial to conserve power by only using sufficient power to ensure reliable communication but not excessive power . this prolongs battery life in the remotely distributed rams and ltus . determination of optimum power settings is done experimentally for different types and lengths of cables and the cru is programmed to use these settings for the given cable , in the preferred embodiment . power settings are controllable independently of frequency of transmission . however , optimum power settings will be different for different frequencies of transmission , hence the cru is programmed to recognize different optimum settings for different frequencies of transmission , as well as for different types and lengths of communication conduits . by conserving battery power , productivity and cost effectiveness of the system are enhanced over that available from prior art . the graph and associated table of fig1 illustrate the operation of the present interrogation signal strategies as described above with two cables of differing conductor size and construction . this fig1 graph plots the relation of transmission bit rate and cable length at the limits of signal definition . to be noted from this comparison is the influence that cable construction has upon data transmission capacity . for example , a 28 awg conductor of construction “ a ” will transmit reliably discernable data over a cable length of 288 meters at 7 . 5 mbits per second . comparatively , a 26 awg conductor of construction “ b ” may transmit reliable data over a cable length of 342 meters at the same transmission rate ; a 54 meter extension that represents a 15 % advantage . the advantages of the invention are further illustrated by the tabulated data of fig1 . here , the capacity of the system is organized into 3 groups respective to the number of geophone channels connected to each ram in an array . specifically , the data of group i corresponds to an equipment distribution matrix that connects 8 geophone analog channels 32 to a single ram . the group ii data corresponds to an equipment matrix having 6 geophone analog channels 32 connected to a single ram . group iii data corresponds to a 4 - channel connection . referring to the schematic of fig1 , the to / cable ( takeouts per cable ) _column of the fig1 table shows the preferred maximum number of analog geophone channel connections to a receiver line cable . the to interval ( takeout interval ) is the distance , in meters , between adjacent analog connections along a cable length . the weight column , is , in pounds , the weight of a corresponding cable of the tabulated length . the distance / ram column is the spacial distance , in meters , between adjacent rams in a receiver line . the cable length column is , in meters , the length of a corresponding cable . the 8 columns of data respective to 8 sampling frequency values ( i . e . interrogation frequency ), 500 hz , 400 hz , etc ., correspond to the maximum number of analog channels 32 that may be connected to a single receiver line of the tabulated length . the xmit rate column corresponds to the transmission bit rate_charging the respective receiver line . a specific number of analog channels 32 per receiver line listed by fig1 relates to the corresponding sampling frequency column and xmit rate row . fig1 depicts a typical land 3d seismic survey with receiver lines and base lines that are perpendicular to the receiver lines . in some types of 3d surveys the distance between receiver lines may be significantly less than the distance between rams along the receiver lines . in this situation it is advantageous in terms of optimizing base line telemetry to be able to select a higher transmission bit rate_than the rate selected to optimize receiver line telemetry , because the cable segments connecting ltus may be much shorter than the cable segments connecting rams . the cru therefore , elects to use an appropriate higher rate of transmission for the base lines , setting it independently from the receiver line transmission rate . by using a higher transmission rate the base line capacity is increased and more channels may be accommodated on one base line communication conduit . using a lower transmission rate on the receiver line communication conduit may be advantageous in particular survey projects because it allows a greater distance between rams and hence fewer total rams to cover a given area . thus , in the preferred embodiment , the transmission rate of the base line may be set to be higher , lower or the same as the receiver line transmission rate . the system sets the transmission rates to be used under the control of the operator at the cru and the cru programs each device in the network accordingly . seismic surveys have spatial and temporal sampling requirements that are a function of the local geology , geophysical objectives , seismic noise and signal characteristics and other factors . sampling density requirements in time and space are both affected and in a similar manner . seismic surveys that have very shallow geologic targets generally have the potential to retain signals at relatively high frequency , e . g . 250 hz . however to successfully image the shallow targets at up to 250 hz requires relatively dense spatial sampling as well as dense time sampling . conversely , deep geologic targets have the potential to retain only lower frequency signal , e . g . up to 50 hz . imaging deep targets thus requires less dense time sampling ( to define up to 50 hz ) but beneficially also requires less dense spatial sampling . as an example , a first seismic survey targeting very shallow geologic horizons may require very dense time sampling at a high sampling rate of 500 hz ( to preserve with fidelity 250 hz signal ). to maintain reliable signal definition , a short separation distance between adjacent rams is appropriate . from the table of fig1 , an extreme layout would connect 1984 analog channels in a single receiver line to one side of an ltu . cooperatively , the signal transmission rate ( xmit rate ) should be set at about 16 . 25 mbits per second . these analog channels could have maximum take - out intervals of 17 meters along a maximum single cable length of 136 meters . only one cable would span between adjacent rams which are also separated by a maximum of 136 meters . at each take - out point , the cable channel is broken and a geophone set is connected to an analog conduit line from the take - out point . a single analog conduit is broken twice and reports in opposite directions to respective rams whereby each ram in the array is connected to 8 analog channels . in the preceding example , although only 1984 channels may be connected along the receiver line to one side of the ltu , another 1984 channels may be connected along an extension of the receiver line if it is connected to the opposite side of the ltu . thus the operator may in practice utilize double the number of channels per receiver line with respect to the number of channels shown in the table , if he follows this practice . a subsequent survey targeting deep geologic layers with the same equipment may require a very sparse sub - surface sampling that is distributed over a large area . long distances between geophone groups and accordingly wide spacing between rams may be appropriate for such a survey . referring to fig1 , by adjusting the ram sampling rate to about 100 hz and setting a transmission rate of about 3 . 5 mbits per second ; this low density survey could accommodate 416 analog channels per receiver line ( or 932 if receiver lines are connected on both sides of the ltu ). the rams could be spaced along the line at 528 meter intervals and connected to receive only 4 analog channels per ram . geophone take - out intervals along the data cable in this case may be a maximum of about 132 meters . thus , the adjustable sampling rate and signal transmission rate of the present invention , along with variability in the number of channels per ram , allows optimization of the equipment investment for varying survey requirements . a variable bit rate translates directly into operational and logistical advantages in the field . the transmit power control feature of the present invention is one more tool the user has to make data transmission more robust under varying survey conditions , while optimizing power consumption . data packet transmission control minimizes the time gaps between data packet groups according to the cable type and lengths used in the network . this benefit provides the survey crew with close to 100 % time utilization of the cable with extra time available for more channels to be added to the line resulting in higher communication conduit limits . in the preferred embodiment of the system , the cru 18 software is programmed to understand the 3 - dimensional earth &# 39 ; s surface and the location of geographic features , both natural and man - made , as well as the location and operating status of all items of the seismic data acquisition equipment . the cru software understands the configuration and interconnections of the network of rams , receiver - line cable , ltus , base - line cables and the cru . the system operator is provided a substantially true - scale map view of all of this information as exemplified in fig1 . the network connections may be established and modified at any time by the operator or automatically by the software at the request of the operator . in this way the desired subset of the total set of deployed rams may be made active to record and transmit seismic data when required to do so by the operator . standard computer tools including keyboard , mouse , touchpad and touch screen may be provided as tools to the operator to assist him to manipulate the network to achieve the geophysical objectives . the operator may request the system software to optimize the network configuration to take best advantage of the communication capacity of the individual equipment items to reduce the required transmission time to a minimum . looping of receiver lines ( by joining ends of adjacent pairs of receiver lines using jumper cables 17 ) is a recommended practice in the preferred embodiment so that in event of failure of any ram or breakage in the receiver line cable , connection to the cru may be re - established by use of the bi - directional communication capability of the ram . the operator is notified on the map screen of the failure and needs simply to re - direct the otherwise stranded rams to communicate in the opposite direction to reach the cru . this is done by re - positioning the logical break in the receiver line . this is illustrated by the schematics of fig1 and 16 . the originally expected data transmission routing is shown by fig1 wherein the data of rams 1 - 6 is transmitted along receiver lines r - 1 to ltu 14 1 . the data of rams 7 - 12 is transmitted along receiver line r - 2 to ltu 14 2 . although ram 6 is physically connected to ram 12 by loop 17 , the loop is off - line to the respective r - 1 and r - 2 interrogate command transmissions from rams 6 and 12 . after the equipment array has been positioned and connected , unexpected circumstances cause a signal continuity interruption along receiver line r - 1 between ram 3 and ram 4 as shown by the x on fig1 . responsively the operator of the present invention terminates the r - 1 interrogate command retransmission at ram 3 ( by insertion of a logical break ), activates the r - 2 interrogate command from ram 12 and also terminates the r - 2 interrogate command from ram 4 . failure of one of the two communication conduits in a receiver line cable during transmission will not result in loss of data because of two key aspects of the system , ( 1 ) the storage of data in the memory of the ram until the cru confirms receipt of the data , and ( 2 ) the ability of the system to transmit all of the data over the remaining receiver line communication conduit . although throughput capacity of the cable is cut in half , no data is lost . similarly , if a base line loses a portion of its communication conduits , for example due to physical damage during operation , all data may be directed over the remaining conduits . the flexible network design allows this adaptability to unanticipated conditions . data storage is also available in the ltu ( as it is with the ram ) which allows saving of data while it awaits re - transmission to the cru . the capacity of the base line to communicate seismic data is provided by eight ( 8 ) independent communication conduits . in addition to providing redundancy useful in overcoming failure of some of the conduits as described immediately above , this design facilitates the distribution of base - line capacity around both sides of physical obstacles . this is illustrated in fig1 . the base line needs to be connected to receiver lines on both sides of the obstacle . in prior art systems this would inevitably require the provision of two complete base lines distributed all the way from the cru to the maximum extent of the area to be covered , an unnecessary burden in the preferred embodiment . using the base line splitter device 19 , shown in fig1 , the capacity of the single base line from the cru may be positioned on both sides of the obstacle . on the far side of the obstacle the base line may be re - joined by use of another base - line splitter device 19 . the eight selected communication conduits may be spread evenly , four to each side , or in any combination totaling to eight . conduits not selected at the split are not connected and are unused around the obstacle . the base line could be designed with a number of communication conduits different from eight without changing the principles of this method , of course . instead of requiring two complete base lines from the cru to the edge of the recording area , one suffices , except at the obstacle itself , resulting in a significant savings in labor and equipment . the basic concept of providing base lines with sub - dividable capacity makes this achievable . prior art systems that use a high capacity base line cannot achieve this savings and are more subject to total loss of transmission capacity due to equipment failure . the preferred embodiment also provides inter - connectability of network devices to make the total network more flexible and adaptable to different layout requirements . either a base line cable or a receiver line cable may be connected to any port of the ltu . an ltu may be connected to a receiver line between any pair of rams . physical receiver lines may be connected at both ends to base lines , or to the same base line at different ltus . base lines may be split and rejoined . receiver lines may be used to carry base line telemetry . fig1 illustrates the benefits to seismic data acquisition operations of the inter - connectability of the preferred embodiment . the operator with the guidance of the system software , uses the true scale map of the area and the seismic equipment , and builds the network in the optimum way , given the nature of the obstructions . in this example there are three kinds of physical obstacles that obstruct the layout of the desired ideal grid of seismic receiver lines . there is a river running across the area , a highway inhibits access and a series of sandstone cliffs blocks access . the operator at the cru views the map as depicted in fig1 . this map changes as often as necessary to depict the current equipment configuration . as the operator constructs the network he has the advantage of viewing the exact locations of equipment items with respect to the physical features of the terrain . he also sees the operability status of equipment items , for example whether a particular base line and the receiver lines with rams connected to it are operating within specifications . he makes decisions which best utilize available equipment to build the network . the operator has chosen to establish a separate base line south of the highway to reduce safety concerns by limiting the number of cables and workers on the highway . he has also chosen to establish a base line running north and to split it several times , one part staying below the cliffs , the other climbing the cliff at the easiest point , where it divides again and again to take advantage of the topography . at the ne corner of the area , the operator has chosen to use receiver line cable with rams used solely as repeaters and with no geophones connected to these rams . here the receiver line cable has been used to carry the base line telemetry and therefore acts as a base line with only two communication conduits . an ltu at the end of this section of cable joins a receiver line with the rams at the ne extremity of the area . this illustrates the dual roles the rams may serve , i . e . as pure repeaters to overcome distance limitations , and as data acquisition devices for the geophone arrays . also , the ability of the receiver line cable to substitute for base line cable , although with reduced number of communication conduits , is another feature which increases system flexibility and hence productivity . prior art systems do not have these capabilities . jumper cables 17 are used to connect segments of receiver line cable to create loops at the ends of pairs of receiver lines . this allows extension of receiver lines but also may provide alternate transmission paths that can be used to overcome cable breaks and failure of one of the rams in the pair of receiver lines . thus the operator with the aid of the map view and layout tools provided by the software , devises the most practical and cost - effective way to acquire the seismic data . the flexibility of the network improves ease and safety of deployment , but also improves productivity after deployment , as the multiple paths available from each ram to the cru allow continued production without need for re - deployment in event of equipment damage or failure . fig1 depicts the cru and a typical ram in the network that is separated from the cru and connected to it by a base - line cable with a series of ltus and a receiver line with several intervening rams . a desirable objective of all seismic data acquisition systems is that amplitude samples are recorded by all rams in the network that , in effect are all taken at the exact same instant . it is not necessary , however , to actually sample the amplitudes simultaneously if a means is available to know the varied actual times of sampling respective to each ram and a means is provided to calculate the probable values of amplitude at the ideal sample time . the preferred embodiment of the invention incorporates unique means to accomplish the sampling objective stated above . the method of the invention recognizes that there are two categories of errors that cause the time of an amplitude sample to differ from the intended ideal time . the first category of errors includes those caused by the successive delays in the network as the interrogate command travels from the cru through the series of intervening network elements to the ram . the second category of error occurs within the ram . transmission delays in the base line cable , ltus , receiver line cable , and intervening rams all contribute to the first category of error . these delays may be either physically measured in the laboratory prior to the seismic survey and tabulated in cru system software for each type of network element , or in the case of deliberately - imposed delays of interrogate command retransmission , may be computed by the system software . the cru is programmed to simply sum up these predictable delays for the given network configuration and thereby compute the total predictable transmission delay for each ram in the network . this predicted value equates to the total delay between the time the interrogate command is sent from the cru until the given ram takes the corresponding initial amplitude samples for its channels at the beginning of the period of recording . in the preferred embodiment , after the first sample of a seismic record is taken , the ram continues to take samples at increments of time equal to the programmed sample period , for example every 2 ms , according to the ram &# 39 ; s own internal clock . the ram &# 39 ; s internal clock may be a relatively low - powered and drift - prone clock , such as temperature - compensated crystal oscillator ( tcxo ), with a drift such as 2 . 5 parts per million ( ppm ). however the system master clock in the cru is much more accurate and also consumes much more power . typically it might have a drift rate such as 0 . 02 ppm . the system master clock may be periodically corrected using an external time source such as from a gps clock . freeing the ram from dependence upon receiving each and every interrogate command from the cru prior to taking the next sample has advantages in terms of system efficiency and in error prevention in case of sporadic errors in transmission from the cru to the ram and is a novel feature of the invention . as the ram proceeds to take amplitude samples after the initial sample in the recording period , say every 2 ms according to its clock , the samples increasingly may drift away from the intended sampling times due to increasing buildup of error in its clock . the error may become so great as to invalidate and render useless the amplitude data when the length of the recording period is great if the method of the preferred embodiment is not used . fig1 illustrates the buildup of clock drift error between the time of the initial sample and the time of a later sample . this ram clock drift can be monitored in the following way which is the method of the preferred embodiment . 1 . the ram stores its clock times periodically on a predetermined schedule of receipt of interrogate commands , e . g . every 100 receipts , beginning with the first interrogate command at the beginning of a period of recording . 2 . at the end of the period of recording , or when requested by the cru , the ram sends back its table of stored clock times to the cru . 3 . the cru , knowing the times on its internal clock that correspond to the times in the table containing the ram clock times , and knowing the total predictable delay for the ram , constructs a drift curve for the ram &# 39 ; s clock consisting of values of ram clock time versus master clock time . any interrogate command which fails in transmission and is thus not received by the ram will decrease its count by one and cause a diagnostic shift in the drift curve . unless transmission errors are rampant , the method includes detection and correction of such interrogate command transmission errors . using the drift curve and the total predicted delay for each channel of each ram , the cru computes the actual times at which each ram took its amplitude samples . fig2 shows the two sets of times , the desired times and the actual times , marked off against a representative analog seismic waveform . the actual samples provide a basis for estimation of the amplitudes at the intended sample times according to the master clock . a simple regression or curve - fitting method may be used to compute the estimated amplitude values at the intended times . alternatively , more elaborate methods well - known in the art such as ( sin x )/ x or optimum least - mean - square - error ( lsme ) interpolation filtering may be used . the cru thus computes amplitude values for the ideal intended time of sampling for each recorded channel , effectively achieving the objective . accounting for drift of the ram clock may be of minimal importance if the duration of the recording period is short , for example , 10 sec . for very long periods of recording such as 300 sec or longer , it is essential , and therefore is invaluable in implementation of continuous or quasi - continuous recording required by methods such as vibroseis slip - sweep . an average time error for a channel , computed over a time - window of relatively short duration , e . g . 10 sec , may be used to time - shift all of the amplitude samples within this window , if the amount of relative drift of the ram clock is insignificant within the window ( e . g . & lt ; 0 . 2 ms ). the ram clock drift being different for each of the many rams in the recording system dictates that the original amplitude samples for different rams to be taken at differing times . in this respect the recording system in this invention is an asynchronous system rather than a synchronous system as in the prior art . furthermore the deliberately - imposed delays in transmission of interrogate commands contribute to the asynchronous nature of the system ( while at the same time allowing maximization of data throughput along base lines and receiver lines ). the novel method of correcting the time samples enables an asynchronous system to achieve the desired sampling which is in effect synchronous . because the system is initially asynchronous it is able to achieve network and system efficiencies not possible with synchronous systems . although our invention has been described in terms of specified embodiments which are set forth in detail , it should be understood that this is by illustration only and that the invention is not necessarily limited thereto . alternative embodiments and operating techniques will become apparent to those of ordinary skill in the art in view of the present disclosure . accordingly , modifications of the invention are contemplated which may be made without departing from the spirit of the claimed invention
6
the fastener of the type which these tools is to install or place is illustrated in fig1 to 6 . the fastener is in the form of a blind rivet 10 ( a blind rivet is one which can be placed by access to one side only of the workpiece ), and comprises three members . the first member is a tubular shell 12 , the second member is a stem 11 , and the third member is an annular lock creator washer 13 , all three members being made of steel . the shell 12 has a preformed head 14 , which in this example is of countersunk form , at one end . the stem 11 comprises an elongated pin 15 , formed with an enlarged head 16 at one end . the stem and shell are assembled together with the stem head 16 adjacent the end ( the tail end ) of the shell remote from the shell head 14 , with the pin 15 protruding from the shell head . the lock creator washer 13 comprises a washer body 17 formed integrally with a circular sharp - edged rim 18 ( more clearly seen in fig2 and 7 ). the washer 13 is assembled on the stem pin with the sharp edge of the rim 18 facing towards , and in contact with , the shell head 14 . in use , the rivet is inserted through an appropriate hole 19 in panels 21 , 22 to be riveted together ( see fig2 and 7 ), until the shell head 14 abuts the nearer panel face . a progressively increasing pulling force is then applied to the stem pin 15 , the reaction to the pulling force on the stem being applied to the shell 12 through the washer 13 . the stem head 16 enters the shell 12 and enlarges it to form a blind head 23 ( fig2 and 7 ) which clamps the panels 21 , 22 together between the shell head 14 and the blind head 23 . when the stem head 16 can enter no further into the shell because of the resistance to expansion provided by the rear panel 22 , increasing force on the washer 13 causes the sharp edged rim 18 to deform the material of the shell head so as to engage with the stem pin and lock the stem into the shell . further increase in tension on the stem pin causes the pin to break , the broken pin tail 24 ( fig2 and 7 ) and the washer 13 then being free from the placed rivet . the broken off pin tail is ejected down a bore 20 through the tool . such rivets , and the manner of placing them as described , above are well known in the art of blind riveting . also well known is the use of installation apparatus , in the form of a hydraulically - powered placing tool for placing such rivets . such a tool is illustrated in fig1 to 5 , and comprises a first part in the form of a nosepiece 35 having an annular anvil face 25 for engaging with the lock creator 13 to transmit force thereby to the shell 12 as aforesaid , and a second part in the form of gripping and pulling means 26 for engaging the pin 15 of the stem 11 to apply tension to it relative to the shell as aforesaid . as is well known in the art of blind riveting , the gripping and pulling means comprises a set of gripping jaws 27 retained within an internally tapered jaw housing 28 which is secured to the front end of the draw rod 29 . the rear end of the draw rod 29 is secured to a piston 31 sliding in a cylinder 32 formed within a body casting 33 . the tool is actuated by supplying hydraulic fluid under pressure to the space 34 in front of the piston 31 , so that the draw rod is urged backwards with respect to the body housing . the annular anvil face 25 is provided at the front end of a tubular nose piece 35 which is secured to the body casting 31 so that the jaw housing 28 is inside the nose piece 35 and the jaws are behind , and aligned with , the annular anvil face 25 . in use of the tool to place a blind rivet , the gripping means 26 is initially in its forwards position ( fig1 ) under the urging of a return spring 37 . the pin 15 of the stem is inserted through the aperture 36 in the annular anvil 25 and pushes the jaws 27 rearwardly and apart until the pin enters between them and is gripped by them . this is the position shown in fig1 . the rivet shell is inserted in the workpiece panels as previously described . the tool is then actuated by supplying hydraulic fluid at a progressively increasing pressure to the space 34 in front of the piston 31 in the cylinder 32 , thus actuating the tool to pull the gripping jaws 27 rearwardly to grip and apply increasing tension to the stem pins the reaction force on the shell being applied by the anvil face 25 through the washer 13 . the blind rivet is placed as previously described . when the stem has broken , hydraulic pressure to the cylinder is removed , and the gripping means 26 moves forwards again under the urging of return spring 37 . in prior art tools , when the stem pin breaks the washer 13 is free to fall off the anvil face 25 and thereby create a hazard , as previously described . the tool of the present example is provided with means for temporarily retaining the lock creator washer on the anvil of the nosepiece after the stem has broken , by resiliently gripping the washer . the resilient gripping is arranged to come into effect when the stem gripping means 26 retracts , and to remain gripping the washer until the stem gripping means 26 returns to its forwards position . thus , after placing a rivet , the tool operator can remove the tool from the workpiece and position it with the anvil in a convenient position ( e . g . over a waste receptacle ) before releasing the hydraulic pressure in the cylinder space 34 to allow the gripping means 26 to return forwards and release the washer in a safe position . the resilient gripping means is provided by a relatively simple modification to the nosepiece 35 . the modification comprises three features . firstly , the nosepiece is provided with three longitudinal slots 38 ( fig4 and 5 ), spaced 120 degrees apart around the nosepiece barrel and extending the anvil aperture 36 rearwardly for the major part of the length of the barrel . the barrel is thus split into three arms 40 , which are integral with each other at the rear end of the barrel beyond the ends of the slots 38 , and the anvil 25 is also split into three parts , which can move radially inwardly and outwardly with respect to the aperture 36 by flexing of the three arms of the barrel . to reduce fatigue , the rear of each slot 38 ends in a small circular enlargement 39 . secondly , the anvil is provided with gripping surfaces around its periphery , in the form of a wall 41 which surrounds the anvil and projects forwardly from it . the wall is split into three parts by the slots 38 , and thus provides three gripping faces 42 ( fig5 ) which extend transversely to the anvil face 25 . it is arranged that , when the arms of the barrel 35 are in the unstressed or undeflected position , the diameter between the gripping faces 42 is slightly less than the outside diameter of the washers 13 of the rivets which the tool is to be used to place . thirdly , the inside of the forward end of the nosepiece barrel is provided with a slightly converging taper face 43 . the arrangement is such that , when the gripping means 26 is withdrawn rearwardly ( fig2 ), the front of the jaw housing 28 is disengaged from the nosepiece taper 43 , so that the nosepiece arms close together under their own resilient urging , so as to grip a washer 13 , on the anvil 25 , between the gripping faces 42 , as shown in fig2 . when the gripping means is moved forwards , under the urging of the return spring 37 , the peripheral edge 44 of the front of the jaw housing 28 enters and engages the nosepiece internal taper 43 , and pushes the nosepiece arms apart slightly . this moves the anvil gripping faces 42 apart slightly , so that they no longer grip the washer , as shown in fig3 ( and in fig1 ), and are thus in their releasing position . limitation of outward movement of the nosepiece arms is provided by a steel ring 45 received in an annular groove 46 around the barrel near its front end . the operation of the temporary gripping means will thus be clear . when the placing tool is in the unactuated position ( fig1 ), the jaw housing 28 is in its forwards position and the anvil gripping faces 42 are held apart in their releasing position . when the rivet stem pin 15 is inserted through the anvil aperture 36 and into the jaws 27 , the rivet washer 13 can enter between the gripping faces 42 and into contact with the anvil face 25 . when the tool is actuated to place the rivet , the jaw housing 28 retracts and allows the nosepiece barrel arms to close together under their own resilient urging , into their retaining position to grip and retain the washer 13 . after the pin 24 of the stem has broken on completion of placing of the fastener , the washer continues to be gripped until the tool is de - actuated , so that the tool can be moved and positioned to release the washer in a convenient and non - hazardous place . since the gripping of the washer simply results from the resilience of the arms 40 , the washer is not substantially deformed thereby . a similar tool provided with a second form of temporary retaining means is illustrated in fig6 to 10 , like parts in fig6 to 10 being indicated by the same numerals as in fig1 to 5 . in this form , the nosepiece barrel 50 is rigid and non - slotted , and the anvil face 25 is provided by a separate anvil nosetip assembly 47 . this is generally tubular and is split along an axial plane , and comprises two identical mirror - image halves 48 . each half nosetip can rock about a position substantially mid - way along its junction with the other half . to this end , each half has a forwards contact face 49 and a rearwards contact face 51 which are at a slight angle to each other , meeting at an apex 52 . the two halves together form the nosetip 47 , which has a rearwards flange 53 , and a forwards flange 60 which forms the anvil face 25 and , around its periphery , extends forwards to provide the gripping faces 42 . the rear and front flanges are joined by a body part 54 which extends through an aperture 55 at the front of the nosetip . the washer gripping faces 42 of the nosetip halves are resiliently urged towards each other , into their retaining position , by a garter spring 56 ( which may be in the form of a rubber 0 - ring }, received in a peripheral groove around the outside of the front ends of the nosetip halves . in order to facilitate assembly of the nosetip 47 in the barrel 35 , the latter is provided with a side slot 59 extending radially from the aperture 55 ( fig1 ). this slot 59 is wide enough to pass the body portions of only one of the nosetip halves at a time , and ends in a crossslot 57 through which the rear flange portions 53 of the nosetip can pass . the action of this form of temporary retaining means will be understood by reference to fig6 and 8 . when the jaw housing 28 is in its forwards position ( fig6 and 8 ), its front end contacts the rear flange 53 of the nosetip and pushes the nosetip forwards , pushing the rear flange halves 53 flat against a flat transverse face 57 on the back of the front end of the nosepiece barrel 35 . this causes the fronts of the nosetip halves to be pushed apart , against the urging of the spring 56 , so that the gripping faces 42 are in their releasing position . the rear faces 51 of the nosetip halves are in contact ( or nearly so ), with the forward faces 49 diverging from each other . when the tool is actuated and the jaw housing 28 retracts , the nosetip halves can rock about their apexes 52 , under the urging of the spring 56 . the washer - gripping faces 42 at the front of the nosetip move towards each other into their gripping position , so that the forwards nosetip faces 49 come into contact with each other ( or nearly so ), whilst the rearwards faces move apart from each other and the engagement of the outer ends of the flange halves 53 on the nosepiece back face 57 pulls the nosetip slightly rearwardly . the action of the temporary retaining means in use of the placing tool has the same function as that described with respect to fig1 to 5 . it should be noted that , in both fig1 to 3 and 6 to 8 , the amount of movement of the washer gripping walls 42 and of the associated parts of the anvil are exaggerated for clarity of illustration . in practice the movement of the gripping walls may be only a few thousands of an inch or a few tenths of a millimetre . the invention is not restricted to the details of the foregoing examples .
8
referring to fig1 - 5 , an apparatus or osteotome 100 is shown that is configured for accessing the interior of a vertebral body and for creating a pathway in vertebral cancellous bone to receive bone cement . in one embodiment , the apparatus is configured with an extension portion or member 105 for introducing through a pedicle and wherein a working end 110 of the extension member can be progressively actuated to curve a selected degree and / or rotated to create a curved pathway and cavity in the direction of the midline of the vertebral body . the apparatus can be withdrawn and bone fill material can be introduced through a bone cement injection cannula . alternatively , the apparatus 100 itself can be used as a cement injector with the subsequent injection of cement through a lumen 112 of the apparatus . in one embodiment , the apparatus 100 comprises a handle 115 that is coupled to a proximal end of the extension member 105 . the extension member 105 comprises an assembly of first ( outer ) sleeve 120 and a second ( inner ) sleeve 122 , with the first sleeve 120 having a proximal end 124 and distal end 126 . the second sleeve 122 has a proximal end 134 and distal end 136 . the extension member 105 is coupled to the handle 115 , as will be described below , to allow a physician to drive the extension member 105 into bone while contemporaneously actuating the working end 110 into an actuated or curved configuration ( see fig6 ). the handle 115 can be fabricated of a polymer , metal or any other material suitable to withstand hammering or impact forces used to drive the assembly into bone ( e . g ., via use of a hammer or similar device on the handle 115 ). the inner and outer sleeves are fabricated of a suitable metal alloy , such as stainless steel or niti . the wall thicknesses of the inner and outer sleeves can range from about 0 . 005 ″ to 0 . 010 ″ with the outer diameter the outer sleeve ranging from about 2 . 5 mm to 5 . 0 mm . referring to fig1 , 3 and 4 , the handle 115 comprises both a first grip portion 140 and a second actuator portion indicated at 142 . the grip portion 140 is coupled to the first sleeve 120 as will be described below . the actuator portion 142 is operatively coupled to the second sleeve 122 as will be described below . the actuator portion 142 is rotatable relative to the grip portion 140 and one or more plastic flex tabs 145 of the grip portion 140 are configured to engage notches 146 in the rotatable actuator portion 142 to provide tactile indication and temporary locking of the handle portions 140 and 142 in a certain degree of rotation . the flex tabs 145 thus engage and disengage with the notches 146 to permit ratcheting ( rotation and locking ) of the handle portions and the respective sleeve coupled thereto . the notches or slots in any of the sleeves can comprise a uniform width along the length of the working end or can comprise a varying width . alternatively , the width can be selected in certain areas to effectuate a particular curved profile . in other variation , the width can increase or decrease along the working end to create a curve having a varying radius . clearly , it is understood that any number of variations are within the scope of this disclosure . fig4 is a sectional view of the handle showing a mechanism for actuating the second inner sleeve 122 relative to the first outer sleeve 120 . the actuator portion 142 of the handle 115 is configured with a fast - lead helical groove indicated at 150 that cooperates with a protruding thread 149 of the grip portion 140 of the handle . thus , it can be understood that rotation of the actuation portion 142 will move this portion to the position indicated at 150 ( phantom view ). in one embodiment , when the actuator portion 142 is rotated a selected amount from about 45 ° to 720 °, or from about 90 ° to 360 °, the inner sleeve 122 is lifted proximally relative to the grip portion 140 and outer sleeve 120 to actuate the working end 110 . as can be seen in fig4 the actuator portion 142 engages flange 152 that is welded to the proximal end 132 of inner sleeve 122 . the flange 152 is lifted by means of a ball bearing assembly 154 disposed between the flange 152 and metal bearing surface 155 inserted into the grip portion 140 of the handle . thus , the rotation of actuator 142 can lift the inner sleeve 122 without creating torque on the inner sleeve . now turning to fig5 , 6 a and 6 b , it can be seen that the working end 110 of the extension member 105 is articulated by cooperating slotted portions of the distal portions of outer sleeve 120 and inner sleeve 122 that are both thus capable of bending in a substantially tight radius . the outer sleeve 120 has a plurality of slots or notches 162 therein that can be any slots that are perpendicular or angled relative to the axis of the sleeve . the inner sleeve 122 has a plurality of slots or notches indicated at 164 that can be on an opposite side of the assembly relative to the slots 162 in the outer sleeve 120 . the outer and inner sleeves are welded together at the distal region indicated at weld 160 . it thus can be understood that when inner sleeve 122 is translated in the proximal direction , the outer sleeve will be flexed as depicted in fig6 b . it can be understood that by rotating the actuator handle portion 142 a selected amount , the working end can be articulated to a selected degree . fig4 , 5 , 6 a and 6 b further illustrate another element of the apparatus that comprises a flexible flat wire member 170 with a proximal end 171 and flange 172 that is engages the proximal side of flange 152 of the inner sleeve 122 . at least the distal portion 174 of the flat wire member 170 is welded to the inner sleeve at weld 175 . this flat wire member thus provides a safety feature to retain the working end in the event that the inner sleeve fails at one of the slots 164 . another safety feature of the apparatus comprises a torque limiter and release system that allows the entire handle assembly 115 to freely rotate — for example if the working end 110 is articulated , as in fig6 b , when the physician rotates the handle and when the working end is engaged in strong cancellous bone . referring to fig4 , the grip portion 142 of the handle 115 engages a collar 180 that is fixed to a proximal end 124 of the outer sleeve 120 . the collar 180 further comprises notches 185 that are radially spaced about the collar and are engaged by a ball member 186 that is pushed by a spring 188 into notches 185 . at a selected force , for example a torque ranging from greater than about 0 . 5 inch * lbs but less that about 7 . 5 inch * lbs , 5 . 0 inch * lbs or 2 . 5 inch * lbs , the rotation of the handle 115 overcomes the predetermined limit . when the torque limiter assembly is in its locked position , the ball bearing 186 is forced into one of the notches 185 in the collar 180 . when too much torque is provided to the handle and outer sleeve , the ball bearing 186 disengages the notch 185 allowing the collar 180 to turn , and then reengages at the next notch , releasing anywhere from 0 . 5 inch * lbs to 7 . 5 inch * lbs of torque . referring to fig6 a and 6b , it can be understood that the inner sleeve 122 is weakened on one side at its distal portion so as to permit the inner sleeve 122 to bend in either direction but is limited by the location of the notches in the outer sleeve 120 . the curvature of any articulated configuration is controlled by the spacing of the notches as well as the distance between each notch peak . the inner sleeve 122 also has a beveled tip for entry through the cortical bone of a vertebral body . either the inner sleeve or outer sleeve can form the distal tip . referring to fig7 a - 7c , in one variation of use of the device , a physician taps or otherwise drives a stylet 200 and introducer sleeve 205 into a vertebral body 206 typically until the stylet tip 208 is within the anterior ⅓ of the vertebral body toward cortical bone 210 ( fig7 a ). thereafter , the stylet 200 is removed and the sleeve 205 is moved proximally ( fig7 b ). as can be seen in fig7 b , the tool or osteotome 100 is inserted through the introducer sleeve 205 and articulated in a series of steps as described above . the working end 110 can be articulated intermittently while applying driving forces and optionally rotational forces to the handle 115 to advance the working end through the cancellous bone 212 to create path or cavity 215 . the tool is then tapped to further drive the working end 110 to , toward or past the midline of the vertebra . the physician can alternatively articulate the working end 110 , and drive and rotate the working end further until imaging shows that the working end 100 has created a cavity 215 of an optimal configuration . thereafter , as depicted in fig7 c , the physician reverses the sequence and progressively straightens the working end 110 as the extension member is withdrawn from the vertebral body 206 . thereafter , the physician can insert a bone cement injector 220 into the path or cavity 215 created by osteotome 100 . fig7 c illustrates a bone cement 222 , for example a pmma cement , being injected from a bone cement source 225 . in another embodiment ( not shown ), the apparatus 100 can have a handle 115 with a luer fitting for coupling a bone cement syringe and the bone cement can be injected through the lumen 112 of the apparatus . in such an embodiment fig9 , the lumen can have a lubricious surface layer or polymeric lining 250 to insure least resistance to bone cement as it flows through the lumen . in one embodiment , the surface or lining 250 can be a fluorinated polymer such as teflon ® or polytetrafluroethylene ( ptfe ). other suitable fluoropolymer resins can be used such as fep and pfa . other materials also can be used such as fep ( fluorinated ethylenepropylene ), ectfe ( ethylenechlorotrifluoro - ethylene ), etfe , polyethylene , polyamide , pvdf , polyvinyl chloride and silicone . the scope of the invention can include providing a polymeric material having a static coefficient of friction of less than 0 . 5 , less than 0 . 2 or less than 0 . 1 . fig9 also shows the extension member or shaft 105 can be configured with an exterior flexible sleeve indicated at 255 . the flexible sleeve can be any commonly known biocompatible material , for example , the sleeve can comprise any of the materials described in the preceding paragraph . as also can be seen in fig9 , in one variation of the device 100 , the working end 110 can be configured to deflect over a length indicated at 260 in a substantially smooth curve . the degree of articulation of the working end 100 can be at least 45 °, 90 °, 135 ° or at least 180 ° as indicated at 265 ( fig9 ). in additional variations , the slots of the outer 120 and inner sleeves 120 can be varied to produce a device having a radius of curvature that varies among the length 260 of the device 100 . in another embodiment of the invention , the inner sleeve can be spring loaded relative the outer sleeve , in such a way as to allow the working end to straighten under a selected level of force when pulled in a linear direction . this feature allows the physician to withdraw the assembly from the vertebral body partly or completely without further rotation the actuating portion 142 of handle 115 . in some variations , the force - limiter can be provided to allow less than about 10 inch * lbs of force to be applied to bone . in another embodiment shown in fig8 , the working end 110 is configured with a tip 240 that deflects to the position indicated at 240 ′ when driven into bone . the tip 240 is coupled to the sleeve assembly by resilient member 242 , for example a flexible metal such as stainless steel or niti . it has been found that the flexing of the tip 240 causes its distal surface area to engage cancellous bone which can assist in deflecting the working end 110 as it is hammered into bone . in another embodiment of the invention ( not shown ), the actuator handle can include a secondary ( or optional ) mechanism for actuating the working end . the mechanism would include a hammer - able member with a ratchet such that each tap of the hammer would advance assembly and progressively actuate the working end into a curved configuration . a ratchet mechanism as known in the art would maintain the assembly in each of a plurality of articulated configurations . a release would be provided to allow for release of the ratchet to provide for straightening the extension member 105 for withdrawal from the vertebral body . fig1 and 11 illustrate another variation of a bone treatment device 400 with a handle 402 and extension member 405 extending to working end 410 having a similar construction to that fig1 to 6b . the device 400 operates as described previously with notched first ( outer ) sleeve 120 and cooperating notched second ( inner ) sleeve 122 . however , the variation shown in fig1 and 11 also includes a third concentric notched sleeve 420 , exterior to the first 120 and second 122 sleeves . the notches or slots in sleeve 420 at the working end 410 permit deflection of the sleeve as indicated at 265 in fig1 . fig1 also illustrates the treatment device 400 as including a luer fitting 412 that allows the device 402 to be coupled to a source of a filler material ( e . g ., a bone filler or bone cement material ). the luer can be removable from the handle 402 to allow application of an impact force on the handle as described above . moreover , the luer fitting 402 can be located on the actuating portion of the handle , the stationary part of the handle or even along the sleeve . in any case , variations of the device 400 permit coupling the filler material with a lumen extending through the sleeves ( or between adjacent sleeves ) to deposit filler material at the working end 410 . as shown by arrows 416 , filler material can be deposited through a distal end of the sleeves ( where the sharp tip is solid ) or can be deposited through openings in a side - wall of the sleeves . clearly , variations of this configuration are within the scope of those familiar in the field . in some variations , the third notched sleeve 420 is configured with its smooth ( non - notched ) surface 424 disposed to face inwardly on the articulated working end ( fig1 ) such that a solid surface forms the interior of the curved portion of the working end 410 . the smooth surface 424 allows withdrawal of the device 110 into a cannula or introducer 205 without creating a risk that the slots or notches become caught on a cannula 205 ( see e . g ., fig7 b ). as shown in fig1 - 11 , the third ( outermost ) sleeve 420 can extend from an intermediate location on the extension member 405 to a distal end of the working end 410 . however , variations of the device include the third sleeve 420 extending to the handle 402 . however , the third sleeve 420 is typically not coupled to the handle 402 so that any rotational force or torque generated by the handle 402 is not directly transmitted to the third sleeve 420 . in one variation , the third sleeve 420 is coupled to the second sleeve 120 at only one axial location . in the illustrated example shown in fig1 , the third sleeve 420 is affixed to second sleeve 420 by welds 428 at the distal end of the working end 410 . however , the welds or other attachment means ( e . g ., a pin , key / keyway , protrusion , etc .) can be located on a medial part of the sleeve 420 . the sleeve 420 can be fabricated of any bio - compatible material . for example , in one variation , the third sleeve is fabricated form a 3 . 00 mm diameter stainless steel material with a wall thickness of 0 . 007 ″. the first , second and third sleeves are sized to have dimensions to allow a sliding fit between the sleeves . fig1 a is a sectional view of extension member 405 of another variation , similar to that shown in fig1 - 11 . however , the variation depicted by fig1 a comprises non - round configurations of concentric slidable sleeves ( double or triple sleeve devices ). this configuration limits or prevents rotation between the sleeves and allows the physician to apply greater forces to the bone to create a cavity . while fig1 a illustrates an oval configuration , any non - round shape is within the scope of this disclosure . for example , the cross - sectional shape can comprise a square , polygonal , or other radially keyed configuration as shown in fig1 b and 12c . as shown in fig1 c the sleeves can include a key 407 and a receiving keyway 409 to prevent rotation but allow relative or axial sliding of the sleeves . the key can comprise any protrusion or member that slides within a receiving keyway . furthermore , the key can comprise a pin or any raised protrusion on an exterior or interior of a respective sleeve . in this illustration , only the first 122 and second 120 sleeves are illustrated . however , any of the sleeves can be configured with the key / keyway . preventing rotation between sleeves improves the ability to apply force to bone at the articulated working end . fig1 - 14 illustrate another variation of a working end 410 of an osteotome device . in this variation , the working end 410 includes one or more flat spring elements 450 , 460 a , 460 b , 460 c , 460 d , that prevent relative rotation of the sleeves of the assembly thus allowing greater rotational forces to be applied to cancellous bone from an articulated working end . the spring elements further urge the working end assembly into a linear configuration . to articulate the sleeves , a rotational force is applied to the handle as described above , once this rotational force is removed , the spring elements urge the working end into a linear configuration . as shown in fig1 , one or more of the spring elements can extend through the sleeves for affixing to a handle to prevent rotation . furthermore , the distal end 454 of flat spring element 450 is fixed to sleeve assembly by weld 455 . thus , the spring element is fixed at each end to prevent its rotation . alternate variations include one or more spring elements being affixed to the inner sleeve assembly at a medial section of the sleeve . as shown in fig1 - 14 , variations of the osteotome can include any number of spring elements 460 a - 460 d . these additional spring elements 460 a - 460 d can be welded at either a proximal or distal end thereof to an adjacent element or a sleeve to allow the element to function as a leaf spring . in an additional variation , the osteotome device can include one or more electrodes 310 , 312 as shown in fig1 . in this particular example , the device 300 includes spaced apart electrodes having opposite polarity to function in a bi - polar manner . however , the device can include a monopolar configuration . furthermore , one or more electrodes can be coupled to individual channels of a power supply so that the electrodes can be energized as needed . any variation of the device described above can be configured with one or more electrodes as described herein . fig1 illustrates an osteotome device 300 after being advanced into the body as discussed above . as shown by lines 315 representing current flow between electrodes , when required , the physician can conduct rf current between electrodes 310 and 312 to apply coagulative or ablative energy within the bone structure of the vertebral body ( or other hard tissue ). while fig1 illustrates rf current 315 flow between electrodes 310 and 312 , variations of the device can include a number of electrodes along the device to apply the proper therapeutic energy . furthermore , an electrode can be spaced from the end of the osteotome rather than being placed on the sharp tip as shown by electrode 310 . in some variations , the power supply is coupled to the inner sharp tip or other working end of the first sleeve . in those variations with only two sleeves , the second pole of the power supply is coupled with the second sleeve ( that is the exterior of the device ) to form a return electrode . however , in those variations having three sleeves , the power supply can alternatively be coupled with the third outer sleeve . in yet additional variations , the second and third sleeves can both function as return electrodes . however , in those devices that are monopolar , the return electrode will be placed outside of the body on a large area of skin fig1 to 20 illustrate another variation of an articulating probe or osteotome device 500 . in this variation , the device 500 includes a working end 505 that carries one or more rf electrodes that can be used to conduct current therethrough . accordingly , the device can be used to sense impedance of tissue , locate nerves , or simply apply electrosurgical energy to tissue to coagulate or ablate tissue . in one potential use , the device 500 can apply ablative energy to a tumor or other tissue within the vertebra as well as create a cavity . fig1 , 18 a , 18 b and 19 , illustrate a variation of the device 500 as having a handle portion 506 coupled to a shaft assembly 510 that extends along axis 512 to the articulating working end 505 . the articulating working end 505 can be actuatable as described above . in addition , fig1 shows that handle component 514 a can be rotated relative to handle component 514 b to cause relative axial movement between a first outer sleeve 520 and second inner sleeve 522 ( fig1 ) to cause the slotted working ends of the sleeve assembly to articulate as described above . the working end 505 of fig1 shows two sleeves 520 and 522 that are actuatable to articulate the working end , but it should be appreciated that a third outer articulating sleeve can be added as depicted above . in one variation , the articulating working end can articulate 90 ° by rotating handle component 514 a between ¼ turn and ¾ turn . the rotating handle component 514 a can include detents at various rotational positions to allow for controlled hammering of the working end into bone . for example , the detents can be located at every 45 ° rotation or can be located at any other rotational increment . fig1 depict an rf generator 530 a and rf controller 530 b connectable to an electrical connector 532 in the handle component 514 a with a plug connector indicated at 536 . the rf generator is of the type known in the art for electrosurgical ablation . the outer sleeve 520 comprises a first polarity electrode indicated at 540 a (+). however , any energy modality can be employed with the device . fig1 a and 18b illustrate yet another variation of a working end of a device for creating cavities in hard tissue . as shown , the device 500 can include a central extendable sleeve 550 with a sharp tip 552 that is axially extendable from passageway 554 of the assembly of first and second sleeves 520 and 522 ( fig1 ). the sleeve 550 can also include a second polarity electrode indicated at 540 b (−). clearly , the first and second electrodes will be electrically insulated from one another . in one variation , and as shown in fig1 , the sleeve assembly can carry a thin sleeve 555 or coating of an insulative polymer such as peek to electrically isolate the first polarity electrode 540 a (+) from the second polarity electrode 540 b (−). the electrode can be deployed by rotating knob 558 on the striking surface of handle component 514 a ( fig1 ). the degree of extension of central sleeve 550 can optionally be indicated by a slider tab 557 on the handle . in the illustrated variation , the slider tab is located on either side of handle component 514 a ( fig1 ). sleeve 550 can be configured to extend distally beyond the assembly of sleeves 520 and 522 a distance of about 5 to 15 mm . referring to fig1 , the central extendable sleeve 550 can have a series of slots in at least a distal portion thereof to allow it to bend in cooperation with the assembly of first and second sleeves 520 and 522 . in the embodiment shown in fig1 b , the central sleeve 550 can optionally include a distal portion that does not contain any slots . however , additional variations include slots on the distal portion of the sleeve . fig1 further depicts an electrically insulative collar 560 that extends length a to axially space apart the first polarity electrode 540 a (+) from the second polarity electrode 540 b (−). the axial length a can be from about 0 . 5 to 10 mm , and usually is from 1 to 5 mm . the collar can be a ceramic or temperature resistant polymer . fig1 also depicts a polymer sleeve 565 that extends through the lumen in the center of electrode sleeve 550 . the polymer sleeve 565 can provide saline infusion or other fluids to the working end and / or be used to aspirate from the working end when in use . the distal portion of sleeve 550 can include one or more ports 566 therein for delivering fluid or aspirating from the site . in all other respects , the osteotome system 500 can be driven into bone and articulated as described above . the electrodes 540 a and 540 b are operatively coupled to a radiofrequency generator as is known in the art for applying coagulative or ablative electrosurgical energy to tissue . in fig2 , it can be seen that rf current 575 is indicated in paths between electrodes 540 a and 540 b as shown by lines 575 . rf generator 530 a and controller 530 b for use with the devices described herein can include any number of power settings to control the size of targeted coagulation or ablation area . for example , the rf generator and controller can have low ( 5 watts ), medium ( 15 watts ) and high ( 25 watts ) power settings . the controller 530 b can have a control algorithm that monitors the temperature of the electrodes and changes the power input in order to maintain a constant temperature . at least one temperature sensing element ( e . g ., a thermocouple ) can be provided on various portions of the device . for example , and as shown in fig1 , a temperature sensing element 577 can be provided at the distal tip of sleeve 550 tip while a second temperature sensing element 578 can be provided proximal from the distal tip to provide temperature feedback to the operator to indicate the region of ablated tissue during the application of rf energy . in one example , the second temperature sensing element was located approximately 15 to 20 mm from the distal tip . fig2 illustrates another variation of articulating osteotome 600 with rf ablation features . variations of the illustrated osteotome 600 can be similar to the osteotome of fig1 - 18b . in this variation , the osteotome 600 has a handle 602 coupled to shaft assembly 610 as described above . the working end 610 again has an extendable assembly indicated at 615 in fig2 that can be extended by rotation of handle portion 622 relative to handle 602 . the osteotome can be articulated as described previously by rotating handle portion 620 relative to handle 602 . fig2 a - 22b are views of the working end 610 of fig2 in a first non - extended configuration ( fig2 a ) and a second extended configuration ( fig2 b ). as can be seen in fig2 a - 22b , the extension portion 615 comprises an axial shaft 624 together with a helical spring element 625 that is axially collapsible and extendible . in one embodiment , the shaft can be a tube member with ports 626 fluidly coupled to a lumen 628 therein . in some variations , the ports can carry a fluid to the working end or can aspirate fluid from the working end . in fig2 a - 22b , it can be seen that axial shaft 624 , helical spring element 625 together with sharp tip 630 comprise a first polarity electrode (+) coupled to electrical source 530 a and controller 530 b as described previously . an insulator 632 separates the helical spring 625 electrode from the more proximal portion of the sleeve which comprises opposing polarity electrode 640 (−). the rf electrodes can function as described above ( see fig2 ) to ablate tissue or otherwise deliver energy to tissue . in one variation , the extension portion 615 can extend from a collapsed spring length of 2 mm , 3 mm , 4 mm or 5 mm to an extended spring length of 6 mm , 7 mm , 8 mm , 9 mm 10 mm or more . in the working end embodiment 615 in fig2 b , the spring can comprise a flat rectangular wire that assists in centering the spring 625 about shaft 624 but still can collapse to short overall length , with the flat surfaces of rectangular wire oriented for stacking . however , other variations are within the scope of the variations described herein . the use of the spring 625 as an electrode provides significant improvements in delivering energy . this spring provides ( i ) greatly increased electrode surface area and ( ii ) a very greatly increased length of relatively sharp edges provided by the rectangular wire — which provides for edges . because the edges provide low surface area the concentration or density of rf current is greater at the edges and allows for theh rf current to jump or arc . both these aspects of the invention — increased electrode surface area and increased electrode edge length — allow for much more rapid tissue ablation . in one aspect of the invention , the surface area of the spring electrode 625 can be at least 40 mm 2 , at least 50 mm 2 , or at least 60 mm 2 over the spring electrode lengths described above . in another aspect of the invention , the total length of the 4 edges of rectangular wire spring can be greater than 50 mm , greater than 100 mm or greater than 150 mm over the spring electrode lengths described above . in one example used in testing , an osteotome 600 ( as in fig2 - 22b ) was configured with a helical spring that had a collapsed length of 1 . 8 mm and an extended length of 7 . 5 mm . in this embodiment , the surface area of the spring electrode 625 when extended was 64 . 24 mm 2 and the total length of the electrodes edges was 171 . 52 mm ( four edges at 42 . 88 mm per edge ). in a comparison test , a first osteotome without a helical electrode was compared against a second osteotome 600 with a helical electrode as in fig2 b . these devices were evaluated at different power levels and different energy delivery intervals to determine volume of ablation . the working ends of the devices had similar dimensions excepting for the helical spring electrode . referring to fig2 c , rf energy was delivered at a low power setting of 5 watts . it can be seen in fig2 c that at a treatment interval of 120 seconds and 5 w , the volume of ablation was about 3 times faster with the helical electrode compared to the working end without the helical electrode ( 1 . 29 cc vs . 0 . 44 cc ). another comparison test of the same first osteotome 500 ( fig1 b ) and second osteotome 600 with a helical electrode ( fig2 b ) were evaluated at higher 15 watt power level . as can be seen in fig2 d , rf energy at a treatment interval of 25 seconds and 15 w , the volume of ablation was again was about 3 times faster with the helical electrode compared to the working end without the helical electrode ( 1 . 00 cc vs . 0 . 37 cc ). referring to fig2 d , the device without the helical electrode impeded out before 60 seconds passed , so that data was not provided . the testing shows that the helical electrode is well suited for any type of tissue or tumor ablation , with a 60 second ablation resulting in 1 . 63 cc of ablated tissue . fig2 schematically illustrates the osteotome 600 in use in a vertebral body , wherein the rf current between the electrodes 625 and 640 ablate a tissue volume indicated at 640 . although particular embodiments of the present invention have been described above in detail , it will be understood that this description is merely for purposes of illustration and the above description of the invention is not exhaustive . specific features of the invention are shown in some drawings and not in others , and this is for convenience only and any feature may be combined with another in accordance with the invention . a number of variations and alternatives will be apparent to one having ordinary skills in the art . such alternatives and variations are intended to be included within the scope of the claims . particular features that are presented in dependent claims can be combined and fall within the scope of the invention . the invention also encompasses embodiments as if dependent claims were alternatively written in a multiple dependent claim format with reference to other independent claims .
0
the system arrangement of one preferred form of the invention is depicted in fig1 . that system includes a compressor 10 , a condenser 12 , and a combined evaporator and cold storage unit 14 . the compressor is driven by a compressor motor 16 the power for which is supplied from an external power source represented by the block 18 through a power controller 20 . the compressor 10 , condenser 12 , and the evaporator portion of the unit 14 are connected in series in a fluid circuit . the compressor delivers high - pressure gas refrigerant to the condenser 12 through a line 24 . the function of the condenser is to dissipate the heat in the compressed gas refrigerant and to deliver cool liquid refrigerant by capillary line 26 to the evaporator conduit 28 . the liquid is permitted to escape through an orifice or a metering valve . it expands and becomes a gas in the flow conduits 28 within the unit 14 . those conduits are represented by dashed lines . as the liquid expands to a gas in the evaporator conduits it draws heat from its surroundings , cooling them . in this invention , the conduit 28 is surrounded by a medium whose particular property is the ability to store cold . that medium may be any one of a number of well known substances and is called the &# 34 ; core &# 34 ; material . one example is salt water ; another is ethylene glycol solution . that cold storage medium is housed in an enclosure which , because of its design or its material , transfers heat into the storage medium , i . e . releases cold to the refrigerator space , at a relatively low rate until some special means is provided for increasing the rate of the heat input or cold output . thus it is that the cold storage portion of unit 14 has a special character and function . on the other hand , the compressor 10 , the condenser 12 , and the compressor motor 16 , and the evaporator element may have conventional design and , in this embodiment , do have conventional design . a means is employed by which to increase the rate of cold output from the cold storage portion of the unit 14 . in this embodiment , that means comprises a fan , or blower , 30 which , when operated , forces air to pass through an encompassing shroud 32 . the shroud surrounds the unit 14 . the shroud is fitted with a number of internal vanes , two of which have been numbered 34 for identification . those vanes are a preferred form of a means for causing the motion of air over the unit 14 to be turbulent so that there is a greater degree of contact between that air and the surface of the unit 14 . in this case , the vanes 34 , or at least most of them , do not actually engage the surface of unit 14 . they are not heat conduction fins . they are removed from significant heat conducting contact with unit 14 to avoid formation of ice at the junction between the fins and heat storage unit . the use of heat conduction fins is not foreclosed in the invention , but in this preferred embodiment they are not used . in this embodiment a resistance wire is applied to the outer surface of the unit 14 . it is arranged so that when energized it will melt quickly any frost which is in direct contact with its outer surface . the resistance wire is identified by the numeral 36 . the energization path for the heater extends through a transformer 37 to the power controller 20 . a means is provided for measuring the quantity of cold that is stored in the cold storage portion of unit 14 . since the storage material has a fixed volume and mass , the quantity of cold stored within it can be determined simply by measuring its temperature , and that is what is done in this preferred embodiment . the temperature sensor 40 is disposed in temperature sensing relation to the cold storage medium and supplies a signal which is indicative of temperature to the power controller 20 by sensor lines 42 . the fan , or blower , 30 is powered through power controller 20 and supply lines which include , in series , a switch 46 and a switch 44 whose operation is controlled by a temperature sensor 47 . that sensor senses the ambient air temperature within the refrigerator of which this system is a part , and it closes switch 44 when the ambient temperature rises above some preset level . the shroud 32 , the evaporator and cold storage unit 14 , the fan 30 , the temperature sensor and a door switch 46 are all enclosed in a cold box or enclosure which is represented in fig1 by the dashed line 50 . the enclosure includes a door 52 which affords access to the interior of the enclosure from its exterior . operation of that door operates the switch 46 . the exterior surface of a refrigerator may become sufficiently cold to condense moisture from the air in humid weather . it is common practice to include a heater element in the enclosure whose function is to heat the enclosure walls . operation of the heater is controlled by a moisture sensor . the unit of fig1 includes such a heater , case heater 38 , and a moisture sensor 94 . the power controller 20 of fig1 is shown in expanded form in fig2 together with some of the sensors , switches and other elements of fig1 . more particularly , the heater 36 and transformer 37 of fig1 is represented by the block labelled &# 34 ; evaporator heater &# 34 ; and numbered 36 . also shown in fig2 are the fan 30 , the door 52 , the door switch 46 , the compressor motor 16 , the ambient sensor 47 , and its switch 44 , the moisture sensor 97 , the case heater 38 , and the core temperature sensor which has an upper and lower limit . the remainder of the elements in fig2 form the power controller 20 . power is applied to lines p - 1 and p - 2 . that power is employed to operate clock 60 . the clock is connected to a source of battery power 62 which supplies power automatically in the event that no power is available at lines p - 1 and p - 2 . that source of battery power is effective to keep the clock running during periods of power outage and when the apparatus is being moved from one place to another or when , for any other reason , power is disconnected from the line . in preferred form , that battery is capable of running the clock for at least two years and has a shelf life approaching the expected useful life of the refrigerator . the function of the clock is to make power available for operating the compressor , motor , and any other element of the system whose operation is to be prevented at selected times . in the embodiment shown , only the compressor motor must be prevented as a function of time . to perform its function , the clock rotates cams . the cams actuate switches which control application of power to relay coils 72 and 74 . the cam set 64 in this embodiment is arranged to apply power to relay coil 72 at all times except during time interval beginning at time x and ending at time y . power is applied to relay coil 74 at all times except during inervals beginning at time w and ending at time x . in practice , the power controller might be a micro - processor as illustrated in fig3 but micro - processors do not lend themselves to diagrammatic representation in readily understandable form . for the sake of clarity , and to meet the obligation to describe the best embodiment and form , the functional operation of the micro - processor has been depicted in fig2 using symbols taken from the electro - magnetic controller art . given the diagram of fig2 it is well within the skill of workers in the computer arts to reproduce the functional equivalent in a micro - processor using the instruction sets published by the manufacturers of the selected micro - processor devices . in fig2 a relay coil 72 is included in the output line x - y . the relay coil 74 is included in the output line w - x . coil 74 operates normally open relay contact 78 . coil 72 operates normally open relay contact 80 . contact 80 is connected in a line that extends from line p - 1 to line p - 2 and which includes the compressor motor 16 , a relay coil 76 , and a normally open switch 82 which is operated at high limit temperature by the core temperature sensor 40 . switch 78 is connected in a line that extends between power lines p - 1 and p - 2 and which includes the compressor motor 16 and a normally closed switch 86 which is operated at the low limit temperature by temperature sensor 40 . finally , the compressor circuit includes a manual over - ride switch 110 which is connected in parallel with the switch 78 . the high limit section of the temperature sensor 40 also operates switch 111 which is connected in a line that extends from power line p - 1 to power line p - 2 and includes the blower or fan 30 and the door switch 46 . the fan or blower 30 and the door switch 46 are also connected in a second line that extends from power line p - 1 and p02 . that second line includes switch contacts 93 which are controlled by relay coil 92 , and it includes the switch 44 which , as previously described , is operated by an ambient temperature sensor 47 . a third line extends from power line p - 1 to power line p - 2 and includes a switch 95 operated by moisture sensor 97 and case ( enclosure ) heater 38 . the relay 92 is in series with a fourth line that extends from power line p - 1 to power line p - 2 . that line includes , in series , a switch 94 which is under the control of a frost sensor 96 and the evaporator heater 36 . the frost sensor includes a timer and is powered from lines p - 1 and p - 2 . it closes switch 94 when frost is sensed and keeps it closed for a fixed time . summarizing , the contro - ler controls five separate electrical control circuits . one of them includes the compressor motor 16 . that motor can be energized through the combination of time control switch 80 and core temperature sensor switch 82 and it can be energized through a time controlled switch 78 . a second circuit controls operation of the fan or blower 30 . it can be energized through either of two sub - circuits both of which include the make - break door switch 46 . one of those circuits includes ambient temperature switch 44 and a switch 90 by which fan operation is coordinated with heater operation . the other energizing circuit includes a switch 111 by which operation of the fan is coordinated with the core temperature sensor 40 . the third circuit includes the moisture sensor and case heater . the fourth circuit includes the frost sensor and evaporator heater , and the fifth controls the on time of the evaporator heater . the moisture sensor continuously senses the presence of moisture so that the case heater is energized only until the moisture is removed and is not energized if moisture is not present . the sensor is set to a predetermined level so that it will not energize the case heater until a certain level of moisture is present . it is desired to operate the evaporator heater only when the frost accumulation exceeds a prescribed amount so that frost sensor 96 is arranged to determine whether that amount of frost exists and to close switch 94 when it does . the circuit is arranged so that the blower will not operate while the heater is operating , and that is accomplished by an interlock between the two circuits . more specifically , when the heater is energized , the relay coil 92 will be energized , it opens switch 93 so that the ambient temperature switch 44 is ineffective to control fan operation . further , the circuit is arranged so that the evaporator heater will not operate when the compressor motor is energized , which is accomplished by an interlock between the two circuits . when the compressor is energized , the relay coil 76 is energized , opening switch 112 so that the frost sensor switch 94 is ineffective to control evaporator heater operation . the clock and cam set combination make it possible to prevent operation of the compressor motor during periods that represent high energy cost peak load periods of the public utility which supplies energy to the refrigeration system . that is done by using the clock to open switches 78 and 80 . the time when the compressor is prevented from operating by the opening of those switches is conveniently identified as the &# 34 ; peak load period ,&# 34 ; and is the period from x to y . it is a feature of this embodiment to provide assurance that the cold stored in the evaporator will be at its maximum immediately preceding a high cost peak load period when the compressor will normally be restricted from use . the relay 74 is arranged so that within the time period shown as w - x in fig2 ( typically one - half hour ) immediately prior to the beginning of a peak load period it will close switch 78 and permit energization of the compressor motor through switch 86 . the core temperature sensor 40 is arranged so that it will close switch 86 if the core temperature is higher ( warmer ) than minus 15 degrees . it is a further feature of this embodiment that the cold storage level of the evaporator be maintained separately from the requirement for cooling the air within the refrigerator compartment and that the storage level be maintained at a temperature range consistent with the most efficient operation intervals of the compressor and within prescribed limits during hours other than the peak load period . the core temperature sensor 40 is arranged so that at the high limit ( warmer ) core temperatures above zero degrees fahrenheit it will close switch 82 and open when the core temperature reaches the lower ( colder ) limit of minus 15 degrees . it is a further feature that the structural material of the evaporator provide for efficient low cost manufacture while at the same time providing for maximum retention of cold stored in the evaporator core material . in a preferred embodiment the structural evaporator material is plastic of a sanitary formulation readily formed by continuous extrusion , assuring manufacture at low cost . the plastic formulation selected has the further characteristic of high thermal conductivity at low temperatures . the family of polystyrenes are among the preferred formulations . in its arrangement of the evaporator in relation to its shroud and the internal vanes of the shroud , as shown in fig1 the preferred embodiment provides for restriction of air flow when the fan is off . this arrangement also restricts convection and assures the retention of cold through capturing and minimizing air flow when the door to the refrigerator compartment is opened . the greater heat transfer efficiency of the refrigerant circuit ( compressor to condenser to evaporator ) is captured and stored , thereby enabling the compressor to be restricted from operation during high energy cost periods , resulting in reduced cost of operation for refrigeration . a further advantage of the storage feature is that the compressor runs for a longer time per start , resulting in a total reduction in energy required for refrigeration due to the initial high energy use required to start electric motors . the less efficient heat transfer from the evaporator to the load through use of the air circuit is the subject of separate control . air , having low conductivity and poor thermal transfer , requires that its efficient use in refrigeration provide for the greatest cold saturation of the air as possible . cold saturation of the air medium through the turbulation of the air is achieved by means of vanes provided in the shroud and by an extended path of exposure provided by the maze created by the juxtapositioning of the vanes in the shroud . to maintain an efficient operation , frost must be removed from the cold storage unit . to perform that task efficiently requires the input of heat , and that is done by installing a full contact electric heater on the several working surfaces of the cold storage unit . the heater is arranged to melt frost rapidly while introducing a minimum amount of heat into the ambient air and the cold storage unit . this is accomplished with a limited use of energy as the frost accumulates directly on the heater surface , permitting direct melting through contact application of heat . a preferred method is to sense the presence of frost and turn the heater on only in those periods when the frost exceeds some predetermined amount and for a limited time for each on period . ordinarily , it is preferred that the heat exchange between the air and the cold storage unit be suspended at times when the heater is on . the logic scheme depicted in fig2 prevents the fan from operating when the heater is energized . to aid the understanding of the timing of the several events that make up system operation , reference is made to fig4 , and 6 . fig4 is a graph showing the time when it is permissible to use energy to operate the compressor motor in a representative situation . the graph assumes that the public utility which supplies energy for the refrigerator experiences its peak load in the period between time x and time y , and that occurs on regular working days but does not occur on holidays or weekends . accordingly , a combination of the clock 60 and programming element 64 is arranged so that it is possible to energize the compressor motor at any time on a holiday , at any time except during the high energy cost period during a working day , and at any time during a weekend day . fig5 assumes the use of a core temperature sensor with a high and low limit so that it is possible to measure a high core temperature , such , for example , as zero degrees ; and a low temperature , such , for example , as minus 15 degrees . it also assumes that the timer is capable of energizing line w - x in the period from time w to time x . fig5 shows that the compressor can be turned on in the time preceding time w when the core temperature is high . in the anticipatory interval , which is defined as the time between time w and time x , the compressor motor is energized if the core temperature is above the lower limit . finally , no use of the compressor motor is permissible in the interval from time x to time y . fig6 shows that fan operation is permissible if the ambient temperature is high . fig7 shows that the fan may be operated only when the heater is off . a wide variety of mechanical arrangements for the evaporator and the cold storage unit is possible . nonetheless , there are some preferred forms , and the best form thus far devised is depicted in fig8 and 9 . fig8 is an enlarged cross - sectional view of the shroud structure 32 and the combined evaporator and cold storage unit 14 that is depicted in fig1 . in a representative home refrigerator installation the shroud might measure 12 inches wide , four inches high and about 28 inches long . the shroud comprises an elongated tube , rectangular in cross - section and formed of metal or plastic . the upper and lower surfaces of the tube are fitted with a series of vanes that extend from the interior wall inwardly toward the unit 14 . they are placed only in that portion of the length of the rectangular tube over which the unit 14 extends . again , several of them have been marked with reference numeral 34 for identification . a fragment of that shroud is shown in fig9 . it comprises a side wall 150 and a lower wall 151 . the vanes 34 are arranged in rows that extend transversely across the width of the shroud . the vanes in this embodiment are formed by cutting away portions of a series of barrier walls each of which extends continuously across the shroud . openings in the barriers are spaced apart a distance of approximately equal to their width . alternate rows along the length of the shroud are arranged so that their openings are disposed at a position opposite the closed area of the vanes in the row ahead and the row behind . the effect is to create a longer path for air flow through the shroud and to render air flow very turbulent whereby the degree in which that air makes contact with the surface of the cold storage unit 14 is increased . as a consequence , the absorption of heat from the air to storage unit is accomplished more efficiently . in the absence of air being forced through the shroud , very little movement of air occurs within the shroud , and heat transfer is minimized and retained cold storage maximized . the unit 14 comprises a central elongated section 152 , an end connector section 154 at each end , and a covering plate 156 at each end . the central section is arranged as best depicted in fig9 . this unit is formed of plastic or metal , and it is arranged so that a number of through passages for the flow of refrigerant is formed . the space around those passages is filled with a cold storage medium . that space and the cold storage medium are called the &# 34 ; core .&# 34 ; the material of the medium has been omitted from the drawing for the sake of clarity . the end members 154 are attached to the respectively associated ends of the member 152 , and they serve to complete a connection from one channel to another so that all of the channels of the member 152 are connected in the series . thus , for example , the passageways 160 and 162 of member 152 are interconnected when the member 154 of fig9 is placed into engagement with end of member 152 . the connection from conduit 160 to conduit 162 is completed in element 164 . that element has an entrance opening 166 which mates with conduit 160 , and it has an exit opening 168 which mates with conduit 162 . those two openings are interconnected with the element 164 . when the end plate 156 is applied over the end of member 154 , that interconnecting channel is sealed . in like fashion , the end members 154 and the end plates 156 operate to complete the series connection of the several conduits . in this application , the members 152 , 154 and 156 are formed of a plastic material possessing the property of improved conductivity at lower temperatures . the efficiency with which heat is removed from the core , or , conversely , the efficiency with which cold is stored in the core , can be improved by forming the several conductors within member 152 of metal or other material that is a good conductor of heat . however , the efficiency of the cold storage process is sufficiently high to make it unnecessary to increase cost or to complicate construction of the unit by use of multiple materials . returning to the clock , for some applications it is preferred to use a digital clock including an oscillator , counters , comparitors and a rom in which are stored the times and dates for comparison with the count in the counters . the times and dates referred to define the times and dates when the compressor may be used and is not to be used . that is conveniently accomplished , as in business computer clocks , by using a julian calendar clock and defining days by julian day number and hours and minutes as conventional hours and minutes . there are many micro - processors capable of performing not only the clock functions but all of the control functions . the intel 8080a family of microcomputer devices is preferred now for several reasons . it is fully documented , there are several sources , it is familiar to many computer technicians and engineers , and it employs separate timer and clock devices . the latter is advantageous because they can be powered separately from a battery during shipping and moving and during utility power outages . the clock functions can be continued without need to supply power to the entire of the micro - processor whereby less battery power is required . the frost sensor function may be performed by a comparison of the actual operating rate of heat transfer achieved over a stated time interval of evaporator fan operation as measured by the ambient temperature sensor and counted by the clock , against a standard of performance representing heat transfer effect during a similar time period on the ambient sensor when the evaporator is defrosted . an unfavorable comparison of actual performance to standard will in that practice initiate a command to energize the defrost heater . to form the micro - processor , an 8080a central computing unit , an 8224 system clock generator and drive and an 8228 system controller are combined with an 8253 programmable timer and an 8255 parallel i / o and an 8259 priority interrupt control . these are connected as described in the intel corporation documentation to drive switches either electromechanically as shown in fig2 or equivalent solid state switches in the arrangement depicted in fig3 . whether it be the intel 8080a family or another , it is a feature of the invention to put the time - on / time - off data in a memory device that is attachable to the unit . similarly , the minimum - run - time - per - start - feature will be incorporated in the memory device . the programmable memory device feature , whether in a rom or in an electromechanical cam set , makes it possible to manufacture the unit complete except for loading of the memory device without regard to its ultimate destination . the data that is loaded into memory is to be defined by the utility which serves the area in which the refrigerator is installed . the memory unit can be loaded by the retail seller or by the utility company or the utility company may elect to furnish pre - loaded memory units . that feature makes the invention very practical , and it makes it possible for the advantages offered by the invention to be made available to users and to energy suppliers without any major change in selling or business procedures . in fig2 it is the cam unit 64 that is the memory device that contains the compressor off - time program specified by the utility company . like the read - only memory unit or rom described above , it may be different for each utility company service area . in this embodiment , like the rom , it is replaceable . cams 200 and 201 are seven - day cams , one to interrupt power in the x - y period on week days and the other 201 to interrupt power in the w - x period on week days . cam 203 is a daylight savings time cam driven through a gear box 204 and cam 205 is a holiday gear driven through a gear box 206 which includes both a speed reducer and a leap year geneva gear . gear 203 controls the flow of energy in series with gears 201 and 200 to relay coils 74 and 72 , respectively . gear 205 supplies energy directly to the relay coils on holidays . although we have shown and described certain specific embodiments of our invention , we are fully aware that many modifications thereof are possible . our invention , therefore , is not to be restricted except insofar as is necessitated by the prior art .
8
accordingly , in the embodiments of this invention , a p - type & lt ; 100 & gt ; oriented silicon substrate ( wafer ) is provided . the embodiments use , as an example , an integrated circuit process for the manufacture of cmos devices . it is to be understood that the application of this invention is not confined to cmos integrated circuits but could be applied to any semiconductor fabrication process . referring to fig3 semiconductor devices are formed within the surface of a silicon wafer 10 in a pattern consisting of an array of rectangular integrated circuit dice 62 . test structures of various kinds are simultaneously formed in the narrow regions 60 between the dice 62 which comprise the kerf area . this is the region that will be consumed by a saw cut which separates the dice at the completion of processing . among these test structures are those designed for inspection of dimensional and structural integrity with an sem . in the first and second embodiments there will be discussed , those structures which have direct conductive paths to the silicon substrate ground for the purpose of draining away charge from the electron beam . the conductive path for the first embodiment passes through a conventional metal contact while in the second embodiment , a polysilicon buried contact is employed . a third embodiment incorporates the use of pseudo - grounded discharge paths formed by means of large area conductive attachments to the conductive regions to be inspected . these attachments provide a means to spread out the charge while the inspection takes place and thereby lowering the charge in the region of interest . the fourth and fifth embodiments address the inspection of contact openings . after the wafer has undergone all processing steps preceding and including the growth of gate oxide , the processing of the inspection test sites within the kerf area is begun . thus field oxide isolation regions and other ion implants or diffusions as , for example , n - wells or p - wells are in place . the photomask set must have been designed to mask the growth of isolation oxide and any implants or diffusions within the kerf area allotted for the test structures except for an implant which reinforces the conductivity type of the substrate material . the first embodiment , shown in cross section in fig4 a , is a contact opening which , in the integrated circuit , would be insulated from substrate ground by a p - n junction . designed as a special structure for sem inspection without a subjacent p - n junction , the base of the contact opening 14 in the interlevel - dielectric ( ild ) layer 12 forms an unhampered conductive path to the sem ground 8 via the substrate 10 . a boron implant 11 in the test structure reinforces the surface conductivity of the silicon at the contact assuring the absence of carrier depletion at the silicon interface . the surface of the ild layer 12 can accumulate some surface charge , especially if the sem is operated at high potentials to achieve high resolution or if the inspection time is too long . with judicious procedure , this charging can be moderated sufficiently to allow ample contour inspection . the elimination of charging in the base of the contact 14 by eliminating the p - n junction reveals pits and debris which would otherwise be obscured . after sem inspection , the test structure shown in fig4 a is processed further and used as the inspection structure for the next level opening which in this embodiment is a via opening shown in fig4 b . the contact opening is filled with conductive material 16 such as is used for tungsten plug metallurgy and a patterned layer of first metal 18 is formed over the ild layer . sem inspection and measurement of the metal pattern features are then performed . again , the discharge path provided by the test structure permits inspection and measurement without image distortion due to charging . the pattern dimensions incorporated into the metal 18 in the test structure are representative of those found in the accompanying integrated circuit . the via opening 22 is etched into the insulating layer 20 at which point sem inspection is again performed to verify dimensional and structural compliance of the via opening . the electron discharge path of the contact opening 14 is now extended to the via opening 22 through the contact 16 and first metal layer 18 . further extension of this grounding concept to via openings and metal patterns in higher levels of metallization should now be apparent . an advantage of this scheme is that each successive level of inspection can focus on the same structures thereby minimizing the number of required inspection sites required . a second embodiment of this invention is shown in fig5 a and 5b . as in the first embodiment a p - type & lt ; 100 & gt ; oriented silicon substrate is provided . the embodiment uses as an example , an integrated circuit process for the manufacture of cmos devices . semiconductor devices are formed within the surface of the silicon wafer in a pattern consisting of an array of rectangular integrated circuit dice . test structures are formed in the narrow regions 60 between the dice 62 which comprises the kerf area ( fig3 ). referring to fig5 a , there is shown a substrate 10 grounded to the sem by a connection 8 . the inspection test site contains no p - n junctions and the surface conductivity is reinforced by an implanted layer 11 . a buried contact opening 36 is formed within the gate oxide layer 30 . typically , when buried contacts are used , the gate oxide over the device area is first covered by a thin layer of polysilicon 32 and the buried contact opening 36 is then formed by etching through both layer 32 and the gate oxide 30 as shown in the figure . at this point the critical dimensions and the integrity of the buried contact opening 36 are validated by sem inspection . electrons from the beam are discharged during the inspection by the conductive path through the wafer 10 to the ground 8 permitting a crisp and undistorted image . a polysilicon layer 34 is next deposited and patterned over the buried contact . the polysilicon gates and buried contact conductors in the integrated circuit dice are subsequently patterned in this layer and the subjacent layer 32 . the test structure pattern 34 contains polysilicon lines whose widths correspond to those found in the product dice . fig5 c shows an example of the top view of the polysilicon pattern 34 . the sem inspections of this pattern permits measurements of line widths corresponding to gates t g and buried contact stripes t bc . referring also to fig5 b , further processing of these test structures wherein an insulator 38 with a via opening 40 has been formed , now permits sem inspection and measurement of this via opening 40 with the benefit of a conductive path to ground through the buried contact 36 . this via might , for example , represent the contact of a load resistor formed in a second polysilicon layer to a gate electrode formed in a first polysilicon layer . such a configuration can be found in poly - load sram cells . the top view of the test structure in fig5 c shows this via opening 40 as well as the location of the buried contact 36 . as in the first embodiment the conductive path provided in the second embodiment may be propagated through higher levels of metallization for other sem inspections . a third embodiment of this invention consists of a metal test pattern lying over an insulated surface wherein the portion to be inspected for dimensional compliance is attached to a larger region of metal as shown in fig6 . the conductive structure 70 contains a portion 74 which has the dimensions of corresponding features in the product dice which is attached to a large area of conductor 72 . the presence of the area 72 permits the spreading out of the sem charge build - up over a large area , thereby minimizing image distortion by reducing the charge in the region of interest . the effectiveness of these structures depends upon the area of the conductive ballast 72 . a fourth embodiment of this invention is illustrated by fig7 and 8 . in fig7 there is shown a cross section of a test structure having a plurality of contact openings designated by l , m , n , o , and p . the substrate 10 is p - type and is grounded to the sem at the connection 8 . alternate openings l , n , and p are formed over n + regions in the substrate , while the openings m and o are formed over p + regions . the contact openings are formed in the insulative layer 82 by reactive - ion - etching . if the contact openings are properly exposed by the rie , charging occurs in openings l , n , and p because the p - n junction prevents electron flow to ground . the exposed silicon surfaces in openings m and o , however , are grounded through the p + region and therefore do not become charged . the appearance of this test structure with properly opened contacts is shown in fig8 a . the alternating shades along the row of contacts can be easily recognized and interpreted . residual insulating layer within the contact openings will not allow proper electron discharge and the row of contacts appear with equal shades as shown in fig8 b . partially open contacts display slight but easily discernable variations in tone . whereas the fourth embodiment is a test structure designed to examine contact openings for completeness of insulator etching , a fifth embodiment is next described which utilizes the same principle as the fourth embodiment to inspect contact openings having a metal silicide layer over the silicon at their base . such contacts are encountered in integrated circuits utilizing the self - aligned silicide ( salicide ) process . see for example wolf , s .,&# 34 ; silicon processing for the vlsi era &# 34 ;, vol . 2 , lattice press , sunset beach , calif ., vol . 3 ( 1990 ), p144ff . the test structure is shown in cross section in fig9 . the silicide layer 84 , frequently tisi 2 , is formed over the silicon surface by depositing the metal and annealing to form the silicide . the insulative layer 82 has the contact openings designated by l , m , n , o , and p . the substrate 10 is p - type and is grounded to the sem at the connection 8 . alternate openings l , n , and p are formed over n + regions in the substrate , while the openings m and o are formed over p + regions . the contact openings are formed in the insulative layer 82 by reactive - ion - etching . when examined in the sem , all the openings appear of equal shade if the etching step terminated within the silicide layer 84 as illustrated by fig1 a . this layer 84 is grounded through contact with the p + regions and through the substrate contact 8 . if the silicide layer has been penetrated by the etchant , differences in contrast are observed between the n + and p + contact openings as illustrated by fig1 b . partially penetrated silicide layers display slight but easily discernable variations in tone . by using a string of contacts with alternating n - and p - regions as illustrated for the fourth and fifth embodiments by fig7 and 9 , even slight differences in sem charging can easily be resolved . while this invention has been particularly shown and described with reference to the preferred embodiments thereof , it will be understood by those skilled in the art that various changes in form and details may be made without departing from the spirit and scope of the invention . while the embodiments of this invention utilize a p - type silicon substrate , an n - type silicon substrate could also be used without departing from the concepts therein provided . it should be further understood that the substrate conductivity type as referred to herein does not necessarily refer to the conductivity of the starting wafer but could also be the conductivity of a diffused region within a wafer wherein the semiconductor devices are incorporated .
7
before explaining the invention in detail , it is to be understood that the invention is not limited in its application to the detail of construction and arrangement of parts illustrated in the drawings since the invention is capable of other embodiments and of being practiced or carried out in various ways . it is also to be understood that the phraseology or terminology employed is for the purpose of description only and not of limitation . referring to fig1 - 6 , passenger car 16 includes flexible front and back decorative bumper covers 17 over front bumper system 20 and rear bumper system 21 . cover 17 is shown in cross section , and only in fig1 and 2 . on each of the front and back bumpers , inflatable bag 30 is held in steel insert shell 40 by a pair of longitudinal ribs 32 which extend into the recesses 38 of longitudinal channels 56 of the shell . inflatable bag 30 is pressurized by way of valve 34 so than when the inflatable bag is fully expanded it is locked into the shell by the ribs in the recesses . impact support beam 44 is attached to insert shell 40 by bolts 62 in two reinforcement plates 42 in the front bumper system . in the rear bumper system impact support beam 45 , which is shorter than impact support beam 44 , is attached to insert shell 40 by bolts 70 in two reinforcement plates 42 . the reinforcement plates are designed to bolt to shock absorbers 58 which presently support vehicle bumpers , so that aftermarket replacement of a stock bumper on a vehicle with the invention is a simple matter of unbolting the stock bumpers from the shock absorber and bolting on the invention . reinforcement plates 42 are welded to insert shell 40 , but may be bolted to the shell . if bolting is used , the inner side of the shell may be recessed to receive the bolt head or a nut so that the head or nut will not damage the inflatable bag . alternatively , as shown in fig6 , and 8 , impact support beam 44 may be attached to the back 52 of insert shell 40 by two reinforcement plates 42 which are spot welded 78 to the front 80 of the beam and the back of the shell . threaded attachment means 86 are provided on the back of the reinforcement plates . alternatively , impact support beam 44 may be connected , bolted , or welded to the insert shell without direct attachment to reinforcement plates 42 . this is done , for example by making the impact support beam shorter than the distance between the reinforcement plates , or making clearance openings in the impact support beam in order to clear the reinforcement plates , or by a vertical displacement between the impact support beam and the reinforcement plates . lightening holes 84 are included in support beam 44 to reduce weight . rear bumper system 21 further includes on each side of the car , a load transfer element such as wheel 50 . wheel 50 is mounted on bracket 66 which is attached to reinforcement plate 42 by bolts 70 . transfer wheel 50 is mounted on a rim 54 that is free to rotate on bearing 74 . fig9 - 11 , inflatable bag 30 comprises a hollow elongated tube preferably made from reinforced rubber having the strength and durability of rubber used in the walls of car and truck tires . bolts 36 are molded into solid ends 28 of the inflatable bag , and attach the inflatable bag to insert shell 40 as shown in fig3 and 4 . mounting the bumper system on a new vehicle , is quick and easy . at the front of the vehicle , bumper system 20 is attached to the shock absorbers by running bolts through shock absorber flanges 92 , impact support beam 44 , and reinforcement plate 42 . insert shell 40 is u - shaped so that it wraps around the front of the vehicle . this provides very good impact protection against oblique hits on the vehicle , and provides support for a wrap around cover 17 for aesthetic value . after insert shell 40 is installed on the vehicle , a deflated inflatable bag is installed in the concave front of the shell by setting it in the concavity and bolting it 36 to ends 94 of the insert shell . then the inflatable bag is inflated by way of valve 34 until the ribs 32 are forced outward into the recess 38 of the longitudinal channels 56 . the ribs and recesses may be designed so that once they engage they interlock like the bead in a good tire , so that the inflatable bag is not dislodged by impacts . for this , the ribs may be solid , preferably rubber or elastomeric . the same procedure is applied to mounting bumper system 21 at the rear of the vehicle , except that two brackets 66 for two transfer wheels 50 are also mounted on the back of the insert shell . advantages and benefits of the invention may also be provided for the side of a vehicle by bolting a straight insert shell to the side of the car . the impact support beam is curved so that it provides back - up support for insert shell 40 . when inflated bag 30 receives a localized impact normal to the length of the bag , the energy of impact is spread lengthwise in the fluid in the bag , and absorbed over the larger area of the walls of the bag and the wall of the insert shell . the fluid may be a compressible fluid such as air or other gas , and the bag may be made with elastic walls such as rubber , so that the energy of impact is absorbed by the fluid and the walls of the bag . if the impact falls to the left or right of a reinforcement plate , the insert shell may spring back toward the impact support beam which provides further support against the force of the impact , and keeps the insert shell from twisting . the insert shell may also be made flexible enough to expand backwards under expanding force from the impacted inflatable bag until it is received by a stiffer impact support beam . in the rear bumper system , fig4 the transfer wheel 50 is spaced from adjacent rear wheel 68 of car 16 , that is inward on the car with respect to the rear insert shell . axis 60 of the transfer wheel is parallel with axis 64 of the car &# 39 ; s wheel . the transfer wheel engages the rear wheel of the car when the portion of the insert shell to which the rear wheel is attached , moves inward on the car . as the transfer wheel is under the car , generally out of sight , and inconvenient to reach to pressurize by pumping , the transfer wheel tire 72 is preferably a solid rubber or elastomeric material , such as a foam rubber requiring no maintenance or pumping . any rotatable element may be used in place of a wheel for transfer wheel 50 , such as a large ball , which is free to rotate on axis 60 . alternatively to installing the transfer wheel assembly on the rear bumper system , a front bumper system which has the wider impact beam may also be installed at the rear of the vehicle . installation of the invention on a vehicle is not limited to attachment to shock absorbers , nor are they required for operation of the invention . it is practical , however , to attach the invention to existing shock absorbers for ease of installation and for the added shock protection that they provide . the insert shell and impact support beam may be designed to ultimately crush and sacrifice under high impact in order to provide further protection for the passengers and vehicle . the bumper system is inexpensive to manufacture . the insert shell , impact support beams , reinforcement plates and brackets may be made of stamped and welded steel , and the inflatable bag and free wheels may be made from recycled elastomeric materials such as rubber tires . from the foregoing , it is seen that with the present invention installed on a vehicle , the vehicle and passengers are protected from injury by shock and crushing , and from cost by collapsing of portions of the vehicle , by a bumper system which has many stages of protection . for example , the bumper system spreads the force of impact sideways where much of the force is absorbed along the length and radially in all directions by the inflatable bag . additional absorption of the force is taken radially by the insert shell along the length of the insert shell . further absorption is taken by expansion of the insert shell , and further by movement of the shell to the impact support beam which adds further protection . at the back of the vehicle , further protection is provided by absorption of energy in the free wheels and the rear wheels of the vehicle , wherein that energy may have overwhelmed the inflatable bag , insert shell , and impact support beam . although the present invention has been described with respect to details of certain embodiments thereof , it is not intended that such details be limitations upon the scope of the invention . it will be obvious to those skilled in the art that various modifications and substitutions may be made without departing from the spirit and scope of the invention as set forth in the following claims .
1
reference will now be made in detail to one or more embodiments of the invention , one or more examples of which are shown in the drawings . each example is provided by way of explanation of the invention , and not meant as a limitation of the invention . it is intended that the invention include modifications and variations to the embodiments illustrated and described herein . fig1 shows a first exemplary embodiment of waste - water installation 1 in accordance with the invention in a schematic , sectional view . waste - water installation 1 comprises inflow side 11 and outflow side 12 that are arranged in a so - called relief basin . inflow side 11 and outflow side 12 are separated from one another by intermediate wall 14 . a cleaning device 2 is arranged on the top of intermediate wall 14 on its bottom area 15 . inflow side 11 is connected to an inflow line ( not shown ) via which rainwater is delivered , e . g ., during heavy rain events to waste - water installation 1 . the rainwater is mixed thereby without separation with normal waste water and delivered to waste - water installation 1 . in the normal instance , the water supplied to inflow side 11 , that is , during dry periods and light rainfalls , is conducted out of inflow side 11 to waste - water installation 1 via a conduit connection ( not shown ) into a sewage treatment plant . inflow side 11 of relief basin 13 can additionally communicate with a retention basin that assures an at least partial intermediate storage for the increased accumulation of water to be cleaned so that as much of the water as possible supplied via the inflow side of waste - water installation 1 can be delivered to the sewage treatment plant . the retention basin also assures that the accumulation of water to be cleaned in the sewage treatment plant is stretched out in time . however , if the amount of accumulating water is so great , e . g ., during a heavy rain event , that it can not be received by the retention basin and by inflow side 11 of waste - water installation 1 , the liquid level in inflow side 11 rises at first until it reaches level n 1 of bottom area 15 of intermediate wall 14 . a further rise of the liquid on inflow side 11 would , without further measures , have the result that water would pass by the sewage treatment plant into the area of outflow side 12 of waste - water installation 1 , from where this water is then discharged , e . g ., into a natural body of water . however , in order to avoid that non - cleaned water passes , e . g ., into a natural body of water , cleaning device 2 is arranged between inflow side 11 and outflow side 12 . this cleaning device is designed in the exemplary embodiment of fig1 as sieve rake 22 , that is capable in a known manner , with rake rods 23 running in parallel and horizontally arranged , of retaining dirt components out of the water flowing through it . in order that sieve rake does not clog up , cleaning device 2 comprises rake cleaner 24 , shown only schematically in fig1 , with the aid of which the intermediate spaces between rake rods 23 are continuously cleaned and dirt components deposited in front of the rake are removed . in one exemplary embodiment , as shown in fig1 , the dirt removed by rake cleaner 24 from the sieve rake is returned into the waste water located in inflow side 11 since if the water in waste - water installation 1 recedes , this dirt can then be removed by the normal cleaning by the sewage treatment plant . in addition to cleaning device 2 , it is also known in the state of the art that a damming element 3 can be provided in the direction of flowthrough after sieve rake 22 , that is , between cleaning device 2 and outflow side 12 , which damming element 3 is supposed to increase the amount of water retained at first by further damming so that as little water as possible is removed from a cleaning action by the sewage treatment plant . fig1 shows a damming element 3 in accordance with the present invention . damming element 3 is capable of damming the backup level of the liquid in inflow side 11 above level n 1 backed up by intermediate wall 14 up to level n 2 located above level n 1 . without the use of a damming element in accordance with the invention , still no water would pass onto outflow side 12 at damming level n 2 , that corresponds to the level of damming element 3 in fig1 . however , according to the present invention , damming element 3 is mounted so that it can move in such a manner that it executes , effected by the forces of the backup pressure by liquid level n 2 , a pivoting motion about shaft 7 . during this time , partial surface 32 of damming element 3 pivots away from cleaning device 2 , thus freeing the area between shaft 7 and bottom area 15 . the open position of damming element 3 is shown in dotted lines in fig1 . the folding back in accordance with the invention of partial surface 32 of damming element 3 brings it about that in the area of bottom area 15 water flows over bottom area 15 at a high rate , thus cleaning bottom area 15 . the water flowing underneath shaft 7 passes to outflow side 12 of waste - water installation 1 and leaves it in the direction of , e . g ., a natural body of water . the designing of damming element 3 as a multi - part damming element brings it about that the part of the damming element located above shaft 7 continues to dam the water located on the inflow side . as a result , the water on inflow side 11 can continue to be retained for the most part , and nevertheless , due to the designing in accordance with the invention of damming element 3 , a current can be produced in the area of bottom area 15 that cleans bottom area 15 of deposits such as , e . g ., sand , so that these deposits do not cause any problems in the area of the sieve rake , e . g ., during the cooperation of sieve rake 22 with rack cleaner 24 . basically , the attempt is made to operate the waste - water installation in such a manner that all the accumulating water is removed to the extent possible by the conduit line ( not shown ) from the area of inflow side 11 in order to clean it in a sewage treatment plant . consequently , damming element 3 and / or its partial surface 32 is / are advantageously designed so that an opening of the damming element only takes place when an overflowing of damming element 3 on its upper edge 36 takes place in any case by the great accumulation of water on inflow side 11 . in order to bring this about , partial surface 32 of damming element 3 can be pre - tensioned with a spring ( not shown ) in such a manner that the water pressure only succeeds in pivoting partial surface 32 about shaft 7 when a sufficient dammed pressure of the water is present , that is , when the liquid level n 2 has been practically reached . in addition to loading damming element 3 with a spring , it is also possible to assure by skillful distributions of mass on partial surface 32 of damming element 3 , which partial surface is located under shaft 7 , that a moment is exerted on this partial surface 32 so that it rests in a sealing manner on stop 16 . a further elevation of the water level on inflow side 11 , e . g ., up to over level n 2 , would then be capable , given the appropriate shaping of the forces acting on partial surface 32 , to pivot this partial surface and free therewith the flowthrough of water . damming element 3 shown in fig1 is designed in the area of its partial surface 32 as a flap that can pivot about shaft 7 , and with the aid of which the effects intended by the invention can be achieved . in addition to a flap pivotable about shaft 7 , it is just as possible , in an especially advantageous manner , to design partial surface 32 as an elastically deformable structural component , e . g ., in the form of a sealing lip capable by virtue of its deformation of effecting the release of the flowthrough of the liquid in the area of bottom area 15 . given a rather low liquid pressure on the elastically deformable structural component , its deformational return forces bring it about that it rests in a sealing manner on stop 16 of waste - water installation 1 so that this installation can retain a rather large ( greater ) amount of water on inflow side 11 with the aid of its damming element 3 before this water must be discharged into , e . g ., a natural body of water . the impurities of the water that accumulate in waste - water installation 1 and pass with the rainwater and the waste water mixed with it into the area of inflow side 11 are retained in a known manner by cleaning device 2 when the water in waste - water installation 1 passes from inflow side 11 directly to outflow side 12 . cleaning device 2 is designed as sieve rake 22 and consists substantially of rake rods arranged superposed horizontally , e . g ., with a slot width between the rake rods of 3 mm to 11 mm . sieve rake 22 comprises rake cleaner 24 for keeping the intermediate spaces between the individual rake rods free from the dirt particles pressed on the inflow side of the rake in the area of the rake rods by the flow of the liquid . this rake cleaner is designed to be movable and is arranged on the side of sieve rake 22 facing outflow side 12 . rake cleaner 24 travels for cleaning along sieve rake 22 and engages thereby with cleaning elements into the intermediate spaces between rake rods 23 . the intermediate space between rake rods 22 is filled thereby with cleaning elements 22 of rake cleaner 24 so that dirt components located there , e . g ., grains of sand , substantially aggravate the movement of the rake cleaner and can result in wear to the rake rods and especially to the cleaning elements of rake cleaner 24 , depending of the hardness of the dirt components . this is especially critical in the area of the components of cleaning device 2 located in the vicinity of bottom area 15 . suspended particles settle with preference on the latter , especially when the water level on inflow side 11 is only slightly higher than level n 1 up to a water level in the range of n 2 , since up to that point no flow can take place in the area between damming element 3 and cleaning device 2 . moving rake cleaner 24 back and forth will then always stir up just enough of the sinking material that its damaging influence can be tolerated since it passes thereby into the range of the rake cleaner . in addition to the positive effects of a waste - water installation 1 in accordance with the invention as shown in fig1 with its damming element 3 , the present invention has the further advantage that in the event of a heavy rain with a large accumulation of dirty water on inflow side 11 , the flowthrough of the oncoming water through sieve rake 22 is distributed over its entire surface if , in such an event , damming element 3 frees the flowthrough , even if only partially as in the exemplary embodiment of fig1 , and to a particular extent if a damming element like the one shown in fig2 is used . this brings it about that the liquid flowing through the rake is distributed over its entire height so that the passage rate is uniformly the same over the entire height of cleaning device 2 . this achieves an especially advantageous action of cleaning device 2 . fig2 shows a schematic view of a section through waste - water installation 1 similar to fig1 ; however , only the area of the intermediate wall , bottom area 15 and a partial area of cleaning device 2 are shown . sieve rake 22 arranged on intermediate wall 14 , which rake is also associated with a rake cleaner 24 , is followed by damming element 3 in flowthrough direction f . damming element 3 is designed in the exemplary embodiment of fig2 as damming flap 36 that can pivot about shaft 7 . damming flap 36 is shown in its position that it assumes when liquid flows in flowthrough direction f , that is , a state in which damming element 3 has changed following the damming pressure of the backed - up water from a closed position into a flowthrough position . the closed position of damming flap 36 is sketched with an interrupted line from which it is clear that damming element 3 consists in the exemplary design of fig2 of two partial surfaces 32 , 320 separated from one another by shaft 7 . partial surface 32 shown above shaft 7 has a greater height and therewith also greater surface than partial surface 320 arranged below shaft 7 . this geometric shape has the effect that at a liquid level with level n 21 the forces act on the two partial surfaces 32 , 320 in such a manner that a torque acts around shaft 7 so that partial surface 320 located beneath shaft 7 is pressed away from sieve rake 22 and rests sealingly on stop 16 formed in the area of bottom area 15 . if the liquid rises further , the force acting on upper partial surface 32 becomes greater and greater until it is capable of rotating damming flap 36 clockwise about shaft 7 . as a result thereof , damming element 3 of fig2 frees the flowthrough in a practically unhindered manner so that practically no more damming action is effected . in order that damming flap 36 retains its open position , as shown in fig2 with an uninterrupted line , in such an instance , even if the water level drops , the damming flap comprises guide device 35 on its partial surface arranged below shaft 7 which guide device directs the force of the liquid flowing by in such a manner onto damming flap 36 that the latter remains in the open position even if the liquid level has already dropped down to approximately the level of shaft 7 . fig3 shows a diagrammatic view similar to that of fig2 but with a damming element 3 that consists of two partial surfaces 32 , 320 pivotably mounted about horizontal shaft 7 running between them . in order to form an effective damming element , several of flap elements 37 shown in fig3 are arranged along the back side of cleaning device 2 . the individual flap elements forming damming element 3 comprise an articulating lever ( not shown ) with which they can be pivoted , e . g ., via a control rod from the open position into the closed position . the drive energy necessary for this can be generated , e . g ., by a suitable power transfer means via the backed - up water or via the flowing water . however , it is also advantageously possible in addition to move flap elements 37 from the open position into the closed position and vice versa via , e . g ., a hydraulic system or an electromotor . this design of the damming element has the advantage that only relatively low forces are required to move the flap elements , independently of the water level . fig4 shows another advantageous exemplary embodiment of the present invention in which a multi - part damming element 3 is also arranged in the direction of the flowthrough of the water behind cleaning device 2 . damming element 3 consists of partial surface 32 installed in a fixed manner in waste - water installation 1 and of partial surface 320 also movably arranged transversely to the direction of flowthrough of the flowing medium . in the exemplary embodiment of fig4 , movably arranged partial surface 320 is arranged on partial surface 32 in a fixed manner in waste - water installation 1 on the side facing away from cleaning device 2 . an arrangement of movable partial surface 320 in the direction of flow in front or after the fixed part of damming element 3 makes no difference in principle but rather is a function of the practical situation such as , e . g ., sliding surfaces and guide surfaces for movable partial surface 320 . just as in the case of damming element 3 in the exemplary embodiment of fig3 , a drive device operating with outside energy should preferably be provided for shifting movable partial surface 320 . however , it is also conceivable to perform the opening and closing of movable partial surface 320 via the backed - up or flowing water with the aid of suitable means , e . g ., floats or baffles . in addition to an embodiment of the invention like the one shown in fig4 , it is also conceivable to arrange the entire damming element 3 movably in the waste - water installation so that the flowthrough of water below the damming element is released by a shift in the vertical direction . such a design makes it possible not only to realize a small slot or interval between damming element 3 and bottom area 15 that is especially suited for generating high flow rates in the area of bottom area 15 and therewith removing the deposited suspended material and sinking material in an especially reliable manner , but it is also additionally possible therewith to move the damming element vertically in such a manner that the entire surface of cleaning device 2 is freed for an unimpeded passage of the liquid . this mode of operation should particularly be provided if there is a danger that cleaning device 2 is inundated as a consequence of a large amount of accumulating water . fig5 shows another embodiment of the invention in which damming element 3 can be opened in a pivoting motion similar to a door about vertical shaft 7 . fig5 shows a top view of a diagrammatic view of a cleaning device 2 built into the wall of a waste - water installation 1 . damming element 3 frees the passage of the water in the area of bottom area 15 in that it is pivoted substantially in the direction of flow s away from cleaning device 2 . the pivoting takes place via drive device 8 that can be designed , e . g ., as a hydraulic piston . this embodiment of a movable damming element 3 in accordance with the invention has the advantage that damming element 3 can be moved away rapidly and in a simple manner , e . g ., for maintenance , so that sieve rake 22 is readily accessible from both sides . fig6 shows a section of a diagrammatic view similar to that of fig1 . damming element 3 is divided into partial surface 32 installed in a fixed manner and into movable partial surface 320 . damming element 3 is also arranged in the direction of flow s behind cleaning device 2 . movable partial surface 320 of damming element 3 closes off the area between bottom area 15 and stationary partial surface 32 of damming element 3 in its closed position . to this end movable partial surface 320 is loaded by drive device 8 that presses movable partial surface 320 onto bottom area 15 so that a seal is created . it is provided for opening and closing movable partial surface 320 that drive device 8 is supplied via control device 81 with control signals and driving energy . control device 81 is connected via control leads 82 to sensors 83 with whose aid the level of the liquid in front of damming element 3 can be measured . the measuring takes place in a known manner , e . g ., by measuring the pressure or optically . it is therefore possible with the aid of this advantageous design of the invention to open or close movable partial surface 320 as a function of the level of the backed - up water . in addition , an opening and closing of damming element 3 can be regulated with the aid of control device 81 as a function of time intervals . this makes it possible to assure at regular intervals that bottom area 15 and therewith cleaning device 2 and its rake cleaner are regularly rinsed and washed in such a manner that deposited sinking material is removed from their area . it is , of course , a prerequisite for this that the amount of water in inflow side 11 has reached a sufficient dammed height ( level ) that a flow of water over bottom area 15 is possible at all . it is , of course , also possible to combine a sensor control and a time control or to make a cleaning of bottom area 15 possible by a manual intervention . fig7 shows a diagrammatic view of a waste - water installation in accordance with the invention similar to that of fig1 . in the waste - water installation of fig7 , damming element 3 is also designed in a multi - part manner in which damming element 3 consists of two separate structural components 33 of which one , the pivotably mounted one , is arranged in the plane of bottom area 15 so that it can pivot about shaft 7 . the movable partial surface 320 is designed so that in its closed state it rests practically in a plane with bottom area 15 . as the dammed pressure of the water backing up on damming element 3 increases , movable partial surface 320 of damming element 3 begins to pivot in the direction of arrow p downward about shaft 7 and opens the flowthrough of the water underneath the stationary partial surface of damming element 3 in the direction of arrow w . in its closed position , movable partial surface 320 is held by elastic elements ( not shown ). the pressure force of the elastic elements is overcome by a certain dammed level of the water in front of damming element 3 so that the flowthrough takes place in the direction of arrow w . intermediate wall 14 is designed in a corresponding manner so that it can receive movable partial surface 320 . another embodiment is shown with an interrupted line in which movable partial surface 320 is arranged substantially below bottom area 15 even though its shaft 7 also runs substantially at the level of bottom area 15 . fig8 shows a section of a device 1 in accordance with the invention in a top view onto bottom area 15 with movable partial surfaces 320 of damming element 3 arranged in it , which damming element consists of several partial surfaces 32 . the uppermost rake rod 23 of sieve rake 22 can be recognized in the top view as well as the top view onto movable partial surfaces 320 of damming element 3 , whose top view is represented by two parallel lines . the top view onto outflow side 12 is recognizable to the right of damming element 3 . movable partial surface 320 shown above is presented in its closed position whereas the movable partial surface 320 shown below is pivoted about shaft 7 so that it is shown in its half - open position . intermediate wall 14 is provided in a manner similar to that in fig7 with a perforation through which the water passes in the direction of arrow w into outflow side 12 of waste - water installation 1 . as is clear from fig8 , especially on the movable partial surface 320 shown at the bottom , shaft 7 is arranged substantially vertically relative to cleaning device 2 . in addition to the cited embodiment , other cleaning devices that are not based on a principle of a sieve rake can be used just as well in a waste - water installation in accordance with the invention . the invention makes it possible , independently of the embodiment of the individual elements , to intervene in a waste - water installation in such a manner that the disadvantages of the state of the art are avoided by making possible a flowthrough of water from inflow side 11 to outflow side 12 . it should be appreciated by those skilled in the art that modifications and variations can be made to the embodiments of the invention described or illustrated herein without departing from the scope and spirit of the invention as set forth in the appended claims and their equivalents .
1
specific embodiments are herein described in detail to explain the present invention , and numerous advantages and effects will become readily apparent to those skilled in the art once the disclosure is fully appreciated . it should be noted that the present invention may be implemented with various embodiments . fig1 is a flow diagram of the method of managing light energy according to the present invention . as shown in fig1 , the method comprises the following steps . in step s 10 , a detecting apparatus detects input information related to coordinate positions , input light energy and environmental information related to efficiency of inputting light energy in real time or at preset time intervals . the information related to input light energy include sources , positions , distance , time , intensity and environmental parameters regarding the input light energy , and the environmental information related to efficiency of inputting light energy is sunlight incident angle , distribution of sunlight , weather conditions , air quality , corresponding time , operational status of the energy guiding device , refractive index , or light transmittance . the aforementioned light energy is a form of energy that can be transmitted and utilized in the form of light . in step s 11 , an analysis and management apparatus analyzes and manages the input information by predetermined parameters or rules in real time or at preset time intervals , and determines whether to take a corresponding action according to results of analysis or management . in a preferred embodiment , the analysis and management apparatus outputs information related to evaluation of industrial value , information related to profit and loss of business , and / or information related to optimized utilization of light energy after analyzing results of analysis or management . as a result , investors and / or information user can understand the status of their investment environment by reference to information related to evaluation of industrial value , while the energy companies can plan their strategies for light energy industry through the information related to business profit and loss and / or the optimized utilization . fig2 is a flow diagram showing an embodiment of detecting light according to the present invention . as shown in fig2 , it involves the following steps . in step s 20 , a detecting apparatus detects sources , positions , distance , and intensity regarding input light energy and environmental information related to efficiency of inputting light energy in real time or at preset time intervals . in step s 21 , an analysis and management apparatus analyzes or manages the input information and environmental information by predetermined parameters or rules , and detects light according to results of analysis or management , so as to determine relative positions of light - emitting devices and intensity of the light emitted therefrom . in embodiments , the method of the present invention can be used in detecting the positions of luminaries . for example , when performing a search or detection in a dim environment , the present invention can detect light emitted by target devices and exactly determine the intensity and characteristics of the light emitted by the target devices and relative positions of the target devices . the present invention may further be applied to solar energy industry . fig3 is a flow diagram showing an embodiment applied to the solar energy industry according to the present invention . it involves the following steps . in step s 30 , input - related data and environmental data related to solar energy and acquired by the detecting apparatus are analyzed , evaluated and processed . in step s 31 , at least an energy guiding device is installed according to the input - related data and environmental data acquired in real time or at preset time intervals . the energy guiding device is capable of guiding - in , guiding - out , refracting , reflecting , intensifying , dispersing , and collecting light . for example , the energy guiding device could be any kinds of parabolic mirrors , reflective mirrors , and csp ( concentrated solar power ). the above steps are also known as field work . in embodiments , the field work is performed in real time or at preset time intervals , so as to obtain various environmental data related to solar energy , like distribution of solar energy , weather and terrain status . the data are further analyzed and evaluated in order to determine the positions where the energy guiding devices are to be installed . for instance , when solar energy companies plan to build multiple sets of energy guiding devices in a certain area , the field work of the present invention can be utilized to obtain environmental data . by making reference to the environmental data , installation of solar energy guiding devices can be optimized , and the energy guided by the solar energy guiding devices can be accurately understood . in step s 32 , the energy guiding device guides solar energy . in step s 33 , a conversion device converting the guided solar energy so that the converted energy is produced and utilized . in embodiments , the energy guiding device guides solar energy . then , a solar energy conversion device converts the guided solar energy and produces energy of many kinds so the converted energy can be further utilized . the energy produced by the conversion device includes electrical energy , thermal energy , and energy of other forms . for example , the conversion device may be a temperature - controlling boiler / furnace / kiln or photovoltaic panel or optical and / or utilization device , and the temperature - controlling boiler / furnace / kiln can convert received solar energy into thermal energy to manage and control the temperature of the boiler / furnace / kiln . in order to upgrade the temperature - controlling boiler / furnace / kiln to an industrial - graded boiler / furnace / kiln , another form of energy is used to increase the temperature of the temperature - controlling boiler / furnace / kiln to a predetermined value when the energy converted from the solar energy is not sufficient to heat the temperature - controlling boiler / furnace / kiln to reach the predetermined temperature . for example , the directions and angles of the energy guiding device is controlled or adjusted to guide in more solar energy , so as to increase the temperature of the temperature - controlling boiler / furnace / kiln to the predetermined value . in case the solar energy is inadequate , another accompanied energy device can supply thermal energy , plasma and / or induction heat source so as to maintain the operating temperature of the temperature - controlling boiler / furnace / kiln . other accompanied energy devices may include electric heater coils , plasma , gas torches , and thermal power gas pipes , to provide coal direct burning , fuel thermal power , waste heat recycling , geotherm , and other kinds of thermal energy . if the energy converted from the solar energy renders the temperature of the temperature - controlling boiler / furnace / kiln higher than the predetermined value , the temperature of the temperature - controlling boiler / furnace / kiln is decreased to below the predetermined value by reducing temperature of the energy guiding device or abating efficiency of the energy guiding device in guiding - in solar energy . alternatively , the extra energy can be transmitted to other boiler / furnace / kilns or energy conversion devices . for example , the temperature can be lowered by gas cooling via a gas flow ; increasing the contact surface area between a thermoelectric material and the temperature - controlling boiler / furnace / kiln to convert heat power into electric power ; increasing volume of process materials by adding more materials ; or increasing the open surface area of the temperature - controlling boiler / furnace / kiln to quickly lower its temperature . in step s 34 , an analysis and management apparatus analyzing or managing the information related to input solar energy and the environmental data related to efficiency of inputting solar energy according to the predetermined parameters or rules , and adjusting , maintaining or controlling energy produced by the conversion device in accordance with results of analysis and management . in a preferred embodiment , an analysis and management apparatus of the present invention analyzes data acquired in real time or at preset time intervals , so as to determine what action to take . for example , the detecting apparatus acquires information related to the variations of the sunlight incident angle in real time or at preset time intervals , and then the analysis and management apparatus determines the action to take according to the acquired information . in a preferred embodiment , a solar energy guiding device maintains a constant quantity of energy to be guided and supplied to an environment required for the operation of boiler / furnace / kilns . the solar energy guiding device is adjustable to the sunlight incident angle in order to track the sun , so that it can adjust and control the quantity of received sunlight . a conversion device may also maintain a constant quantity of energy to be produced , or turn on / off the solar energy guiding device to facilitate real - time , precise adjustment . fig4 shows the architecture of the system 40 of managing light energy according to the present invention . its components are described in detail below . the detecting module 401 detects input information related to input light energy and environmental information related to efficiency of inputting light energy in real time or at preset time intervals . the analysis and management module 402 analyzes and manages the input information and environmental information by predetermined parameters or rules , and determines whether to take a corresponding action according to results of analysis or management . hence the system of the present invention can accurately handle sources of light energy and thereby control and optimize the light energy . in a preferred embodiment , the analysis and management module further evaluates profit and loss of business of the related light energy industry by the predetermined real or simulated parameters . fig5 is a schematic diagram of the system of managing light energy according to the present invention , wherein the system is implemented with computer software . the software 501 of managing light energy , which is an embodiment of the system in fig4 , is installed on a computer 50 . the software 501 is stored on various storage media , like memory , hard drives , network or optical disks . in a preferred embodiment , the computer 50 receives from ambience or from an external device the information related to input light energy and environmental information related to efficiency of inputting light energy . the software 501 of managing light energy calculates and analyzes the information and determines whether a corresponding action is to be taken according to results of analysis . for example , the computer 50 outputs data related to evaluation of industrial value , data related to profit and loss of business , and / or data related to optimized utilization of the light energy . investors can better understand terrain status and production capacity of a specific light energy industry , so that they can estimate the risk in advance . another example is that the computer 50 can upload analytical data about various characteristics of light energy to a website 51 for public queries . fig6 shows the architecture of the system of managing light energy applied for energy conversion according to one embodiment of the present invention . the solar energy guiding device 61 is configured to guide solar energy . for example , the energy guiding device could be any kinds of parabolic mirrors , reflective mirrors , and csp ( concentrated solar power ). the temperature - controlling boiler / furnace / kiln 62 is configured to convert the solar energy guided by the solar energy guiding device 61 in order to produce energy . it should be noted that there is no limit for the types of the conversion device in the present invention . the energy produced by the conversion device may include electrical energy , thermal energy , and energy of other forms . the detecting apparatus 60 detects and acquires information related to input solar energy and environmental information related to efficiency of inputting solar energy , like sunlight incident angle , weather conditions , air quality , index of light refraction and light transmittance . the analysis and management host 63 determines whether to take a corresponding action according to the information acquired by the detecting apparatus 60 , in order to adjust , maintain or control energy produced by the temperature - controlling boiler / furnace / kiln 62 . for example , the analysis and management host 63 instructs , according to the information acquired by the detecting apparatus 60 , the solar energy guiding device 61 to turn on , partially turn on , turn off , and partially turn off , so that the energy produced by the temperature - controlling boiler / furnace / kiln 62 is adjusted , maintained or controlled . in a preferred embodiment , the system of managing light energy according to the present invention further includes a database for storing any data related to solar energy and acquired by the system . in another preferred embodiment , the solar energy guiding device 61 is adjustable to the sunlight incident angle so as to track the sun , thereby adjusting and controlling the quantity of sunlight received by the solar energy guiding device 61 . in another preferred embodiment , when the energy converted from the solar energy is not sufficient to heat the temperature - controlling boiler / furnace / kiln 62 to the predetermined temperature , the directions and angles of the energy guiding device 61 is controlled or adjusted by the analysis and management host 63 in real time or at preset time intervals , in order to guide - in more solar energy to increase the temperature of the temperature - controlling boiler / furnace / kiln to the predetermined value . if the energy converted from the solar energy renders the temperature of the temperature - controlling boiler / furnace / kiln 62 higher than the predetermined value , the temperature or efficiency of the solar energy guiding device 61 will be lowered by the analysis and management host 63 , so that the temperature of the temperature - controlling boiler / furnace / kiln 62 is lowered to below the predetermined value . in conclusion , the system and method of managing light energy according to the present invention have the following advantages : ( 1 ) the information related to input light energy is detected and then further analyzed and managed so that every characteristic of the input light energy can be mastered ; ( 2 ) the analysis and management is conducted according to every mastered characteristic of light energy , in order to determine whether to perform a corresponding act or take a corresponding action , which are beneficial installation and use of solar energy equipment in the solar energy industry . the foregoing descriptions of the detailed embodiments are only illustrated to disclose the principles and functions of the present invention , but not restrictive of the scope of the present invention . it should be understood to those skilled in the art that all modifications and variations according to the spirit and principle of the present invention can be made to the aforementioned embodiments .
6
the present inventions are directed to an integrated circuit having a mixed - radix and / or mixed - mode switch matrix interconnect architectures for implementation in / on , for example , integrated circuits ( for example , a processor , controller , state machine , gate array , pga , fpga and soc ). with that in mind , in one aspect , the present inventions are directed to an integrated circuit having a mixed - radix hierarchal interconnect architecture . in one embodiment , an integrated circuit includes a plurality of computing elements ( for example , a look - up - table , processor circuit , controller circuit and / or combinational logic circuit ) wherein each computing element is associated with plurality of switch matrices which are configured in at least two different radices in relation to an interconnect network of the switch matrices associated with other computing elements of the integrated circuit . for example , the switch matrices of a first stage ( which are directly connected to one or more associated computing elements ) are configured in a first radix interconnect ( for example , radix - 4 ), the switch matrices of a second stage are configured in a second radix interconnect ( for example , boundary - less radix - 3 ), the switch matrices of a third stage are configured in a third radix interconnect ( for example , boundary - less radix - 3 or radix - 2 ) and the switch matrices of a fourth stage are configured in a fourth radix interconnect ( for example , radix - 2 ). with reference to fig2 a and 2b , the hierarchal interconnect network may include a plurality of switch matrix stages ( stages 1 , 2 . . . n ) that are configured in two or more different radix or boundary - less radix interconnects . the mixed - radix interconnect architecture include hierarchy conductors to connect the switch matrices and computing elements — albeit detailed interconnections between switch matrices of each stage have been eliminated for purposes clarity . the design of the interconnect may depend on a plurality of tradeoffs including , for example , operating / response speed of the network , switching time of the matrices , die area considerations / constraints of the network and conductor routing considerations / constraints . for example , with reference to fig3 a - 3c , in one exemplary embodiment , it may be advantageous to employ a radix - 4 interconnect ( stage 1 ), in comparison to radix - 2 ( r2 ) interconnects , in order to reduce the switching time ( which may provide in a faster network ) because a radix - 4 ( r4 ) requires ½ the number of switch matrix ( sm ) stages to communicate between four computing elements ( ces )— that is , a radix - 4 interconnect network requires one switch matrix ( sm ) stage ( compared to two switch matrix ( sm ) stages in the context of a radix - 2 interconnect ). this may be balanced against the fact that a radix - 4 interconnect requires more wiring resources ( e . g . if sufficient wiring resources exist , or the wiring distances are sufficiently short ). thus , where wiring resources are less of a consideration , it may be advantageous to employ a radix - 4 interconnect for stage 1 ( such as short connections , where radix - 4 does not result in excessive routing congestion and increase in interconnect power / capacitance ). under these scenarios , a reduction of a sm stage is beneficial . however , in the higher / upper stages , smaller radix may be advantageous ( for example , a radix - 2 interconnects ) due to the fact that radix - 2 has lower routing resources relative to radix - 4 which may result in or provide reduced wiring congestion , capacitance , and power . because wire delay typically dominates over switch delay for longer wires , the additional delay incurred in sm stages becomes a beneficial tradeoff to reduce routing resources . with reference to fig4 a and 4b , in addition to radix - 2 / 4 tradeoffs ( of course , higher radices are suitable as well ), the boundary - less radix - 3 ( br3 ) interconnect may be well suited to implement with switch matrices organized as radix - 4 ( r4 ) and / or radix - 2 ( r2 ) interconnects in mixed - radix switch matrix network . unlike traditional radix - based networks , br3 networks maintains spatial locality between each computing element ( ce ) or switch matrix macro ( sm macro ) and its nearest neighbors and improves path diversity ( more path diversity often translates into less routing resource requirements ) and may be implemented using fewer switch matrix stages to make required connection ( compared to radix - 2 networks ). however , br3 network may use more routing resources compared to radix - 2 — and , as such , it may be advantageous to employ the br3 interconnect at lower hierarchies ( e . g ., closer to the computing elements and / or between the computing elements and a switch matrices stage of radix - 2 interconnect ). in this exemplary architecture , radix - 4 interconnect is employed as the stage 1 ( ce sm1 ), followed by stage 2 of br3 ( sm1 sm2 ), and followed by stage 3 of radix - 2 network ( sm2 sm3 ). notably , certain design - tradeoff include : one stage of radix - 4 requires 2 × the routing resources relative to two stages of radix - 2 switches , but requires only one switch delay to reach three of the nearest switch “ neighbors ”. one stage of br3 network requires 2 × the routing resources as 1 stage of radix - 2 switches . two stages of br3 network requires 2 × the routing resources as two stages of radix - 2 switches , which is same amount of routing resource as 1 stage of radix - 4 switch , but requires two switch delays . however , two stages of br3 switches allow each ce to reach eight “ neighbors ”, while one stage of radix - 4 switch allows each ce to only reach three “ neighbors ”. one stage of radix - 2 switches allows each ce to reach one “ neighbor ”. it requires the fewest routing resources , but requires the most number of switch and therefore switch delays . thus , in the exemplary embodiment of fig4 a , due to its large resource requirement but fast switches , it may be advantageous to employ radix - 4 switches where wiring is short ( local routes ), for example , for those interconnects in / on the lower or lowest hierarchies — such as , the first or second switch matrix ( sm ) stages ( i . e ., sm1 or sm2 ). notably , higher radices ( 8 , 16 , etc .) may also be employed for the lower sm stage hierarchies ( i . e ., sm1 and / or sm2 ). between the lower or lowest hierarchies / stages and upper or highest hierarchies / stages ( e . g ., in the middle hierarchies — such as , sm2 and / or sm3 ), it may be advantageous to employ boundary - less radix - 3 ( br3 ) configuration / interconnects to increase path diversity that facilitates communication to or reaching more neighboring switches without routing to an upper hierarchy , which may improve performance ( using fewer stages ) and reduce the resource requirements for the upper hierarchies . in the higher or upper hierarchies ( e . g ., sm3 and / or sm4 ), which are often dominated by wiring resource considerations , radix - 2 ( r2 ) interconnect may be employed which may reduce or minimize wiring resources / lengths . in another aspect of the present inventions , the integrated circuit includes mixed - mode interconnect architectures wherein ( i ) the switch matrices of at least one switch stage are configured in a hierarchical network ( in relation to the switch stages of the other switch matrices and / or computing elements ) and ( ii ) the switch matrices of at least one stage are configured in a mesh network . for example , in one embodiment , the integrated circuit includes n stage of switch matrices ( for example , four stages of switch matrices ) including , for example , a first stage of switch matrices ( which are directly connected to one or more associated computing elements ) configured in hierarchical interconnect / network ( for example , radix - 4 or radix - 3 ), a second stage of switch matrices ( which are connected to switch matrices of the first stage and a third stage of switch matrices ) configured in hierarchical interconnects / networks ( for example , radix - 4 or radix - 3 ), a third stage of switch matrices ( which are connected to switch matrices of the second stage and a fourth stage of switch matrices ) configured in hierarchical interconnects / networks ( for example , radix - 3 and radix - 2 ) and the fourth stage configured in a mesh interconnect / network , wherein each switch matrix of the mesh - type interconnect is connected to another switch matrix of the same stage ( i . e ., the fourth stage ). with reference to fig5 a - 5c , exemplary mixed - mode interconnect architectures of a programmable logic tiles , according to at least one aspect of the present inventions , include a plurality of computing elements ( for example , a look - up - table , processor circuit , controller circuit and / or combinational logic circuit ) and switch matrices of at least one stage are configured in a hierarchical network ( in relation to the switch stages of the other switch matrices and / or computing elements ) and switch matrices of at least one stage are configured in a mesh network . in these illustrative embodiments , switch matrices of certain stages are configured in a hierarchical network and other switch matrices are configured in a mesh network according to at least one aspect of the present inventions , for example , in fig5 a , switch matrices of stages 1 and 2 are configured in a hierarchical architecture and switch matrices of stage n are configured in a mesh architecture wherein , as a mesh architecture ( and unlike a hierarchical architecture ), the outputs of the switches of stage n are routed to selected other switches of stage n — that is , the output routing remains within stage 4 ( see , fig5 a wherein the signal travels between switches 1 . n and 9 . n , and thereafter the signal may travel within the other stages connected to the mesh network — e . g ., to the ce by entering the hierarchical network via stage n − 1 ) ( see also , fig5 b wherein switch matrices of stage 2 are configured in a mesh architecture and , as such , the signal travels between switches 1 . 2 and 9 . 2 , and thereafter the signal may travel within the other stages connected to the mesh network via the hierarchical network of stages 9 . . . n ,— e . g ., to one or more computing elements by entering the hierarchical network via stage 1 ). notably , mesh interconnects may be implemented in more than one stage of a logic tile . with reference to fig5 c , switch matrices of stage 1 is configured in a hierarchical architecture ( and other stages may as well ) and switch matrices of stages 2 and n are configured in a mesh architecture wherein , as a mesh architecture ( and unlike a hierarchical architecture ), the outputs of the switches of stages 2 and n are routed to selected other switches of stages 2 and n , respectively — that is , the output routing remains within stage 2 and stage n , respectively . here , for the purposes of clarity , much of the detailed interconnections between switch matrices of the stages have been eliminated . the switch matrices of stage 3 through stage n may be configured in a hierarchical architecture ( e . g ., one or more radix and / or boundary - less radix organizations ) or a mesh network architecture ( i . e ., a mesh , torus or the like network architecture ). indeed , the mixed mode techniques / interconnects and mixed - radix techniques / interconnects may be implemented together in network of a logic tile . ( see , for example , fig6 a - 6d ). here , mixed - radix , mixed - mode interconnect architectures ( i . e ., a plurality of switch matrices ( sm ) stages implementing either hierarchy or mesh interconnects ) provide advantages of mixed - radix interconnects and mixed - mode interconnects wherein the logic tile includes each interconnect . again , detailed interconnections between switch matrices of the stages have been eliminated for purposes clarity . with reference to fig7 a - 7c , in one exemplary embodiment , the network includes has a mix - radix ( with br3 ) hierarchical network similar to fig4 a for the lower 3 stages ( lower stages are those stages that are disposed , positioned or located closer to the computing elements within the architecture ) which connects to a mesh - style network for stage 4 . notably , a key difference for mesh - style architecture is that a signal does not change hierarchy when traversing between switch matrices ; that is , the signal may be transmitted to other switches within the switch matrices ( sm ) of stage 4 . in a hierarchical network , the signal would travel from ce up to the required sm hierarchy , and then travel back down . here , the signal generally does not travel within the same hierarchy — as in a mesh interconnect . thus , a mesh - style switch configuration is different ( from a switch implemented in a hierarchal configuration ), for example , when a signal travels from switch 1 . 4 to switch 9 . 4 , it remains within switch matrices of stage 4 ; thereafter , the signal can then travel somewhere else on the mesh network , or travel downwards towards a ce ( for example , ce 3 ) by entering , for example , the switch 3 . 4 and then propagate within the hierarchical network via stage 3 ( e . g ., switches 3 . 3 , 3 . 2 , 3 . 1 to ce 3 ). ( see , for example , fig7 a and 7b ). there are many inventions described and illustrated herein . while certain embodiments , features , attributes and advantages of the inventions have been described and illustrated , it should be understood that many others , as well as different and / or similar embodiments , features , attributes and advantages of the present inventions , are apparent from the description and illustrations . as such , the embodiments , features , attributes and advantages of the inventions described and illustrated herein are not exhaustive and it should be understood that such other , similar , as well as different , embodiments , features , attributes and advantages of the present inventions are within the scope of the present inventions . indeed , the present inventions are neither limited to any single aspect nor embodiment thereof , nor to any combinations and / or permutations of such aspects and / or embodiments . moreover , each of the aspects of the present inventions , and / or embodiments thereof , may be employed alone or in combination with one or more of the other aspects of the present inventions and / or embodiments thereof . notably , “ circuitry ”, means , among other things , a circuit ( whether integrated or otherwise ), a group of such circuits , one or more processors , one or more state machines , one or more processors implementing software , one or more gate arrays , programmable gate arrays and / or field programmable gate arrays , or a combination of one or more circuits ( whether integrated or otherwise ), one or more state machines , one or more processors , one or more processors implementing software , one or more gate arrays , programmable gate arrays and / or field programmable gate arrays . the layout , organization and interconnection techniques described herein may be implemented using one or more processors ( suitably programmed ) to perform , execute and / or assess one or more of the functions or operations of the present inventions . notably , various circuits , circuitry , layout and routing disclosed herein may be described using computer aided design tools and expressed ( or represented ), as data and / or instructions embodied in various computer - readable media , in terms of their behavioral , register transfer , logic component , transistor , layout geometries , and / or other characteristics . formats of files and other objects in which such circuit , circuitry , layout and routing expressions may be implemented include , but are not limited to , formats supporting behavioral languages such as c , verilog , and hldl , formats supporting register level description languages like rtl , and formats supporting geometry description languages such as gdsii , gdsiii , gdsiv , cif , mebes and any other formats and / or languages now known or later developed . computer - readable media in which such formatted data and / or instructions may be embodied include , but are not limited to , non - volatile storage media in various forms ( e . g ., optical , magnetic or semiconductor storage media ) and carrier waves that may be used to transfer such formatted data and / or instructions through wireless , optical , or wired signaling media or any combination thereof . examples of transfers of such formatted data and / or instructions by carrier waves include , but are not limited to , transfers ( uploads , downloads , e - mail , etc .) over the internet and / or other computer networks via one or more data transfer protocols ( e . g ., http , ftp , smtp , etc .). indeed , when received within a computer system via one or more computer - readable media , such data and / or instruction - based expressions of the above described circuits may be processed by a processing entity ( e . g ., one or more processors ) within the computer system in conjunction with execution of one or more other computer programs including , without limitation , net - list generation programs , place and route programs and the like , to generate a representation or image of a physical manifestation of such circuits . such representation or image may thereafter be used in device fabrication , for example , by enabling generation of one or more masks that are used to form various components of the circuits in a device fabrication process . moreover , the various circuits , circuitry , layout and routing , as well as techniques , disclosed herein may be represented via simulations using computer aided design and / or testing tools . the simulation of the inventive circuits , circuitry , layout and routing , and / or techniques implemented thereby , may be implemented by a computer system wherein characteristics and operations of such circuits , circuitry , layout and routing , and techniques implemented thereby , are imitated , replicated and / or predicted via a computer system . the present inventions are also directed to such simulations of the inventive circuits , circuitry , layout and routing , and / or techniques implemented thereby , and , as such , are intended to fall within the scope of the present inventions . the computer - readable media corresponding to such simulations and / or testing tools are also intended to fall within the scope of the present inventions . notably , reference herein to “ one embodiment ” or “ an embodiment ” ( or the like ) means that a particular feature , structure , or characteristic described in connection with the embodiment may be included , employed and / or incorporated in one , some or all of the embodiments of the present inventions . the usages or appearances of the phrase “ in one embodiment ” or “ in another embodiment ” ( or the like ) in the specification are not referring to the same embodiment , nor are separate or alternative embodiments necessarily mutually exclusive of one or more other embodiments , nor limited to a single exclusive embodiment . the same applies to the term “ implementation .” the present inventions are neither limited to any single aspect nor embodiment thereof , nor to any combinations and / or permutations of such aspects and / or embodiments . moreover , each of the aspects of the present inventions , and / or embodiments thereof , may be employed alone or in combination with one or more of the other aspects of the present inventions and / or embodiments thereof . for the sake of brevity , certain permutations and combinations are not discussed and / or illustrated separately herein . further , an embodiment or implementation described herein as “ exemplary ” is not to be construed as preferred or advantageous , for example , over other embodiments or implementations ; rather , it is intended convey or indicate the embodiment or embodiments are example embodiment ( s ). although the present inventions have been described in certain specific aspects , many additional modifications and variations would be apparent to those skilled in the art . it is therefore to be understood that the present inventions may be practiced otherwise than specifically described without departing from the scope and spirit of the present inventions . thus , embodiments of the present inventions should be considered in all respects as illustrative and not restrictive . as used in the claims , the terms “ comprises ,” “ comprising ,” “ includes ,” “ including ,” “ have ,” and “ having ” or any other variation thereof , are intended to cover a non - exclusive inclusion , such that a process , method , circuit , 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 . in the claims , and elsewhere , the terms “ first ,” “ second ,” and the like , herein do not denote any order , quantity , or importance , but rather are used to distinguish one element from another . moreover , the terms “ a ” and “ an ” herein do not denote a limitation of quantity , but rather denote the presence of at least one of the referenced item . the term “ data ” may mean , among other things , a current or voltage signal ( s ) whether in analog or a digital form ( which may be a single bit ( or the like ) or multiple bits ( or the like )). further , the term “ logic tile ” means a design unit or block of a plurality of transistors ( typically thousands to millions ), which , in this application , is capable of connecting or connected to a plurality of neighboring “ tile ”, “ core ” or “ block ” ( for example , in or during operation ). moreover , as noted above , the term ( i ) “ integrated circuit ” means , among other things , a processor , controller , state machine , gate array , soc , pga and / or fpga , and ( ii ) “ computing elements ” means , among other things , a look - up - table , processor circuit , controller circuit and / or combinational logic circuit .
7
in fig1 of the accompanying drawings there is schematically depicted an overall view of a printhead assembly . fig2 shows the core components of the assembly in an exploded configuration . the printhead assembly 10 of the preferred embodiment comprises eleven printhead modules 11 situated along a metal “ invar ” channel 16 . at the heart of each printhead module 11 is a “ memjet ” chip 23 ( fig3 ). the particular chip chosen in the preferred embodiment being a six - color configuration . the “ memjet ” printhead modules 11 are comprised of the “ memjet ” chip 23 , a fine pitch flex pcb 26 and two micro - moldings 28 and 34 sandwiching a mid - package film 35 . each module 11 forms a sealed unit with independent ink chambers 63 ( fig9 ) which feed the chip 23 . the modules 11 plug directly onto a flexible elastomeric extrusion 15 which carries air , ink and fixitive . the upper surface of the extrusion 15 has repeated patterns of holes 21 which align with ink inlets 32 ( fig3 a ) on the underside of each module 11 . the extrusion 15 is bonded onto a flex pcb ( flexible printed circuit board ). the fine pitch flex pcb 26 wraps down the side of each printhead module 11 and makes contact with the flex pcb 17 ( fig9 ). the flex pcb 17 carries two busbars 19 ( positive ) and 20 ( negative ) for powering each module 11 , as well as all data connections . the flex pcb 17 is bonded onto the continuous metal “ invar ” channel 16 . the metal channel 16 serves to hold the modules 11 in place and is designed to have a similar coefficient of thermal expansion to that of silicon used in the modules . a capping device 12 is used to cover the “ memjet ” chips 23 when not in use . the capping device is typically made of spring steel with an onsert molded elastomeric pad 47 ( fig1 a ). the pad 47 serves to duct air into the “ memjet ” chip 23 when uncapped and cut off air and cover a nozzle guard 24 ( fig9 ) when capped . the capping device 12 is actuated by a camshaft 13 that typically rotates throughout 180 °. the overall thickness of the “ memjet ” chip is typically 0 . 6 mm which includes a 150 - micron inlet backing layer 27 and a nozzle guard 24 of 150 - micron thickness . these elements are assembled at the wafer scale . the nozzle guard 24 allows filtered air into an 80 - micron cavity 64 ( fig1 ) above the “ memjet ” ink nozzles 62 . the pressurized air flows through microdroplet holes 45 in the nozzle guard 24 ( with the ink during a printing operation ) and serves to protect the delicate “ memjet ” nozzles 62 by repelling foreign particles . a silicon chip backing layer 27 ducts ink from the printhead module packaging directly into the rows of “ memjet ” nozzles 62 . the “ memjet ” chip 23 is wire bonded 25 from bond pads on the chip at 116 positions to the fine pitch flex pcb 26 . the wire bonds are on a 120 - micron pitch and are cut as they are bonded onto the fine pitch flex pcb pads ( fig3 ). the fine pitch flex pcb 26 carries data and power from the flex pcb 17 via a series of gold contact pads 69 along the edge of the flex pcb . the wire bonding operation between chip and fine pitch flex pcb 26 may be done remotely , before transporting , placing and adhering the chip assembly into the printhead module assembly . alternatively , the “ memjet ” chips 23 can be adhered into the upper micro - molding 28 first and then the fine pitch flex pcb 26 can be adhered into place . the wire bonding operation could then take place in situ , with no danger of distorting the moldings 28 and 34 . the upper micro - molding 28 can be made of a liquid crystal polymer ( lcp ) blend . since the crystal structure of the upper micro - molding 28 is minute , the heat distortion temperature ( 180 ° c .– 260 ° c . ), the continuous usage temperature ( 200 ° c .– 240 ° c .) and soldering heat durability ( 260 ° c . for 10 seconds to 310 ° c . for 10 seconds ) are high , regardless of the relatively low melting point . each printhead module 11 includes an upper micro - molding 28 and a lower micro - molding 34 separated by a mid - package film layer 35 shown in fig3 . the mid - package film layer 35 can be an inert polymer such as polyimide , which has good chemical resistance and dimensional stability . the mid - package film layer 35 can have laser ablated holes 65 and can comprise a double - sided adhesive ( ie . an adhesive layer on both faces ) providing adhesion between the upper micro - molding , the mid - package film layer and the lower micro - molding . the upper micro - molding 28 has a pair of alignment pins 29 passing through corresponding apertures in the mid - package film layer 35 to be received within corresponding recesses 66 in the lower micro - molding 34 . this serves to align the components when they are bonded together . once bonded together , the upper and lower micro - moldings form a tortuous ink and air path in the complete “ memjet ” printhead module 11 . there are annular ink inlets 32 in the underside of the lower micro - molding 34 . in a preferred embodiment , there are six such inlets 32 for various inks ( black , yellow , magenta , cyan , fixitive and infrared ). there is also provided an air inlet slot 67 . the air inlet slot 67 extends across the lower micro - molding 34 to a secondary inlet which expels air through an exhaust hole 33 , through an aligned hole 68 in fine pitch flex pcb 26 . this serves to repel the print media from the printhead during printing . the ink inlets 32 continue in the undersurface of the upper micro - molding 28 as does a path from the air inlet slot 67 . the ink inlets lead to 200 micron exit holes also indicated at 32 in fig3 . these holes correspond to the inlets on the silicon backing layer 27 of the “ memjet ” chip 23 . there is a pair of elastomeric pads 36 on an edge of the lower micro - molding 34 . these serve to take up tolerance and positively located the printhead modules 11 into the metal channel 16 when the modules are micro - placed during assembly . a preferred material for the “ memjet ” micro - moldings is a lcp . this has suitable flow characteristics for the fine detail in the moldings and has a relatively low coefficient of thermal expansion . robot picker details are included in the upper micro - molding 28 to enable accurate placement of the printhead modules 11 during assembly . the upper surface of the upper micro - molding 28 as shown in fig3 has a series of alternating air inlets and outlets 31 . these act in conjunction with the capping device 12 and are either sealed off or grouped into air inlet / outlet chambers , depending upon the position of the capping device 12 . they connect air diverted from the inlet slot 67 to the chip 23 depending upon whether the unit is capped or uncapped . a capper cam detail 40 including a ramp for the capping device is shown at two locations in the upper surface of the upper micro - molding 28 . this facilitates a desirable movement of the capping device 12 to cap or uncap the chip and the air chambers . that is , as the capping device is caused to move laterally across the print chip during a capping or uncapping operation , the ramp of the capper cam detail 40 serves to elastically distort and capping device as it is moved by operation of the camshaft 13 so as to prevent scraping of the device against the nozzle guard 24 . the “ memjet ” chip assembly 23 is picked and bonded into the upper micro - molding 28 on the printhead module 11 . the fine pitch flex pcb 26 is bonded and wrapped around the side of the assembled printhead module 11 as shown in fig4 . after this initial bonding operation , the chip 23 has more sealant or adhesive 46 applied to its long edges . this serves to “ pot ” the bond wires 25 ( fig6 ), seal the “ memjet ” chip 23 to the molding 28 and form a sealed gallery into which filtered air can flow and exhaust through the nozzle guard 24 . the flex pcb 17 carries all data and power connections from the main pcb ( not shown ) to each “ memjet ” printhead module 11 . the flex pcb 17 has a series of gold plated , domed contacts 69 ( fig2 ) which interface with contact pads 41 , 42 and 43 on the fine pitch flex pcb 26 of each “ memjet ” printhead module 11 . two copper busbar strips 19 and 20 , typically of 200 micron thickness , are jigged and soldered into place on the flex pcb 17 . the busbars 19 and 20 connect to a flex termination which also carries data the flex pcb 17 is approximately 340 mm in length and is formed from a 14 mm wide strip . it is bonded into the metal channel 16 during assembly and exits from one end of the printhead assembly only . the metal u - channel 16 into which the main components are place is of a special alloy called “ invar 36 ”. it is a 36 % nickel iron alloy possessing a coefficient of thermal expansion of 1 / 10 th that of carbon steel at temperatures up to 400 ° f . the invar is annealed for optimal dimensional stability . additionally , the invar is nickel plated to a 0 . 056 % thickness of the wall section . this helps to further match it to the coefficient of thermal expansion of silicon which is 2 × 10 − 6 per ° c . the invar channel 16 functions to capture the “ memjet ” printhead modules 11 in a precise alignment relative to each other and to impart enough force on the modules 11 so as to form a seal between the ink inlets 32 on each printhead module and the outlet holes 21 that are laser ablated into the elastomeric ink delivery extrusion 15 . the similar coefficient of thermal expansion of the invar channel to the silicon chips allows similar relative movement during temperature changes . the elastomeric pads 36 on one side of each printhead module 11 serve to “ lubricate ” them within the channel 16 to take up any further lateral coefficient of thermal expansion tolerances without losing alignment . the invar channel is a cold rolled , annealed and nickel plated strip . apart from two bends that are required in its formation , the channel has two square cut - outs 80 at each end . these mate with snap fittings 81 on the printhead location moldings 14 ( fig1 ). the elastomeric ink delivery extrusion 15 is a non - hydrophobic , precision component . its function is to transport ink and air to the “ memjet ” printhead modules 11 . the extrusion is bonded onto the top of the flex pcb 17 during assembly and it has two types of molded end caps . one of these end caps is shown at 70 in fig1 a . a series of patterned holes 21 are present on the upper surface of the extrusion 15 . these are laser ablated into the upper surface . to this end , a mask is made and placed on the surface of the extrusion , which then has focused laser light applied to it . the holes 21 are evaporated from the upper surface , but the laser does not cut into the lower surface of extrusion 15 due to the focal length of the laser light . eleven repeated patterns of the laser ablated holes 21 form the ink and air outlets 21 of the extrusion 15 . these interface with the annular ring inlets 32 on the underside of the “ memjet ” printhead module lower micro - molding 34 . a different pattern of larger holes ( not shown but concealed beneath the upper plate 71 of end cap 70 in fig1 a ) is ablated into one end of the extrusion 15 . these mate with apertures 75 having annular ribs formed in the same way as those on the underside of each lower micro - molding 34 described earlier . ink and air delivery hoses 78 are connected to respective connectors 76 that extend from the upper plate 71 . due to the inherent flexibility of the extrusion 15 , it can contort into many ink connection mounting configurations without restricting ink and air flow . the molded end cap 70 has a spine 73 from which the upper and lower plates are integrally hinged . the spine 73 includes a row of plugs 74 that are received within the ends of the respective flow passages of the extrusion 15 . the other end of the extrusion 15 is capped with simple plugs which block the channels in a similar way as the plugs 74 on spine 17 . the end cap 70 clamps onto the ink extrusion 15 by way of snap engagement tabs 77 . once assembled with the delivery hoses 78 , ink and air can be received from ink reservoirs and an air pump , possibly with filtration means . the end cap 70 can be connected to either end of the extrusion , ie . at either end of the printhead . the plugs 74 are pushed into the channels of the extrusion 15 and the plates 71 and 72 are folded over . the snap engagement tabs 77 clamp the molding and prevent it from slipping off the extrusion . as the plates are snapped together , they form a sealed collar arrangement around the end of the extrusion . instead of providing individual hoses 78 pushed onto the connectors 76 , the molding 70 might interface directly with an ink cartridge . a sealing pin arrangement can also be applied to this molding 70 . for example , a perforated , hollow metal pin with an elastomeric collar can be fitted to the top of the inlet connectors 76 . this would allow the inlets to automatically seal with an ink cartridge when the cartridge is inserted . the air inlet and hose might be smaller than the other inlets in order to avoid accidental charging of the airways with ink . the capping device 12 for the “ memjet ” printhead would typically be formed of stainless spring steel . an elastomeric seal or onsert molding 47 is attached to the capping device as shown in fig1 a and 12 b . the metal part from which the capping device is made is punched as a blank and then inserted into an injection molding tool ready for the elastomeric onsert to be shot onto its underside . small holes 79 ( fig1 b ) are present on the upper surface of the metal capping device 12 and can be formed as burst holes . they serve to key the onsert molding 47 to the metal . after the molding 47 is applied , the blank is inserted into a press tool , where additional bending operations and forming of integral springs 48 takes place . the elastomeric onsert molding 47 has a series of rectangular recesses or air chambers 56 . these create chambers when uncapped . the chambers 56 are positioned over the air inlet and exhaust holes 30 of the upper micro - molding 28 in the “ memjet ” printhead module 11 . these allow the air to flow from one inlet to the next outlet . when the capping device 12 is moved forward to the “ home ” capped position as depicted in fig1 , these airways 32 are sealed off with a blank section of the onsert molding 47 cutting off airflow to the “ memjet ” chip 23 . this prevents the filtered air from drying out and therefore blocking the delicate “ memjet ” nozzles . another function of the onsert molding 47 is to cover and clamp against the nozzle guard 24 on the “ memjet ” chip 23 . this protects against drying out , but primarily keeps foreign particles such as paper dust from entering the chip and damaging the nozzles . the chip is only exposed during a printing operation , when filtered air is also exiting along with the ink drops through the nozzle guard 24 . this positive air pressure repels foreign particles during the printing process and the capping device protects the chip in times of inactivity . the integral springs 48 bias the capping device 12 away from the side of the metal channel 16 . the capping device 12 applies a compressive force to the top of the printhead module 11 and the underside of the metal channel 16 . the lateral capping motion of the capping device 12 is governed by an eccentric camshaft 13 mounted against the side of the capping device . it pushes the device 12 against the metal channel 16 . during this movement , the bosses 57 beneath the upper surface of the capping device 12 ride over the respective ramps 40 formed in the upper micro - molding 28 . this action flexes the capping device and raises its top surface to raise the onsert molding 47 as it is moved laterally into position onto the top of the nozzle guard 24 . the camshaft 13 , which is reversible , is held in position by two printhead location moldings 14 . the camshaft 11 can have a flat surface built in one end or be otherwise provided with a spline or keyway to accept gear 22 or another type of motion controller . 1 . the “ memjet ” chip 23 is dry tested in flight by a pick and place robot , which also dices the wafer and transports individual chips to a fine pitch flex pcb bonding area . 2 . when accepted , the “ memjet ” chip 23 is placed 530 microns apart from the fine pitch flex pcb 26 and has wire bonds 25 applied between the bond pads on the chip and the conductive pads on the fine pitch flex pcb . this constitutes the “ memjet ” chip assembly . 3 . an alternative to step 2 is to apply adhesive to the internal walls of the chip cavity in the upper micro - molding 28 of the printhead module and bond the chip into place first . the fine pitch flex pcb 26 can then be applied to the upper surface of the micro - molding and wrapped over the side . wire bonds 25 are then applied between the bond pads on the chip and the fine pitch flex pcb . 4 . the “ memjet ” chip assembly is vacuum transported to a bonding area where the printhead modules are stored . 5 . adhesive is applied to the lower internal walls of the chip cavity and to the area where the fine pitch flex pcb is going to be located in the upper micro - molding of the printhead module . 6 . the chip assembly ( and fine pitch flex pcb ) are bonded into place . the fine pitch flex pcb is carefully wrapped around the side of the upper micro - molding so as not to strain the wire bonds . this may be considered as a two step gluing operation if it is deemed that the fine pitch flex pcb might stress the wire bonds . a line of adhesive running parallel to the chip can be applied at the same time as the internal chip cavity walls are coated . this allows the chip assembly and fine pitch flex pcb to be seated into the chip cavity and the fine pitch flex pcb allowed to bond to the micro - molding without additional stress . after curing , a secondary gluing operation could apply adhesive to the short side wall of the upper micro - molding in the fine pitch flex pcb area . this allows the fine pitch flex pcb to be wrapped around the micro - molding and secured , while still being firmly bonded in place along on the top edge under the wire bonds . 7 . in the final bonding operation , the upper part of the nozzle guard is adhered to the upper micro - molding , forming a sealed air chamber . adhesive is also applied to the opposite long edge of the “ memjet ” chip , where the bond wires become ‘ potted ’ during the process . 8 . the modules are ‘ wet ’ tested with pure water to ensure reliable performance and then dried out . 9 . the modules are transported to a clean storage area , prior to inclusion into a printhead assembly , or packaged as individual units . this completes the assembly of the “ memjet ” printhead module assembly . 10 . the metal invar channel 16 is picked and placed in a jig . 11 . the flex pcb 17 is picked and primed with adhesive on the busbar side , positioned and bonded into place on the floor and one side of the metal channel . 12 . the flexible ink extrusion 15 is picked and has adhesive applied to the underside . it is then positioned and bonded into place on top of the flex pcb 17 . one of the printhead location end caps is also fitted to the extrusion exit end . this constitutes the channel assembly . 13 . the channel assembly is transported to an eximir laser ablation area . 14 . the assembly is put into a jig , the extrusion positioned , masked and laser ablated . this forms the ink holes in the upper surface . 15 . the ink extrusion 15 has the ink and air connector molding 70 applied . pressurized air or pure water is flushed through the extrusion to clear any debris . 16 . the end cap molding 70 is applied to the extrusion 15 . it is then dried with hot air . 17 . the channel assembly is transported to the printhead module area for immediate module assembly . alternatively , a thin film can be applied over the ablated holes and the channel assembly can be stored until required . 18 . the channel assembly is picked , placed and clamped into place in a transverse stage in the printhead assembly area . 19 . as shown in fig1 , a robot tool 58 grips the sides of the metal channel and pivots at pivot point against the underside face to effectively flex the channel apart by 200 to 300 microns . the forces applied are shown generally as force vectors f in fig1 . this allows the first “ memjet ” printhead module to be robot picked and placed ( relative to the first contact pads on the flex pcb 17 and ink extrusion holes ) into the channel assembly . 20 . the tool 58 is relaxed , the printhead module captured by the resilience of the invar channel and the transverse stage moves the assembly forward by 19 . 81 mm . 21 . the tool 58 grips the sides of the channel again and flexes it apart ready for the next printhead module . 22 . a second printhead module 11 is picked and placed into the channel 50 microns from the previous module . 23 . an adjustment actuator arm locates the end of the second printhead module . the arm is guided by the optical alignment of fiducials on each strip . as the adjustment arm pushes the printhead module over , the gap between the fiducials is closed until they reach an exact pitch of 19 . 812 mm . 24 . the tool 58 is relaxed and the adjustment arm is removed , securing the second printhead module in place . 25 . this process is repeated until the channel assembly has been fully loaded with printhead modules . the unit is removed from the transverse stage and transported to the capping assembly area . alternatively , a thin film can be applied over the nozzle guards of the printhead modules to act as a cap and the unit can be stored as required . 26 . the printhead assembly is transported to a capping area . the capping device 12 is picked , flexed apart slightly and pushed over the first module 11 and the metal channel 16 in the printhead assembly . it automatically seats itself into the assembly by virtue of the bosses 57 in the steel locating in the recesses 83 in the upper micro - molding in which a respective ramp 40 is located . 27 . subsequent capping devices are applied to all the printhead modules . 28 . when completed , the camshaft 13 is seated into the printhead location molding 14 of the assembly . it has the second printhead location molding seated onto the free end and this molding is snapped over the end of the metal channel , holding the camshaft and capping devices captive . 29 . a molded gear 22 or other motion control device can be added to either end of the camshaft 13 at this point . 30 . the capping assembly is mechanically tested . 31 . the printhead assembly 10 is moved to the testing area . inks are applied through the “ memjet ” modular printhead under pressure . air is expelled through the “ memjet ” nozzles during priming . when charged , the printhead can be electrically connected and tested . 32 . electrical connections are made and tested as follows : 33 . power and data connections are made to the pcb . final testing can commence , and when passed , the “ memjet ” modular printhead is capped and has a plastic sealing film applied over the underside that protects the printhead until product installation .
1
turning first to fig2 therein fragmentarily illustrated is microprism sheeting of the type which is employed in the present invention and which is generally designated by the numeral 8 . the sheeting 8 is conveniently formed by casting a resin formulation to form closely spaced microprisms 12 on a base film 10 as described in the aforementioned rowland patents . as illustrated in fig3 the sheeting 8 of fig2 is shown with a reflective metallic deposit generally designated by the numeral 14 . this is comprised of a base layer 16 of silver and superposed layer 18 of copper as seen in fig4 . thereafter , an adhesive or other coating material 20 may be deposited thereon , as seen in fig5 . turning now to fig1 the apparatus to develop the metallic deposit 14 is illustrated schematically as comprising a vacuum chamber 22 connected to vacuum pumps 24 by the conduits 26 . a roll 28 of the microprism sheeting 8 seen in fig2 is supported therein on the roll shaft 29 , and the sheeting 8 passes about tensioning rolls 30 , 32 and thence about the cooling drum 34 . from the drum 34 , it passes about the tensioning rolls 36 , 38 and is coiled on the roll shaft 40 which is being driven . the direction of motion of the sheeting can be reversed since both the shafts 29 and 40 can be driven . as the sheeting 8 passes about the cooling drum 34 , it is exposed to sputtered metal from the silver cathode 42 and then the copper cathode 44 which form the composite metallic deposit 14 seen in fig3 - 5 . after the sheeting 8 has been metallized in one or more passes , the vacuum in the chamber 22 can be broken , and the roll 28 of now metallized sheeting 8 can be removed . subsequently , the sheeting 8 may be coated with an adhesive or other coating and a protective sheet material backing provided thereon as is conventional . the thickness of the silver and copper layers may vary . generally , however , the silver layer should be at least 300 angstroms and may be as thick as 5000 angstroms or even thicker if so desired , but at greater cost . however , thicknesses of about 600 - 2000 angstroms exhibit a high degree of reflectivity and are easily obtained , albeit in multiple passes . moreover , thicknesses in this range appear to form an intermetallic layer with the copper layer being deposited thereon , possibly as the result of diffusion or concurrent deposition . a copper layer of as little as 200 angstroms will provide the desired composite coating but thicknesses on the order of 400 - 2500 angstroms are preferred and provide the opportunity to form an intermetallic layer as well as a good protective layer for the underlying silver layer . the process employed for the deposition of the composite metallic deposit is one in which the metal is sputtered in a vacuum by high energy inert gas ions striking a target of the metal . as the gas ions strike the target metal with energies in the range of 100 - 1000 electron volts , the metal at the surface of the target is evaporated to form a vapor of atoms having energy in the range of 10 - 50 electron volts and the metal deposits on the surface of the sheeting as it passes by the target . such high energy sputtering processes are described by john a . thornton in &# 34 ; coating deposition by sputtering &# 34 ; in deposition technologies for films and coatings , published in noyes publications of park ridge , n . j ., in 1982 . using a dc sputtering technique of the type described in this reference , the vacuum drawn in the vacuum chamber is typically 5 × 10 - 4 - 5 × 10 - 7 torr with a pressure of argon or other inert gas of 1 - 100 mtorr . the target voltage may be within the range of 1000 - 5000 volts and the target current in the range of 5 - 25 amperes with the target power being in the range of 5 - 15 kilowatts . because it is difficult to measure the thickness of the metal deposits on the angled surfaces of the prisms , two techniques may be employed to determine appropriate conditions for the silver deposit . in one technique the optical density of the unmetallized and metallized sheeting is measured . the silver deposit should provide an increase of 2 . 0 - 2 . 5 in density . another technique is to place a flat glass slide adjacent the roll and to one side of the sheeting in the path of the metal atoms moving from the target toward the sheeting . the thickness of the metal deposited on the surface of the flat slide may be readily measured . typically , the linear speed of the sheeting will be varied to control the thickness of the deposit , but it must be sufficient to avoid overheating of the resin sheeting which would cause softening and even melting . to obtain a desired thickness for the deposit , two or more passes may be required , and generally a circumferential or lineal speed of 20 - 40 feet per minute is desirable . the distance from the metal targets to the surface of the sheeting is generally within the range of 1 - 3 inches . by having the copper deposited closely following the point of the silver deposit , it is believed that the high energy copper atoms initially form an intermetallic layer with the surface portion of the silver and that this intermetallic layer provides the high degree of corrosion resistance . samples of retroreflective sheeting with only a silver deposit and the protective coating thereover corrode inwardly from the edges of the sheeting . preferably , the sheeting passes about a water cooled drum to extract from the sheeting the heat resulting from the deposition of the hot atoms of the vaporized metal . as is known , the size of the target and the energy of the electrons impinging thereon will also affect the thickness of the deposit . the target should be of greater width than the sheeting to ensure a uniform deposit adjacent the edges . the nature of the protective synthetic resin placed over the metallic deposit may vary , but it should be resistant to passage of polar substances . if a backing member is to be placed thereover , it is conveniently an adhesive which will bond a synthetic resin sheet material thereto to provide a laminate . it may also be a thermoplastic material which may be heated to render it tacky to provide adhesion to the surface . the coating itself may serve as the final backing or it may serve as the means for adhering the reflective sheeting to a substrate by use of an ever - tacky pressure sensitive adhesive and placing a release paper or film thereover . however , for most applications , a protective sheeting of synthetic plastic sheet material will be bonded to the synthetic resin coating . this in turn may be provided with a pressure sensitive adhesive coating and a release film or paper thereon . a microprism sheeting of the type seen in fig2 is produced by casting an uv - curing acrylic - modified polyester resin formulation into microprism cavities of a mold surface , pressing a polyester film of 0 . 002 inch thickness thereagainst and curing the polyester resin by ultraviolet light . the resultant microprisms have a height of about 0 . 0028 inch and center to center spacing of 0 . 006 inch . a roll of the resultant sheeting on 18 inches width is placed in a vacuum apparatus of the type illustrated in fig1 and the microprism surface is provided with a sputter coating of silver in three passes by a silver target at a linear speed of 30 feet per minute . the silver target is 24 inches long and is spaced 21 / 8 inches from the sheeting . the argon pressure is 10 - 12 mtorr and the flow rate is 65 - 70 cubic centimeters per minute ; the vacuum is 6 × 10 - 6 torr . in the last pass by the silver target , power is also applied to the copper target , which is spaced 1 11 / 16 inches from the sheeting . the power applied to both targets is 10 kilowatts , and the amperage is 15 - 18 . the now metallized sheeting is removed from the vacuum chamber and a section is examined . the sheeting as viewed through the planar face is bright white ; the microprism face has a golden color . an adhesive strip applied to the metallic deposit does not lift the deposit . next , a coating of a silicone pressure sensitive adhesive marketed by dow chemical company is applied to the surface to a thickness of about 0 . 002 inch above the apices of the prisms . specimens immersed in four percent sodium chloride solution show no signs of discoloration after seven weeks . specimens subjected to accelerated weathering in a carbon arc weatherometer show no signs of corrosion after 1000 hours of exposure . it is also observed that the sheeting provides greater retroreflection at increasing angles of incidence as compared to an aluminum metallized equivalent product . the daytime luminance represented by the tri - stimulus co - ordinate capy is increased to a value of 27 as compared to al metallized sheeting with a capy value of 11 photometric measurements at 0 . 2 ° observation angle and - 4 ° entrance angle produce values in excess of 1300 cd / lx / m 2 . samples of sheeting exposed to an outdoor atmosphere for 12 weeks exhibit no signs of corrosion of the metallic deposit . sheeting is prepared substantially in the manner described in example one except that the coating of silicone resin is stopped short of the edges to leave exposed portions of the metal deposit along the sides of the sheeting . specimens of this material placed in a salt solution begin to turn black in the uncoated areas within 24 hours , but corrosion does not proceed under the coated portion of the sheeting . thus , it can be seen from the foregoing detailed specification that the method of the present invention provides retroreflective sheeting which exhibits a bright white daylight appearance and which is highly resistant to corrosion in salt atmosphere . the metallic deposit is well bonded to the microprism surface and provides high retroreflectivity when exposed to abeam of incandescent light at night .
8
as stated above , the present invention relates to doped semiconductor wires having constant lateral dimensions and methods of manufacturing the same , which are now described in detail with accompanying figures . it is noted that like and corresponding elements are referred to by like reference numerals , and that the figures are not drawn to scale . referring to fig3 a and 3b , an exemplary semiconductor nanowire structure according to the present invention is shown , which comprises a substrate 10 , an undoped semiconductor nanowire 50 , and a catalyst particle 20 . the exemplary semiconductor nanowire is provided by first growing an undoped semiconductor nanowire 50 on the substrate 10 by catalytic growth induced by the catalyst particle 20 . the substrate 10 may comprise a semiconductor material , or an insulator material . semiconductor materials that may be employed in the substrate 10 include group iv semiconductor materials , iii - v compound semiconductor materials , ii - vi compound semiconductor materials , and alloys thereof . the insulator materials that may be employed in the substrate include dielectric oxides and dielectric nitrides . exemplary dielectric oxides include silicon oxide and dielectric metal oxides including high dielectric constant dielectric material having a dielectric constant greater than 4 . 0 such as hfo 2 , zro 2 , la 2 o 3 , al 2 o 3 , tio 2 , srtio 3 laalo 3 , and y 2 o 3 . exemplary dielectric nitrides include silicon nitride and ceramic nitrides such as aluminum nitride , strontium nitride , boron nitride , and beryllium nitride . the substrate 10 may be single crystalline , polycrystalline , or amorphous . the catalyst particle 20 comprises a material that induces catalytic growth of a semiconductor nanowire in a suitable environment . exemplary materials for the catalyst particle 20 include , but are not limited to , au , ag , cu , pt , fe , co , ni , in , ta , ti , zn , cd , and sn . the catalyst particle 20 has lateral dimensions from about 1 nm to about 1 , 000 nm , and preferably from about 1 nm to about 30 nm . the catalyst particle 20 may , or may not have a radial symmetry , i . e ., horizontal cross - sectional areas may , or may not be , a circle . the catalyst particle 20 may be a sphere , an ellipsoid , a cylinder , a cone , a regular polyhedron , an irregular polyhedron , or a combination thereof . the lateral dimensions of the catalyst particle 20 refer to characteristic dimensions of the catalyst particle 20 if such a characteristic dimension exists . for example , in case a horizontal cross - sectional area is a circle or an ellipse , the characteristic dimension may be a diameter , a major axis , and / or a minor axis . in case the catalyst particle 20 does not have a regular shaped cross - sectional area , the lateral dimensions refer to the maximum of lateral extent of a cross - sectional area . if multiple cross - sectional areas provide different lateral extents , the cross - sectional area that provides the maximum lateral extent is employed to characterize the lateral dimensions of the catalyst particle 20 . once the catalyst particle 20 is placed on the substrate 10 , the catalyst particle 20 and the substrate 10 are subjected to a condition conducive to the growth of the undoped semiconductor nanowire 50 in a process chamber , which may be a low pressure chemical vapor deposition ( lpcvd ) chamber or an ultra - high vacuum chemical vapor deposition ( uhvcvd ) chamber . the undoped semiconductor nanowire 50 is grown by catalytic growth of a semiconductor material , which is known in the art and described , for example , in u . s . pat . nos . 7 , 105 , 428 ; 7 , 211 , 464 ; and 6 , 962 , 823 supra . specifically , the catalytic growth of the undoped semiconductor wire 50 is effected by supplying a reactant containing a semiconductor material to be incorporated into the undoped semiconductor wire 50 at an elevated temperature , which is herein referred to as a first temperature . the semiconductor material of the undoped semiconductor nanowire 50 may be a group iv semiconductor material such as silicon and germanium . in case the semiconductor material comprises silicon , the reactant may be sih 4 , si 2 h 6 , sih 2 cl 2 , sihcl 3 , sicl 4 , geh 4 , or a combination thereof in case the semiconductor material comprises germanium , the reactant may be one of geh 4 , geh 4 , ge 2 h 6 , geh 3 cl , geh 2 cl 2 , gehcl 3 , and gecl 4 . alternately , the semiconductor material of the undoped semiconductor nanowire 50 may be a iii - v compound semiconductor material , or a ii - vi compound semiconductor material . in this case , the reactant comprises a mixture of precursors that provide the semiconductor material to the undoped semiconductor nanowire upon reaction with the catalyst particle 20 . the semiconductor material of the undoped semiconductor nanowire 50 may be a mixture of any semiconductor material , in which case the reactant is a combination of the various gases and / or precursors described above . the first temperature , which is the temperature employed for growth of the undoped semiconductor nanowire 50 , is selected to avoid lateral growth of the semiconductor material on sidewalls of the undoped semiconductor nanowire . pyrolysis of the reactant in the absence of the catalyst particle 20 is effected at a higher temperature than catalytic pyrolysis effected on the surface of the catalyst particle 20 . in other words , one of the functions of the catalyst particle 20 is to enable catalytic pyrolysis of the reactant at a temperature at which normal pyrolysis of the reactant would not occur without the catalyst particle 20 . the first temperature is selected so that catalytic pyrolysis of the reactant occurs directly beneath the catalyst particle 20 , while pyrolysis of the reactant does not occur on normal surfaces including sidewalls of the undoped semiconductor nanowire 50 . in case the undoped semiconductor nanowire 50 comprises silicon or germanium , the first temperature may be from about 350 ° c . to about 500 ° c ., and preferably from about 350 ° c . to about 450 ° c ., and most preferably from about 350 ° c . to about 400 ° c . typically , the undoped semiconductor nanowire 50 is entirely single crystalline since the catalytic growth induces epitaxial alignment of the semiconductor atoms during the growth . the lateral dimensions of the undoped semiconductor nanowire 50 may be substantially the same as the lateral dimensions of the catalyst particle 20 . lack of pyrolysis on sidewalls of the undoped semiconductor nanowire 50 preserves the lateral dimensions of portions of the undoped semiconductor nanowire even after the catalyst particle 20 moves away from the portion as the growth of the undoped semiconductor nanowire 50 continues . thus , the undoped semiconductor nanowire 50 has a constant cross - sectional area independent of the location within the undoped semiconductor nanowire 50 . the cross - sectional area of the undoped semiconductor nanowire 50 may be circular , elliptical , polygonal , or may be a composite shape of a curved portion and a polygonal portion . in case the cross - sectional area of the undoped semiconductor nanowire 50 is a circle , the radius ri of the circle may be from about 0 . 5 nm to about 500 nm with a corresponding radius from about 1 nm to about 1 , 000 nm , and preferably from about 0 . 5 nm to about 15 nm with a corresponding radius from about 1 nm to about 30 nm . the undoped semiconductor nanowire 50 is substantially undoped , i . e ., any dopant , if present , is at a trace level or at a level that does not increase conductivity of the undoped semiconductor nanowire to any significant level . dopants herein refer to electrical dopants that confer p - type doping or n - type doping on a semiconductor material as well known in the art . p - type dopants include b , ga , and in . n - type dopants include p , as , and sb . typically , a doping concentration of less than 1 . 0 × 10 17 / cm 3 is insufficient to induce any significant increase in the conductivity of a semiconductor material . preferably , no dopant is supplied into the process chamber during the growth of the undoped semiconductor nanowire 50 , and any dopant in the undoped semiconductor nanowire 50 is at a trace level . it is to be noted that even if dopant gases are provided within the process chamber during the growth of the undoped semiconductor nanowire 50 at the first temperature , the first temperature is insufficient to effect any significant level of dopant incorporation of the dopant gases into the undoped semiconductor nanowire . this is because the catalytic growth selectively incorporates the semiconductor material at the expense of dopant atoms that may be provided from the dopant gases . thus , even if any dopant gas is supplied into the gas stream along with the reactant , the doping concentration of the undoped semiconductor nanowire 50 is much less than 1 . 0 × 10 17 / cm 3 , thus rendering the undoped semiconductor nanowire 50 “ undoped ,” i . e ., having a doping at a level that renders the properties of the undoped semiconductor nanowire 50 essentially the same as the corresponding properties of a semiconductor nanowire with no doping . referring to fig4 a and 4b , a shell 60 of a doped semiconductor material is grown directly on and around the sidewall of the undoped semiconductor nanowire 50 by exposing the undoped semiconductor nanowire 50 to a mixture of a reactant and a dopant gas at another elevated temperature , which is herein referred to as a second temperature . this processing step may employ the same process chamber as , or a different process chamber from , the process chamber employed for the growth of the undoped semiconductor nanowire 50 . use of the same process chamber provides the advantage of preventing exposure of the surfaces of the undoped semiconductor wire 50 to an ambient gas outside the process chamber . the doped semiconductor material may comprise the same semiconductor material as , or a different semiconductor material from , the undoped semiconductor nanowire 50 . in general , any of the semiconductor material that may be employed for the undoped semiconductor nanowire 50 as listed above may be employed for the doped semiconductor material for the shell 60 . the reactant for the growth of the shell 60 is selected based on the material of the shell , and may be the same as the reactants listed above , i . e ., sih 4 , si 2 h 6 , sih 2 cl 2 , sihcl 3 , sicl 4 , geh 4 , geh 4 , ge 2 h 6 , geh 3 cl , geh 2 cl 2 , gehcl 3 , gecl 4 , and other precursors for compound semiconductors . the dopant gas comprises a gas phase compound of a dopant atom . exemplary dopant gases include , but are not limited to , b 2 h 6 , gah 3 , gacl 3 , ga 2 cl 6 , ph 3 , pocl 3 , ash 3 , sbh 3 , and sbf 3 . the dopant gas may be supplied concurrently and continuously with the reactant into the process chamber so that the composition of the shell 60 is uniform , or alternately , may be supplied intermittently into the process chamber so that the shell 60 has a layered structure with modulations in the dopant concentration within the shell 60 . dopant concentration in the shell 60 may be controlled by adjusting the partial pressure of the dopant gas and / or the ratio of the partial pressure of the dopant gas to the partial pressure of the reactant . the shell 60 grows on sidewalls of the undoped semiconductor wire 50 and at the top of the undoped semiconductor wire 50 . the catalyst particle 20 may be separated from the undoped semiconductor nanowire 50 by the growth of the shell 60 . due to the in - situ doping of the shell , i . e ., the incorporation of dopants into the shell 60 during the growth , the shell 60 comprises both a semiconductor material and a dopant . preferably , the doping concentration of the shell is from about 1 . 0 × 10 18 / cm 3 to about 5 . 0 × 10 21 / cm 3 , more preferably , from about 5 . 0 × 10 19 / cm 3 to about 5 . 0 × 10 21 / cm 3 to effect a high doping concentration level in the undoped semiconductor wire 50 after an anneal to be subsequently performed . the growth of the shell 60 is not catalytic , i . e ., the presence of the catalyst particle 20 is not necessary for precipitating the growth of the shell , although the catalyst particle 20 may enhance deposition rate of the shell 60 over the undoped semiconductor nanowire 50 . to insure that growth of the shell 60 occurs on the sidewalls of the undoped semiconductor nanowire 50 , the second temperature , i . e ., the temperature of the growth of the shell 60 , is set at a sufficiently high temperature at which pyrolysis of the reactant proceeds even without the catalyst particle 20 . in the case the shell 60 comprises silicon or germanium , the second temperature may be from about 500 ° c . to about 1 , 100 ° c ., and preferably from about 500 ° c . to about 700 ° c . the shell is typically single crystalline as the doped semiconductor material of the shell 60 is grown in epitaxial registry with the underlying undoped semiconductor nanowire 50 . the cross - sectional area of the shell 60 is independent of the location along the shell 60 . since the shell 60 laterally encloses the undoped semiconductor nanowire 50 , the inner surface of the shell 60 conforms to the outer surface of the undoped semiconductor nanowire 50 . the cross - sectional area of the shell 60 may be annular , or may comprise an expanded shape of the cross - sectional area of the undoped semiconductor nanowire 50 from which the shape of the cross - sectional area of the undoped semiconductor nanowire is subtracted . the thickness of the shell 60 may be from about 0 . 5 nm to about 100 nm , and typically from about 1 nm to about 10 n . the thickness of the shell 60 may be from about 5 % to about 100 % of the lateral dimensions of the undoped semiconductor nanowire 50 , and preferably from about 20 % to about 50 % of the lateral dimensions of the undoped semiconductor nanowire 50 , although lesser and greater percentages are explicitly contemplated herein also . in case the cross - sectional area of the undoped semiconductor nanowire 50 is a circle , the cross - sectional area of the shell is an annulus or a ring having an inner radius and an outer radius r 2 . the inner radius is the same as the radius r 1 of the circle of the cross - sectional area of the inner semiconductor nanowire 50 . referring to fig5 a and 5b , the catalyst particle 20 may be removed by a heating cycle , during which the catalyst 20 is separated from the assembly of the undoped semiconductor nanowire 50 and the shell 60 . methods of separating a catalyst particle from a nanowire after formation of the nanowire are known in the art . concurrently with the heating cycle , or subsequent to the heating cycle , the assembly of the undoped semiconductor nanowire 50 and the shell 60 is subjected to an anneal at an elevated temperature , which is typically performed at a higher temperature than the second temperature to induce diffusion of dopants in the shell 60 into the undoped semiconductor nanowire 50 , thereby converting the assembly into a uniformly doped semiconductor nanowire 70 . if the undoped semiconductor nanowire 50 and the shell 60 are single crystalline , the resulting structure after the anneal , which is the uniformly doped semiconductor nanowire 70 , is also single crystalline . the temperature of the anneal is selected to effect sufficient bulk diffusion of the dopants in the shell 60 into the undoped semiconductor nanowire 50 so that the dopant concentration in the uniformly doped semiconductor nanowire 70 is substantially uniform . for example , the anneal temperature may be from about 600 ° c . to about 1 , 200 ° c . the anneal may be performed in a furnace or in a rapid thermal anneal chamber . the duration of the anneal may be from about 1 second to about 12 hours , and typically from about 10 seconds to about 1 hour . typically , use of a high anneal temperature requires a short duration of the anneal process , while use a low anneal temperature requires a long duration of the anneal process . the doping concentration of the uniformly doped semiconductor nanowire 70 is the volume weighted average of the doping concentration of the undoped semiconductor nanowire 50 prior to the anneal , which is substantially zero , and the doping concentration of the shell 60 prior to the anneal . for example , if the volume of the undoped semiconductor nanowire 50 is v 1 , the volume of the shell 60 is v 2 , and the doping concentration of the shell 60 before the anneal is cb , the doping concentration of the uniformly doped semiconductor nanowire 70 after the anneal ca is given by : ca = cb × v 2 /( v 1 + v 2 ). in case the doping concentration of the shell is from about 1 . 0 × 10 18 / cm 3 to about 5 . 0 × 10 21 / cm 3 , the doping concentration of the uniformly doped semiconductor nanowire 70 may be from about 1 . 0 × 10 17 / cm 3 to about 5 . 0 × 10 20 / cm 3 , although higher and lower doping concentrations for the uniformly doped semiconductor nanowire 70 may be obtained by manipulation of the dimensions of the undoped semiconductor nanowire 50 and / or the dimensions of the shell 60 . thus , the present invention provides a method of forming a semiconductor nanowire having a high doping level , i . e ., a doping concentration of about 1 . 0 × 10 17 / cm 3 or greater , while maintaining the diameter of the semiconductor constant . further , the lateral dimensions of the uniformly doped semiconductor nanowire 70 may be kept at a small dimension , i . e . from about 1 nm to about 30 nm , by keeping the lateral dimensions of the undoped semiconductor nanowire 50 at such a small dimension and avoiding pyrolysis of reactants at sidewalls of the undoped semiconductor nanowire 50 . referring to fig6 . the conversion process of the assembly of the undoped semiconductor nanowire 50 and the shell 60 into the uniformly doped semiconductor nanowire 70 by an anneal is schematically shown . the anneal homogenizes the dopant distribution within the assembly of the semiconductor nanowire 50 and the shell 60 so that the uniformly doped semiconductor nanowire 70 has a substantially “ uniform ” doping concentration . referring to fig7 , two measured photoelectron spectra are shown as a demonstration of the present invention . in this experimental set up , two nanowires were subjected to a beam of photons having 6 . 2 ev of kinetic energy . photoemitted electrons were extracted with a bias potential of 15 ev so that 15 ev of energy would be added to the initial kinetic energy of the photoemitted electrons through the electrical biasing of the set up . the first nanowire comprised an undoped silicon nanowire having a diameter of 20 nm . the second nanowire comprised a uniformly doped silicon nanowire having a diameter of 29 nm and manufactured by the methods of the present invention by first forming an undoped silicon nanowire of diameter of 20 nm , followed by formation of a 4 . 5 nm thick doped silicon shell and a subsequent anneal . the doped silicon shell contained boron ( a p - type dopant ) as a doping material . a shift in the energy of the photoemitted electrons is observed in the photoelectron spectrum of the second nanowire , which is the doped silicon nanowire , relative to the photoelectron spectrum of the first nanowire , which is the undoped silicon nanowire . the shift in the energy of the photoelectron spectrum shows that the fermi level of the second nanowire shifted due to the doping of the second nanowire . in other words , the shift in the photoelectron spectra demonstrates that the second silicon nanowire is indeed doped with p - type dopants as disclosed in the present invention . referring to fig8 a - 8c , fenni level diagrams for an undoped semiconductor nanowire , a p - doped semiconductor nanowire , and an n - doped semiconductor nanowire are shown , respectively . the present invention enables formation of p - type or n - type doped semiconductor nanowires having a shifted fermi level relative to the fermi level of the undoped semiconductor nanowire shown in fig8 a . thus , the manipulation of the fermi level according to the present invention enables changes in the conductivity of a semiconductor nanowire as well as determination of charge carrier types in the semiconductor nanowire . while the invention has been described in terms of specific embodiments , it is evident in view of the foregoing description that numerous alternatives , modifications and variations will be apparent to those skilled in the art . accordingly , the invention is intended to encompass all such alternatives , modifications and variations which fall within the scope and spirit of the invention and the following claims .
8
amino acid sequences of vl and vh domains of ab 19 and ab 17 in order to determine the formulation that would provide a high degree of stability to antibodies ab 17 and ab 19 , different excipients were tested by profiling the antibodies &# 39 ; structural stability while undergoing changes ( over time and ph ) and exposure to stressful conditions ( e . g . shear stress and slow freeze - thaw cycles ) including accelerated stability studies via incubation at 50 ° c . for one - to two - weeks . at several time points ( e . g . t 0 , t 7 , t 14 ) the stability of the molecules was examined with and without stress using the following tools : right angle light scatter ( rals ), intrinsic and extrinsic fluorescence ( if , ef ) in conjunction with analytical methods like high - performance size exclusion chromatography ( hp - sec ). rals is employed to detect and monitor the subtle changes in the associative behavior of the molecule , which can result in aggregation and / or precipitation . rals monitors macroscopic changes as a soluble molecule transitions to insoluble aggregates . the if assay measures stress - induced conformational changes in proteins as observed by changes in the tryptophan environment . ef utilizes an external , non - covalent , polarity - sensitive fluorescent probe to examine a protein &# 39 ; s apparent exposure of hydrophobic clefts and to monitor possible changes in this parameter as a function of various environmental stresses and conditions . after reading initial rals or turbidity , approximately 400 ˜ μl of sample was frozen slowly in an eppendorf tube by placing it in a − 80 ° c . freezer . after freezing was complete ( minimum of four hours ), all samples were thawed on the bench top ( room temperature ). the process was repeated for a total of 5 cycles . 750 ˜ μl of the tested formulation were shear stressed in a conical glass vial using a triangular stir bar . the samples were spun at 300 rpm ( no cavitation ) for 24 hours before removal from the magnetic stirrer for analysis . sodium dodecyl sulphate poly acrylamide gel electrophoresis ( sds - page ) was performed using bis - tris gradient of 4 - 12 %. 2 μg of the antibody combination were mixed with a native sample buffer ( invitrogen ) containing 50 mm dtt and incubated for 10 min at 100 ° c . prior to loading . the gels were run at 200v for about 30 min , and then rinsed twice in ddw for 3 min . the gels were then stained with coomasie blue ( gelcode ; pierce ) while shaking for one hour , and then rinsed in ddw over night . photographs of the gels were taken using the lis - cap program in a renium camera this example describes the selection of excipients for a liquid formulation comprising the human anti hbsag antibodies ab 19 and ab 17 , ab 19 having the amino acid sequence shown in fig1 a ( light chain ; seq id no . 1 ) and 1 b ( heavy chain ; seq id no . 2 ) and ab 17 having the amino acid sequence shown in fig1 c ( light chain ; seq id no . 3 ) and id ( heavy chain ; seq id no . 4 ). ab 19 and ab 17 may be produced by hybridoma cells ( deposited at the ecacc under accession nos . 96052169 and 96052168 ), or may be prepared by recombinant methods well known in the art , e . g . by cho expression systems transfected with the genes encoding the heavy and light chain of each antibody . several ph values for the formulation were compared ranging from 5 . 0 to 7 . 5 generated using different buffers : sodium citrate , histidine or succinic acid . ab 17 and ab 19 in the different buffers were examined by if , rals , ef and sec - hplc under different conditions : incubation at 50 ° c . for seven and fourteen days , exposure to shear stress and slow freeze - thaw cycles . the formulation containing citrate at ph 6 . 5 performed best in the assays and therefore sodium citrate was chosen as the preferred buffer for the formulation . using sodium citrate as a buffer , a set of formulations containing different amino acids at a concentration of 50 mm was generated . these formulations were examined by if , rals , ef and sec - hplc , and were subjected to shear stress and slow freeze - thaw cycles . the formulations containing glutamic acid and proline scored highest , followed by the formulation containing alanine . these three amino acids were further analyzed in order to establish the feasibility of concentrating the antibodies to 100 mg / ml . the formulation containing alanine scored best in the concentration studies . since glutamic acid had scored best in the previous study , these two amino acids were chosen as the preferred amino acid stabilizers and were reexamined in a combination study including additional formulation excipients as will be described below . carbohydrates are typically used as stabilizers , isotonic adjusters , and / or bulking agents ( in the case of lyophilization ). surfactants are typically used to protect proteins against shear stress . several formulations were generated containing each 20 mm sodium citrate , 50 mm glutamic acid and a different carbohydrate or surfactant . the following excipients were examined : lactose , mannose , mannitol , sorbitol , sucrose and trehalose ( 3 %), peg - 3350 and peg - 4000 ( 1 %), tween - 20 and tween - 80 ( 0 . 1 %). all formulations were examined by if , rals , ef and sec - hplc and were stressed by shear stress and slow freeze - thaw . the formulations containing trehalose and sorbitol scored the best over time . therefore both of these carbohydrates were chosen as preferred carbohydrates for the antibody formulation and would be further examined in the combination study . the formulation containing tween - 80 ( t80 ) scored best among the surfactants and therefore t80 was chosen as the preferred surfactant for the antibody formulation . finally , based on the data described above several formulations of the antibodies were prepared examining different combinations of stabilizing excipients in order to determine the preferred combination . these combinations were tested by if , rals , ef and sec - hplc . these assays indicated that sodium citrate at ph 6 . 5 provided the greatest stability to ab 17 and ab 19 . the amino acids alanine and glutamic acid were identified as lead stabilizers for ab 17 and ab 19 , and trehalose was selected over the other strong carbohydrate stabilizer , sorbitol . the surfactant , tween 80 , was found to reduce the shear stress of the molecule . based on these findings four liquid formulations containing the preferred excipients were evaluated for selection of a preferred clinical formulation for use in treatment or prevention of hbv infections . the formulations were as shown in table 1 below . these formulations were again examined using the assays described above . under subjection to temperature , shear and freeze - thaw stress , all formulations maintained both high purities and recoveries . overall , formulation 3 performed slightly better over a 28 day stability study . this suggests that a higher alanine concentration may help to stabilize the antibodies . the stock of ab 17 ( in pbs ) was diluted 1 : 1 prior to concentrating with a solution of 20 mm sodium citrate , 50 mm alanine and 100 mm nacl in order to provide stability while concentrating . the protein was then concentrated to ˜ 89 mg / ml by tangential - flow filtration ( tff ) over the course of 4 days . the concentrated ab 17 was slightly cloudy , and there was an 80 % recovery from the tff . the antibody was buffer exchanged using dialysis tubing ( mw cutoff = 25 , 000 ) into the preferred formulation as described above . this example describes the stability tests performed on the combination of antibodies ab 17 and ab 19 in formulation 3 . stability studies were performed on samples stored under controlled temperatures at 5 ° c ., 25 ° c . and 40 ° c . combination samples were prepared containing 90 mg / ml of ab 17 + 30 mg / ml of ab 19 in 2 ml ( final concentration 60 mg / ml ) in formulation 3 containing either 0 . 1 % tween 80 or 0 . 01 % tween 80 . the samples were subjected to sds - page under reduced conditions in order to check the purity of the sample and the presence of degradation products . fig2 and 3 show antibody samples after incubation for 4 weeks in different storage temperatures ( fig2 : formulation 3 containing 0 . 1 % t80 ; fig3 : formulation 3 containing 0 . 01 % t80 ). the antibody chains remain intact in all temperatures measured as can be seen by the two distinct bands representing each the heavy and light antibody chains . no impurities and no degradation products were detected . both tween 80 concentrations tested ( 0 . 1 % and 0 . 01 %) were effective in stabilizing the antibodies . a functional property of the antibodies , i . e . binding to hbsag was measured using an immuno assay and is shown in table 3 . the specific activity ( iu / mg ) was measured at time 0 ( t 0 ) at the beginning of the incubation and compared with the specific activity 4 weeks ( t 4 ) after incubation in different temperatures . as can be seen in table 3 the specific activity of the antibodies was not significantly changed after 4 weeks incubation , providing another indication to their stability in the tested formulations . the three month stability data above shows that some 40 ° c . formulations of 17 and 19 in combination fared as well or better than similar formulations of 17 or 19 alone . following the term “ about ” used to described amounts herein , the precise amount following the term “ about ” is also contemplated in each instance . all publications , patents , and patent applications cited herein are specifically incorporated herein by reference .
0
reference is now made to fig1 which illustrates a bend - responsive catheter 20 , in accordance with a preferred embodiment of the present invention . catheter 20 includes a distal end 22 , which is preferably inserted in the heart of a subject , and a proximal end 24 , which is coupled to a control console 26 . adjacent to distal end 22 , catheter 20 includes a first position - sensing element 28 and , proximal thereto , a second position - sensing element 30 , which serves to enable determination of a bending angle of catheter 20 , as will be described below . preferably , each of elements 28 and 30 comprises three substantially orthogonal , non - concentric coils , as described in the above - mentioned pct publication wo96 / 05768 , which generate signals responsive to magnetic fields applied by field generators 32 . these signals are conveyed via wires 34 to signal processing and computing circuitry 36 in console 26 , which preferably also provides driver and control signals to generators 32 . circuitry 36 analyzes the signals , as further described in the pct publication , in order to determine the six - dimensional translational and orientational coordinates of elements 28 and 30 in relation to a frame of reference established by generators 32 . alternatively , it is sufficient that one of elements 28 and 30 comprise three such coils , and that the other of the elements comprise a single coil , as described in the above - mentioned u . s . pat . no . 5 , 391 , 199 patent . as described in the patent , three - dimensional translational coordinates of the single - coil element are determined . further alternatively , sensors 28 and 30 may comprise other types and combinations of position sensors , known in the art . it is sufficient , for example , that element 28 be such as to enable determination of three - dimensional translational coordinates and two - dimensional angular elevation and azimuth coordinates with respect thereto , while three - dimensional coordinates are determined with respect to element 30 . if bending of catheter 20 is constrained to a plane , as shown in fig2 a and described below , it is sufficient to determine two - dimensional coordinates of element 30 . catheter 20 preferably includes a resilient longitudinal member 38 , for example , a coil spring element , which is fixed within the catheter along a longitudinal axis thereof . preferably , there is a sufficient distance between metal parts of member 38 and sensors 28 and 30 so that the metal parts do not significantly distort the magnetic fields at the sensors . such distortion may be caused , for example , by eddy currents induced in the metal parts or by bending of the magnetic field lines by ferromagnetic materials . on account of member 38 , catheter 20 has a generally constant elasticity over at least a portion 40 of its length , preferably extending at least from element 30 , or from another point proximal thereto , out to distal end 22 , or at least to element 28 . portion 40 of catheter 20 is preferably short enough , generally less that about 9 cm long , so that it is inserted entirely into a chamber of the heart with no more than a single bend in the portion . as a result , when portion 40 is bent , whereby element 30 is translationally displaced and orientationally rotated by a known angle relative to element 28 , portion 40 will assume an arcuate or helical shape having a known radius of curvature , determined by the known angle . fig2 a illustrates , for example , a case in which portion 40 of catheter 20 is bent in a plane , which we take to be the plane of the page without loss of generality . the length of portion 40 is taken to be l , as shown . respective first and second local coordinate axes 50 ( x o , y o , z o ) and 52 ( x 1 , y 1 , z 1 ) are defined at the positions of first and second elements 28 and 30 , wherein the local z - axis is taken in every case taken to be aligned with the longitudinal axis of catheter 20 , generally parallel to member 38 . the six - dimensional position coordinates of first element 28 are determined and used to define the element &# 39 ; s translational position and first local coordinate axes 50 . the orientation coordinates of second element 30 define second local axes 52 , which together with axes 50 determine a bend angle θ , as shown . an arc is thus defined having a radius of curvature given by r = l / θ , and a center of curvature 54 at a position y = r defined with respect to coordinate axes 50 or 52 . the elasticity of member 38 ensures that portion 40 will generally follow this arc , so that the position of any point within portion 40 of catheter 20 may be conveniently determined . fig2 b schematically illustrates the more general case , in which catheter 20 is free to twist in three dimensions . in the case shown here , portion 40 of catheter 20 has been twisted about its longitudinal axis by approximately 180 °, so that axes x 1 and y 1 of second local axes 52 are oriented in generally opposite respective directions to axes x 0 and y 0 of local axes 50 . the elasticity of member 38 causes portion 40 to assume a generally right - helical form , within the bounds of a cylinder 54 having a diameter r c and length d , as shown in the figure . the length d is defined by the translational displacement of element 30 relative to element 28 , but determining r c generally requires solving an integral equation . preferably , solutions to the equation are stored in the form of a look - up table , preferably within signal processing circuitry 36 , as is known in the art . r c and d then determine the pitch of the helical form , so that the position of any point within portion 40 of catheter 20 may again be conveniently determined . preferably , portion 40 of catheter 20 will not be allowed to twist by more than 180 ° in either the clockwise or counterclockwise direction , so that the relative rotational coordinates of elements 28 and 30 will be unambiguous . if necessary , however , the twist of portion 40 may be continuously monitored , by analyzing the signals received from the elements , as catheter 20 is being inserted into and manipulated inside the body , so that rotations of greater than 180 ° will be detected . these greater twist angles are then used in appropriately determining r c , as described above . in the preferred embodiments described above , it is assumed that portion 40 of catheter 20 is free to move within a body cavity , and that the shape and configuration of portion 40 are determined substantially by its own elasticity . portion 40 is caused to bend by a combination of a compressive axial force , generally exerted from proximal end 24 of catheter 20 by a user , such as a physician , and a lateral deflecting force exerted on distal end 22 by body tissue with which the distal end is in contact . fig3 schematically illustrates an alternative preferred embodiment of the present invention , in which catheter 20 bends controllably , not necessarily in an arcuate or helical form , by means of a steering mechanism 56 . preferably , mechanism 56 comprises an electronically - or mechanically - controlled deflection element , operating under the control of console 26 , as described in the above - mentioned pct patent application no . pct / il97 / 00159 . alternatively , mechanism 56 may comprise any suitable catheter steering or deflection device known in the art . catheter 20 is sufficiently rigid , except in an immediate vicinity of mechanism 56 , so as to bend only in the immediate vicinity of the mechanism . the position coordinates of elements 28 and 30 are used to measure the deflection angle θ , whereby the location of any point along portion 40 of catheter 20 may be determined . preferably , the measured deflection angle is also used to provide feedback for closed - loop control of mechanism 56 . fig4 schematically illustrates another preferred embodiment of the present invention , which is similar to the embodiments described above except that in place of second position - sensing element 30 , catheter 20 as shown here includes a bend sensor 80 , responsive to the angle of bending of the catheter . bend sensor 80 preferably comprises at least one piezoelectric element , or more preferably , three such elements 82 , 84 and 86 as shown in the figure . the piezoelectric elements are mechanically coupled to resilient member 38 , so that when member 38 is bent , as described above , the bending force is conveyed to and acts upon the elements . as is known in the art , the piezoelectric crystals generate voltage signals that are generally proportional to this bending force , which signals are conveyed by wires 34 to signal processing circuitry 36 in console 26 . each of elements 82 , 84 and 86 includes a piezoelectric crystal having a crystal axis aligned orthogonally to the axes of the other two elements , so that each crystal generates signals responsive to bending of catheter 20 about a different axis . thus , as shown in fig4 element 82 generates signals responsive to twisting of catheter 20 about its longitudinal axis , and elements 84 and 86 generate signals responsive to left - right and up - down bending , respectively . due to the generally constant elasticity of member 38 , the signals generated by elements 82 , 84 and 86 can be used to derive the bend and twist angles of portion 40 of catheter 20 . these angles are taken together with the translational and orientational coordinates determined with respect to position - sensing element 28 , in order to determine the positions of the plurality of points of interest along the length of catheter 20 . other types of bend sensors may be used in place of sensor 80 shown in fig4 . for example , strain gauges may be substituted - for piezoelectric elements 82 , 84 and 86 . such strain gauges have an electrical resistance that varies as a function of mechanical strain applied thereto , as is known in the art . alternatively , fiberoptic sensors , as are known in the art , may be used to determine the bend angle of catheter 20 , by measuring the loss and back - reflection of light conveyed through an optical fiber embedded in the catheter . furthermore , additional bend sensors of other types may be positioned at different locations along the length of catheter 20 , so that multiple bends or bends of non - constant radius of curvature can be detected . more generally speaking , while the preferred embodiments of the present invention have been described above with reference to one or two position - sensing elements 28 and 30 and a single bend sensor 80 , it will be appreciated that for some applications , catheter 20 may preferably comprise a greater number of position sensors and / or of bend sensors . such additional sensors may be particularly useful when a portion of the length of the catheter must be tracked within a convoluted passage , or when the catheter is brought to bear against and is desired to conform to a convoluted surface within a body cavity . preferably , however , the number of such sensors is held to the minimum needed to achieve the desired accuracy of determination of the plurality of points along the length of the catheter . although for simplicity of illustration , catheter 20 has been shown and described above as comprising only the sensors and other elements necessary for the operation of the present invention , in preferred embodiments of the present invention , the catheter preferably includes other sensing and / or therapeutic devices , as are known in the art . the principles of the present invention may then be applied , for example , to map physiological activity or apply local therapeutic treatment within a body cavity , such as a chamber of the heart , with greater ease and accuracy than methods and devices known in the art . it will be appreciated that the principles of the present invention may be applied , as well , to other flexible medical probes , such as endoscopes . it will further be appreciated that the preferred embodiments described above are cited by way of example , and the full scope of the invention is limited only by the claims .
0
the present invention is a culling device 2 comprising a cable element 4 , a retainer element 6 and a floating element 8 . the retainer element 6 may attach the device 2 to an animal , preferably a fish . the floating element 8 comprises a center section 10 and two dial sections 12 , the two dial sections being controllably adjustable to indicate the weight of the animal to which the device 2 is attached or to be attached . the cable element 4 is attached at one end to the retainer element 6 and is attached at the other end to the floating element 8 . the retainer element 6 may be comprised of any suitable material , though metal is preferred . the metal should be resilient and rustproof , given the exposure to water and the natural elements encountered when fishing . it is preferred that the retainer element 6 be a closable loop hook , one that can easily puncture the mouth of a fish and is sturdy enough to remain attached on the fish through fish activity , including struggling , swimming , diving and collision . the cable element 4 may be comprised of any suitable material , though coated wire is preferred , and plastic - coated wire is more preferred . the cable element 4 should be resilient , non - frayable and rustproof , given the exposure to water and the natural elements encountered when fishing , and may be of any practical length . it is preferred that the cable element 4 be between about twelve inches to about eighteen inches in length . the floating element 8 may be comprised of any suitable material that floats . it is preferred that the floating element 8 substantially consist of plastic with a specific gravity of less than one , and it is more preferred that the floating element 8 substantially consist of high density polyethylene . in an embodiment , the floating element 8 is comprised of plastic and a foam , such as polystyrene , and in such an embodiment it is preferred that the plastic completely enclose the foam , and in such an embodiment it is possible for the plastic to have a specific gravity of more than one , as long as the foam present in the floating element causes the floating element as a whole to be buoyant . the floating element 8 may further comprise one or more dial display openings 16 . one of the dial sections 12 may further comprise pound number surface 32 and the other dial section 12 may further comprise an ounce number surface 36 . in a preferred embodiment , the dial display openings 16 permit the view of only the desired numbers and that have been printed on the pound number surface 32 and ounce number surface 36 to be readable , while not revealing the other numbers printed on the pound number surface 32 and ounce number surface 36 . this is a preferred , though not required , configuration , as it improves readability of the device . it is preferred that , on the surface of the center section 10 , adjacent to the dial display opening 16 which permits the view of the pound number surface 32 is a pound indicator 34 , which indicates to the user that the number being viewed through that particular display opening 16 is a weight in pounds . similarly , it is preferred that , on the surface of the center section 10 , adjacent to the dial display opening 16 which permits the view of the ounce number surface 36 is an ounce indicator 38 , which indicates to the user that the number being viewed through that particular display opening 16 is a weight in ounces . the floating element 8 may further comprise a ring extension 30 . the ring extension 30 permits the attachment of the cable element 4 to the floating element 8 . any suitable manner known by those of ordinary skill in the art for attaching the cable element 4 to the floating element 8 is acceptable , and the ring extension 30 may be of any suitable general shape , though a substantially circular protrusion from the center section 10 is preferred . in a particularly preferred embodiment of the present invention , the floating element 8 comprises a center section 10 and two dial sections 12 . the center section 10 comprises a ring extension 30 , two dial mount mechanisms 14 , and two dial display openings 16 . the dial mount mechanisms 14 are on substantially opposite sides of the center section 10 . each dial section 12 is attached to the center section 10 on substantially opposite sides of the center section through rotatable attachment to a dial mount mechanism 14 . in this particularly preferred embodiment , each dial mount mechanism 14 comprises a button 18 , an axle 20 , and a spring 22 . the axle 20 is a substantially cylindrical piece extending from the center section 10 and having a groove 24 bisecting the axle 20 through a diameter of the axle . the button 18 is a substantially flat piece residing at least partially within the groove 24 and having at least one locking peg 26 extending therefrom . the spring 22 resides at the base of and at least partially within the groove 24 such that the spring 22 , when compressed , provides a force parallel to the height of the axle 20 and along the groove 24 against the button 18 away from the center of the center section 10 . the angler may press and release the button 18 through a depression extension 42 , which is a protrusion on the button 18 extending through the dial section 12 and at least partially beyond the end of the axle 20 . in this particularly preferred embodiment , the dial sections 12 each comprise a series of peg - accepting notches 28 , and the peg - accepting notches 28 are circumferentially equidistant from one another . each dial section 12 may be independently rotated around the axle 20 upon depression of the button 18 and compression of the spring 22 , thereby disengaging the at least one locking peg 26 from a peg - accepting notch 28 . upon raising the button 18 and the expansion of the spring 22 , the at least one locking peg 26 may engage a peg - accepting notch 28 . in this particularly preferred embodiment , one end of the cable element 4 is attached to the ring extension 30 of the center section 10 , and the other end of the cable element 4 is attached to the retainer element 6 . the cable element 4 comprises a flexible metal cable that has been coated in a thin plastic layer . in this particularly preferred embodiment , each dial section 12 has sixteen peg - accepting notches 28 . the peg - accepting notches 28 on each dial are circumferentially equidistant from one another , are substantially identical in size and shape , reside within a concave portion of the dial section 12 , which faces towards the center section 10 , and are substantially complimentary in shape to the one or more locking pegs 26 . one dial section 12 further comprises a pound number surface 32 , and the other dial section 12 further comprises an ounce number surface 36 . both the pound number surface 32 and the ounce number surface 36 are numbered in consecutive whole number integers from zero to fifteen . the center section 10 further comprises a pound indicator 34 and an ounce indicator 38 . in this particularly preferred embodiment , each dial section 12 further comprises eight dial grips 40 , circumferentially equidistant from one another . in this particularly preferred embodiment , a number on the pound number surface 32 is visible through the dial display opening 16 adjacent to the pound indicator 34 , and a number on the ounce number surface 36 is visible through the dial display opening 16 adjacent to the ounce indicator 38 . the angler may adjust the number visible on the pound number surface 32 , the ounce number surface 36 , or both , by pressing the depression extension 42 on the button 18 downward , thereby compressing the spring 22 and disengaging one or more locking pegs 26 from one or more peg - accepting notches 28 , and rotating the desired dial 12 until the desired number appears in the respective dial display opening 16 . then the angler will release the depression extension 42 , thereby expanding the spring 22 , and engaging the one or more locking pegs 26 into one or more peg - accepting notches 28 . in an embodiment , the dial sections 12 may further comprise dial grips 40 , which may be of any suitable shape or size known to those of ordinary skill in the art , to serve the purpose of enabling the angler to grip the dial section 12 and rotate it around the axle 20 . the present invention further includes an embodiment where the floating element 8 comprises a center section 10 and a single dial section 12 , wherein the pound number surface 32 and ounce number surface 36 are one in the same . the present invention further comprises a method of culling fish , the method comprising the steps of catching a first fish , weighing the first fish , adjusting a culling device 2 to indicate the weight of the first fish , and attaching the culling device to the first fish . preferably , the method further comprises the steps of catching a second fish , weighing the second fish , determining that the second fish has a greater weight than the first fish , adjusting a culling device 2 to indicate the weight of the second fish , and attaching the culling device to the second fish . the culling device being used on the aforementioned second fish may or may not be the same culling device being used on the aforementioned first fish . the angler may optionally remove the culling device from the first fish , and use that device on the second fish , or he may place a different culling device on the second fish , and subsequently remove the culling device from the first fish and return the first fish to the wild . the present invention further includes a kit , the kit potentially comprising a plurality of culling devices 2 . the kit may also further comprise a scale . it should be understood that the aforementioned embodiments are for exemplary purposes only and are merely illustrative of the many possible specific embodiments that can represent applications of the principles of the invention . without departing from the spirit and scope of this invention , one of ordinary skill in the art can make various changes and modifications to the invention to adapt it to various usages and conditions , including those not specifically laid out herein . as such , those changes and modifications are properly , equitably , and intended to be , within the full range and scope of equivalents of the invention disclosed and described herein .
0
as shown in fig1 , a computer is connected to the internet . computer includes an internal bus that facilitates communication of information ( i . e ., digital data ) between and among the various devices of the computer and that also facilitates communication between the computer and external devices and systems via a communication interface . a processor coupled to the bus processes information within the computer . the computer also includes a memory such as , for example , random access memory ( ram ) and / or other equivalent dynamic memory storage devices , coupled to bus for receiving and storing instructions communicated from the processor . memory may also be used to temporarily store variable or other intermediate information while the processor executes instructions . read - only - memory ( rom ) is also coupled to the bus for storing static data and instructions for use by the processor . various input and output devices are provided as part of computer , including , by way of non - limiting example , a display 154 ( e . g ., cathode ray tube ( crt ), liquid crystal display ( lcd ), etc . ), an input device such as a keyboard , and a cursor control device such as a mouse , or trackball , for example . a data storage device such as , for example , a magnetic disk drive and magnetic disk , a cd - rom drive and cd - rom , a dvd - rom drive and dvd - rom , or other equivalent devices and data storage mediums , is coupled to the bus for communication with the processor , main memory , and communication interface . the storage device preferably has an operating system and an internet browser software program ( i . e ., a browser ) stored thereon . as will be discussed in greater detail below , a client - side module may also be stored on the data storage device . the computer may communicatively connect to the internet via the communication interface over one or more transmission media including , but not limited to , coaxial cable , copper wires , and fiber optical cables . communication between the computer and the internet may also be via a wireless or cellular interface . the communication interface facilitates two - way communication between the computer and another electronic device or system , e . g ., a server computer or computers provided by a content provider . an internet user using the computer may gain access to the internet by causing the browser to execute , thereby opening a communication link between the communication interface of the computer and an internet site of content provider , via an internet service provider ( isp ). internet content is communicated by the content provider to the computer for display by browser . alternatively , a content provider may also be an isp . in alternative embodiments , computer may be a desktop or notebook computer , pda , hand held device , or wireless phone ( with graphics capability ), or any other device now known or hereafter developed that is capable of performing the functions as described herein . in accordance with an embodiment of the invention , toolbar , the content provider for the toolbar , may provide an internet user with access to a program for controlling the browser . when executed by the user , the controlling program downloads or creates a client - side module such as , for example , a dynamic link library ( dll ), on the data storage device of the internet user &# 39 ; s computer . the client - side module preferably includes activex control or plug - in functionality . thereafter , when the internet user accesses the internet using the browser , the browser opens the client - side module and preferably automatically establishes a connection to the content provider &# 39 ; s internet site . the content provider , in response to the connection established by the browser , loads information and / or functional data into a shell operating within the browser and created by the client - side module . for example , if the user has an account with toolbar , customized information and / or functionality may be loaded into the client - side module . if the user does not have an account , more generalized ( e . g ., guest ) information and / or functionality may be loaded . the client - side module essentially opens a shell ( or a plurality of shells ) within the browser that contains the activex control or plug - in code that may control , i . e ., add , remove , and / or modify , the internet browser , alternatively the current invention may reside in a stand alone window . when loaded with the activex control or plug - in , the client - side module preferably contains functions , objects , data , and other software , referred to generally herein as information , that may be used to control the browser . the present invention ensures that the client - side module ( and shell ) does not close when the internet user moves , for example , from internet to another . thus , the information and / or functionality provided via the activex control or plug - in is not lost when the internet user disconnects from the internet site that loaded the activex control or plug - in , and connects to another internet site . in alternate embodiments client - side module may be located at a remote location from the internet user . the client - side module takes the form of customizable toolbars . an embodiment of the invention may be provided as a feature of a method of controlling an internet browser interface displayable by an internet browser on a display of a computer , and enabling a user of the computer and internet browser to access and navigate the internet , receive updated information on targeted websites and to receive and display on the computer display one or more web pages from one or more internet sites , including the display of a web page from a predetermined internet site , the internet browser having at least one internet browser toolbar having at least one toolbar button providing a predetermined functionality to the user of the computer and internet browser , the method can comprise providing , at the predetermined internet site , access to a program for controlling the internet browser interface and making available for downloading by the predetermined internet site , a file for causing the display of a persistent user toolbar adjacent to said internet browser toolbar so as to create the visual impression that the user toolbar is an integrated part of the internet browser , the user toolbar making additional functionality that is not part of the internet browser prior to download available to the user after download as part of the internet browser interface , such that once the user toolbar is displayed the user toolbar remains displayed and said additional functionality remains available to the user regardless of a subsequent internet site to which the internet browser is caused to navigate after download . the method of controlling a browser may be implemented using , by way of non - limiting example , a downloadable toolbar . an internet user may customize the browser so that each time the user accesses the internet using the browser , user - defined information and / or functionality , e . g ., a customizable button on a toolbar , will be displayed with the browser interface . in addition , the toolbar may also include mybartab , search , tabbers tablet , add tablet , bookmark tablet , feeds tablet , photos tablet , videos tablet , podcast tablet , music tablet , email tablet , news tablet , and inbox tablet . the customizable button acts like a typical toolbar button , except an internet user can edit the title , the uniform resource identifier ( uri ), and displayed icon related to the button . when the toolbar is executed , the client - side module can receive some , none or all of the toolbar buttons from toolbar . the toolbar buttons and their characteristics may be obtained through a feed from toolbar , the content provider to the client computer . the request for customizable buttons may be part of a request for the contents of a downloadable toolbar . the request may be an explicit request for customizable button characteristics and / or a content provider may automatically send customizable button characteristics in response to a general request for toolbar content . in an embodiment of the invention , before the request for customizable button characteristics is received by the server , the user at client would sign into or open a new account with the toolbar . in that embodiment , no customizable button is displayed until the user signs into an account . having an account with the content provider and allowing toolbar to store button characteristics allows multiple users who use the same computer to each have their own button characteristics when using the same computer . another benefit of certain embodiments is that the same user can use his or her personalized button characteristics at different computers without having to re - set those characteristics at the different computers . alternatively , if the client does not have an account with the content provider or the client is not signed in , the content provider may transmit standard or generic button characteristics . in the preferred embodiment , users can create tablets on the toolbar which launches multiple applications in a tablet window . this tablet window can serve as a startup page , a collection of modules , or information for a particular interest . with the ajax features it will make it easy for users to organize and personalize their toolbars and tablets . alternatively , users can browse other user &# 39 ; s toolbar and tablets in the community and replicate their toolbar and tablet if they find it useful . users can add on and improve on existing toolbars and tablets making it even more useful and contain more content for everyone in the community . users can share and improve on toolbar — adding more functions and content for users . users may also share and improve on tablet — adding more functions and content for users . users can create specific toolbar that they can use and share only with people they choose . ideally toolbar will eventually be a central place where users can do anything online , just from a toolbar by bypassing useless information on the internet . in an alternate embodiment toolbar will allow users to share and send useful content to other users . a toolbar community will exists where users can not only network with each other but contribute back to their community by sharing their content — news , photos , videos , bookmarks , feeds , toolbars and tablets which others might find useful and can pass along to their friends . users can discover new sites from other user &# 39 ; s bookmarks . users can receive instant alerts / deals on their toolbar . toolbar allows users in the community to actually share toolbars and tablets that they personally created . users would also be able to easily share any of their digital content with other users . one aspect of the current invention to provide a platform where tabbers can easily send each other messages , videos , photos , games , bookmarks of sites they find interesting , and whatever they would like to share . the toolbar community aims to provide tabbers with a central place that they can share , give and help each other in making their online experience a more productive , efficient , and fulfilling one . toolbar homepage will allow users to choose and navigate from at least 5 different selections . the first selection is for users to sign up and download our toolbar . users will come to our website and see the different functionalities and possibilities of our toolbar . users will be able to see a demo of how they can customize their own toolbar , share their toolbar with others , add other users &# 39 ; toolbars for their own use , and communicate with other users in our toolbar community . once users decide to sign up for our toolbar , there will be a download button . as shown in fig2 , the preferred user selection of content for personalized toolbars . there will be at least two methods users will be prompted to our download page . one is when they click the join toolbar button from our homepage . second is when first time users browse through our website and see a toolbar or tablet they are interested in and click the add toolbar button . either method will prompt them to a sign up page which they will be required to fill out their personal info — name , birthday , location , email , and toolbars they are interested in having on their toolbar . once user identification process is complete users will be able to download our toolbar . if the users came from clicking the add toolbar button , then that toolbar or tablet will automatically be added to their toolbar toolbar when the download process is finished . once the download is complete , a screen will appear which introduces said users to their default toolbar , the other toolbars they have selected , and the functions in their toolbar . they will also be shown that they have successfully downloaded their toolbar and only a few short steps from using the most customizable toolbar available on the internet . in the profile page , users will be shown how they can customize their profile . they can either go through with the demo or skip . next , users will be prompted to the last step which leads them to a page that shows a demo on how they can start customizing their toolbars . this demo will elaborate a little bit more on tablets ( ref . tablet page ) and the applications and features they can add to their toolbar — allowing them to either skip that page and start using their toolbar . they can either skip this demo or press finish which ends their sign up process . the other way a user will be prompted to our download page is simply to click on sign up on our homepage . the same steps will apply as above . once users have downloaded the toolbar and start using it , every tablet that they click on will have a demo on that particular tablet or tab . as shown in fig3 , the preferred method for users to customize their toolbars . the second selection is for users to search , browse , and add toolbars as well as see other users that have the same toolbar . on bartabs , bars page , users will be able to search by category , enter a search term in our search area , or search by tags for the toolbar that they might want to add . ex : if they are into sports , they can browse under sports and see all the different toolbars created for that category . users will also see a list of the most popular and most recently added toolbars . users will also see a preview of the different toolbars which contains a title , description , tags , who created the toolbar , when it was last updated , how many times it has been added as well as comments and ratings of the toolbar . the bar page also displays all the tabbers that have a particular toolbar . ex : if someone searches for a sports toolbar , it will display a list of all the tabbers that own a sports bar . once users click on the preview for a particular toolbar , it will open another page that gives more details of that specific toolbar . once a user arrives at bartabs toolbars page ; they will see a list of most popular toolbars . in the preffered embodiment , users will see a list of toolbars by categories , tags , and most recently added . once category is selected , the category will collapse into subcategories that list all the toolbars in that subcategory . the page will also display a preview of the toolbar in the main category as well as a preview of the toolbars in the subcategory . ex . users click on the main category sports , it will collapse into all subcategories for sports such as basketball , football , baseball , hockey , golf , soccer , tennis , motor racing , cycling and other sports . the page will display a preview of the sports toolbar and all the subcategory toolbars such as basketball , football , baseball , soccer , golf , and so forth . the toolbar toolbar comprise at least five parts ; the options menu , the tablets on the toolbar which are the main features of the toolbar , the tabs on the toolbar which are the other toolbars broken down into tabs , an add bar button , and a search function . the option menu allow for users to adjust any settings on their toolbar and customize the colors of their tablets and toolbars . the option menu also contains a function for sign in / out , an about us , and settings . tablets are buttons which launch applications such as bookmarks , feeds for photos , videos , news , sports , comics , stocks , and alerts . tablets can also launch other interactive applications such as calendars , weather , calculator , maps , music players , and many more . the tabs on the toolbar are other toolbars a user has added on their browser . new tabs are created once a user adds any additional toolbar to their browser . the default tab would be called mybar which is their default toolbar . once a user clicks on a different tab on their toolbar , the tablets will change accordingly to the new toolbar chosen . the add bar button allows users to add an additional toolbar on their browser . the search function on the toolbar is powered by google and allows users to search anything they want . the results would be the search results from google . there is a drop down menu next to the search box that allows users to choose the type of content they are searching for : image , videos , news , blogs , or local . here is a list of the different tablets that would be on the default toolbar once a user downloads it . users then can add the toolbar they want by clicking on the add button icon on the preview of the toolbar . the tabs on the toolbar are other toolbars a user has added on their browser . new tabs are created once a user adds any additional toolbar to their browser . once a user clicks on a tab the toolbar will update to that tab as well as all the tablets on the toolbar . from there users can use the tablets on the toolbar they have chosen . users can click a button on their tab which will allow users to share , edit or delete the tab . once they click add , the toolbar will be added on their browser . the user also has the option of clicking on the preview of the toolbar for more information . once they do this , a new page will open where users would be able to see all the details of that toolbar . the page will show the toolbar and all the tablets in that toolbar . on this page there will be two tabs : one will be called mytab and the other will be called all . under the mytab tab , there is a list of all the tablets that were originally created for the toolbar . then under the all tab , there will be a list of all the tablets for that toolbar that have been added by other users since it was first created . once they click add , the toolbar will be added on their browser . then they can choose to add additional tablets that are available for the toolbar they just added . users will also be able to click on other users on the toolbar page since the site will show the users that have the same toolbars as them and this will lead them to the user &# 39 ; s profile page . through the users profile page , they can see the different toolbars and tablets they have and can add their toolbars and tablets . the add bar button on the toolbar will direct user &# 39 ; s to our toolbar page where users can select from a list of popular toolbars , a list of categories , or search for a specific toolbar they are looking for . once they have found the toolbar they want , they can easily add it by the click of a button . then a new tab would be automatically created with the new toolbar they added . when a user decides to add a toolbar , they can add a toolbar from a list of existing toolbars or they can customize their own toolbar . if a user decides to customize their own toolbar , they will be prompted to add a title , description , and tags for their toolbar . from there , users will be offered a list of suggested tablets that can be added based on the keywords they tagged their toolbar with . if they choose not to add any of the suggested tablets , they can search for other tablets . another option would be for the user to create personalized tablets which can be added to their toolbar . once users have finished customizing their new toolbar , they will have the option of sharing it to others or making it for personal use . as shown in fig4 , the preferred method of customizing tablets . tablets are buttons which launch applications such as bookmarks , feeds for photos , videos , news , sports , comics , stocks , and alerts to name a few . tablets can also launch other interactive applications such as calendars , weather , calculator , radio , maps , music players and games . tablets can include feeds , podcasts , apps , menus and allow users to customize them according to their needs . once a user clicks any tablet on their toolbar , a new page will drop down . the drop down page would contain all the content or applications a user has in their tablet . users can also add more content to their tablets from the drop down page . there would also be a settings feature where users can edit the privacy of their tablet allowing only for private use , sharing it with friends only , or sharing it with the toolbar community . in the settings feature , users can also edit or delete tablet , change the title , description , tags , layout , colors and display . the page would also show all the tabbers that have the same tablet , enabling them to interact with each other and potentially share other useful content . users may search , browse , and add tablets as well as see other users that have the same tablets . tablets are buttons which launch applications such as bookmarks , feeds for photos , videos , news , sports , comics , stocks , and alerts . in an alternative embodiment , tablets can also launch other interactive applications such as calendars , weather , calculator , radio , maps , music players , and many other uses . tablets can include feeds , modules , and allow users to customize the tablet according to their needs . on our tablets page , users will be able to search by category or tags for the tablet that they might want to add . ex : if they are interested in sports , they can browse under sports and see all the different tablets created for that category . users can also see a list of the most popular , most recent , and the most tagged tablets . users can also see a preview of tablets which contains a title , description , tags , who created the tablet , when it was last updated , how many times it has been added as well as comments and ratings of the tablet . users would also be able to choose the type of tablet that they are looking for — whether they are feeds , apps , tablets which can contain both feeds and apps in them , or menus which can contain multiple tablets . the tablet page also displays all the tabbers that have a particular tablet . ex : if someone searches for a sports tablet , it will display a list of all the tabbers that own a sports tablet . once users click on the preview for a particular tablet , it will open another page that gives more details of that specific tablet . the tablet page will also allow developers and users to create new tablets from our api section . once a user arrives at the mytab tablets page ; they will see a list of our most popular tablets . they will also see a list of tablets by categories , tags , and most recently added . once a user clicks on a category , the category will collapse into subcategories that list all the tablets in that subcategory . the page will also display a preview of the tablet in the main category as well as a preview of the tablets in the subcategory . ex . users click on the main category sports , it will collapse into all subcategories for sports such as basketball , football , baseball , hockey , golf , soccer , tennis , motor racing , cycling and other sports . the page will display a preview of all the tablets in that category such as basketball , football , baseball , soccer , golf , and so forth . users then can add the tablet they want by clicking on the add button icon on the preview of the tablet . once they click add , the tablet will be added on their toolbar . the user also has the option of clicking on the preview of the tablet for more information . once they do this , a new page will open where users would be able to see all the details of that tablet . on this page there will be two tabs : one will be called mytab and the other will be called all . under the mytab tab , there is a list of all the contents that were originally created for the tablet . then under the all tab , there will be a list of all the different content for that tablet that have been added by other users since it was first created . once they click add , the tablet will be added to their toolbar . then they can choose to add additional content for the tablet they just added such as feeds or apps . users will also be able to click on other users on the tablet page since the site will show the users that have the same tablets as them and this will lead them to the user &# 39 ; s profile page . through the users profile page , they can see the different toolbars and tablets they have and can add their toolbars and tablets . when a user decides to add a tablet , they can add a tablet from a list of existing tablets or they can customize their own tablet . the existing list of tablets that would be available includes tablet , feeds , apps , or menus . users can then choose the different types of tablet they would like to add to their toolbar . ex : if they choose to add a feed tablet , they will only be shown tablets that perform feed functions such as a scores feeds or stats feeds . if they choose an apps tablet , they will be shown a list of apps tablet such as games , maps , currency exchanger , and so forth . if a user decides to create their own tablet , they will be prompted to add a title , description , and tags for their tablet . then a user must choose the type of tablet they want to create . there choices would be : feed template , apps template which will bring them to our developers api section , or menu template . from there , users will be offered a list of suggested content that can be added based on the keywords they tagged their tablet with . if they choose not to add any of the suggested content , they can search for other content . a person that decides to create a feed tablet would be offered a suggested list of feeds to add to that template . however they can enter their own feed url on our feed tablet template and add as many feeds as they want . once they &# 39 ; re done with the feeds , they can click finish and now have their own customized tablet . once users have finished customizing their new tablet , they will have the option of sharing it to others or making it only for personal use . as shown in fig5 , the preferred embodiment of the method to customize the tabbers . tabbers are users who have downloaded our toolbar toolbar . each tabber would be assigned their own website and inbox . each tabber would be able to personalize and customize their toolbar according to their needs . tabbers will also have a profile that they can customize to their level of content . tabbers can add photos , videos , bookmarks , blogs , instant messaging , to do lists , bulletin board , games , and many other unique features on their profile . each tabber has the option of setting different privacy options which can set their toolbars , tablets , and profile to private , allowing no one to see any of their content . they can also set it so that only they &# 39 ; re friends have access to their content or they may make it available for all users to see . the same privacy options would be considered when other users are trying to contact each other . we aim to build a toolbar community where tabbers can easily communicate and share with each their content , but also respect each tabber &# 39 ; s preference to keep their content private . we aim to be able to provide a platform where tabbers can easily send each other messages , videos , photos , games , bookmarks of sites they find interesting , and whatever they would like to share . we want tabbers to be able to discover , meet , network , connect , learn , help , share , and give to other tabbers within our unique toolbar community . the tabbers page contains all users and contains a search function that one can search by location , age , gender , interest , or other tabbers that have the same toolbars or tablets . the tabbers page also lists tabbers by most popular , most recent , last login , and most active . the tabbers page also displays a list of popular groups where users can join , add photos , videos , music , blogs , forums , share and discuss matters they have in common . once a user arrives at our the tabbers page , they will have the option to search for tabbers based on their preference such as age , gender , location , interest and so forth . the search result will bring about the tabbers within their query . users can also see a list of the most popular , recently joined , or most active tabbers . once a user clicks on a tabber they find interesting , they can explore their page and if they find that tabber interesting , they can contact them or request to add them as a friend . users can also join groups by clicking on the groups they are interested in . once they click on groups , they will see all the tabbers in that group and what the group is about and join that group . 1 . toolbar toolbar having a tablet + addbar if user clicked on that it will display a slider window with the options like add to videos , add to feeds , . . . and add to site tracker , from this option user can add urls or some content on the web page to site tracker for monitoring . 2 . we need to provide some interface to user from where he can manage there web pages information , given below . b . adding new web page url c . editing existing web pages url d . removing existing url ( s ) e . setting frequency each url ( if user want then only , other wise it is set to default frequency which is set by site tracker admin ), user can set minimum 3 hr or more frequency . 3 . if any change exist in user added content / url from toolbar it will display a slider window with in it highlighting the changed content , if user clicked on the slider window it will display the same page ( actual url ) in browser with changed content highlighting . 1 . url limit : every user having there own limit value for adding number of web pages to site tracker for now it is fixed to 100 , for all users initially this value is set to default value which is set from the site tracker admin panel by site tracker admin . . . . 2 . even site tracker admin can set the urls adding limit to particular user ( s ). ex :— like i want to allow my corporate people to 200 urls / contents . 3 . crawler frequency : site tracker admin can set the crawler ( s ) default crawling frequency value from control panel by default this value will be applicable for all crawler . . . . 4 . even site tracker admin can set frequency value for selected crawler . 5 . managing number of crawlers : site tracker admin can add crawlers and can set the crawler details from admin panel . like . . . . a . crawler1 — visit sites 1 to 1000 with default frequency 1 day . . . . b . crawler2 — visit sites 1001 to 1500 with default frequency 2 days . . . . 6 . and admin should be able to manage the crawlers information adding / removing / modifying frequency . 1 . site tracker web server will be a dedicated server , which will serve all site tracker information to toolbar , users . 2 . site tracker database server will be a dedicated server with high bandwidth capacity , it contain all the information about site tracker system . 3 . site tracker crawler server this will be a dedicated server with high bandwidth capacity , it always depend upon the site tracker database for getting frequency , sites information , . . . and after crawling site tracker crawler server will keep information in site tracker database . 4 . and the site tracker deployment may contain more than one site tracker crawler server and it can be added at any time with out disturbing the existing system and those servers can be located in any location . 5 . site tracker crawling logic may improve at any time with out affecting the existing system . 6 . site tracker crawling frequency logic may improve at any time with out effecting existing system . 7 . all servers are located at remote places . while the above invention has been described with reference to certain preferred embodiments , the scope of the present invention is not limited to these embodiments . one skilled in the art may find variations of these preferred embodiments which , nevertheless , fall within the spirit of the present invention , whose scope is defined by the claims set forth below .
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[ 0032 ] fig1 is a perspective view of a representative heat exchange plate 3 used in the indirect evaporative cooling apparatus and processes of this patent disclosure . such a plate forms a common wall between a dry channel and a wet channel of applicants &# 39 ; indirect evaporative cooling apparatus . as indicated previously , the term “ plate ”, as used herein , is not intended to be limited to a flat plane . such a plate can be shaped for a particular installation and include curved , angled , spiraled , corrugated or otherwise contoured configuration to better function as a heat transfer surface in a given application . in all cases , one side of the plate is one wall of the wet side channel and the other side is a wall of the dry side channel . applicants &# 39 ; indirect evaporative cooling processes begin by passing an incoming stream of gas 2 ( such as air , nitrogen , carbon dioxide , industrial waste gas , etc . and / or mixtures thereof ) over a dry side , heat transfer surface 3 d of the heat exchange plate 3 . the opposite , wet side of this plate 3 is designated 3 w . in certain embodiments of this invention , such a plate 3 is made from a single layer of a hard , smooth , waterproof or low permeability material 4 such as a sheet of plastic , metal or ceramic material . during the course of some of the hereindescribed indirect evaporative cooling processes , the dry side 3 d of plate 3 is cooled by an evaporation process that has taken place on the plate &# 39 ; s opposite , wet side 3 w . this cooled condition of the dry side surface 3 d of the plate 3 can be used to reduce the temperature of the incoming gas ( e . g ., air ) 2 ( preferably , without increasing the humidity of the incoming gas ). thus , the incoming gas 2 is given a lower wet bulb temperature . again , such a lower temperature can be utilized to great advantage in the process of evaporating a coolant liquid 1 ( such as water ) in applicants &# 39 ; wet side channel . the heat required for the evaporation of a portion of the evaporative liquid coolant ( e . g ., water ) into the cooled gas stream in the wet side channel is gained from heat flow across the heat exchange plate 3 ( i . e ., from its dry side 3 d to its wet side 3 w ). that is to say that the heat flow across plate 3 creates a heat flux on the wet side of the plate that serves to increase the evaporation rate of the evaporative liquid into that portion of the gas stream 2 which is then passing through the wet side channel . thus , the dry side 3 d of the plate 3 , and the gas stream 2 passing by the dry side 3 d of the plate 3 ( and through it ) are cooled . this dry side channel cooling will often be referred to as “ pre - cooling ” for the purposes of this patent disclosure . the temperature , pressure , relative humidity and flow speed of the gas stream 2 in the wet side channel — in conjunction with the heat passing through the heat exchange plate — will cause a portion of the evaporative liquid ( e . g ., water 1 ) to be evaporated into that portion of the gas stream 2 then passing through the wet side channel . this evaporation , in turn , causes cooling of the wet side surface 3 w of the plate 3 as well as cooling of the remaining evaporative liquid that continues to flow down the wet side surface 3 w of the plate 3 . in other words , a portion of the evaporative liquid has taken up its heat of vaporization and passed into a vapor phase that is taken up into the gas stream 2 as it passes through the wet side channel . the temperature of the remaining evaporative liquid , in its still liquid state , is also thereby lowered . in the ideal case , the temperature of the remaining liquid at the bottom of the heat exchange plate will approach the dew point temperature of the gas ( e . g ., air ) passing through the plate to the wet side channel . the evaporation of the evaporative ( coolant ) liquid 1 in applicants &# 39 ; wet channel also causes the gas stream 2 in the wet channel to increases in humidity . the temperature of the gas stream passing through the wet channel is also increased . the resulting warmer , more humid gas stream is then removed from the wet side channel . it can be discarded or utilized as desired . [ 0036 ] fig1 also depicts how a portion of the incoming gas stream 2 ( e . g ., from about 5 % to about 100 %, and more preferably from about 20 % to about 100 % thereof ) passes from the dry side 3 d of the plate 3 to its wet side 3 w through an array of holes , perforations , micro sieves or gas - permeable portions h 1 , h 2 , h 3 . . . h n in the otherwise impermeable plate 3 . it might also be noted here that the impermeable quality of the remainder of the surface area of the plate 3 serves to reduce the overall pressure drop between a relatively higher dry side channel pressure and a relatively lower wet side channel pressure . this , in turn , reduces the energy required to operate ( and the necessary size of ) applicants &# 39 ; indirect evaporative cooling apparatus . thus , the size and / or spacing of the holes in the plate ( s ) can be varied to meet various operating requirements for a given indirect evaporative cooling duty . [ 0037 ] fig1 also illustrates another preferred embodiment of this invention . it is concerned with the direction of gas flow in a wet side channel relative to the direction of gas flow in a dry side channel . for example in fig1 the passage of the incoming gas stream 2 is initially directed in a generally downward direction 2 a on the dry side 3 d of the plate 3 . after passing through the array of holes ( h 1 , h 2 , h 3 . . . h n ) in the plate 3 , the resulting sub - streams ( e . g ., 2 x , 2 y , 2 z ) of the gas portion that passed through the holes ( h 1 , h 2 , h 3 . . . h n ) can then be directed through a wet side channel in a substantially horizontal , cross - flow direction 2 b such as that depicted in fig1 . a gas moving device 11 such as a fan can be used to produce this cross - flow . flow through the wet channel also can be directed in the generally vertically upward , direction 2 c depicted in fig1 . this vertically upward direction 2 c is in a substantially counter - flow direction ( i . e ., 180 ° opposite ), relative to the vertically downward flow direction 2 a of the gas stream 2 on the dry side 3 d of the plate 3 . gas flow 2 through the wet side channel also could be at some angle θ that is neither vertical ( a counter - flow direction approximating direction 2 c ) nor horizontal ( a cross - flow direction approximating direction 2 b ). for example this angle θ could be 30 °, 45 °, 60 °, etc . that portion ( e . g ., 5 % to 100 % of the original air volume ) that passes through holes h 1 , h 2 , h 3 . . . h n , then goes into direct contact with the evaporative cooling liquid 1 moving down the wet side 3 w of the plate 3 . after passing through the body of the plate 3 , the gas can then flow in a cross - flow , counter - flow ( or some combination of cross and counter - flow suggested by the angle symbol θ ) direction defined by the orientation of the wet side channel walls . here again , tradeoffs are involved . for example , use of a cross - flow direction 2 b ( or its direct opposite direction ) in the wet channel requires less pressure drop between the dry side channel and the wet side channel . the advantage of a counter - flow direction in the wet side channel is that it allows a lower temperature to be obtained as relatively more of the gas is drawn from near its dew point temperature ( more likely resulting from a longer travel distance down the dry side , 3 d ). thus , another preferred embodiment of this invention is to cause the incoming gas 2 undergoing the pre - cooling processes , to flow in the same direction ( e . g ., downward ) as the coolant flow in the wet channel ( e . g ., downward ). that is to say that , under these flow direction conditions , the remaining evaporative liquid is progressively cooled to progressively lower and lower temperatures as it flows further and further downward along the heat exchange plate 3 . any gas 2 flowing deeper ( e . g ., downward ) in to the dry channel is likewise progressively cooled to lower and lower temperatures . [ 0040 ] fig1 also suggests that if the incoming gas 2 is heated by some outside heat source 7 before the gas is pre - cooled in the dry side channel ( for example , by using waste , heat or solar energy ), the available latent heat / cooling capacity of the indirect evaporative cooling processes and apparatus of this patent disclosure can be increased by a greater amount than the sensible heat which is added . this is especially true in high absolute humidity climates where the dew point temperature of ambient air is higher than about 60 ° f . to 70 ° f . ( depending upon the elevation of the site ). above these dew point temperatures , the effect of changing absolute humidity , with changing temperature , will become even larger . it should be emphasized , however , that it is only through a process of pre - cooling the gas 2 entering the dry channel that the hereindescribed psychometric principles can be fully applied . similar principles are applicable to the use of a warmer incoming evaporative liquid ( see item 8 ) as such heating of an incoming evaporative liquid stream 10 will have the same effect as pre - heating the incoming gas 2 . although the heating as illustrated in fig1 ( e . g ., by heat source 7 ) is positioned to heat the incoming gas 2 , the particulars of the individual application or process may dictate that such heating of the gas may occur in the middle of the flow , or for only a portion of the gas . [ 0041 ] fig2 depicts an evaporative liquid flowing , in the form of a series of droplets 1 , descending along the wet side 3 w of a plate 3 . the plate 3 is depicted as being comprised of a single layer of an impermeable , solid material . for example , such a heat exchange plate can be made of a sheet of plastic , metal or ceramic material . item 2 a of fig2 depicts how a remaining portion ( e . g ., 0 % to 95 %) of the incoming gas volume can be routed around the bottom 3 b of the plate 3 and then forced to flow in a counter - flow direction 2 c ( relative to the incoming flow direction 2 a ) in a wet side channel ( not otherwise shown ). by way of contrast with the single layer plate shown in fig2 fig3 depicts a two layered plate 3 . it has a layer of a solid , impermeable material 4 and a layer of a porous , absorbent material 9 . evaporative liquid droplets 1 are shown flowing through the body of the porous , absorbent layer material . the porous , absorbent material 9 , can absorb , adsorb and / or , to some degree , hold back the evaporative liquid 1 as it flows downward along the wet side 3 w of the plate 3 under the influence of gravity . applicants have found that if the downward flow of an evaporative liquid is hindered by its passage through a porous , absorbent material 9 ( e . g ., burlap , cotton , metal shavings , ceramic or cellulose ), in close proximity to the wet side of a solid , impermeable layer material 4 of the two layered plate 3 , the evaporation rate of the coolant liquid will be significantly increased . in effect , the surface tension of the evaporative liquid ( e . g ., water ) is reduced , and thereby allowing easier evaporation of that liquid . [ 0043 ] fig4 depicts a hole - containing heat exchange plate 3 having two layers 3 ( 1 ) and 3 ( 2 ). that is to say this plate 3 has two sub - layers i . e ., a dry side impermeable layer 3 ( 1 ), a wet side porous layer 3 ( 2 ). the porous layer is shown being provided with an evaporative liquid 1 . fig4 also shows the wet side layer 3 ( 2 ) provided with baffles or spacer blocks 6 ( a ), 6 ( b ) and 6 ( c ). these spacer blocks are useful in constructing indirect evaporative cooling apparatus having a series of ( spacer block - abutting ) heat exchange plates . such baffles or spacer blocks should not impede a cross - current flow in the wet side channel if that is the desired flow direction . another preferred embodiment of this invention , shown in fig5 is depicted as being constructed from a series of hole - containing heat exchange plates 3 ( 1 ), 3 ( 2 ), 3 ( 3 ), etc . that are held in a spaced - apart relationship by virtue of the fact that these plates are all affixed to a common base 14 . these plates are so adapted and arranged such that an alternating series of dry channels 15 ( a ), 15 ( b ), 15 ( c ), etc . and an alternating series of wet channels 16 ( a ) and 16 ( b ) etc . are created . the common base 14 to which the plates are attached also can form a pan or reservoir ( or multiple reservoirs ) for a liquid coolant and / or for a liquid desiccant . both the incoming evaporative liquid 1 and the incoming gas 2 are shown entering this indirect evaporative cooler from its top side . the incoming gas 2 eventually leaves this apparatus in a plurality of horizontally directed sub - streams 2 ( a ), 2 ( b ), etc . that are shown respectively exiting the wet channels 16 ( a ) and 16 ( b ) formed by spaced - apart heat exchange plates 3 ( 2 ), 3 ( 3 ) and 3 ( 4 ), 3 ( 5 ). an outlet for the evaporative liquid 1 can be a drain pipe ( not shown ) from the pan ( s ) or other liquid reservoir ( s ) in the base 14 of this apparatus . some of the plates of fig5 can be two layered in nature . for example , one side of plates 3 ( 3 ) and 3 ( 4 ) could be made of a solid , impermeable material ( plastic materials are especially well suited for this purpose ) while the other side of these plates can be provided with an evaporative liquid — wettable , absorbent material 9 ( e . g ., burlap ). layers of such absorbent materials are preferably laminated or otherwise attached to the solid , impermeable plate material . [ 0045 ] fig6 depicts a particularly preferred embodiment of this invention wherein the heat exchange plates are horizontally and vertically alternating arrays of corrugated sheets . for example , the corrugated sheets that produce vertically directed channels are designated v ( a ), v ( b ) and v ( c ). the downwardly directed arrows 2 depict a gas entering these vertical channels . those corrugated sheets whose channels having a horizontal orientation are designated h ( a ), h ( b ) and h ( c ). thus , the resulting array is one having a vertical series of channels , a horizontal series of channels , another vertical series of channels and so on . these two kinds of sheets are fixedly attached to each other in this “ alternating ” ( vertical flow / horizontal flow / vertical flow , etc .) fashion . some or all of these sheets can be provided with holes such as those holes 5 shown in vertical corrugated sheet v ( a ). thus , incoming gas 2 entering vertical channel 1 vc ( 1 ) can pass through hole 5 ( a ) and then , for example , flow in the downward direction 2 ( x ) suggested in fig6 . similarly , air entering vertical channel 2 vc ( 2 ) can pass through and exit another hole 5 ( b ) and then flow in the downward flow direction 2 y and so on . [ 0046 ] fig7 depicts another indirect evaporative cooling apparatus made according to the teachings of this patent disclosure . it has an series of vertically directed channels ( formed from an array of corrugated sheets ) and an alternating series of horizontally directed channels ( formed from a cross - current carrying array of corrugated sheets ). these corrugated sheets are separated by hole - containing plates 3 ( 1 ), 3 ( 2 ) . . . 3 ( n ). by way of example only , an evaporative liquid 1 is shown running down the wet side surface of the outside plate 3 ( 1 ). these plates may also be provided with solid or liquid desiccant materials and / or layers of porous , absorbent materials 9 . [ 0047 ] fig8 depicts an array of plates having respective vertical and horizontal gas flow orientations . these spaced - apart , heat exchange plates 3 ( a ), 3 ( b ), 3 ( c ) and 3 ( d ) can be provided with liquids in various ways . for example , the wet side 3 w of plate 3 ( a ) is shown being provided with droplets 1 of an evaporative liquid . fig8 also suggests how a porous material 9 could be placed between plate 3 ( b ) and 3 ( c ). this apparatus can be further modified by providing the dry surface of certain plates , e . g ., the dry side of plate 3 ( a ), with a desiccant 12 . such a desiccant can be a wet , flowing desiccant or a dry desiccant that is attached to the dry side surface of the plate . the holes could be a micro sieve or similarly selective porosity material to create a higher pressure drop across the plate and only allow certain size molecules to pass through . for example , the material could pass air but not a liquid desiccant . thus , a lower pressure created in a wet channel will allow regeneration of a desiccant in the dry channel as the water vapor can pass through the porous plate into the wet channel . [ 0048 ] fig9 shows yet another preferred embodiment of applicants &# 39 ; apparatus . the vertical channels 15 ( 1 ) and 15 ( 2 ) are the dry channels that receive an incoming gas such as air . the horizontal channels 16 ( a ) and 16 ( b ) are wet channels that receive the gas that has passed through holes in the plates , e . g ., holes h 1 , h 2 , h 3 . . . h n in plate 3 ( 1 ). fig9 also suggests how a porous , absorbent material 9 can be attached to the wet side of at least one of these plates . a dry desiccant also can be attached to at least one dry side of another plate . moreover , a plate with a porous absorbent material 9 laminated thereon can be backed up to a waterproof side of a desiccant carrying plate . these various kinds of plates can be assembled in alternate fashion . the coolant liquid 1 can be directed into the apparatus through a pipe 10 from which said coolant liquid is further distributed in troughs positioned along the upper regions of the apparatus . used liquid desiccant can be collected in a pan 14 and thereafter concentrated by passing said used liquid desiccant down a wet plate side of a wet channel . as a result of this , any water contained in the used ( and hence , water - containing ) liquid desiccant is evaporated from a liquid desiccant / water system . as more and more water is evaporated from such a liquid desiccant / water system , the liquid desiccant becomes more and more concentrated . the resulting regenerated liquid desiccant can then be sent back to the dry side channel ( by devices not shown ) where it is again used to dehumidify incoming gas . [ 0050 ] fig1 shows another embodiment of the present apparatus wherein two dry channels 15 ( 1 ) and 15 ( 2 ) and two wet channels 16 ( 1 ) and 16 ( 2 ) are created by assembling a series of plates . a given plate can be further provided with a layer of absorbent material 9 on the wet channel side of any given plate . a liquid desiccant 13 is shown entering the top of the device so that it can flow ( preferably as a film ) along a dry side of a given plate . the liquid desiccant can be regenerated outside the device in known ways or it can be regenerated within this apparatus by replacing an incoming evaporative liquid ( e . g ., water ) with a weak solution ( e . g ., one containing more water ), of a liquid desiccant 13 taken from a dry side channel reservoir 14 . use of the weak liquid desiccant in place of a water coolant in the wet channel will allow evaporation of water from the liquid desiccant owing to a relatively lower pressure in the wet side channel relative to a relatively higher pressure in the dry side channel . again , the weak liquid desiccant will become more concentrated as water is evaporated from the liquid desiccant . the resulting cooled and reconcentrated desiccant in reservoir 17 could be used as a coolant before being again used to dehumidify air entering the dry side channel 15 . it might also be noted here that the cooled liquid desiccant leaving the dry channel and reservoir 14 could also be used as a process coolant liquid before it is returned to the hereindescribed process . yet another embodiment of the present invention is shown in fig1 . in cross section , it shows how certain dry channels 15 and wet channels 16 can be created by use of pairs of matching , rectangular shaped , corrugated plates 20 . these plates are preferably made from an impermeable material . the wet channels 16 also can contain a porous material 21 that is positioned between the corrugated plates 20 . pairs of matching rectangular corrugated plates 20 are set , in symmetrical fashion , opposite each other , to form the dry channels 15 and they , in turn , are offset to form the wet channels 16 . the rectangular corrugations formed between the plates 20 are comprised of ridges 22 and valleys 23 . the ridges 22 are shown to be longer than the valleys 23 . the corrugations in the valleys 23 contain holes or perforations 5 which allow a gas such as air to flow between the dry channels 15 and the wet channels 16 . this also allows gas flow through a wetted porous material 21 positioned between the corrugated plates 20 . this corrugated configuration has the advantage of creating a relatively large surface area that allows greater heat transfer between the dry channels 15 and wet channels 16 . there is also less thermal resistance for heat flux between the channels themselves . therefore , the overall heat transfer rate is increased by this arrangement . [ 0052 ] fig1 also shows a solid desiccant film 12 applied to the inner surfaces of the dry channels 15 , preferably on the outside of the valleys 23 . thus , this apparatus is capable of dehumidifying the incoming gas . it is also capable of internally regenerating the desiccant 12 . for example , regeneration of the desiccant can be accomplished by a pressure drop across the dry channel 15 to the wet channel 16 . it also should be noted that with this arrangement only one type of plate is needed since the valleys 23 have an existing dry side on the plate within a wet channel 16 . this plate uniformity also serves to reduce the manufacturing cost of this apparatus . [ 0053 ] fig1 shows another embodiment of the present invention wherein incoming air 2 enters from both the left side and the right side of the indirect evaporative cooling apparatus , through its dry channels 15 . the respective streams of air ( e . g ., streams 2 ( l ) and 2 ( r )) flow inwardly and pass inward through a respective array of holes 5 in each plate 3 . a porous , absorbent material 9 can be provided on the opposite side of such plates within the wet channels 16 . the coolant liquid 1 can be distributed evenly over the top surfaces of the wet channels 16 so that , by gravity , the coolant liquid 1 passes downward through a porous material layer 9 attached to the wet side of the plates 3 . baffles or spacers 6 can be provided within the wet channels 16 to guide the exhaust gas sub - streams 2 ex 1 , 2 ex 2 . . . 2 ex 6 as they leave the apparatus . in this embodiment , the exhaust gas is shown being directed upwardly in a counter - flow direction to the downward flow of the incoming coolant liquid 1 . [ 0054 ] fig1 depicts applicants &# 39 ; indirect evaporative cooling apparatus 100 being used as a component of a more complex apparatus comprising a fan system 106 , applicants &# 39 ; cooling apparatus 100 and a water cooling tower 104 . applicants &# 39 ; cooling apparatus 100 takes ambient air 2 delivered by the fan system 106 , cools that air 2 and then delivers it ( e . g ., in one or more streams such as the three separate streams 120 , 122 and 124 depicted in fig1 ) to the water cooling tower 104 . the top of the water cooling tower 104 is shown receiving a stream of water 108 in need of cooling . the cooling apparatus 100 is depicted as having two cooling regions 112 and 114 . cooling region 114 is not a separate and distinct region from region 112 , but rather region 114 is merely an extension of region 112 . that is to say that the two cooling regions are created by virtue of some of the incoming air 2 passing over a greater length of any given cooled plate ( not otherwise shown in fig1 ). the incoming air 2 is delivered to an array of dry side channel openings . this air 2 passes through the dry side channels in a direct flow direction ( e . g ., from left to right ) over an initial portion of an array of heat exchange plates ( e . g ., such as the array shown in fig8 ). a first portion of this air 2 flows through a first group of holes in the heat exchange plates and then is directed in an upwardly directed , cross - current flow direction . this first portion of air is shown leaving the first region 112 and passing over a baffle plate 118 that is attached to the outside of the cooling apparatus 100 . the portion of air passing over the top of the baffle plate is shown flowing rightwardly through a top region of the water cooling tower 104 . it is generally designated as sub - streams 120 . these sub - streams 120 are relatively warm and relatively humid air . a second portion of the rightwardly flowing air 2 passes over an extended portion of the same array of heat exchange plates . consequently , this second portion of the rightwardly moving air is in longer contact with the cooled plates . hence , this second portion of air becomes relatively cooler than the first portion of air removed from region 112 . the second portion of air flows through a second group of holes in the plates that are further downstream from the first group of holes through which the first portion of air passed . the second portion of air leaving region 114 is also directed in an upwardly direction , cross - current flow direction . this second portion of air is shown leaving the second region 114 and then flowing rightwardly through a middle level of the water cooling tower 104 . this second portion of air is generally lower than the first portion of air and is generally designated as sub - streams 122 . these sub - streams 122 are relatively cooler than sub - streams 120 . they also may be relatively more humid . a third portion of the air 2 entering the cooling apparatus lob is shown passing directly through the dry side channels ( i . e ., without passing through holes in the plates and without being directed in an upward cross - current flow direction ). this third portion of air is shown leaving the second region 114 and flowing through a lower level of the cooling tower 104 . this third portion of air is generally designated as sub - streams 124 . these sub - streams 124 are relatively cooler than sub - streams 122 . these sub - streams 124 will however be relatively dryer than sub - streams 122 and 120 . thus , a stream of water 108 entering the top of the water cooling tower 104 will be progressively cooled as it descends down said tower to a reservoir 125 from which a stream 126 of cooled water can be removed . the embodiments , described in the specifications and drawings of this patent disclosure are illustrative of the present invention , but are not intended to limit the scope thereof . it also is to be understood that this invention can be applied to a wide variety of cooling devices e . g ., cooling towers , industrial heat exchangers , air conditioning apparatus , etc . it also should be appreciated that the indirect cooling devices described herein can be expanded to any desired size to accommodate the cooling duties of a given cooling operation . therefore , changes in the processes disclosed herein , as well as changes in the details of construction of various physical components thereof , may be made without departing from the spirit of this invention .
5
fig1 represents a conventional train system 1 comprising a vehicle body v , one bogie frame g , and two solid axle wheelsets w , wherein each wheelset comprises two wheels either side of the axle . the body v is equivalent to the body of half a vehicle or carriage in a high speed train vehicle . the bogie g is used to carry and guide the body along a track or line . bogies have traditionally been used in train designs as a “ cushion ” between vehicle body and wheels to reduce the vibration experienced by passengers or cargo as the train moves along the track . the wheelsets w and bogie g are connected by a primary suspension system k p / c p . only longitudinal ( x direction ) and lateral ( y direction ) connections are represented in fig1 . any suitable suspension system may be used , such as a steel coil or steel plate framed bogie g with laminated spring axlebox suspension . the ( lateral and longitudinal ) connections of the primary suspension system k p / c p are represented by equivalent ‘ spring - damper ’ circuits , each circuit comprising a spring of stiffness k p in parallel with a damper of damping constant c p . a secondary suspension system k s / c s is included between the body v and the bogie g , e . g ., making use of an air suspension . the secondary suspension system k s / c s may also be represented by equivalent “ spring - damper ” circuits , wherein each circuit comprises a spring k s in parallel with a damper c s . accordingly , the train system 1 shown in fig1 represents an example of a “ two stage suspension system ,” which includes a primary suspension system and a secondary suspension system . it will be appreciated , however , that the train system may be a “ single stage suspension system ,” which includes a single suspension system between the body and the wheelsets . the longitudinal connections in the system of fig1 contribute to the yaw modes and only these contributions are accounted for in the model described below . vertical , longitudinal and roll modes are not included in this model . the conventional train system 1 of fig1 may be described by a seven degrees - of freedom ( 7 - dof ) model including lateral and yaw modes for each wheelset ( y w1 ; θ w1 ; y w2 ; θ w2 ) and for the bogie frame ( y g ; θ g ), and a lateral mode for the vehicle body ( y v ). system 1 may be modeled by eqs . ( 1 )-( 7 ) listed below , with parameters defined in table 1 shown in fig2 : a state - space form can be derived from equations ( 1 )-( 7 ) as given by : x =[{ hacek over ( y )} w1 , y w1 , { hacek over ( θ )} w1 , θ w1 , ŷ w2 , y w2 , θ w2 , θ w2 , ŷ g , y g , { grave over ( θ )} g , θ g , { hacek over ( y )} v , y v ] t . w =[ 1 / r 1 , θ c1 , y t1 , 1 / r 2 , θ c2 , y t2 ] t . the vector w is used to define the inputs from the railway track ( curvature , cant and track lateral stochastic displacement ). when entering a curve , the track cannot change from straight to the nominal value of the radius ( r 1 ; r 2 ) and cant angle ( θ c1 ; θ c2 ) immediately . a conservative assumption is made in that r 1 ; r 2 and θ c1 ; θ c2 are ramped with 3 seconds transition time . in fact , for high speed trains a longer transition time is appropriate depending on the vehicle and track type . the straight track lateral stochastic inputs ( y t1 ; y t2 ) are of a broad frequency spectrum with a relatively high level of irregularities . in the example provided below , y t1 ( t ) is defined to be the output of a second order filter h ( s )=( 21 . 69 s 2 + 105 . 6s + 14 . 42 )/( s 3 + 30 . 64s 2 + 24 . 07s ) whose input is a process with a single sided power spectrum given by : s s ( f s )= a v /( f s ) 2 in which a v is the track roughness factor , f s is a spatial frequency in cycles / meter . the body lateral acceleration is quantified in terms of the root mean square ( r . m . s .) acceleration j1 , and evaluated using the covariance method , time domain simulation method and frequency calculation method . the results by the three methods are all consistent . for the frequency calculation , j 1 is expressed by : t d is the time delay of the track input between the front and rear wheelsets , which equals 21 wx / v seconds , where 1 wx is the semi - longitudinal spacing of the wheels and v is the system &# 39 ; s speed in the longitudinal direction x . a nominal speed v is assumed to be equal to 55 m / s . using the default suspension layout and parameter settings , with velocity v varying between 1 m / s and 55 m / s , it can be calculated that the least damping ratio ( ldmp ) equals 6 . 45 % ( which is achieved at the nominal speed ). using the covariance method , it can also be calculated that , with y t1 and y t2 as input , the maximum lateral body acceleration ( macc ) equals 0 . 2204 m / s 2 when the velocity equals 55 m / s . recent investigations ( see for example ingenia online , “ why railscrack ,” andy doherty , steve clark , robert care and mark dembosky , issue 23 june 2005 ) have shown that the main cause for track wear is the phenomenon called rolling contact fatigue ( rcf ) which occurs in bodies in rolling contact . such bodies can damage one another in various ways depending upon the severity of the contact pressure and the shear in the area where the bodies come into contact . in the case of railway systems , rcf is primarily due to excess wheel — rail forces . these are primarily caused by the axle shifting relative to the rail . excess wheel - rail forces in train systems such as the system 1 shown in fig1 are directly related to high values of the primary longitudinal spring stiffness k px , which provides high yaw stiffness . high yaw stiffness k px gives good high speed stability but results in very high creep forces that are responsible for rcf . apart from yaw stiffness , there are direct measures of track wear such as the wear work which is a measure of energy dissipated at the wheel - rail interface . to reduce track wear , a system according to the present invention uses inerters in the lateral suspensions . this has the effect of reducing track wear by reducing , for example , yaw stiffness k px , as will be described below . in accordance with the present invention , the system 2 of fig3 comprises the same elements of the conventional system 1 of fig1 described above ( see also fig4 ( a ) and 5 ( a ) ), and additionally comprises inerter devices b in the lateral connections of the primary and / or secondary suspension systems ( in the y direction ) as shown in fig4 ( b ), 4 ( c ), 5 ( b ), and 5 ( c ) . in its most general form , an “ inerter ” represents a mechanical two - terminal element comprising means connected between the terminals to control the mechanical forces at the terminals such that they are proportional to the relative acceleration between the terminals . inerters are defined by the following equation : f = b ⁢ ⅆ ( v 2 - v 1 ) ⅆ t , where f is the applied force and b is either a fixed term or a variable function representing the ‘ inertance ’ of the system ; v 1 and v 2 are the corresponding velocities of the two terminals . in the 7 - dof model defined above according to equations ( 1 )-( 7 ), the yaw stiffness k px is minimized . the restrictions are for ldmp to be above 5 % across all velocity values ( 1 - 55 m / s ) and macc to be at least as good as the nominal value ( 0 . 2204 m / s 2 ). the primary and secondary lateral spring stiffness ( k py , k sy ) is fixed , and the optimization is made firstly for the secondary lateral suspension only and then for both the primary and secondary suspensions . results for a conventional system 1 ( without inerters ) as shown in fig1 are compared with results obtained for a system 2 in accordance with the present invention . these results show that a 6 % improvement in the value of k px can be obtained by using the inerter devices . all parameter values have been constrained to be within physically reasonable ranges , e . g ., the values of spring stiffness cannot be arbitrarily large . fig7 ( a ) and 7 ( b ) show the lateral body acceleration ( macc ) and least damping ratio ( ldmp ) as a function of velocity for the optimization only including the secondary lateral suspensions . the continuous curves represent the conventional system system 1 , as shown in fig1 ( without inerters ). the dashed curves represent system 2 in accordance with the present invention as shown in fig4 ( c ) . fig8 ( a ) and 8 ( b ) show the lateral body acceleration ( macc ) and the least damping ratio ( ldmp ) as a function of velocity for the optimization involving both the primary and secondary lateral suspensions . the continuous curves represent the conventional system 1 , as shown in fig1 ( without inerters ). the dashed curves represent system 2 in accordance with the present invention as shown in fig4 ( c ) and fig5 ( c ) . from fig5 ( a )- 5 ( c ) and fig6 , it can be seen that the constraints on ldmp and macc are all satisfied ( ldmp is above 5 % and macc is at least as good as the nominal value 0 . 2204 m / s 2 ). preferably , a system 2 in accordance with the invention comprises at least one series damper - inerter system in the lateral primary or secondary suspension system . however , it will be appreciated that it is possible to have many combinations of inerters with dampers or other mechanical parts of the lateral suspension systems . embodiments in accordance with the invention may comprise inerter - damper combinations at one or more connection points between the wheelsets w and bogie g , as well as between the bogie and body v shown in fig3 .
1
this invention relates to compounds of the general formula i useful in this novel method of treatment : ## str2 ## or a pharmaceutically acceptable salt thereof wherein : r 1 is : ( b ) ( c 1 - c 6 )- alkyl , ( c 2 - c 6 )- alkenyl or ( c 2 - c 6 )- alkynyl each of which is unsubstituted or substituted with a substituent selected from the group consisting of : i ) phenyl or naphthyl as defined in r 1 ( c ), ( c ) aryl , wherein aryl is defined as phenyl or naphthyl which is unsubstituted , mono - or disubstituted with substituents selected from the group consisting of : ( d ) heteroaryl , wherein heteroaryl is defined as a 5 - or 6 - membered heteroaromatic moiety selected from the group consisting of thiophene , furan , thiazole , oxazole , pyridine or pyrimidine , which is unsubstituted , mono - or disubstituted with substituents selected from the group consisting of : -- a 1 -- a 2 -- a 3 -- a 4 -- is : ## str3 ## n is : 0 to 2 ; and r 2 is : ( b ) ( c 1 - c 6 )- alkyl or ( c 2 - c 6 )- alkenyl each of which is unsubstituted or substituted with one of the following substituents , ( c ) aryl , wherein aryl is phenyl or naphthyl , which is unsubstituted or substituted as defined in r 1 ( c ), ( d ) -- ch 2 - aryl , wherein aryl is phenyl or naphthyl , which is unsubstituted or substituted as defined in r 1 ( c ), or r 6 and r 7 on adjacent carbon atoms can be joined together to form a ring structure : ## str4 ## a represents : a ) -- y -- c ( r 4 )═ c ( r 4 )--, y is -- o --, -- s ( o ) n -- and nr 5 ; and ( b ) ( c 1 - c 6 )- alkyl , unsubstituted or substituted with ( c 3 - c 7 )- cycloalkyl , ( g ) when r 9 and r 10 are on adjacent carbons , they can be joined to form a phenyl ring , ( i ) ( c 3 - c 7 )- cycloalkyl , unsubstituted or substituted with ( c 1 - c 6 )- alkyl , ( k ) ( c 1 - c 6 )- alkyl - s ( o ) n --( ch 2 ) n --, ( q ) --[( c 1 - c 6 )- alkyl ] nr 5 r 13 , ( b ) ( c 1 - c 6 )- alkyl , unsubstituted or substituted with a substituent selected from the group consisting of : ( c ) aryl , wherein aryl is phenyl or naphthyl , which is unsubstituted or substituted with a substituent selected from the group consisting of : ( b ) ( c 1 - c 4 )- alkyl unsubstituted or substituted with one of the following substituents : ( e ) -- conhso 2 - phenyl or -- conhso 2 - naphthyl , wherein phenyl or naphthyl is unsubstituted or substituted as defined in r 1 ( c ), ( f ) -- conhso 2 -( c 1 - c 8 )- alkyl , wherein the alkyl group is unsubstituted or substituted with a substituent selected from the group consisting of : -- oh , -- sh , -- o ( c 1 - c 4 )- alkyl , -- s --( c 1 - c 4 )- alkyl , -- cf 3 , cl , br , f , i , -- no 2 , -- co 2 h , -- co 2 -( c 1 - c 4 )- alkyl , -- nh 2 , -- nh [( c 1 - c 4 )- alkyl ], or -- n [( c 1 - c 4 )- alkyl ] 2 , ( h ) -- conhso 2 - heteroaryl , wherein heteroaryl is as defined in r 1 ( d ), ( j ) -- so 2 nhco - phenyl or -- so 2 nhco - naphthyl , wherein phenyl or naphthyl is unsubstituted or substituted as defined in r 1 ( c ), ( k ) -- so 2 nhco -( c 1 - c 8 )- alkyl , wherein the alkyl group is unsubstituted or substituted with a substituent selected from the group consisting of : -- oh , -- sh , -- o ( c 1 - c 4 )- alkyl , -- s -( c 1 - c 4 )- alkyl , -- cf 3 , cl , br , f , i , -- no 2 , -- co 2 h , -- co 2 -( c 1 - c 4 )- alkyl , -- nh 2 , -- nh [( c 1 - c 4 )- alkyl ], or -- n [( c 1 - c 4 )- alkyl ] 2 , ( m ) -- so 2 nhco - heteroaryl , wherein heteroaryl is as defined in r 1 ( d ), ( e ) ( ch 2 ch 2 o ) y - o --[( c 1 - c 4 )- alkyl ], wherein y is 1 or 2 , ( f ) phenyl , naphthyl , ch 2 - phenyl or ch 2 - naphthyl , where phenyl or naphthyl is substituted or unsubstituted with co 2 -( c 1 - c 4 )- alkyl , ## str5 ## r 15 and r 16 independently are ( c 1 - c 6 )- alkyl or phenyl . ( b ) ( c 1 - c 6 )- alkyl , ( c 2 - c 6 )- alkenyl or ( c 2 - c 6 )- alkynyl each of which is unsubstituted or substituted with a substituent selected from the group consisting of : -- a 1 -- a 2 -- a 3 -- a 4 -- is : ## str6 ## n is : 0 , 1 , or 2 ; and r 2 is : ( b ) ( c 1 - c 6 )- alkyl which is unsubstituted or substituted with one of the following substituents , r 6 and r 7 on adjacent carbon atoms can be joined together to form a ring structure : ## str7 ## a represents : a ) -- y -- c ( r 4 )═ c ( r 4 )--, y is -- o --, -- s ( o ) n -- and nr 5 ; and ( b ) ( c 1 - c 6 )- alkyl , unsubstituted or substituted with ( c 3 - c 7 )- cycloaklyl , ( e ) hydroxy -( c 1 - c 6 )- alkyl or dihydroxy -( c 1 - c 6 )- alkyl ; and ( b ) ( c 1 - c 6 )- alkyl , unsubstituted or substituted with : ( c ) aryl , wherein aryl is phenyl or naphthyl , which is unsubstituted or substituted with a substituent selected from the group consisting of : ( b ) ( c 1 - c 4 )- alkyl unsubstituted or substituted with one of the following substituents : ( e ) -- conhso 2 - phenyl or -- conhso 2 - naphthyl , wherein phenyl or naphthyl is unsubstituted or substituted as defined in r 1 ( c ), ( f ) -- conhso 2 -( c 1 - c 8 )- alkyl , wherein the alkyl group is unsubstituted or substituted with a substituent selected from the group consisting of : -- oh , -- sh , -- o ( c 1 - c 4 )- alkyl , -- s -( c 1 - c 4 )- alkyl , -- cf 3 , cl , br , f , i , -- no 2 , -- co 2 h , -- co 2 -( c 1 - c 4 )- alkyl , -- nh 2 , -- nh [( c 1 - c 4 )- alkyl ], or -- n [( c 1 - c 4 )- alkyl ] 2 , ( h ) -- conhso 2 - heteroaryl , wherein heteroaryl is as defined in r 1 ( d ), ( j ) -- so 2 nhco - phenyl or -- so 2 nhco - naphthyl , wherein phenyl or naphthyl is unsubstituted or substituted as defined in r 1 ( c ), ( k ) -- so 2 nhco -( c 1 - c 8 )- alkyl , wherein the alkyl group is unsubstituted or substituted with a substituent selected from the group consisting of : -- oh , -- sh , -- o ( c 1 - c 4 )- alkyl , -- s -( c 1 - c 4 )- alkyl , -- cf 3 , cl , br , f , i , -- no 2 , -- co 2 h , -- co 2 -( c 1 - c 4 )- alkyl , -- nh 2 , -- nh [( c 1 - c 4 )- alkyl ], or -- n [( c 1 - c 4 )- alkyl ] 2 , ( m ) -- so 2 nhco - heteroaryl , wherein heteroaryl is as defined in r 1 ( d ), ( e ) ( ch 2 ch 2 o ) y -- o -[( c 1 - c 4 )- alkyl ], wherein y is 1 or 2 , ( f ) phenyl , naphthyl , -- ch 2 - phenyl or -- ch 2 - naphthyl , wherein phenyl or naphthyl is substituted or unsubstituted with co 2 -( c 1 - c 4 )- alkyl , ## str8 ## r 15 and r 16 independently are ( c 1 - c 6 )- alkyl or phenyl . a class of this embodiment of the invention is a compound of formula ii : ## str9 ## wherein r 1 is : -- a 1 -- a 2 -- a 3 -- a 4 -- is : ## str10 ## n is : 0 , 1 , or 2 ; and r 9 and r 10 are each independently : ( d ) ( c 1 - c 6 )- alkyl -( c 3 - c 7 )- cycloalkyl , or ( e ) hydroxy ( c 1 - c 6 )- alkyl or dihydroxy ( c 1 - c 6 )- alkyl ; and ( e ) -- conhso 2 -( c 1 - c 4 )- phenyl or -- conhso 2 -( c 1 - c 4 )- naphthyl , wherein phenyl or naphthyl is unsubstituted or substituted as defined in r 1 ( c ), or ( f ) -- conhso 2 -( c 1 - c 4 )- heteroaryl , wherein heteroaryl is as defined in r 1 ( d ). another embodiment of the invention is a compound of formula iii : ## str11 ## r 1 is : ( a ) h , -- a 1 -- a 2 -- a 3 -- a 4 -- is : ## str12 ## r 4 groups are independently : ( a ) h , r 6 and r 7 on adjacent carbon atoms can be joined together to form a ring structure : ## str13 ## a represents : a ) -- o -- c ( r 4 )═ c ( r 4 )--, the following tables ( i - v ) further exemplify the scope of the invention described by formula ii ( wherein x is -- o -- and r 7 , r 8a and r 8b are h , unless specified otherwise ). table i__________________________________________________________________________ ## str14 ## r . sup . 1 r . sup . 4a r . sup . 4b r . sup . 9 r . sup . 10 r . sup . 6 , r . sup . 7 , r . sup . 8a , r . sup . 8b z__________________________________________________________________________pr 4 - me 7 - me me me 3 - ome coohbu 5 - phco h bu h 3 - ome coohph h h pr h 3 - ome coohpr h h cl h 3 - ome coohbu h h br br 3 - ome coohph h h cl cl 3 - ome cooht - bu h h pr pr 3 - ome coohpr h h pr pr 3 - ome coohbu h h pr h 4 - ome coohph h h pr pr 3 - ome tetrazol - 5 - ylbu h h pr pr 3 - ome conhso . sub . 2 meh h h pr pr 3 - ome coohh h h pr pr 3 , 4 - methylenedioxy coohh h h pr pr 2 - ome cooh . __________________________________________________________________________ table ii__________________________________________________________________________ ## str15 ## r . sup . 1 r . sup . 4a r . sup . 4b r . sup . 9 r . sup . 10 r . sup . 6 , r . sup . 7 , r . sup . 8a , r . sup . 8b z__________________________________________________________________________et 5 - me 7 - me pr pr 2 - br , 3 - ome , 4 - ome , 5 - br coohh h 7 - me pr pr 2 - br , 3 - ome , 4 - ome , 5 - br coohet 5 - me 7 - me me me 3 - ome coohpr 6 - phconh h bu h 3 - ome coohet 5 - me 7 - me pr h 3 - om coohet 5 - me 7 - me cl h 3 - ome coohet 5 - me 7 - me br br 3 - ome coohph h h cl cl 3 - ome coohme h h br br 3 - ome coohet 5 - me 7 - me pr pr 3 - ome coohet 5 - me 7 - me pr pr 4 - ome coohet 5 - me 7 - me me me 4 - ome coohet 5 - me 7 - me bu h 4 - ome coohbu h h cl cl 4 - ome coohme 5 - me 7 - me br br 4 - ome coohet 5 - me 7 - me pr pr 2 - ome coohpr 5 - me 7 - me pr h 2 - ome coohpr h 7 - me h h 2 - ome coohpr 6 - phconh h bu h 2 - ome , 4 - ome coohet 5 - me 7 - me cl cl 2 - ome , 4 - ome coohph h h pr pr 2 - ome , 4 - ome coohet 5 - me 7 - me me me 2 - ome , 5 - ome coohph h h cl cl 2 - ome , 5 - ome coohme h h br br 3 - ome , 4 - ome coohph h h pr pr 3 - ome , 4 - ome coohh h h pr pr 3 - ome , 4 - ome coohet 5 - me 7 - me pr pr 3 - ome conhso . sub . 2 meme 5 - me 7 - me pr pr 3 - ome conhso . sub . 2 phet 5 - me 7 - me pr pr 3 - ome , 5 - ome coohh 5 - me 7 - me pr pr 3 - ome , 5 - ome coohet 5 - me 7 - me pr pr 3 - ome , 5 - ome conhso . sub . 2 meet 5 - me 7 - me pr pr 2 - ome , 3 - ome coohh 5 - me 7 - me pr pr 2 - ome , 3 - ome coohet 5 - me 7 - me pr pr 2 - ome , 3 - ome conhso . sub . 2 meet h 7 - me pr pr 2 , 3 - methylenedioxy coohet h 7 - me pr pr 3 , 4 - methylenedioxy coohet 5 - me 7 - me pr pr 3 , 4 - methylenedioxy conhso . sub . 2 meet h 7 - me pr pr 3 , 4 - methylenedioxy coohh h 7 - me pr pr 3 , 4 - methylenedioxy coohme h h pr pr 3 , 4 - methylenedioxy coohme h h pr pr 3 - ome , 5 - ome coohet me 6 - nhcoph pr pr 3 - ome , 5 - ome coohh h 6 - nhcoph pr pr 3 - ome , 5 - ome coohet 5 - me 7 - me h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) et 5 - me 7 - me h pr 3 - ome , 5 - ome conhso . sub . 2 ph ( 4 - ipr ) h h h h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) h h h pr pr 5 - br , 3 , 4 - methylenedioxy coohh 5 - me 7 - me pr pr 5 - br , 3 , 4 - methylenedioxy coohh h h pr h 5 - br , 3 , 4 - methylenedioxy coohh h h pr h 5 - br , 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) et 5 - me 7 - me h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - tbu ) et 5 - me 7 - me h ch . sub . 2 - c - pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) h h h h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - tbu ) h h h h ch . sub . 2 - c - pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - tbu ). __________________________________________________________________________ table iii__________________________________________________________________________ ## str16 ## r . sup . 1 r . sup . 4a r . sup . 4b r . sup . 9 r . sup . 10 r . sup . 6 , r . sup . 7 , r . sup . 8a , r . sup . 8b z__________________________________________________________________________pr 4 - me 7 - me pr h 3 - ome coohph 4 - cl h cl h 3 - ome coohph 4 - cl h br br 2 - ome coohme 4 - cl h pr pr 2 - ome coohph 4 - me h pr pr 3 - ome coohme 4 - cl h pr pr 4 - ome coohpr 4 - me h me me 4 - ome coohph 4 - cl h pr pr 3 - ome , 4 - ome coohph 4 - cl h pr pr 3 - ome , 5 - ome coohet 4 - me h pr h 2 - ome coohph 4 - cl h cl cl 2 - ome , 3 - ome coohme 4 - cl h br br 2 , 3 - methylenedioxy coohme 4 - cl h pr pr 3 , 4 - methylenedioxy coohh 4 - cl h pr pr 3 , 4 - methylenedioxy coohh h h pr pr 3 , 4 - methylenedioxy coohh h h pr pr 3 - ome , 5 - ome coohet 5 - me 7 - me h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) et 5 - me 7 - me h pr 3 - ome , 5 - ome conhso . sub . 2 ph ( 4 - ipr ) h h h h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) h h h h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - tbu ) h h h h pr 3 , 4 - methylenedioxy conhso . sub . 2 phh h h h pr 3 - ome , 5 - ome conhso . sub . 2 ph ( 4 - ipr ) me h h pr pr 3 , 4 - methylenedioxy coohme h h h pr 3 , 4 - methylenedioxy coohme h h h pr 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ) h h 7 - sme pr pr 3 , 4 - methylenedioxy coohh h 7 - nme . sub . 2 pr pr 3 , 4 - methylenedioxy coohh h h pr pr 5 - br - 3 , 4 - methylenedioxy coohme h h pr pr 5 - br - 3 , 4 - methylenedioxy cooh . __________________________________________________________________________ table iv__________________________________________________________________________ ## str17 ## r . sup . 1 r . sup . 4a r . sup . 4b r . sup . 9 r . sup . 10 r . sup . 6 , r . sup . 7 , r . sup . 8a , r . sup . 8b z__________________________________________________________________________pr 4 - me 7 - me pr h 3 - ome coohph 4 - cl h cl h 3 - ome coohph 4 - cl h br br 2 - ome coohme 4 - cl h pr pr 2 - ome coohph 4 - me h pr pr 3 - ome coohme 4 - cl h pr pr 4 - ome coohpr 4 - me h me me 4 - ome coohph 4 - cl h pr pr 3 - ome , 4 - ome coohph 4 - cl h pr pr 3 - ome , 5 - ome coohet 4 - me h pr h 2 - ome coohph 4 - cl h cl cl 2 - ome , 3 - ome coohme 4 - cl h br br 2 , 3 - methylenedioxy coohme 4 - cl h pr pr 3 , 4 - methylenedioxy coohh 4 - cl h pr pr 3 , 4 - methylenedioxy coohh h h pr pr 3 , 4 - methylenedioxy coohh h h pr pr 3 - ome , 5 - ome coohh h h pr h 3 , 4 - methylenedioxy conhso . sub . 2 ph ( 4 - ipr ). __________________________________________________________________________ table v__________________________________________________________________________ ## str18 ## r . sup . 1 r . sup . 4a r . sup . 4b r . sup . 9 r . sup . 10 r . sup . 6 , r . sup . 7 , r . sup . 8a , r . sup . 8b z__________________________________________________________________________me n ( me ). sub . 2 h pr pr 3 - ome coohme me me pr h 3 - ome coohph h h pr pr 3 - ome coohbu h h pr pr 4 - ome coohph me h me me 2 - ome coohph cl h pr pr 3 - ome , 5 - ome coohh cl h pr pr 3 - ome , 5 - ome coohh cl h pr pr 3 , 4 - methylenedioxy coohh cl h pr pr 2 , 3 - methylenedioxy cooh . __________________________________________________________________________ the alkyl substituents recited above denote straight and branched chain hydrocarbons of the length specified such as methyl , ethyl , isopropyl , isobutyl , neopentyl , isopentyl , etc . the alkenyl and alkynyl substituents denote alkyl groups as described above which are modified so that each contains a carbon to carbon double bond or triple bond , respectively , such as vinyl , allyl and 2 - butenyl . cycloalkyl denotes rings composed of 3 to 8 methylene groups , each which may be substituted or unsubstituted with other hydrocarbon substituents , and include for example cyclopropyl , cyclopentyl , cyclohexyl and 4 - methylcyclohexyl . the alkoxy substituent represents an alkyl group as described above attached through an oxygen bridge . the heteroaryl substituent recited above represents any 5 - or 6 - membered aromatic ring containing from one to three heteroatoms selected from the group consisting of nitrogen , oxygen , and sulfur , for example , pyridyl , furyl , pyrrolyl , thienyl , isothiazolyl , imidazolyl , pyrazinyl , pyrimidyl , pyrazolyl , purinyl , carbazolyl , isoxazolyl , thiazolyl , and oxazolyl . although the reaction schemes described below are reasonably general , it will be understood by those skilled in the art of organic synthesis that one or more functional groups present in a given compound of formula i may render the molecule incompatible with a s particular synthetic sequence . in such a case an alternative synthetic route , an altered order of steps , or a strategy of protection and deprotection may be employed . in all cases the particular reaction conditions , including reagents , solvent , temperature and time , should be chosen so that they are consistent with the nature of the functionality present in the molecule . the compounds of formula i , and more specifically compounds where r 11 is hydrogen , can be synthesized using the reactions and techniques described for the synthesis of the non - heterocyclic components in the patent application wo91 / 11999 ( merck & amp ; co . ; published on aug . 22 , 1991 under the patent cooperation treaty ) and also u . s . pat . no . 5 , 177 , 095 ( merck & amp ; co . ; jan . 5 , 1993 ). the reaction schemes described below have been generalized for simplicity . it is further to be understood that in the generalized schemes below , unless specified more narrowly in the text , the alkyl and aryl groups represent unfunctionalized or functionalized derivatives as described before . the leaving group q present in the alkylating agents is either chloro , bromo , iodo , methanesulfonate , p - toluenesulfonate or triflate . ## str19 ## more specifically , the compounds of formula i ( where x is oxygen , sulphur or appropriately substituted nitrogen and r 11 is h ) can be synthesized as outlined in scheme 1 . the substituted compound 1 may be reacted with the alkylating agent 2 in an appropriate solvent such as alcohols ( methanol , ethanol , isopropanol and like ), dimethylformamide ( dmf ), dimethylsulfoxide ( dmso ), tetrahydrofuran ( thf ) and acetone in the presence of an alkali metal salt such as alkoxides , carbonates , hydroxides and hydrides , or organic bases such as trialkylamines or alkyl lithiums to provide compound 3 . the z 1 group present in compound 3 may then be further transformed to provide desired compounds of formula i . in general , the alkylating agent 2 can be prepared using methods and techniques outlined in u . s . pat . no . 5 , 177 , 095 . more specifically , compound 2 ( where z 1 is coor and q is br ) can be synthesized from the substituted arylacetic acids 4 as outlined in scheme 2 . the substituted arylacetic acid 4 is converted to the corresponding ester either by refluxing the acid in an appropriate alcohol in the presence of a catalytic amount of conc . sulfuric acid , or using other conventional methods of esterification . the resulting ester is then refluxed in carbon tetrachloride with n - bromosuccinimide and a catalytic amount of a radical initiator ( e . g ., aibn or benzoylperoxide ) to provide the 2 - bromo - arylacetic acid ester 5 . ## str20 ## alternatively , the ester 5 may also be prepared from appropriate aryl aldehydes ( scheme 3 ). the aldehyde 6 can be reacted with trimethylsilyl cyanide and catalytic amounts of kcn and 18 - crown - 6 to provide the corresponding trimethylsilyl cyanohydrin 7 , which upon further treatment with the gaseous hcl and alcohol affords the 2 - hydroxy ester 8 . the ester 8 is treated with triphenylphosphine and carbon tetrabromide in methylene chloride to give the 2 - bromoarylacetate derivatives 5 . ## str21 ## scheme 4 illustrates a typical synthesis of an alkylating agent 12 ( where ar represents substituted indoles ). the appropriately substituted cyanoindole 9 ( for a general synthesis of substituted indoles refer to , r . k . brown , indoles , part one , ed . w . j . houlihan , vol . 25 , chapter ii , wiley - interscience , new york , 1972 ) is reduced with dibalh to provide the corresponding aldehyde , which is then convened into the n - boc derivative 10 . reaction of 10 with the trichloromethide anion [ generated from koh and chcl 3 ; j . m . wyvratt et . al ., j . org . chem ., 52 , 944 - 945 ( 1987 )] followed by treatment with aqueous naoh in dmf provides the alcohol 11 . treatment of 11 with diazomethane followed by the reaction with cbr 4 / ph 3 p yields the alkylating agent 12 . a typical synthesis of alkylating agents bearing a substituted benzoxazole or benzthiazole ring is outlined in scheme 5 . the substituted benzoxazole 14 is prepared from the corresponding o - aminophenol 13 by the reaction of an appropriate orthoester under refluxing conditions ( for other methods of synthesis of benzoxazoles see , s . a . lang and y . lin , comprehensive heterocyclic chemistry , vol . 6 , 1 - 130 , ed . c . w . rees ; and references cited therein ). reduction of 14 with nabh 4 provides the alcohol 15 which is then subjected to pyridinium dichromate ( pdc ) oxidation to yield the corresponding aldehyde 16 . further elaboration of 16 as outlined provides the key intermediate 17 . similarly , the benzothiazole 19 can also be prepared form the appropriately substituted o - aminothiophenol 18 . ## str22 ## scheme 6 illustrates the synthesis of benzofuran and dihydrobenzofuran alkylating agents 23 and 25 . the benzofuran 21 can be prepared from the α - phenoxy carbonyl compound 20 via a ring closure reaction [ stoermer and wehln , chem . ber ., 35 , 3549 ( 1902 )] ( for general methods of synthesis of benzofurans and dihydrobenzofurans see , r . c . elderfield and v . b . meyer , heterocyclic compounds , vol . 2 , chapter 1 , ed . r . c . elderfield , wiley ; and references cited therein ). the ester 21 is reduced to provide the aldehyde 22 which is then transformed into the corresponding alkylating agent 23 . the dihydrobenzofuran ester 24 , obtained by catalytic reduction of 21 , can also be transformed into the corresponding alkylating agent 25 using the sequence of reactions outlined in scheme 6 . benzothiophene 26 may be synthesized from the corresponding aldehyde 26b in a manner similar to that outlined in scheme 6 for benzofuran 23 . benzothiophene 26b can be prepared by the oxidative cyclization ( using an alkaline solution of potassium ferricyanide ) of appropriately substituted o - mercaptocinnamic acid 26a [ c . chmelewsky and p . friedlander , chem . ber ., 46 , 1903 ( 1913 )]. ( for general methods of synthesis of benzothiophene , see , e . champaigne in comprehensive heterocyclic chemistry , vol . 4 , chapter 3 - 15 ; eds . a . katritzky and c . w . rees .) scheme 7 outlines a typical synthesis of an α - bromoarylacetates , 30 and 32 , bearing appropriately substituted methylenedioxy or 1 , 4 - dioxane rings . the substituted catechol derivative 27 is treated with an appropriate dibromide ( where m is 1 or 2 ) in the presence of cesium carbonate in dimethylformamide to provide 28 . treatment of 28 with dibalh yields the aldehyde 29 which is then transformed into the desired alkyl bromide as described . ## str23 ## the compounds of formula ( i ) can be synthesized using the reactions and techniques described in the international application wo91 / 11999 published under the patent cooperation treaty to ( merck & amp ; co .) on aug . 22 , 1991 . the reactions are performed in a solvent appropriate to the reagents and materials employed and suitable for the transformation being effected . it is understood by those skilled in the art of organic synthesis that the functionality present on the heterocycle and in the reactants being employed should be consistent with the chemical transformations being conducted . depending upon the reactions and techniques employed , optimal yields may require changing the order of synthetic steps or use of protecting groups followed by deprotection . the compounds useful in the novel method treatment of this invention form salts with various inorganic and organic acids and bases which are also within the scope of the invention . such salts include ammonium salts , alkali metal salts like sodium and potassium salts , alkaline earth metal salts like the calcium and magnesium salts , salts with organic bases ; e . g ., dicyclohexylamine salts , n - methyl - d - glucamine , salts with amino acids like arginine , lysine , and the like . also , salts with organic and inorganic acids may be prepared ; e . g ., hcl , hbr , h 2 so 4 , h 3 po 4 , methanesulfonic , toluenesulfonic , maleic , fumaric , camphorsulfonic . the salts can be formed by conventional means , such as by reacting the free acid or free base forms of the product with one or more equivalents of the appropriate base or acid in a solvent or medium in which the salt is insoluble , or in a solvent such as water which is then removed in vacuo or by freeze - drying or by exchanging the cations of an existing salt for another cation on a suitable ion exchange resin . it will be appreciated that the compounds of general formula i in this invention may be derivatized at functional groups to provide prodrug derivatives which are capable of conversion back to the parent compounds in vivo . the concept of prodrug administration has been extensively reviewed ( e . g . a . a . sinkula in annual reports in medicinal chemistry , vol 10 , r . v . heinzelman , ed ., academic press , new york london , 1975 , ch . 31 , pp . 306 - 326 , h . ferres , drugs of today , vol 19 , 499 - 538 ( 1983 ) and j . med . chem ., 18 , 172 ( 1975 )). examples of such prodrugs include the physiologically acceptable and metabolically labile ester derivatives , such as lower alkyl ( e . g . methyl or ethyl esters ), aryl ( e . g . 5 - indanyl esters ), alkenyl ( e . g . vinyl esters ), alkoxyalkyl ( e . g . methoxymethyl esters ), alkylthioalkyl ( e . g . methylthiomethyl esters ), alkanoyloxyalkyl ( e . g . pivaloyloxymethyl esters ), and substituted or unsubstituted aminoethyl esters ( e . g . 2 - dimethylaminoethyl esters ). additionally , any physiologically acceptable equivalents of the compounds of general formula i , similar to the metabolically labile esters , which are capable of producing the parent compounds of general formula i in vivo , are within the scope of this invention . it will be further appreciated that the majority of compounds of general formula i claimed herein are asymmetric and are produced as racemic mixtures of enantiomers and that both the racemic compounds and the resolved individual enantiomers are considered to be in the scope of this invention . the racemic compounds of this invention may be resolved to provide individual enantiomers utilizing methods known to those skilled in the art of organic synthesis . for example , diastereoisomeric salts , esters or imides may be obtained from a racemic compound of general formula i and a suitable optically active amine , amino acid , alcohol or the like . the diastereoisomeric salts , esters or imides are separated and purified , the optically active enantiomers are regenerated and the preferred enantiomer is the more potent isomer . the resolved enantiomers of the compounds of general formula i , their pharmaceutically acceptable salts and their prodrug forms are also included within the scope of this invention . endothelin ( et - 1 ), and two closely related bioactive peptides , et - 2 and et - 3 , are widely distributed in mammalian tissues , and they can induce numerous biological responses in non - vascular as well as vascular tissues by binding to at least two distinct endothelin receptor subtypes . in addition to smooth muscle , neural and atrial sites , endothelin receptors may be found in gastrointestinal , kidney , lung , urogenital , uteral and placental tissues . endothelin is a potent vasoconstrictor peptide and thus plays an in vivo role in arterial pressure - volume homeostasis . not only peripheral , but coronary vascular resistance as well , is increased by endothelin . cardiac output is decreased , while plasma renin activity is increased . there is a reduction in renal blood flow and glomerular filtration rate , while levels of atrial natriuretic factor , vasopressin , and aldosterone become elevated . it is also considered , in accordance with the present invention , that antagonists for the endothelin receptor may be useful in preventing or reducing restenosis subsequent to denudation following angioplasty . such denudation results from myointimal thickening following angioplasty , which is caused by increased endothelin release . endothelin acts as a growth factor with respect to smooth muscle and fibroblastic cells , and possibly other types of cells , as well . endothelin is also a neuropeptide , acting on the posterior pituitary , where it modulates the release of the neurosecretory hormones vasopressin and oxytocin . endothelin released from the posterior pituitary also acts as a circulating hormone , having a wide range of actions as discussed further above . this includes effects on the endocrine system , especially the adrenal glands . endothelin increases plasma levels of epinephrine . consequently , the novel compounds of the present invention , which are receptor antagonists of endothelin , have therapeutic usefulness in preventing , decreasing or modulating the various physiological effects of endothelin discussed above , by wholly or partially blocking access of endothelin to its receptor . the binding of the novel compound of this invention to the endothelin receptor was determined in accordance with the assay described in detail immediately below . it is similar to the assay described in ambar et al . ( 1989 ) biochem . biophys . res . commun . 158 , 195 - 201 ; and kloog et al . ( 1989 ) febs letters , 253 , 199 - 202 . the endothelins ( ets ) have a number of potent effects on a variety of cells , and exert their action by interacting with specific receptors present on cell membranes . the compound described in the present invention acts as an antagonist of et at the receptors . in order to identify et antagonists and determine their efficacy in vitro , the following three ligand receptor assays were established . thoracic aortae were obtained from fleshly slaughtered calves and brought to the lab on wet ice . the adventitia were removed , and the aorta was opened up lengthwise . the lumenal surface of the tissue was scrubbed with cheesecloth to remove the endothelial layer . the tissue was ground in a meat grinder , and suspended in ice - cold 0 . 25m sucrose , 5 mm tris - hcl , ph 7 . 4 , containing 0 . 5 μg / ml leupeptin and 7 μg / ml pepstatin a . tissue was homogenized twice and then centrifuged for 10 minutes at 750 × g at 4 ° c . the supernatant was filtered through cheesecloth and centrifuged again for 30 minutes at 48 , 000 × g at 4 ° c . the membrane pellet thus obtained was resuspended in the buffer solution described above ( including the protease inhibitors ), and aliquots were quick - frozen and stored at - 70 ° c . until use . membranes were diluted into 50 mm kpi , 5 mm edta ph 7 . 5 containing 0 . 01 % human serum albumin . assays were done in triplicate . test compounds and 100 pm [ 125 i ]- endothelin - 1 ( 2000 - 2200 ci / μmole , obtained from new england nuclear or amersham ) were placed in a tube containing this buffer , and the membranes prepared above were added last . the samples were incubated for 60 min at 37 ° c . at the end of this incubation , samples were filtered onto prewetted ( with 2 % bsa in water ) glass fiber filter pads and washed with 150 mm nacl , 0 . 1 % bsa . the filters were assayed for 125 i radioactivity in a gamma counter . nondisplaceable binding of [ 125 i ]- endothelin - 1 was measured in the presence of 100 nm unlabelled endothelin - 1 [ endothelin - 1 ( et - 1 ) was purchased from peptides international ( louisville , ky .)]. specific binding is defined as total binding minus nondisplaceable binding . the inhibitory concentration ( ic 50 ) which gives 50 % displacement of the total specifically bound [ 125 i ]- endothelin - 1 was presented as a measure of the potency of such compound as et antagonist . rat hippocampi were obtained from freshly sacrificed male sprague - dawley rats and placed in ice cold 0 . 25m sucrose , 5 mm tris - hcl , ph 7 . 4 containing 0 . 5 μg / ml leupeptin , 7 μg / ml pepstatin a . hippocampi were weighed and placed in a dounce homogenizer with 25 volumes ( wet weight to volume ) ice - cold sucrose buffer in the presence of protease inhibitors . hippocampi were homogenized using the dounce ( glass - glass ) homogenizer with type a pestle , with the homogenizer immersed in ice . tissue homogenate was centrifuged at 750 × g for 10 min at 4 ° c . supernatant was filtered through dampened cheesecloth , and centrifuged again at 48 , 000 × g for 30 min at 4 ° c . membrane pellets were resuspended in sucrose buffer with protease inhibitors . aliquots of this preparation were quick frozen and stored at - 70 ° c . until use . membranes were diluted into 50 mm kpi , 5 mm edta ph 7 . 5 containing 0 . 01 % human serum albumin . assays were done in triplicate . test compounds and 25 pm [ 125 i ]- endothelin - 1 ( 2000 - 2200 ci / μmole , obtained from new england nuclear or amersham ) were placed in a tube containing this buffer , and the membranes prepared above were added last . the samples were incubated for 60 min at 37 ° c . at the end of this incubation , samples were filtered onto prewetted ( with 2 % bsa in water ) glass fiber filter pads and washed with 150 mm nacl , 0 . 1 % bsa . the filters were assayed for 125 i radioactivity in a gamma counter . nondisplaceable binding of [ 125 i ]- endothelin - 1 was measured in the presence of 100 nm unlabelled endothelin - 1 [ endothelin - 1 ( et - 1 ) was purchased from peptides international ( louisville , ky .)]. specific binding is defined as total binding minus nondisplaceable binding . the inhibitory concentration ( ic 50 ) which gives 50 % displacement of the total specifically bound [ 125 i ]- endothelin - 1 was presented as a measure of the potency of such compounds as endothelin antagonists . receptor binding assay using cloned human et receptors expressed in chinese hamster ovary cells both endothelin receptor subtypes were cloned from a human cdna library and were individually expressed in chinese hamster ovary cells . cells were harvested by addition of 126 mm nacl , 5 mm kcl , 2 mm edta , 1 mm nah 2 po 4 , 15 mm glucose , 10 mm tris / hepes ph 7 . 4 cells were centrifuged at 250 × g for 5 minutes . the supernatant was aspirated off , and the cells were resuspended in the 50 mm kpi , 5 mm edta ph 7 . 5 containing 0 . 01 % human serum albumin . assays were done in triplicate . test compounds and 25 - 100 pm [ 125 i ]- endothelin - 1 ( 2000 - 2200 ci / μmole , obtained from new england nuclear or amersham ) were placed in a tube containing 50 mm kpi , 5 mm edta ph 7 . 5 containing 0 . 01 % human serum albumin , and the cells prepared above were added last . the samples were incubated for 60 min at 37 ° c . at the end of this incubation , samples were filtered onto prewetted ( with 2 % bsa in water ) glass fiber filter pad and washed with 150 mm nacl , 0 . 1 % bsa . the filters were assayed for 125 i radioactivity in a gamma counter . nondisplaceable binding of [ 125 i ]- endothelin - 1 was measured in the presence of 100 nm unlabelled endothelin - 1 [ endothelin - 1 ( et - 1 ) was purchased from peptides international ( louisville , ky .)]. specific binding is defined as total binding minus nondisplaceable binding . the inhibitory concentration ( ic 50 ) which gives 50 % displacement of the total specifically bound [ 125 i ]- endothelin - 1 was presented as a measure of the potency of such compounds as endothelin antagonists . the binding assays described above were used to evaluate the potency of interaction of the compound of the invention with endothelin receptors . to determine whether this compound was an endothelin antagonist , assays which measure the ability of the compound to inhibit endothelin - stimulated phosphatidylinositol hydrolysis were established . rat uterus contains predominantly one of the known endothelin receptor subtypes ( et a ). diethylstilbestrol primed female sprague - dawley rats were sacrificed and their uteri were collected , dissected of fat and connective tissue and minced . minced tissue was added to oxygenated ( 95 % o 2 , 5 % co 2 ) 127 mm nacl , 25 mm nahco 3 , 10 mm glucose , 2 . 5 mm kcl , 1 . 2 mm kh 2 po 4 , 1 . 2 nm mgso 4 , 1 . 8 mm cacl 2 . to the tissue mince , 1 . 2 μm myo -[ 3 h ]- inositol ( amersham ) was added . the mince was incubated 90 min at 37 ° c ., with constant oxygenation . after incubation , the loaded tissue mince was washed five times with the same oxygenated buffer to remove excess radiolabelled inositol . the tissue mince was resuspended in the above buffer , containing 10 mm licl , aliquotted into tubes , and 3 nm endothelin - 1 with and without test compounds was added to a final concentration of 3 nm to start the assay . assays were done in quadruplicate . samples were incubated at 37 ° c . under blowing o 2 in a hooded water bath for 30 minutes . reaction was stopped by addition of trichloroacetic acid to 6 % concentration . samples were sonicated for 10 min . centrifuged 20 min , then trichloroacetic acid was extracted with water - saturated ethyl ether . an aliquot of each sample was neutrallized and diluted by addition of 50 mm tris - hcl ph 7 . 4 . a 100 μl aliquot of this solution was assayed for radioactivity in a beta counter . the diluted neutralized sample was applied to dowex 1 × 8 - formate columns , washed with water , then washed with 60 mm ammonium formate , 5 mm sodium tetraborate . samples were eluted with 200 mm ammonium formate , 5 mm sodium tetraborate . the radioactivity of each eluted sample was measured in a beta counter . radioactivity was normalized by dividing radioactivity in post column sample by radioactivity in precolumn sample . control values ( 100 % stimulated ) are values in the presence of endothelin minus the values in the absence of endothelin ( basal ). test sample values are the values in the presence of endothelin and test sample minus basal . inhibitory concentration ( ic 50 ) is the concentration of test compound required to give a sample activity of 50 % of control value . sarafotoxin s6c is a member of the endothelin family which binds preferentially to one of the known endothelin receptor subtypes ( et b ). male sprague - dawley rats were sacrificed and their lungs were collected , dissected of fat and connective tissue and minced . minced tissue was added to oxygenated ( 95 % o 2 , 5 % co 2 ) 127 mm nacl , 25 mm nahco 3 , 10 mm glucose , 2 . 5 mm kcl , 1 . 2 mm kh 2 po 4 , 1 . 2 mm mgso 4 , 1 . 8 mm cacl 2 . to the tissue mince , 1 . 2 μm myo -[ 3 h ]- inositol was added . the mince was incubated 60 min at 37 ° c ., with constant oxygenation . after incubation , loaded tissue mince was washed five times with the same oxygenated buffer to remove excess radiolabelled inositol . tissue mince was resuspended in the above buffer , containing 10 mm licl , aliquotted into tubes , and sarafotoxin s6c ( to a final concentration of 3 nm ) with and without test compounds was added to start the assay . assays were done in quadruplicate . samples were incubated at 37 ° c . under blowing o 2 in a hooded water bath for 30 minutes . reaction was stopped by addition of 0 . 5 ml 18 % trichloroacetic acid to 6 % concentration . samples were sonicated for 10 min , centrifuged 20 min , then trichloroacetic acid was extracted with water - saturated ethyl ether . an aliquot of each sample was neutralized and diluted by addition of 50 nm tris - hcl ph 7 . 4 . a 100 μl aliquot of this solution was assayed for radioactivity in a beta counter . the diluted neutralized sample was applied to dowex 1 × 8 - formate columns , washed with water , then washed with 60 mm ammonium formate , 5 mm sodium tetraborate . samples were eluted with 200 mm ammonium formate , 5 mm sodium tetraborate . the radioactivity of each eluted sample was measured in a beta counter . radioactivity was normalized by dividing radioactivity in post column sample by radioactivity in precolumn sample . control values ( 100 % stimulated ) are values in the presence of sarafotoxin minus the values in the absence of sarafotoxin ( basal ). test sample values are the values in the presence of sarafotoxin and test sample minus basal . inhibitory concentration ( ic 50 ) is the concentration of test compound required to give a sample activity of 50 % of control value . phosphatidylinositol hydrolysis assays using cloned human endothelin receptors expressed in chinese hamster ovary cells endothelin receptors of both receptor subtypes were cloned from a human cdna library and were individually expressed in chinese hamster ovary cells . cells were loaded overnight by the addition of 1 . 2 μm myo -[ 3 h ]- inositol to their growth medium . cells were harvested by addition of 126 mm nacl , 5 mm kcl , 2 mm edta , 1 mm nah 2 po 4 , 15 mm glucose , 10 mm tris / hepes ph 7 . 4 cells were washed five times by centrifugation at 250 × g for 5 minutes to remove excess radiolabelled inositol . the supernatant was aspirated off , and the cells were resuspended in the same oxygenated ( 95 % 0 2 , 5 % co 2 ) buffer containing 10 mm licl , aliquotted into tubes , and endothelin - 1 ( to a final concentration of 0 . 3 nm ) with and without test compounds was added to start the assay . assays were done in quadruplicate . samples were incubated at 37 ° c . under blowing o 2 in a hooded water bath for 30 minutes . reaction was stopped by addition of 0 . 5 ml 18 % trichloroacetic acid to 6 % concentration . samples were sonicated for 10 min , centrifuged 20 min , then trichloroacetic acid was extracted with water - saturated ethyl ether . an aliquot of each sample was neutralized and diluted by addition of 50 mm tris - hcl ph 7 . 4 . a 100 μl aliquot of this solution was assayed for radioactivity in a beta counter . the diluted neutralized sample was applied to dowex 1 × 8 - formate columns , washed with water , then washed with 60 mm ammonium formate , 5 mm sodium tetraborate . samples were eluted with 200 mm ammonium formate , 5 mm sodium tetraborate . the radioactivity of each eluted sample was measured in a beta counter . radioactivity was normalized by dividing radioactivity in post column sample by radioactivity in precolumn sample . control values ( 100 % stimulated ) are values in the presence of endothelin minus the values in the absence of endothelin ( basal ). test sample values are the values in the presence of endothelin and test sample minus basal . inhibitory concentration ( ic 50 ) is the concentration of test compound required to give a sample activity of 50 % of control value . using the methodology described above , the compounds of the invention were evaluated and found to exhibit ic50 values of at least & lt ; 50 μm thereby demonstrating and confirming the utility of the compound of this invention as an effective endothelin antagonist . accordingly the novel compounds of the present invention are useful in human therapy for treating asthma , hypertension , pulmonary hypertension , arterioscelerosis , heart failure , renal failure particularly post - ischemic renal failure , cyclosporin nephrotoxicity , vasospasm , vascular restenosis , cerebral and cardiac ischemia and other ischemic states , myocardial infarction , raynaud &# 39 ; s disease , inflammatory bowel diseases , including crohn &# 39 ; s disease and ulcerative colitis , as well as other inflammatory diseases , or endotoxic shock caused by or associated with endothelin , by administration to a patient in need of such treatment of a therapeutically effective amount thereof . in the management of hypertension and the clinical conditions noted above , the compounds of this invention may be utilized in compositions such as tablets , capsules or elixirs for oral administration , suppositories for rectal administration , sterile solutions or suspensions for parenteral or intramuscular administration , and the like . the compounds of this invention can be administered to patients ( animals and human ) in need of such treatment in dosages that will provide optimal pharmaceutical efficacy . although the dose will vary from patient to patient depending upon the nature and severity of disease , the patient &# 39 ; s weight , special diets then being followed by a patient , concurrent medication , and other factors which those skilled in the art will recognize , the dosage range will generally be about 0 . 5 mg .- 1 . 0 g . per patient per day which can be administered in single or multiple doses . preferably , the dosage range will be about 0 . 5 - 500 mg . per patient per day ; more preferably about 0 . 5 - 100 mg . per patient per day . the present invention also relates to pharmaceutical compositions for treating asthma , hypertension , pulmonary hypertension , arterioscelerosis , heart failure , renal failure particularly post - ischemic renal failure , cyclosporin nephrotoxicity , vasospasm , vascular restenosis , cerebral and cardiac ischemia and other ischemic states , myocardial infarction , raynaud &# 39 ; s disease , inflammatory bowel diseases , including crohn &# 39 ; s disease and ulcerative colitis , as well as other inflammatory diseases , or endotoxic shock caused by or associated with endothelin , comprising a therapeutically effective amount of the novel compound of this invention together with a pharmaceutically acceptable carrier therefor . about 1 to 100 mg . of compound or mixture of compounds of formula i or a physiologically acceptable salt is compounded with a physiologically acceptable vehicle , carrier , excipient , binder , preservative , stabilizer , flavor , etc ., in a unit dosage form as called for by accepted pharmaceutical practice . the amount of active substance in these compositions or preparations is such that a suitable dosage in the range indicated is obtained . illustrative of the adjuvants which can be incorporated in tablets , capsules and the like are the following : a binder such as gum tragacanth , acacia , corn starch or gelatin ; an excipient such as microcrystalline cellulose ; a disintegrating agent such as corn starch , pregelatinized starch , alginic acid and the like ; a lubricant such as magnesium stearate ; a sweetening agent such as sucrose , lactose or saccharin ; a flavoring agent such as peppermint , oil of wintergreen or cherry . when the dosage unitform is a capsule , it may contain , in addition to materials of the above type , a liquid carrier such as fatty oil . various other materials may be present as coatings or to otherwise modify the physical form of the dosage unit . for instance , tablets may be coated with shellac , sugar or both . a syrup or elixir may contain the active compound , sucrose as a sweetening agent , methyl and propyl parabens as preservatives , a dye and a flavoring such as cherry or orange flavor . sterile compositions for injection can be formulated according to conventional pharmaceutical practice by dissolving or suspending the active substance in a vehicle such as water for injection , a naturally occurring vegetable oil like sesame oil , coconut oil , peanut oil , cottonseed oil , etc ., or a synthetic fatty vehicle like ethyl oleate or the like . buffers , preservatives , antioxidants and the like can be incorporated as required . the following examples illustrate the preparation of the compounds of formula i and their incorporation into pharmaceutical compositions and as such are not to be considered as limiting the invention set forth in the claims appended hereto . general procedure for the synthesis of 2 - bromophenylacetic esters from substituted aromatic aldehydes to a solution of 8 . 33 mmol of an appropriate aromatic aldehyde dissolved in 20 ml of dichloromethane is added 10 . 0 mmol of trimethylsilylcyanide , 1 - 2 mg of potassium cyanide , 1 - 2 mg of 18 - crown - 6 , and the reaction mixture is stirred at room temperature for 3 - 12 hours . the reaction mixture is then diluted into diethyl ether , washed with 5 % nahco 3 , brine , dried ( mgso 4 ), filtered and evaporated . the residual oil is used directly in the next step . to a stirred 0 ° c . ( ice - water bath ) solution of 8 . 35 mmol of the product of step a dissolved in 10 ml of methanol is introduced a slow stream of anhydrous hydrogen chloride gas . after 5 minutes the hydrogen chloride is turned off and the flask is stoppered and stirred at room temperature 14 hours . the reaction is then poured into ice - water and extracted into chloroform . the chloroform solution is filtered through a pad of silica gel and the silica gel is washed with additional chloroform . the combined filtrate is evaporated in vacuo to give the title compound . to a cooled ( 0 ° c .) solution of 2 . 19 mmol of the product of step b dissolved in 10 ml of dichloromethane is added 2 . 74 mmol of triphenylphosphine followed by 2 . 74 mmol of carbon tetrabromide . after 30 minutes the reaction is allowed to warm to room temperature and stirring is continued for 2 - 12 hours . the reaction mixture is evaporated in vacuo , and the residue is purified on a silica gel flash chromatography column using an appropriate eluting solvent to afford the title compound . a suspension of an appropriate heterocycle ( 5 . 71 mmol ) and nah ( 1 . 1 eq ) in dmf ( 25 ml ) is stirred for 1 hour and then cooled to 0 ° c . an appropriate 4 - benzyloxybenzyl halide ( 1 . 1 eq ) is then added and the ice bath removed . the reaction mixture is stirred for 2 - 4 hours and then concentrated in vacuo . the residue is purified on a silica gel flash chromatography column using an appropriate eluting solvent to yield the desired product . to a solution of the product of step a ( 1 . 62 mmol ) in 10 ml of meoh is added 60 mg of a 10 % pd / c catalyst and stirred under a h 2 atmosphere ( 1 atm ) for 7 hours . the reaction mixture is filtered and concentrated in vacuo to yield the corresponding phenolic compound . to a suspension of 0 . 32 mmol of a 35 % oil dispersion of potassium hydride in 0 . 5 ml of dmf is added 0 . 32 mmol of the phenolic compound ( step b ) and the reaction is stirred under an n 2 atmosphere . after stirring for 15 minutes , a catalytic amount of 18 - crown - 6 is added followed by addition of a solution of 0 . 35 mmol of the product of example 1 ( step c ) dissolved in 1 . 0 ml of dmf . the reaction mixture , after stirring for 4 hours , is concentrated in vacuo , and the residue is purified on a silica gel flash chromatography column using an appropriate solvent system to afford the title compound . to a solution of 0 . 21 mmol of the product of step c dissolved in 3 ml of ethanol is added 1 ml of a 1n naoh solution . the reaction mixture is stirred at room temperature for 1 . 5 hours , neutralized to ph 7 with 1n hcl and then concentrated in vacuo . the residue is purified on a silica gel flash chromatography column to afford the corresponding carboxylic acid . a substituted phenylacetic acid is converted to the corresponding methyl ester by refluxing the acid in methanol in the presence of a catalytic amount of conc . sulfuric acid . the ester , thus obtained , is then refluxed in carbon tetrachloride with n - bromosuccinimide ( 1 . 1 equiv ) and aibn ( 0 . 05 - 0 . 1 equiv ). upon completion of the reaction , the product methyl 2 - bromo - 2 - phenylacetate is purified by flash column chromatography using silica gel and ethyl acetate in hexane as eluent . an appropriately substituted aromatic aldehyde is treated overnight with trimethylsilyl cyanide in the presence of catalytic amounts of kcn and 18 - crown - 6 in methylene chloride . the reaction mixture is quenched with water and extracted with ch 2 cl 2 / ethyl acetate / ether ( 1 / 2 / 2 ) mixture . the organic phase is washed with saturated aq . nahco 3 solution . after drying and concentration of the organic phase , the trimethylsilyl cyanohydrin obtained is used in the next acid hydrolysis step . gaseous hcl is bubbled through an ethanolic solution of the cyanohydrin at 0 ° c . for 0 . 5 h , and the resulting mixture is stirred overnight or for a longer period of time to afford the corresponding crude 2 - hydroxy ester . the ester is then treated with triphenylphosphine and carbon tetrabromide in methylene chloride at 0 ° c . methylene chloride is removed and flash column chromatography of the crude product using silica gel and ethyl acetate / hexane as eluent gives the desired 2 - bromo - 2 - arylacetate derivative . 4 - hydroxy - 3 , 5 - dipropylbenzyl alcohol is alkylated with 2 - bromo - 2 - aryl esters ( step a ) in dmf using either cesium carbonate ( cs 2 co 3 ), or potassium carbonate ( k 2 co 3 ), or sodium hydride ( nah ) at room temperature . the alkylated product is purified by flash column chromatography using silica gel and ethyl acetate / hexane mixture as eluent to give the desired 4 -[( 1 - carbomethoxy - 1 - aryl ) methoxy ]- 3 , 5 - dipropyl - benzyl alcohol . the product ( 1 . 39 mmol ) obtained in step b is reacted with cbr 4 ( 2 . 1 mmol ) and ph 3 p ( 2 . 1 mmol ) in dry thf ( 10 ml ) containing dry acetonitrile ( 5 ml ) at room temperature for 3 - 6 h . the solvent is removed and the crude product is purified by flash column chromatography ( silica gel ) using an appropriate mixture of ethylacetate and hexane to give the titled product as an oil . using the general procedure for the synthesis of 2 - bromophenylacetic esters from benzaldehydes ( steps a - c , example 1 ), 1 . 00 g ( 7 . 35 mmol ) of 2 - methoxybenzaldehyde was converted to 0 . 736 g ( 2 . 69 mmol ) of the title compound in 37 % overall yield . 1 h nmr ( 300 mhz , cdcl 3 , ppm ): δ 1 . 20 - 1 . 30 ( t , 3h ), 3 . 85 ( s , 3h ), 4 . 15 - 4 . 30 ( m , 2h ), 5 . 85 ( s , 1h ), 6 . 80 - 6 . 90 ( d , 1h ), 6 . 90 - 7 . 00 ( t , 1h ), 7 . 25 - 7 . 35 ( t , 1h ), 7 . 55 - 7 . 65 ( d , 1h ). using the general procedure for the alkylation reaction described in step c of example 2 , 0 . 090 g ( 0 . 32 mmol ) of 3 -( 4 - hydroxyphenyl ) methyl - 7 - methyl - 2 - propyl - 3h - imidazo [ 4 , 5 - b ] pyridine ( prepared according to step a - b of example 2 ) was alkylated with 0 . 096 g ( 0 . 35 mmol ) of the product of step a , to afford 0 . 126 g ( 83 %) of the title compound . 1 h nmr ( 300 mhz , cdcl 3 , ppm ): δ 0 . 90 - 1 . 00 ( t , 3h ), 1 . 15 - 1 . 25 ( m , 3h ), 1 . 65 - 1 . 80 ( m , 2h ), 2 . 65 ( s , 3h ), 2 . 70 - 2 . 80 ( t , 2h ), 4 . 05 - 4 . 25 ( m , 2h ), 5 . 35 ( s , 2h ), 6 . 05 ( s , 1h ), 6 . 80 - 7 . 05 ( m , 7h ), 7 . 25 - 7 . 35 ( m , 1h ), 7 . 45 - 7 . 50 ( d , 1h ), 8 . 15 - 8 . 20 ( d , 1h ). using the general procedure for ester hydrolysis described in step d of example 2 , 0 . 123 g ( 0 . 26 mmol ) of the product of step b was converted to 0 . 095 g ( 82 %) of the title compound . 1 h nmr ( 300 mhz , cd 3 od , ppm ): δ 0 . 90 - 1 . 00 ( t , 3h ), 1 . 60 - 1 . 80 ( m , 2h ), 2 . 60 ( s , 3h ), 2 . 80 - 2 . 90 ( t , 2h ), 3 . 90 ( s , 3h ), 5 . 50 ( s , 2h ), 6 . 00 ( s , 1h ), 5 . 90 - 7 . 15 ( m , 6h ), 7 . 15 - 7 . 20 ( d , 1h ), 7 . 20 - 7 . 25 ( t , 1h ), 7 . 45 - 7 . 55 ( d , 1h ), 8 . 20 - 8 . 25 ( d , 1h ). using the k 2 co 3 / acetone conditions for phenol alkylation described in step b of example 3 , 5 , 7 - dimethyl - 2 - ethyl - 3 -[ 4 - hydroxy - 3 - propylphenyl ] methyl - 3h - imidazo [ 4 , 5 - b ] pyridine ( prepared as described in the patent application wo 91 / 11999 ) was alkylated with methyl 2 - bromo - 2 -( 2 - methoxy ) acetate . standard workup and purification by flash chromatography afforded a 69 % yield of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 6 ( d , 1h ), 7 . 38 ( dd , 1h ), 6 . 98 ( dd , 1h ), 6 . 875 ( s , 1h ), 6 . 866 ( dd , 1h ), 6 . 8 - 6 . 75 ( m , 2h ), 6 . 62 ( d , 1h ), 5 . 975 ( s , 1h ), 5 . 35 ( abq , 2h ), 3 . 85 ( s , 3h ), 3 . 68 ( s , 3h ), 2 . 79 ( q , 2h ), 2 . 62 ( s , 3h ), 2 . 575 ( s , 3h ), 2 . 466 ( dd , 1h ), 1 . 65 - 1 . 47 ( m , 2h ), 1 . 27 ( t , 3h ), 0 . 9 ( t , 3h ). using the general procedure for ester hydrolysis described in step d of example 2 , the product of step a was converted to the title compound in 58 % yield . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 8 ( d , 1h ), 7 . 4 ( dd , 1h ), 7 . 16 ( d , 1h ), 6 . 99 ( d , 1h ), 6 . 875 ( s , 1h ), 6 . 825 ( d , 1h ), 6 . 775 ( d , 1h ), 6 . 72 ( d , 1h ), 6 . 02 ( br s , 1h ), 5 . 33 ( abq , 2h ), 3 . 83 ( s , 3h ), 2 . 72 ( q , 2h ), 2 . 575 ( s , 3h ), 2 . 49 ( s , 3h ), 1 . 7 - 1 . 47 ( m , 2h ), 0 . 97 ( t , 3h ), 0 . 9 ( t , 3h ). a mixture of 5 . 0 g ( 25 mmol ) of 3 &# 39 ;, 4 &# 39 ;- dimethoxyphenylacetic acid and thionyl chloride 2 . 32 ml ( 1 . 25 eq .) was stirred and refluxed while bromine 4 . 5 ml , 3 . 5 eq .) was added dropwise to the reaction mixture . the reaction was refluxed overnight then cooled . methanol ( 30 ml ) was cautiously added and the reaction mixture was stirred an additional 1 hour at room temperature . the mixture was then evaporated in vacuo , and the residue was purified on a silica gel flash chromatography column eluted with 10 % ethyl acetate / hexane to afford 0 . 80 g ( 7 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 37 ( s , 1h ), 5 . 94 ( s , 2h ), 3 . 88 ( s , 3h ), 3 . 85 ( s , 3h ), 3 . 79 ( s , 3h ). using the k 2 co 3 / acetone conditions for phenol alkylation described in step b of example 3 , 5 , 7 - dimethyl - 2 - ethyl - 3 -[ 4 - hydroxy - 3 - propylphenyl ] methyl - 3h - imidazo [ 4 , 5 - b ] pyridine was alkylated with the product of step a . standard workup and purification by flash chromatography afforded a 65 % yield of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 15 ( s , 1h ), 6 . 98 ( dd , 1h ), 6 . 86 ( s , 1h ), 6 . 79 ( dd , 1h ), 6 . 54 ( d , 1h , 8 . 42 hz ), 6 . 04 ( s , 1h ), 5 . 22 ( abq , 2h ), 3 . 825 ( s , 3h ), 3 . 8 ( s , 3h ), 3 . 713 ( s , 3h ), 2 . 76 ( q , 2h , 7 . 6 hz ), 2 . 59 ( s , 3h ), 2 . 561 ( s , 3h ), 2 . 477 ( dd , 2h , 7 . 65 hz , 7 . 6 hz ), 1 . 675 - 1 . 45 ( m , 2 h ), 1 . 268 ( t , 3h ), 0 . 889 ( t , 3h ). using the general procedure for ester hydrolysis described in step d of example 2 , the product of step b was convened to the title compound in 72 % yield . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 25 ( br s , 1h ), 6 . 97 ( s , 1h ), 6 . 94 ( s , 1h ), 6 . 82 ( br s , 1h ), 6 . 68 ( br s , 1h ), 5 . 41 ( s , 3h ), 3 . 80 ( s , 3h ), 3 . 78 ( s , 3h ), 2 . 80 ( m , 2h ), 2 . 58 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 22 ( m , 2h ), 1 . 8 - 1 . 45 ( m , 2h ), 1 . 25 ( t , 3h ), 0 . 84 ( t , 3h ). to a solution of 63 mg ( 0 . 09 mmol ) of the product of step b of example 6 in methanol was added 5 mg of palladium chloride , 20 mg of sodium borohydride and the mixture was stirred at room temperature for 2 hours . the reaction mixture was evaporated in vacuo , and the residue was purified on a silica gel flash chromatography column eluted with 50 % ethyl acetate / hexane to afford 22 mg ( 45 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 07 ( s , 1h ), 7 . 04 ( d , 1h , 8 . 13 hz ), 6 . 97 ( s , 1h ), 6 . 85 ( s , 1h ), 6 . 85 ( d , 1h ), 6 . 78 ( dd , 1h ), 6 . 57 ( d , 1h ), 5 . 48 ( s , 1h ), 5 . 33 ( s , 1h ), 3 . 86 ( s , 3h ), 3 . 85 ( s , 3h ), 3 . 65 ( s , 3h ), 2 . 75 ( q , 2h , 7 . 52 hz ), 2 . 59 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 65 - 2 . 5 ( m , 2h ), 1 . 72 - 1 . 47 ( m , 2h ), 1 . 252 ( t , 3h , 7 . 69 hz ), 0 . 89 ( t , 3h , 7 . 34 hz ). using the general procedure for ester hydrolysis described in step d of example 2 , the product of step a was converted to the title compound in 90 % yield . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 2 ( s , 1h ), 7 . 14 ( d , 1h ), 6 . 98 ( s , 1h ), 6 . 84 ( d , 1h ), 6 . 82 ( s , 1h ), 6 . 74 ( d , 1h ), 6 . 65 ( d , 1h ), 5 . 5 ( s , 1h ), 5 . 3 ( abq , 2h ), 3 . 86 ( s , 3h ), 3 . 84 ( s , 3h ), 2 . 62 ( q , 2h ), 2 . 7 - 2 . 55 ( m , 2h ), 2 . 52 ( s , 3h ), 2 . 39 ( s , 3h ), 1 . 7 - 1 . 47 ( m , 2h ), 1 . 22 ( t , 3h ), 0 . 89 ( t , 3h ). a solution of 3 . 04 g ( 15 . 8 mmol ) of methyl 4 - hydroxy - 3 - propenylbenzoate ( prepared by the procedure described in patent application wo91 / 11999 ) was refluxed with anhydrous potassium carbonate ( 4 . 37 g , 2 equiv ) and allyl bromide ( 3 . 5 ml , 2 . 5 equiv ) in acetone overnight . the mixture was filtered through celite and the filter cake was washed with acetone and dichloromethane . after removing the solvents , the resulting oil was distilled under high vacuum to give 3 . 2 g ( 87 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 87 ( dd , 1h ), 7 . 83 ( d , 1h ), 6 . 83 ( d , 1h ), 6 . 07 - 5 . 92 ( m , 2h ), 5 . 41 ( dd , 1h ), 5 . 27 ( dd , 1h ), 5 . 07 ( dd , 1h ), 5 . 05 ( dd , 1h ), 4 . 58 ( d , 2h ), 3 . 83 ( s , 3h ), 3 . 4 ( d , 2h ). the product of step a ( 3 . 2 g , 13 . 8 mmol ) was refluxed in 1 , 2 - dichlorobenzene for 3 days in the presence of a catalytic amount of bht ( 10 mg ). flash column chromatography of the mixture using hexane and then 10 % and 20 % ethyl acetate in hexane afforded 3 . 1 g ( 97 %) of the title compound . 1 h nmr ( 200 mhz , cdcl 3 , ppm ): δ 7 . 73 ( s , 2h ), 6 . 12 - 5 . 92 ( m , 2h ), 5 . 63 ( s , 1h ), 5 . 21 ( dd , 2h ), 5 . 15 ( dd , 2h ), 3 . 87 ( s , 3h ), 3 . 43 ( dd , 4h ). the product of step b ( 3 . 1 g , 13 . 36 mmol ) was treated with tert - butyldimethylsilyl chloride ( 2 . 22 g , 1 . 1 equiv ), triethylamine ( 3 ml ) and dmap ( 0 . 1 equiv ) in dichloromethane overnight . the mixture was concentrated and flash chromatographed with 5 % and then 10 % ethyl acetate in hexane to finish 4 . 5 g ( 97 %) of the title compound . 1 h nmr ( 200 mhz , cdcl 3 , ppm ): δ 7 . 72 ( s , 2h ), 6 . 02 - 5 . 30 ( m , 2h ), 5 . 12 ( dd , 2h ), 5 . 07 ( dd , 2h ), 3 . 86 ( s , 3h ), 3 . 38 ( dd , 4h , 7 hz ), 1 . 02 ( s , 9h ), 0 . 21 ( s , 6h ). a solution of 5 . 0 g ( 14 . 45 mmol ) of the product of step c in 250 ml ethanol containing 5 % rh / c ( 0 . 25 g ) was shaken under a 40 psi pressure of hydrogen . upon completion of reduction , the mixture was filtered through celite , the filter cake was washed with methanol and dichloromethane . removal of solvents afforded 4 . 55 g ( 90 %) of the title compound . 1 h nmr ( 200 mhz , cdcl 3 , ppm ): δ 7 . 66 ( s , 2h ), 3 . 84 ( s , 3h ), 2 . 54 ( dd , 4h , 7 . 91 hz , 7 . 41 hz ), 1 . 56 ( sextet , 4h ), 0 . 98 ( s , 9h ), 0 . 899 ( t , 6h ), 0 . 18 ( s , 6h ). lithium aluminum hydride ( 9 ml of a 1m solution in thf ) was added cautiously to a solution of the product of step d at 0 ° c ., and the reaction mixture was stirred overnight . ethyl acetate was added to the mixture , cooled to 0 ° c . and treated with cold 1n hcl . after separating the organic phase , the aqueous phase was extracted with a mixture of ethyl acetate - ether - dichloromethane . the combined organic extracts were dried and concentrated . the concentrated material was purified by flash column chromatography using 20 % ethyl acetate in hexane to afford 4 . 2 g ( 92 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 6 . 95 ( s , 2h ), 4 . 54 ( s , 2h ), 2 . 52 ( dd , 4h ), 1 . 55 ( sextet , 4h ), 0 . 99 ( s , 9h ), 0 . 90 ( t , 6h ), 0 . 16 ( s , 6h ). to a solution of 4 . 2 g ( 13 . 0 mmol ) of the product of step e , 2 . 5 g ( 14 . 0 mmol ) of 5 , 7 - dimethyl - 2 - ethylimidazo [ 4 , 5 - b ] pyridine ( prepared by the method described in patent application wo 91 / 11999 ), and 5 . 62 ( 20 . 0 mmol ) of triphenylphosphine dissolved in 40 ml of thf , was added 3 . 396 g ( 20 . 0 mmol ) of diethyl azodicarboxylate and the mixture was stirred for 1 hour . the reaction mixture was then concentrated in vacuo and the residual oil was purified on a silica gel flash chromatography column eluted with 25 - 40 % ethyl acetate / hexane to afford 5 g ( 80 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 6 . 84 ( s , 1h ), 6 . 71 ( s , 2h ), 5 . 29 ( s , 2h ), 2 . 75 ( q , 2h ), 2 . 57 ( s , 3h ), 2 . 55 ( s , 3h ), 2 . 4 ( dd , 4h ), 1 . 42 ( sextet , 4h ), 1 . 27 ( t , 3h ), 0 . 94 ( s , 9h ), 0 . 8 ( t , 6h ), 0 . 10 ( s , 6h ). a thf solution of 5 . 0 g ( 10 . 44 mmol ) of the product of step f was treated with tetrabutylammonium fluoride ( 1 . 2 equiv , 1m solution in thf ) overnight . thf was removed in vacuo and the residue was flash chromatographed using 30 - 50 % ethyl acetate in hexane as eluent to afford 3 . 35 g ( 88 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 6 . 86 ( s , 1h ), 6 . 81 ( s , 1h ), 6 . 73 ( s , 2h ), 5 . 37 ( s , 1h ), 5 . 30 ( s , 2h ), 2 . 76 ( q , 2h ), 2 . 6 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 44 ( dd , 4h ), 1 . 52 ( sextet , 4h ), 1 . 23 ( t , 3h ), 0 . 88 ( t , 6h ). using the k 2 co 3 / acetone conditions for phenol alkylation described in step b of example 3 , the product of step g was alkylated with methyl 2 - bromophenylacetate . standard workup and purification by flash chromatography afforded a 96 % yield of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 44 - 7 . 42 ( m , 2h ), 7 . 37 - 7 . 31 ( m , 3h ), 6 . 88 ( s , 1h ), 6 . 74 ( s , 2h ), 5 . 38 ( s , 1h ), 5 . 33 ( s , 2h ), 3 . 7 ( s , 3h ), 2 . 80 ( q , 2h ), 2 . 62 ( s , 3h ), 2 . 57 ( s , 3h ), 2 . 38 ( dd , 2h ), 2 . 3 - 2 . 25 ( m , 2h ), 1 . 55 - 1 . 47 ( m , 2h ), 1 . 46 - 1 . 37 ( m , 2h ), 1 . 36 ( t , 3h ), 0 . 86 ( t , 3h ), 0 . 72 ( t , 3h ). using the general procedure for ester hydrolysis described in step d of example 2 , the product of step h was convened to the title compound in 80 % yield . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 47 - 7 . 34 ( m , 2h ), 7 . 33 - 7 . 22 ( m , 3h ), 6 . 92 ( s , 1h ), 6 . 69 ( s , 2h ), 5 . 35 ( br s , 3h ), 2 . 78 ( q , 2h ), 2 . 58 ( s , 3h ), 2 . 55 ( s , 3h ), 2 . 62 - 2 . 25 ( m , 4h ), 1 . 45 - 1 . 28 ( m , 4h ), 1 . 2 ( t , 3h ), 0 . 7 ( t , 6h ). using the k 2 co 3 / acetone conditions for phenol alkylation described in step b of example 3 , 5 , 7 - dimethyl - 2 - ethyl - 3 -[ 4 - hydroxy - 3 , 5 - dipropylphenyl ] methyl - 3h - imidazo [ 4 , 5 - b ] pyridine was alkylated with methyl 2 - bromo -( 2 &# 39 ;- methoxy ) phenylacetate . standard workup and purification by flash chromatography afforded the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 62 ( dd , 1h , j = 2 . 1 , 1 . 9 hz ), 7 . 40 ( dd , 1h ), 7 . 30 ( dd , 1h ), 6 . 86 ( s , 1h ), 6 . 72 ( s , 2h ), 6 . 70 ( dd , 1h ), 5 . 37 ( s ), 5 . 35 ( s ), 5 . 32 ( s , 2h ), 3 . 69 ( s , 3h ), 3 . 68 ( s , 3h ), 2 . 74 ( q , 2h , j = 7 . 5 hz ), 2 . 61 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 34 - 2 . 19 ( m , 4h ), 1 . 50 - 1 . 29 ( m , 4h ), 1 . 23 ( t , 3h , j = 7 . 54 hz ), 0 . 74 ( t , 6h , j = 7 . 3 hz ). using the general procedure for ester hydrolysis described in step d of example 2 , the product of step a was convened to the title compound in 77 % yield . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 72 - 7 . 66 ( m ), 7 . 55 ( br s , 1h ), 7 . 52 - 7 . 48 ( m ), 7 . 35 ( dd , 1h ), 6 . 86 ( s , 1h ), 6 . 72 ( s , 2h ), 6 . 69 ( dd , 1h ), 5 . 38 ( s , 1h ), 5 . 30 ( abq , 2h ), 3 . 64 ( s , 3h ), 2 . 76 ( q , 2h , 7 . 6 hz ), 2 . 55 ( s , 3h ), 2 . 52 ( s , 3h ), 2 . 28 ( m , 4h ), 1 . 50 - 1 . 18 ( m , 4h ), 1 . 13 ( t , 3h ), 0 . 74 ( t , 6h ). the title compound was prepared according to the synthetic route described for example 8 except for step h where methyl 2 - bromo -( 3 &# 39 ;- methoxy ) phenylacetate was used as the alkylating agent . 1 h nmr ( 200 mhz , cd 3 od , ppm ): δ 7 . 26 ( t , 1h , j = 7 . 8 hz ), 7 . 02 - 6 . 90 ( m , 4h ), 6 . 77 ( s , 2h ), 5 . 44 ( s , 1h ), 5 . 00 ( s , 1h ), 3 . 77 ( s , 3h ), 2 . 84 ( q , 2h , j = 7 . 6 hz ), 2 . 60 ( s , 3h ), 2 . 58 ( s , 3h ), 2 . 31 ( t , 4h , j = 7 . 8 hz ), 1 . 45 - 1 . 29 ( m , 4h ), 1 . 21 ( t , 3h , j = 7 . 6 hz ), 0 . 74 ( t , 6h , j = 7 . 3 hz ). the title compound was prepared according to the synthetic route described for example 8 except for step h where methyl 2 - bromo -( 4 &# 39 ;- methoxy ) phenylacetate was used as the alkylating agent . 1 h nmr ( 200 mhz , cd 3 od , ppm ): δ 7 . 27 ( d , 2h , j = 8 . 8 hz ), 7 . 19 ( s , 1h ), 6 . 92 - 6 . 89 ( m , 4h ), 5 . 53 ( s , 2h ), 5 . 00 ( s , 1h ), 2 . 97 ( q , 2h , j = 7 . 5 hz ), 2 . 62 ( s , 6h ), 2 . 31 ( t , 4h , j = 7 . 8 hz ), 1 . 46 - 1 . 17 ( m , 4h ), 1 . 25 ( t , 3h , j = 7 . 6 hz ), 0 . 75 ( t , 6h , j = 7 . 3 hz ). using the k 2 co 3 / acetone conditions for phenol alkylation described in step b of example 3 , the 5 , 7 - dimethyl - 2 - ethyl - 3 -[ 4 - hydroxy - 3 , 5 - dipropylphenyl ] methyl - 3h - imidazo [ 4 , 5 - b ] pyridine was alkylated with methyl 2 , 2 &# 39 ;, 5 &# 39 ;- tribromo - 3 &# 39 ;, 4 &# 39 ;- dimethoxyphenylacetate . standard workup and purification by flash chromatography afforded a 60 % yield of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 36 ( s , 1h ), 6 . 89 ( s , 1h ), 6 . 75 ( s , 2h ), 5 . 55 ( s , 1h ), 5 . 34 ( abq , 2h ), 3 . 88 ( s , 3h ), 3 . 84 ( s , 3h ), 3 . 69 ( s , 3h ), 2 . 78 ( q , 2h ), 2 . 62 ( s , 3h ), 2 . 41 - 2 . 20 ( m , 4h ), 1 . 45 - 1 . 32 ( m , 4h ), 0 . 85 ( t , 3h ), 0 . 74 ( t , 6h ). using the general procedure for ester hydrolysis described in step d of example 2 , the product of step a was convened to the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 7 . 45 ( br s , 1h ), 7 . 01 ( s , 1h ), 6 . 75 ( s , 2h ), 5 . 51 ( s , 1h ), 5 . 44 ( abq , 2h ), 3 . 88 ( s , 3h ), 3 . 78 ( s , 3h ), 3 . 34 ( s , 3h ), 2 . 82 ( q , j = 7 . 5 hz , 2h ), 2 . 59 ( s , 3h ), 2 . 57 ( s , 3h ), 2 . 24 - 240 ( m , 4h ), 1 . 38 - 1 . 52 ( m , 2h ), 1 . 24 - 1 . 36 ( m , 2h ), 1 . 20 ( t , j = 7 . 5 hz , 3h ), 0 . 74 ( t , j = 7 . 5 hz , 6h ). the titled compound was prepared following the synthetic route described for the synthesis of example 8 except for step h where methyl 2 - bromo -( 3 , 4 - methylenedioxyphenyl ) acetate was used as the alkylating agent . 1 h nmr ( 400 mhz , cd 3 od ): δ 7 . 15 ( s , 1h ); 6 . 95 ( d , 1h , j = 1 . 6 hz ), 6 . 86 ( s , 2h ); 6 . 83 ( dd , 1h , j = 8 . 0 , 1 . 6 hz ), 6 . 77 ( d , 1h , j = 7 . 9 hz ), 5 . 96 ( s , 2h ), 5 . 51 ( s , 2h ), 4 . 96 ( s , 1h ), 2 . 96 ( q , 2h , j = 7 . 6 hz ), 2 . 62 ( s , 3h ), 2 . 61 ( s , 3h ), 2 . 32 ( t , 4h , j = 7 . 9 hz ), 1 . 43 ( sx , 2h , j = 7 . 6 hz ), 1 . 34 ( sx , 2h , j = 7 . 5 hz ), 1 . 24 ( t , 2h , j = 7 . 6 hz ), 0 . 77 ( t , 6h , j = 7 . 3 hz ). the titled compound was prepared following the synthetic route described for the synthesis of example 8 except for step h where methyl 2 - bromo - 2 -( benzofur - 5 - yl ) acetate was used as the alkylating agent . 1 h nmr ( 400 mhz , cd 3 od ): δ 7 . 78 ( d , 1h , j = 2 . 2 hz ), 7 . 66 ( d , 1h , j = 1 . 6 hz ), 7 . 49 ( d , 1h , j = 8 . 4 hz ), 7 . 40 ( dd , 1h , j = 1 . 8 , 8 . 6 hz ), 7 . 03 ( s , 1h ), 6 . 82 ( s , 1h ), 6 . 76 ( s , 2h ), 5 . 44 ( s , 2h ), 5 . 13 ( s , 1h ), 2 . 84 ( q , 2h , j = 7 . 6 hz ), 2 . 60 ( s , 3h ), 2 . 57 ( s , 3h ), 2 . 27 ( t , 4h , j = 8 . 0 hz ), 1 . 34 ( m , 4h ), 1 . 20 ( t , 3h , j = 7 . 6 hz ), 0 . 68 ( t , 6h , j = 7 . 3 hz ). the titled compound was prepared following the synthetic route described for the synthesis of example 8 except for step h where methyl 2 - bromo -( 3 , 4 - dimethoxyphenyl ) acetate was used as the alkylating agent . 1 h nmr ( 400 mhz , cd 3 od / cdcl 3 , ppm ): δ 7 . 06 ( s , 1h ), 6 . 98 ( s , 1h ), 6 . 85 ( m , 2h ), 6 . 73 ( s , 1h ), 5 . 437 ( s , 1h ), 5 . 41 ( s , 2h ), 3 . 81 ( s , 3h ), 3 . 782 ( s , 3h ), 2 . 83 ( q , 2h ), 2 . 59 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 27 ( t , 4h ), 1 . 45 - 1 . 38 ( m , 2h ), 1 . 31 - 1 . 15 ( m , 2h ), 1 . 207 ( t , 3h ), 0 . 73 ( t , 3h ). the titled compound was prepared following the synthetic route described for the synthesis of example 8 except for step h where methyl 2 - bromo -( 3 , 5 - dimethoxyphenyl ) acetate was used as the alkylating agent . 1 h nmr ( 400 mhz , cd 3 od / cdcl 3 , ppm ) δ 6 . 96 ( s , 1h ), 6 . 72 ( s , 2h ), 6 . 57 ( d , 2h ), 6 . 39 ( dt , 1h ), 5 . 41 ( s , 1h ), 5 . 39 ( s , 2h ), 3 . 71 ( s , 6h ), 2 . 81 ( q , 2h ), 2 . 59 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 29 ( t , 4h ), 1 . 417 ( m , 2h ), 1 . 30 ( m , 2h ), 1 . 21 ( t , 3h ), 0 . 73 ( t , 6h ). the titled compound was prepared following the synthetic route described for the synthesis of example 8 except for step h where methyl 2 - bromo - 2 -( indol - 5 - yl ) acetate was used as the alkylating agent . 1 h nmr ( 400 mhz , cd 3 od / cdcl 3 , ppm ): δ 7 . 46 ( s , 1h ), 7 . 22 ( dd , 1h ), 7 . 17 ( d , 1h , j = 3 . 09 hz ), 6 . 99 ( s , 1h ), 6 . 68 ( s , 2h ), 6 . 33 ( d , 1h , j = 3 . 23 hz ), 5 . 41 ( abq , 2h ), 4 . 9 ( s , 1h ), 2 . 81 ( q , 2h ), 2 . 59 ( s , 3h ), 2 . 56 ( s , 3h ), 2 . 24 - 2 . 80 ( m , 4h ), 1 . 43 - 1 . 3 ( m , 2h ), 1 . 18 ( t , 3h ), 1 . 23 - 1 . 12 ( m , 2h ), 0 . 64 ( t , 6h ). a mixture of ( 3 , 4 - methylenedioxyphenyl ) acetic acid ( 4 . 64 g , 25 . 74 mmol ) in dry dmf ( 40 ml ), cesium carbonate ( 9 . 2 g , 25 . 74 mmol ) and methyl iodide ( 3 . 7 g , 26 . 0 mmol ) in dry dmf ( 40 ml ) was stirred at room temperature for 3 h . at the end of this period , the reaction mixture was poured into ice water and extracted with ethyl acetate . the organic phase was washed with saturated nahco 3 , water , brine and then dried ( mgso 4 ) and filtered . the filtrate was concentrated in vacuo to provide pure methyl ( 3 , 4 - methylenedioxyphenyl ) acetate as an oil ( 4 . 38 g ). n - bromosuccinimide ( 3 . 95 g , 22 . 2 mmol ) and aibn ( 0 . 098 g , 0 . 06 mmol ) were added to a solution of methyl ( 3 , 4 - methylenedioxy - phenyl ) acetate ( 3 . 9 g , 21 . 2 mmol ) and the mixture was refluxed for 2 . 5 h . the reaction was cooled and filtered . the filtrate was concentrated in vacuo and the residue was purified by flash chromatography on silica - gel using 10 % ethyl acetate - hexane . yield 2 . 6 g ( oil ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 105 ( d , 1h ), 6 . 93 ( d , 1h ), 6 . 72 ( m , 1h ), 5 . 964 ( s , 2h ), 5 . 28 ( s , 1h ), 3 . 76 ( s , 3h ). to a solution of ( 3 , 5 - dipropyl - 4 - hydroxy ) benzyl alcohol ( 0 . 19 g , 1 . 0 mmol ) in dry dmf ( 4 ml ) were added cesium carbonate ( 0 . 33 g , 1 . 01 mmol ) and methyl 2 - bromo - 2 -( 3 , 4 - methylenedioxyphenyl ) acetate ( 0 . 272 g , 1 . 0 mmol ) and the mixture was stirred at room temperature for 3 h . at the end of this period , the reaction mixture was poured into ice water and extracted with ethyl acetate . the organic phase was washed with water , brine , dried ( mgso 4 ) and then filtered . the filtrate was concentrated in vacuo to provide an oil , which was then purified by flash chromatography on silica - gel using ethyl acetate - hexane ( 1 : 4 ) to provide the titled product as a thick colorless oil ( 0 . 30 g ). 1 h - nmr ( 200 mhz , cdcl 3 , ppm ): δ 7 . 05 ( s , 1h ), 6 . 97 ( s , 2h ), 6 . 88 ( d , 1h ), 6 . 75 ( d , 1h ), 5 . 97 ( s , 2h ), 5 . 00 ( s , 1h ), 4 . 55 ( s , 2h ), 3 . 74 ( s , 3h ), 2 . 38 ( m , 4h ), 1 . 45 ( m , 4h ), 0 . 82 ( t , 6h ). to a solution of the product of step b ( 0 . 53 g , 1 . 38 mmol ) in dry thf ( 10 ml ) were added ph 3 p ( 0 . 49 g , 2 . 06 mmol ), cbr4 ( 0 . 69 g , 2 . 06 mmol ) and ch 3 cn ( 2 ml ), and the mixture was stirred at room temperature for 14 h . at the end of this period , the reaction mixture was concentrated in vacuo to provide an oil , which was then purified by flash chromatography on silica - gel using ethyl acetate - hexane ( 1 : 9 ) to provide the titled product as a thick colorless oil ( 0 . 57 g ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 7 . 04 ( d , 1h ), 7 . 00 ( s , 2h ), 6 . 87 ( dd , 1h ), 6 . 76 ( d , 1h ), 5 . 97 ( s , 2h ), 5 . 00 ( s , 1h ), 4 . 41 ( s , 2h ), 3 . 73 ( s , 3h ), 2 . 36 ( m , 4h ), 1 . 45 ( m , 4h ), 0 . 82 ( t , 6h ). cesium carbonate ( 294 mg , 0 . 902 mmol ) was added to 2 - methylimidazo [ 4 , 5 - b ] pyridine ( 60 mg , 0 . 451 mmol ) in dmf ( 2 ml ) at room temperature under nitrogen . after stirring at 50 ° c . for 15 min , a solution of 4 -( 1 - carbomethoxy - 1 -( 3 , 4 - methylenedioxyphenyl ) methoxy )- 3 , 5 - dipropylbenzyl bromide ( from step c ) ( 27 1 mg , 0 . 585 mmol ) in dmf ( 2 ml ) was added and the mixture stirred at 50 ° c . for 12 h . after cooling to room temperature , the mixture was poured onto ice / water and extracted with ethyl acetate ( 4 times ). the combined organic phase was washed with water twice , brine , dried ( magnesium sulfate ) and the solvent removed in vacuo . the crude product ( a mixture of regioisomers ) was purified by flash chromatography on silica - gel ( 3 , 4 , 5 % methanol / methylene chloride ) to provide the title compound ( 87 mg ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 8 . 31 ( d , 1h ), 7 . 95 ( m , 1h ), 7 . 19 ( m , 1h ), 7 . 00 ( d , 1h ), 6 . 81 ( d , 1h ), 6 . 75 ( s , 2h ), 6 . 72 ( d , 1h ), 5 . 94 ( s , 2h ), 5 . 35 ( s , 2h ), 4 . 94 ( s , 1h ), 3 . 70 ( s , 3h ), 2 . 50 ( s , 3h ), 2 . 29 ( m , 4h ), 1 . 35 ( m , 4h ), 0 . 75 ( t , 6h ). a 5n sodium hydroxide solution ( 0 . 4 ml ) was added to a stirred mixture of the product of step d ( 53 . 5 mg , 0 . 104 mmol ) in methanol ( 4 ml ). a few drops of methylene chloride were added to allow stirring then the mixture was stirred at room temperature for 2 h . the solution volume was reduced to ˜ 10 % in vacuo then 5 % citric acid solution was added . the mixture was extracted with ethyl acetate ( 3 times ). the combined organic phase was washed with water , brine , dried ( magnesium sulfate ) and the solvent removed in vacuo . the residue was chromatographed ( 8 , 10 % methanol / methylene chloride ) to give the titled compound ( 28 . 5 mg ) as a white solid . 1 h - nmr ( 400 mhz , cd 3 od , ppm ): δ 8 . 33 ( d , 1h ) 7 . 98 ( m , 1h ), 7 . 31 ( dd , 1h ), 6 . 98 ( d , 1h ), 6 . 80 ( m , 3h ), 6 . 69 ( m , 1h ), 5 . 91 ( s , 2h ), 5 . 44 ( s , 2h ), 4 . 83 ( s , 1h ), 2 . 52 ( s , 3h ), 2 . 30 ( m , 4h ), 1 . 42 ( m , 2h ), 1 . 29 ( m , 2h ), 0 . 75 ( t , 6h ). the titled compound , 1 -[ 4 -( 1 - carbomethoxy - 1 -( 3 , 4 - methylenedioxyphenyl ) methoxy )- 3 , 5 - dipropylphenylmethyl ]- 2 - methyl - 1h - imidazo [ 4 , 5 - b ] pyridine ( 38 mg ), was isolated from the crude product obtained in step d of example 18 . 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 8 . 47 ( m , 1h ), 7 . 45 ( d , 1h ), 7 . 10 ( m , 1h ), 6 . 99 ( d , 1h ), 6 . 81 ( d , 1h ), 6 . 72 ( d , 1h ), 6 . 63 ( s , 2h ), 5 . 95 ( s , 2h ), 5 . 19 ( s , 2h ), 4 . 96 ( s , 1h ), 3 . 71 ( s , 3h ), 2 . 60 ( s , 3h ), 2 . 30 ( m , 4h ), 1 . 36 ( m , 4h ), 0 . 75 ( t , 6h ). a 5n sodium hydroxide solution ( 0 . 2 ml ) was added to a stirred mixture of the product of step a ( 27 mg , 0 . 0524 mmol ) in methanol ( 2 ml ). a few drops of methylene chloride were added to allow stirring then the mixture was stirred at room temperature for 2 h . the solution volume was reduced to ˜ 10 % in vacuo then 5 % citric acid solution added . the mixture was extracted with ethyl acetate ( 3 times ). the combined organic phase was washed with water , brine , dried ( magnesium sulfate ) and the solvent removed in vacuo . the residue was purified by flash - chromatography using silica gel ( 8 , 10 % methanol / methylene chloride ) to give the titled compound ( 12 . 8 mg ) as a white solid . 1 h - nmr ( 400 mhz , cd 3 od , ppm ): δ 8 . 36 ( d , 1h ), 7 . 85 ( d , 1h ), 7 . 26 ( m , 1h ), 6 . 98 ( s , 1h ), 6 . 78 ( m , 3h ), 6 . 69 ( d , 1h ), 5 . 91 ( s , 2h ), 5 . 40 ( s , 2h ), 4 . 82 ( s , 1h ), 2 . 62 ( s , 3h ), 2 . 32 ( m , 4h ), 1 . 44 ( m , 2h ), 1 . 29 ( m , 2h ), 0 . 75 ( t , 6h ). cesium carbonate ( 117 . 3 mg , 0 . 36 mmol ) was added to 4 - chloroimidazo [ 4 , 5 - c ] pyridine ( 25 mg , 0 . 18 mmol ) in dmf ( 2 ml ) at room temperature under nitrogen . after stirring for 15 min , a solution of 4 -( 1 - carbomethoxy - 1 -( 3 , 4 - methylenedioxyphenyl ) methoxy )- 3 , 5 - dipropylbenzyl bromide ( 106 . 5 mg , 0 . 23 mmol ) in dmf ( 2 ml ) was added and the mixture stirred at room temperature for 12 h . the mixture was poured onto ice / water and the crude product that precipitated was collected by filtration . the crude material was pre - adsorbed on silica gel and chromatographed ( 0 to 50 % hexane / ethyl acetate ) to afford the title compound ( 25 mg ). 1 h - nmr ( cdcl 3 ): δ 8 . 24 ( d , 1h ), 8 . 00 ( s , 1h ), 7 . 68 ( d , 1h ), 7 . 04 ( s , 1h ), 6 . 88 ( d , 1h ), 6 . 82 ( s , 2h ), 6 . 75 ( d , 1h ), 5 . 96 ( s , 2h ), 5 . 60 ( s , 2h ), 5 . 00 ( s , 1h ), 3 . 71 ( s , 3h ), 2 . 35 ( m , 4h ), 1 . 40 ( m , 4h ), 0 . 78 ( t , 6h ). a 5n sodium hydroxide solution ( 0 . 1 ml ) was added to a stirred mixture of the product of step a ( 25 mg , 0 . 0466 mmol ) in methanol ( 1 ml ). a few drops of methylene chloride were added to allow stirring then the mixture was stirred at room temperature for 3 h . the solvent was removed in vacuo then 5 % citric acid solution added . the precipitate was filtered off , washed with water and dried in vacuo to give the titled compound ( 20 mg ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 8 . 22 ( d , 1h ), 8 . 01 ( s , 1h ), 7 . 68 ( d , 1h ), 6 . 99 ( s , 1h ), 6 . 86 ( d , 1h ), 6 . 81 ( s , 2h ), 6 . 75 ( d , 1h ), 5 . 95 ( s , 2h ), 5 . 60 ( s , 2h ), 5 . 05 ( s , 1h ), 2 . 35 ( m , 4h ), 1 . 40 ( m , 4h ), 0 . 78 ( t , 6h ). the titled compound ( 59 mg ) was isolated from the crude product obtained in step a of example 20 . 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 8 . 16 ( d , 1h ), 8 . 00 ( s , 1h ), 7 . 15 ( d , 1h ), 7 . 00 ( s , 1h ), 6 . 85 ( d , 1h ), 6 . 78 ( s , 2h ), 6 . 75 ( d , 1h ), 5 . 95 ( s , 2h ), 5 . 25 ( s , 2h ), 4 . 99 ( s , 1h ), 3 . 71 ( s , 3h ), 2 . 34 ( m , 4h ), 1 . 42 ( m , 4h ), 0 . 78 ( t , 6h ). a 5n sodium hydroxide solution ( 0 . 1 ml ) was added to a stirred mixture of the product of step a ( 22 mg , 0 . 0410 mmol ) in methanol ( 1ml ). a few drops of methylene chloride were added to allow stirring then the mixture was stirred at room temperature for 2 . 5 h . the solvent was removed in vacuo then 5 % citric acid solution added . the precipitate was filtered off , washed with water and dried in vacuo to give the titled carboxylic acid ( 18 mg ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 8 . 18 ( d , 1h ), 8 . 02 ( s , 1h ), 7 . 15 ( d , 1h ), 6 . 99 ( s , 1h ), 6 . 85 ( d , 1h ), 6 . 81 ( s , 2h ), 6 . 75 ( d , 1h ), 5 . 97 ( s , 2h ), 5 . 25 ( s , 2h ), 5 . 06 ( s , 1h ), 2 . 35 ( m , 4h ), 1 . 42 ( m , 4h ), 0 . 78 ( t , 6h ). cesium carbonate ( 156 mg , 0 . 48 mmol ) was added to imidazo [ 4 , 5 - c ] pyridine ( 28 . 6 mg , 0 . 24 mmol ) in dmf ( 3 ml ) at room temperature under nitrogen . after stirring for 15 min , a solution of 4 -( 1 - carbomethoxy - 1 -( 3 , 4 - methylenedioxyphenyl )- methoxy )- 3 , 5 - dipropylbenzyl bromide ( 121 mg , 0 . 26 mmol ) in dmf ( 3 ml ) was added and the mixture stirred at 50 ° c . for 18 h . the mixture was poured onto ice / water and extracted with ethyl acetate ( 3 × 30 ml ). the combined organic phase was washed with water , brine , dried ( magnesium sulfate ) and the solvent removed in vacuo . the crude material was purified by flash column chromatography ( 0 to 5 % methanol / methylene chloride ) to afford the less polar isomer of the titled compound ( 19 mg ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 8 . 92 ( s , 1h ), 8 . 48 ( d , 1h ), 8 . 23 ( s , 1h ), 7 . 91 ( s , 1h ), 7 . 02 ( s , 1h ), 6 . 86 ( d , 1h ), 6 . 84 ( s , 2h ), 6 . 75 ( d , 1h ), 5 . 95 ( s , 2h ), 5 . 38 ( s , 2h ), 4 . 99 ( s , 1h ), 3 . 71 ( s , 3h ), 2 . 35 ( m , 4h ), 1 . 40 ( m , 4h ), 0 . 78 ( t , 6h ). a 5n sodium hydroxide solution ( 0 . 1 ml ) was added to a stirred mixture of the product of step a ( 19 mg , 0 . 038 mmol ) in methanol ( 1 ml ). a few drops of methylene chloride were added to allow stirring then the mixture was stirred at room temperature for 3 h . the solvent was removed in vacuo then 5 % citric acid solution added . the mixture was extracted with ethyl acetate ( 3 × 30 ml ), washed water , brine , dried ( magnesium sulfate ), and the solvent was removed in vacuo to give the titled compound ( 14 mg ). 1 h - nmr ( 400 mhz , cd 3 od , ppm ): δ 8 . 98 ( s , 1h ), 8 . 75 ( s , 1h ), 8 . 46 ( s , 1h ), 7 . 96 ( d , 1h ), 7 . 05 ( s , 2h ), 7 . 00 ( s , 1h ), 6 . 85 ( d , 1h ), 6 . 78 ( d , 1h ), 5 . 96 ( s , 2h ), 5 . 52 ( s , 2h ), 5 . 00 ( s , 1h ), 3 . 71 ( s , 3h ), 2 . 40 ( m , 4h ), 1 . 46 ( m , 4h ), 0 . 80 ( t , 6h ). the titled compound was obtained in step a of example 22 as the more polar isomer ( 30 mg ). 1 h - nmr ( 400 mhz , cdcl 3 , ppm ): δ 9 . 16 ( s , 1h ), 8 . 50 ( d , 1h ), 8 . 18 ( s , 1h ), 7 . 50 ( d , 1h ), 7 . 01 ( s , 1h ), 6 . 86 ( d , 1h ), 6 . 80 ( s , 2h ), 6 . 75 ( d , 1h ), 5 . 96 ( s , 2h ), 5 . 34 ( s , 2h ), 4 . 99 ( s , 1h ), 3 . 71 ( s , 3h ), 2 . 35 ( m , 4h ), 1 . 45 ( m , 4h ), 0 . 78 ( t , 6h ). a 5n sodium hydroxide solution ( 0 . 15 ml ) was added to a stirred mixture of the ester , obtained in step a , ( 29 mg , 0 . 058 mmol ) in methanol ( 1 . 5 ml ). a few drops of methylene chloride were added to allow stirring then the mixture was stirred at room temperature for 3 h . the solvent was removed in vacuo then 5 % citric acid solution added . the precipitate was filtered off , washed with water and dried in vacuo to give the titled carboxylic acid ( 19 mg ). 1 h - nmr ( 400 mhz , cdcl 3 / cd 3 od , ppm ): δ 9 . 02 ( s , 1h ), 8 . 49 ( s , 1h ), 8 . 36 ( d , 1h ), 7 . 65 ( d , 1h ), 6 . 98 ( s , 1h ), 6 . 94 ( s , 2h ), 6 . 84 ( d , 1h ), 6 . 75 ( d , 1h ), 5 . 94 ( s , 2h ), 5 . 43 ( s , 2h ), 4 . 95 ( s , 1h ), 2 . 36 ( t , 4h ), 1 . 41 ( m , 4h ), 0 . 78 ( t , 6h ). a 15 ml capacity high pressure vessel equipped with a magnetic stir bar was charged with a solution of 0 . 400 g ( 0 . 74 mmol ) of the product of example 13 in 5 . 0 ml of anhydrous thf and 0 . 300 g ( 1 . 85 mmol ) of 1 , 1 &# 39 ;- carbonyldiimidazole was added . the vessel was sealed and the contents were stirred and heated at 80 ° c . for 2 hours . the reaction was then cooled to room temperature , opened and a solution of 0 . 290 g ( 1 . 84 mmol ) of benzenesulfonamide and 275 μl ( 1 . 84 mmol ) of 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene in 5 ml thf was added . the reaction vessel was resealed and then stirred and heated at 80 ° c . overnight . the reaction vessel was then cooled , opened and the contents were partitioned between water and etoac . the organic layer was separated washed with 10 % aqueous nahso 4 , brine , dried ( mgso 4 ), filtered and evaporated . the residual oil was purified on a silica gel flash chromatography column eluted with 25 % acetone / chcl 3 which afforded after evaporation of the purified fractions 0 . 220 g ( 44 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 64 ( t , j = 7 . 60 hz , 6h ), 1 . 19 ( t , j = 7 . 60 hz , 3h ), 1 . 15 - 1 . 26 ( m , 2h ), 1 . 28 - 1 . 38 ( m , 2h ), 2 . 10 - 2 . 19 ( m , 4h ), 2 . 56 ( s , 3h ), 2 . 60 ( s , 3h ), 2 . 82 ( q , j = 7 . 60 hz , 2h ), 4 . 80 ( s , 1h ), 5 . 42 ( s , 2h ), 5 . 94 ( s , 2h ), 6 . 71 ( s , 2h ), 6 . 73 ( s , 2h ), 6 . 79 ( s , 1h ), 7 . 02 ( s , 1h ), 7 . 46 - 7 . 60 ( m , 3h ), 7 . 78 - 7 . 81 ( m , 2h ). a 15 ml capacity high pressure vessel equipped with a magnetic stir bar was charged with a solution of 0 . 230 g ( 0 . 42 mmol ) of the product of example 13 in 4 . 0 ml of anhydrous thf and 0 . 172 g ( 1 . 06 mmol ) of 1 , 1 &# 39 ;- carbonyldiimidazole was added . the vessel was sealed and the contents were stirred and heated at 80 ° c . for 2 . 5 hours . the reaction was then cooled to room temperature , opened and a solution of 0 . 172 g ( 1 . 06 mmol ) of thiophene - 2 - ylsulfonamide and 158 μl ( 1 . 06 mmol ) of 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene in 4 ml thf was added . the reaction vessel was resealed and then stirred and heated at 80 ° c . overnight . the reaction vessel was then cooled , opened and the contents were partitioned between water and etoac . the organic layer was separated washed with 10 % aqueous nahso 4 , brine , dried ( mgso 4 ), filtered and evaporated . the residual oil was purified on a silica gel flash chromatography column eluted first with 250 ml of chcl 3 / meoh / nh 4 oh ( 95 : 5 : 0 . 5 ), next with 200 ml of chcl 3 / meoh / nh 4 oh ( 92 : 8 : 0 . 5 ), and finally with 200 ml of chcl 3 / meoh / nh 4 oh ( 90 : 10 : 0 . 5 ). evaporation of the purified fractions and drying in vacuo afforded 0 . 104 g ( 36 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 67 ( t , j = 7 . 60 hz , 6h ), 1 . 19 ( t , j = 7 . 60 hz , 3h ), 1 . 16 - 1 . 40 ( m , 4h ), 2 . 16 - 2 . 28 ( m , 4h ), 2 . 56 ( s , 3h ), 2 . 59 ( s , 3h ), 2 . 82 ( q , j = 7 . 60 hz , 2h ), 4 . 78 ( s , 1h ), 5 . 41 ( s , 2h ), 5 . 90 ( s , 2h ), 6 . 66 ( d , j = 8 . 00 hz , 1h , 6 . 70 - 6 . 74 ( m , 3h ), 6 . 93 ( d , j = 1 . 60 hz , 1h ), 6 . 87 - 6 . 99 ( m , 1h ), 7 . 00 ( s , 1h ), 7 . 54 - 7 . 58 ( m , 2h ). a 15 ml capacity high pressure vessel equipped with a magnetic stir bar was charged with a solution of 0 . 230 g ( 0 . 42 mmol ) of the product of example 13 in 4 . 0 ml of anhydrous thf and 0 . 172 g ( 1 . 06 mmol ) of 1 , 1 &# 39 ;- carbonyldiimidazole was added . the vessel was sealed and the contents were stirred and heated at 80 ° c . for 2 hours . the reaction was then cooled to room temperature , opened and a solution of 0 . 213 g ( 1 . 06 mmol ) of 4 - isobutylthiophene - 2 - ylsulfonamide and 158 μl ( 1 . 06 mmol ) of 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene in 4 ml thf was added . the reaction vessel was resealed and then stirred and heated at 80 ° c . overnight . the reaction vessel was then cooled , opened and the contents were partitioned between water and etoac . the organic layer was separated washed with 10 % aqueous nahso 4 , brine , dried ( mgso 4 ), filtered and evaporated . the residual oil was purified on a silica gel flash chromatography column eluted first with 500 ml 50 % etoac - hexane followed by 500 ml 25 % acetone / chcl 3 . the product containing fractions were combined , evaporated and rechromatographed on a silica gel flash chromatography column eluted first with 250 ml of chcl 3 / meoh / nh 4 oh ( 95 : 5 : 0 . 5 ), next with 200 ml of chcl 3 / meoh / nh 4 oh ( 92 : 8 : 0 . 5 ), and finally with 200 ml of chcl 3 / meoh / nh 4 oh ( 90 : 10 : 0 . 5 ). evaporation of the purified fractions and drying in vacuo afforded 0 . 047 g ( 15 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 68 ( t , j = 7 . 60 hz , 6h ), 0 . 92 ( d , j = 6 . 40 hz , 6h ), 1 . 20 ( t , j = 7 . 60 hz , 3h ), 1 . 20 - 1 . 40 ( m , 4h ), 1 . 85 ( m , j = 6 . 40 hz , 1h ), 2 . 14 - 2 . 26 ( m , 4h ), 2 . 57 ( s , 3h ), 2 . 60 ( s , 3h ), 2 . 69 ( d , j = 7 . 20 hz , 2h ), 2 . 82 ( q , j = 7 . 60 hz , 2h ), 4 . 81 ( s , 1h ), 5 . 42 ( s , 2h ), 5 . 94 ( s , 2h ), 6 . 70 - 6 . 76 ( m , 4h ), 6 . 77 - 6 . 79 ( m , 1h ), 6 . 87 ( s , 1h ), 7 . 02 ( s , 1h ), 7 . 55 ( d , j = 4 . 00 hz , 1h ). a 15 ml capacity high pressure vessel equipped with a magnetic stir bar was charged with a solution of 0 . 230 g ( 0 . 42 mmol ) of the product of example 13 in 4 . 0 ml of anhydrous thf and 0 . 172 g ( 1 . 06 mmol ) of 1 , 1 &# 39 ;- carbonyldiimidazole was added . the vessel was sealed and the contents were stirred and heated at 80 ° c . for 4 hours . the reaction was then cooled to room temperature , opened and a solution of 0 . 130 g ( 1 . 06 mmol ) of isopropylsulfonamide and 158 μl ( 1 . 06 mmol ) of 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene in 4 ml thf was added . the reaction vessel was resealed and then stirred and heated at 80 ° c . overnight . the reaction vessel was then cooled , opened and the contents were partitioned between water and etoac . the organic layer was separated washed with 10 % aqueous nahso 4 , brine , dried ( mgso 4 ), filtered and evaporated . the residual oil was purified on a silica gel flash chromatography column eluted first with 250 ml of chcl 3 / meoh / nh 4 oh ( 95 : 5 : 0 . 5 ), next with 200 ml of chcl 3 / meoh / nh 4 oh ( 92 : 8 : 0 . 5 ), and finally with 200 ml of chcl 3 / meoh / nh 4 oh ( 90 : 10 : 0 . 5 ). evaporation of the purified fractions and drying in vacuo afforded 0 . 074 g ( 27 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 76 ( t , j = 7 . 60 hz , 6h ), 1 . 16 - 1 . 45 ( m , 13 h ), 2 . 25 - 2 . 38 ( m , 4h ), 2 . 57 ( s , 3h ), 2 . 60 ( s , 3h ), 2 . 82 ( q , j = 7 . 60 hz , 2h ), 3 . 61 ( s , j = 7 . 40 hz , 1h ), 4 . 87 ( s , 1h ), 5 . 43 ( s , 2h ), 5 . 94 ( s , 2h ), 6 . 75 ( d , j = 8 . 00 hz , 1h ), 6 . 76 ( s , 2h ), 6 . 85 ( dd , j = 1 . 60 , 8 . 00 hz , 1h ), 7 . 01 ( s , 1h ), 7 . 03 ( d , j = l . 60 hz , 1h ). a 15 ml capacity high pressure vessel equipped with a magnetic stir bar was charged with a solution of 0 . 200 g ( 0 . 37 mmol ) of the product of example 13 in 1 . 0 ml of anhydrous dmf and 0 . 172 g ( 1 . 06 mmol ) of 1 , 1 &# 39 ;- carbonyldiimidazole was added . the vessel was sealed and the contents were stirred and heated at 80 ° c . for 1 hour . the reaction was then cooled to room temperature , opened and 0 . 063 g ( 0 . 74 mmol ) of 5 - aminotetrazole and 110 μl ( 0 . 74 mmol ) of 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - en was added . the reaction vessel was resealed and then stirred and heated at 80 ° c . for 3 hours . the reaction vessel was then cooled , opened and the contents were partitioned between water and etoac . the organic layer was separated washed with 10 % aqueous nahso 4 , brine , dried ( mgso 4 ), filtered and evaporated . the residual oil was purified on a silica gel flash chromatography column eluted first with 300 ml of 8 % isopropanol / ch2cl2 , followed by 300 ml of chcl 3 - meoh - nh 4 oh ( 80 : 15 : 1 ). the product containing fractions were evaporated and dried in vacuo to afford 0 . 043 g of the title compound contaminated with some remaining starting material . to a solution of 0 . 043 g ( 0 . 07 mmol ) of the product of step a dissolved in 1 ml methylene chloride was added 0 . 020 g ( 0 . 07 mmol ) of triphenylmethyl chloride , 20 μl ( 0 . 14 mmol ) of triethylamine , and 0 . 5 mg of 4 - dimethylaminopyridine . the reaction mixture was stirred at room temperature for 4 hours , then evaporated in vacuo . the residue was purified on a silica gel flash chromatography column eluted with 50 % etoac - hexane , and the fractions containing a new less - polar product were separated , evaporated and dried in vacuo to afford 0 . 015 g of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): consistent with structure . to a stirred solution of 0 . 015 g ( 0 . 02 mmol ) of the product of step b dissolved in 0 . 2 ml ethanol was added 0 . 1 ml of 1n hydrochloric acid and the reaction mixture was stirred at room temperature for 2 hours . the reaction mixture was neutralized with 0 . 1 ml of 1n sodium hydroxide to ph = 5 , then concentrated in vacuo . the residue was purified on a silica gel flash chromatography column eluted with chcl 3 - meoh - nh 4 oh ( 80 : 15 : 1 ), the purified fractions were combined , evaporated , and dried in vacuo to afford 7 mg of the title compound free of the corresponding carboxylic acid . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 70 ( t , j = 7 . 60 hz , 6h ), 1 . 21 ( t , j = 7 . 60 hz , 3h ), 1 . 28 - 1 . 45 ( m , 4h ), 2 . 28 - 2 . 34 ( m , 4h ), 2 . 57 ( s , 3h ), 2 . 60 ( s , 3h ), 2 . 82 ( q , j = 7 . 60 hz , 2h ), 5 . 14 ( s , 1h ), 5 . 45 ( s , 2h ), 5 . 94 - 5 . 96 ( m , 2h ), 6 . 78 ( d , j = 8 . 00 hz , 1h ), 6 . 80 ( s , 2h ), 6 . 90 ( dd , j = 1 . 60 , 8 . 00 hz , 1h ), 7 . 02 ( s , 1h ), 7 . 05 ( d , j = 1 . 60 hz , 1h ). to a solution of 0 . 120 g ( 0 . 62 mmol ) of 3 , 5 - dichloro - 4 - hydroxybenzyl alcohol in 1 . 5 ml dmf was added 0 . 223 g ( 0 . 68 mmol ) of cesium carbonate and the reaction was magnetically stirred at room temperature for 15 minutes . a solution of 0 . 196 g ( 0 . 68 mmol ) of ethyl α - bromo - 3 , 4 - methylenedioxyphenylacetate in 0 . 5 ml dmf was added and the reaction was stirred an additional 30 minutes at room temperature . the reaction mixture was partitioned between etoac and 5 % aqueous citric acid , extracted , dried ( mgso 4 ), filtered and evaporated . the residue was purified on a silica gel flash chromatography column eluted with 30 % etoac - hexane , and evaporation of the purified fractions afforded 0 . 214 g ( 86 %) of the title compound . 1 h nmr ( 200 mhz , cdcl 3 , ppm ): δ 1 . 25 ( t , j = 7 . 20 hz , 3h ), 4 . 15 - 4 . 31 ( m , 2h ), 4 . 61 ( s , 2h ), 5 . 68 ( s , 1h ), 5 . 98 ( s , 2h ), 6 . 75 ( d , j = 8 . 00 hz , 1h ), 6 . 93 ( dd , j = 1 . 60 , 8 . 00 hz , 1h ), 7 . 09 ( d , j = 1 . 60 hz , 1h ), 7 . 26 ( s , 2h ). to a magnetically stirred solution of 0 . 206 g ( 0 . 52 mmol ) of the product of step a dissolved in 2 ml methylene chloride was added 0 . 162 g ( 0 . 62 mmol ) of triphenylphosphine followed by 0 . 205 g ( 0 . 62 mmol ) of carbon tetrabromide at 0 ° c . the reaction mixture was held at 0 ° c . for 10 minutes , then allowed to warm to room temperature and stirred for 2 . 5 hours . the reaction mixture was then concentrated in vacuo and the residue was applied to a silica gel flash chromatography column and eluted with 15 % etoac - hexane . the purified fractions were combined , evaporated and dried in vacuo to afford 0 . 220 g ( 92 %) yield of the title compound . 1 h nmr ( 200 mhz , cdcl 3 , ppm ): δ 1 . 24 ( t , j = 7 . 20 hz , 3h ), 4 . 15 - 4 . 32 ( m , 2h ), 4 . 33 ( s , 2h ), 5 . 70 ( s , 1h ), 5 . 97 ( s , 2h ), 6 . 76 ( d , j = 8 . 00 hz , 1h ), 6 . 94 ( dd , j = 1 . 60 , 8 . 00 hz , 1h ), 7 . 10 ( d , j = 1 . 60 hz , 1h ), 7 . 28 ( s , 2h ). to a solution of 0 . 034 g ( 0 . 20 mmol ) of 5 , 7 - dimethyl - 2 - ethylimidazo [ 4 , 5 - b ] pyridine in 0 . 5 ml anhydrous dmf was added 8 . 6 mg ( 0 . 22 mmol ) of a 60 % oil dispersion of sodium hydride and the reaction mixture was stirred under a nitrogen atmosphere at room temperature for 30 minutes . a solution of 0 . 100 g ( 0 . 22 mmol ) of the product of step b in 0 . 9 ml of dmf was added and the reaction was stirred an additional 1 . 5 hour at room temperature . the reaction mixture was partitioned between etoac and 5 % aqueous nh 4 cl , separated , dried ( mgso 4 ), filtered and evaporated . the residue was purified on a silica gel flash chromatography column eluted with 50 % etoac - hexane . evaporation of the purified fractions and drying in vacuo afforded 0 . 081 g ( 74 %) of the title compound . 1 h nmr ( 200 mhz , cdcl 3 , ppm ): δ 1 . 22 ( t , j = 7 . 60 hz , 3h ), 1 . 29 ( t , j = 7 . 40 hz , 3h ), 2 . 59 ( s , 3h ), 2 . 64 ( s , 3h ), 2 . 76 ( q , j = 7 . 60 hz , 2h ), 4 . 12 - 4 . 31 ( m , 2h ), 5 . 33 ( s , 2h ), 5 . 68 ( s , 1h ), 5 . 97 ( s , 2h ), 6 . 72 ( d , j = 8 . 00 hz , 1h ), 6 . 90 ( dd , j = 1 . 60 , 8 . 00 hz , 1h ), 6 . 92 ( s , 1h ), 7 . 05 ( s , 2h ), 7 . 07 ( d , j = 1 . 60 hz , 1h ). to a magnetically stirred solution of 0 . 076 g ( 0 . 14 mmol ) of the product of step c in 1 . 0 ml methanol was added 0 . 1 ml of a 5 . 0n solution of sodium hydroxide and the reaction was stirred at room temperature overnight . the reaction mixture was adjusted to ph = 6 with 1 . 0n hydrochloric acid and then concentrated in vacuo . the residue was then purified on a silica gel flash chromatography column eluted with chcl 3 - meoh -- nh 4 oh ( 80 : 15 : 1 ). evaporation of the purified fractions and drying in vacuo afforded 0 . 059 g ( 82 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 1 . 22 ( t , j = 7 . 60 hz , 3h ), 2 . 57 ( s , 3h ), 2 . 60 ( s , 3h ), 2 . 83 ( q , j = 7 . 60 hz , 2h ), 5 . 44 ( s , 2h ), 5 . 67 ( s , 1h ), 5 . 92 - 5 . 93 ( m , 2h ), 6 . 70 ( d , j = 8 . 00 hz , 1h ), 6 . 84 ( dd , j = 1 . 60 , 8 . 00 hz , 1h ), 6 . 96 ( d , j = 1 . 60 hz , 1h ), 7 . 04 ( s , 1h ), 7 . 07 ( s , 2h ). to a solution of 0 . 257 g ( 0 . 80 mmol ) of 5 , 7 - dimethyl - 2 - ethyl - 3 -[ 4 - hydroxy - 3 - propylphenyl ]- methyl - 3h - imidazo [ 4 , 5 - b ] pyridine in 4 ml of anhydrous dmf was added 0 . 309 g ( 0 . 88 mmol ) of cesium carbonate and the mixture was stirred at room temperature for 15 minutes . ethyl α - bromo - 3 , 4 - methylenedioxyphenylacetate ( 0 . 251 g ; 0 . 88 mmol ) was added and the reaction mixture was then stirred an additional 14 hours at room temperature . the reaction mixture was then partitioned between ethyl acetate and 10 % aqueous citric acid and extracted . the organic layer was washed with saturated nahco 3 , brine , dried ( mgso 4 ), filtered and evaporated . the residue was purified on a silica gel flash chromatography column eluted with 50 % etoac - hexane . evaporation of the purified fractions and drying in vacuo afforded 0 . 346 g ( 82 %) of the title compound . 1 h nmr ( 400 mhz , cdcl 3 , ppm ): δ 0 . 90 ( t , j = 7 . 60 hz , 3h ), 1 . 14 ( t , j = 7 . 20 hz , 3h ), 1 . 27 ( t , j = 7 . 60 hz , 3 ), 1 . 53 - 1 . 68 ( m , 2h ), 2 . 56 - 2 . 67 ( m , 2h ), 2 . 58 ( s , 3h ), 2 . 63 ( s , 3h ), 2 . 78 - 2 . 81 ( m , 2h ), 4 . 08 - 4 . 81 ( m , 2h ), 5 . 35 ( s , 2h ), 5 . 44 ( s , 1h ), 5 . 95 ( br s , 2h ), 6 . 57 ( d , j = 8 . 40 hz , 1h ), 6 . 77 - 6 . 80 ( m , 2h ), 6 . 89 ( s , 1h ), 6 . 96 - 6 . 99 ( m , 2h ), 7 . 02 ( d , j = 2 . 00 hz , 1h ). to a solution of 0 . 340 g ( 0 . 64 mmol ) of the product of step a dissolved in 2 ml methanol was added 130 μl of a 5 . 0n solution of sodium hydroxide and the reaction mixture was stirred at room temperature for 2 hours . at this point the reaction mixture was adjusted to ph = 6 with dropwise addition of 6 . 0n hydrochloric acid and the reaction mixture was concentrated in vacuo . the residue was applied to a silica gel flash chromatography column and eluted with chcl 3 - meoh -- nh 4 oh ( 80 : 15 : 1 ). the purified fractions were combined , evaporated and dried in vacuo to afford 0 . 278 g ( 86 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 84 ( t , j = 7 . 60 hz , 3 ), 1 . 21 ( t , j = 7 . 60 hz , 3h ), 1 . 51 - 158 ( m , 2h ), 2 . 51 - 2 . 58 ( m , 1h ), 2 . 57 ( s , 3h ), 2 . 59 ( s , 3h ), 2 . 64 - 2 . 74 ( m , 1h ), 2 . 83 ( q , j = 7 . 60 hz , 2h ), 5 . 32 ( s , 1h ), 5 . 43 ( s , 2h ), 5 . 92 ( br s , 2h ), 6 . 76 ( d , j = 8 . 00 hz , 2h ), 6 . 85 ( dd , j = 2 . 40 , 8 . 40 hz , 1h ), 6 . 93 ( d , j = 2 . 40 hz , 1h ), 7 . 00 ( s , 1h ), 7 . 04 ( dd , j = 1 . 60 , 7 . 60 hz , 1h ), 7 . 08 ( d , j = 1 . 60 hz , 1h ). to a solution of 0 . 070 g ( 0 . 14 mmol ) of the product of step b in example 30 dissolved in 1ml of anhydrous thf was added 0 . 034 g ( 0 . 21 mmol ) of 1 , 1 &# 39 ;- carbonyldiimidazole and the mixture was refluxed under a nitrogen atmosphere for 20 minutes . the reaction was cooled to room temperature and opened and 31 μl of 1 , 8 - diazabicyclo [ 5 . 4 . 0 ] undec - 7 - ene ( dbu ) and 0 . 042 g ( 0 . 21 mmol ) of 4 - iso - propylbenzenesulfonamide were added . the flask was resealed and the contents were stirred and heated at reflux for an additional 1 . 5 hours . the reaction mixture was then cooled and evaporated in vacuo . the residue was partitioned between etoac and 10 % aqueous citric acid and the organic layer which separated was washed with saturated nahco 3 , brine , dried ( mgso 4 ), filtered and evaporated . the residue was purified on a silica gel flash chromatography column eluted with chcl 3 - meoh -- nh 4 oh ( 92 : 8 : 0 . 5 ). the purified fractions were combined , evaporated , and dried in vacuo to afford 0 . 040 g ( 42 %) of the title compound . 1 h nmr ( 400 mhz , cd 3 od , ppm ): δ 0 . 79 ( t , j = 7 . 60 hz , 3h ), 1 . 17 ( d , j = 7 . 20 hz , 6h ), 1 . 21 ( t , j = 7 . 60 hz , 3h ), 1 . 45 - 1 . 53 ( m , 2h ), 2 . 41 - 2 . 49 ( m , 1h ), 2 . 53 - 2 . 64 ( m , 1h ), 2 . 59 ( s , 3h ), 2 . 61 ( s , 3h ), 2 . 82 ( q , j = 7 . 60 hz , 2h ), 5 . 23 ( s , 1h ), 5 . 41 ( s , 2h ), 5 . 91 ( br s , 2h ), 6 . 57 ( d , j = 8 . 40 hz , 1h ), 6 . 72 - 6 . 76 ( m , 2h ), 6 . 91 ( d , j = 2 . 40 hz , 1h ), 6 . 59 - 6 . 97 ( m , 2h ), 7 . 02 ( s , 1h ), 7 . 15 ( d , j = 8 . 20 hz , 2h ), 7 . 63 ( d , j = 8 . 20 hz , 2h ).
2
[ 0027 ] fig1 is a perspective view of the interbody spinal fusion device 10 . interbody spinal fusion device 10 suitable for implantation in the intervertebral space between two adjacent vertebral bodies ( not shown ), has a pair of bone - engaging plate members , specifically top plate member 12 and bottom plate member 14 . in use , top plate member 12 and bottom plate member 14 are arranged above and below each other , respectively , in spaced apart relationship . the spaced apart relationship is created and maintained in a manner that will be described more completely hereinbelow . bottom plate member 14 has a bottom support plate 18 that is adapted to rest on the endplate of the lower vertebra ( not shown ). bottom support plate 18 has an outer surface 19 that contacts the lower vertebra and an inner surface 20 . as shown in this figure , bottom support plate 18 is generally flat , but may be adapted to follow the contour of the vertebra on which it rests . since the support plates merely contacts the endplates of the vertebrae , and can be bent to the contour of the vertebrae , rather than engage by means of protuberances or engaging teeth , there is less damage to the bone which prevents subsidence . in this embodiment , bottom support plate 18 has three longitudinal members 22 , 23 , and 24 that terminate in a generally curved section 21 at posterior end 17 . longitudinal members 22 , 23 , and 24 define two large openings 25 and 26 . at anterior end 16 , longitudinal members 22 , 23 , and 24 terminate with a generally curved section that is bent substantially orthogonal to the horizontal plane of bottom support plate 18 in the direction of communication of the template and the vertebral body . the generally curved section is herein referred to as bottom template 27 . bottom template 27 has an anterior front face surface 28 at anterior side 16 of the device and an opposing posterior surface 29 ( designated , but not specifically shown in this figure ). posterior surface 29 is adapted to contact and rest flush against the curved anterior cortical surface of the lower vertebra ( not shown ). in this embodiment , bottom template 27 is provided with three pre - drilled holes 31 , 32 and 33 which may , in some embodiments , be internally threaded . fasteners , such as threaded orthopedic bone screws ( not shown ) are inserted through the pre - drilled holes and into the hard cortical bone of the anterior surface of the vertebra . in preferred embodiments , the pre - drilled holes may be configured to adjust the angle of placement of the bone screws so that the bone screws can be set to work against each other in order to stabilize the device . while a total of six bone screws are used in the specific embodiment described herein , it is to be understood that the bone - engaging plate members can be attached to vertebrae using a greater or lesser number of fasteners depending on different variables , including , but certainly not limited to , size or bone density of the vertebrae , spatial positioning of the vertebrae , and the level of attachment required by the physician . orthopedic bone screws of the type suggested for use in the practice of the invention are well - known and available from a variety of suppliers known to those of ordinary skill in the art . however , it is to be understood , that other known or new and improved forms of orthopedic screws and other types of improved orthopedic fasteners and fastening systems are within the contemplated scope of the invention . top plate member 12 is generally equivalent in structure to bottom plate member 14 , and in some embodiments , may be identical in structure to bottom plate member . however , in use , the top plate member 12 is flipped so that top template 44 will be bent substantially orthogonal to the horizontal plane of top support plate 36 in the direction of communication of the template and the vertebral body . referring to fig1 top plate member 12 has a top support plate 36 that is adapted to rest on the endplate of the upper vertebra ( not shown ). top support plate 36 has an outer surface 37 that contacts the upper vertebra and an inner surface 38 ( designated , but not specifically shown in this figure ). top support plate 36 has three longitudinal members 39 , 40 , and 41 that terminate in a generally curved section 42 at posterior end 17 . longitudinal members 39 , 40 and 41 define two large openings 43 an 45 . at anterior end 16 , longitudinal members 39 , 40 and 41 terminate with top template 44 . top template 44 has an anterior front face surface 46 at anterior side 16 of the device and an opposing posterior surface 47 ( designated , but not specifically shown ). posterior surface 47 is adapted to contact and rest flush against the curved anterior cortical surface of the upper vertebra ( not shown ). top template 44 is also provided with three pre - drilled holes 48 , 49 , 50 . bottom template 27 has tabs , illustratively adjacent tabs 34 and 35 , that are integrally formed , and coplanar with , the anterior front face of bottom template 27 , but extend in a direction opposite to the direction that the template is bent . for bottom template 27 , the tabs extend upward from its inner surface 20 . tabs 34 and 35 form an initial guide , or slot 53 , that precludes transverse dislocation of support strut 55 when inserted into the interbody spinal fusion device . in this specific embodiment , the tabs are spaced apart to define an opening having a width approximately equal to the width of central longitudinal member 23 . top template 44 also has tabs , illustratively tabs 51 and 52 , that define a slot 54 . however , in the case of top template 44 , the tabs extend in a direction downward from its inner surface 38 . when top plate member 12 and bottom plate member 14 are mounted to adjacent vertebrae , as will be described hereinbelow , tabs 34 and 35 in combination with tabs 51 and 52 , are aligned to form generally an aperture 56 into which wedge - shaped support strut 55 is inserted . in addition to the foregoing , in some embodiments additional tabs ( shown , but not specifically designated , in fig1 ) may be provided . in these embodiments , the tabs can operate to define additional slots / apertures for the insertion of more than one support strut . the tabs , which extend in an opposing direction to the main body of the template , and in front of the channels into which one graft material will be placed , can also operate to stabilize and anchor the device . the interbody spinal fusion device 10 has a height that is defined by the vertical distance between the outer surface 39 of top support plate 36 and the outer surface 19 of bottom support plate 18 . the height is adjustable by selection and insertion of a strut of the appropriate size into aperture 56 , and preferably , varies along the interbody spinal fusion device 10 between anterior end 16 and posterior end 17 so as to maintain the natural lordosis of the spine . referring to exemplary strut 55 , shown in fig1 prior to insertion , support strut 55 comprises a solid wedge - shaped object of a predetermined maximum height at anterior end 81 and minimum height at posterior end 83 . the angle of the wedge - shaped strut is determined by the height of posterior end 83 relative to the height of anterior end 81 . in a kit embodiment of the invention , a selection of support struts of varying height and / or angle would be provided along with the top and bottom plate members in a surgical kit so that the practitioner can select the appropriate strut for the individual patient . the angle of support strut 55 is chosen to maintain the lordosis of the vertebral column . the height of support strut 55 is chosen to approximate the height of the disc material that previously occupied the intervertebral spacing . it is anticipated that as few as two or three support struts will be all that is required to practice the invention . of course , this number is illustrative and is in no way intended to be limiting . this is a significant reduction in the amount of parts required for a surgical kit for an interbody fusion operation . in use , support strut 55 is inserted in aperture 56 between longitudinal members 23 and 40 , spanning the intervertebral region and resting firmly against the upper and lower vertebrae . in some embodiments , top plate 36 has a protrusion 57 to engage support strut 55 to prevent over - insertion . of course , either one or both the bottom plate 18 or top plate 36 can be provided with a protrusion for this purpose . [ 0041 ] fig2 is a plan view of a portion of the spinal column with interbody fusion device 10 mounted between two vertebrae . elements of structure that are identical to those in fig1 are similarly designated in fig2 . interbody spinal fusion device 10 is placed in intervertebral region 60 between a first vertebra 61 located below intervertebral region 60 and a second vertebra 62 located above intervertebral region 60 . bottom plate member 14 is attached to vertebra 61 by bone screws 63 , 64 , and 65 that are inserted through pre - drilled holes ( see fig1 ) in bottom template 27 . top plate member 12 is attached to vertebra 62 by bones screws 63 ′, 64 ′, and 65 ′ through top template 44 . support strut 55 is shown inserted in aperture 56 . channels 66 and 67 are formed on either side of support strut 55 for packing bone graft material 72 to facilitate fusion of vertebra 61 with vertebra 62 . referring to fig1 openings 25 and 26 in bottom support plate 18 ( not shown in this figure ) and openings 43 and 45 in top support plate 36 ( not shown in this figure ) underlie or overlie , respectively , channels 66 and 67 so that there is a large area of contact of bone graft material with the vertebrae . in some embodiments , an end cap ( not shown in this figure ) is placed over the top and bottom templates to lock the support strut in place . advantageously , the end cap will assist in retaining bone graft material in the channels . preferably , the outermost portions of the lateral and posterior annulus 71 remain intact and serve to confine the bone graft material in lateral and posterior directions . of course , a retaining plate ( not shown ) for the posterior side of spinal fusion device 10 can be devised , by persons of skill in the art , for retaining bone graft material , if required . the components of the interbody spinal fusion device of the present invention are constructed of biocompatible materials , and presently titanium or titanium alloys are preferred . however , it is to be understood that other materials presently known , and to be developed , that have the appropriate strength and biocompatibility , such as ceramics , metals , and carbon composites , are specifically contemplated for use in connection with the invention . in practice , the interbody spinal fusion device of the present invention is installed in accordance with techniques known to those of ordinary skill in the art . illustratively , the technique utilizes an anterior approach to the spine and is particularly suited to fusion of lumbar or thoracic vertebrae . the annulus of the affected disc is sharply incised anteriorly to allow a complete discectomy to be performed . preferably , the entire disc is removed except for the outermost portions of the lateral and posterior annulus . the endplates of the vertebrae are carefully scraped clean of all disc material . the top plate member 12 and the bottom plate member 14 are respectively placed into the intervertebral space , as shown in fig3 which is a cross - sectional side view of spinal fusion device 10 taken along line x - x in fig2 as installed between neighboring vertebrae 61 and 62 . elements of structure that are identical to those in fig1 or fig2 are similarly designated in fig3 . referring to fig3 by way of illustration , top plate member 12 is mounted into intervertebral region 60 by placing template 44 on the anterior surface 73 of the hard cortical endplate of the upper vertebra 62 . this results in the insertion of support plate 36 into intervertebral region so that its outer surface 37 contacts the cleaned , softer center of cancellous bone 75 where the disc has been removed ( designated , but not specifically shown ). template 44 is shown attached to the hard cortical bone by surgical screw 64 ′. bottom plate member 14 is mounted into intervertebral region 60 and attached to vertebra 61 in a similar manner by fastening bottom template 27 on the anterior surface 74 of the hard cortical endplate of the lower vertebra 61 . the height and width of the disc space are measured , and a support strut 55 having the correct height and / or angle to restore and maintain the appropriate intervertebral spacing and normal spinal lordosis is selected by the surgeon . support strut 55 is then inserted into aperture 56 created by center slots 54 and 53 ( see fig1 ) and will rest between central longitudinal members 23 and 40 . protuberance 57 on central longitudinal member 40 will act as a stop to prevent over - insertion of support strut 55 . once the desired height and angle is achieved , bone graft material ( not shown in this figure ) is packed into hollow channels ( shown as channels 66 and 67 in fig2 ) on either side of support strut 55 . the remaining outermost portions of the lateral and posterior annulus ( not shown in this figure ) may serve to retain the packed bone graft material in place . in this particular embodiment , removable end plate 70 , which may be fastened to template members 44 and 27 by force - fit or fasteners , locks spinal fusion device 10 in place and retains bone graft material in the anterior direction . known techniques , such as x - ray imaging or fluoroscopy , can be used to confirm correct placement of the device and selection of size / angle of the support strut . however , in the practice of the invention , the radius of curvature of the anterior vertebral body would dictate the placement of the template . the depth of the support plate , along with the curvature as it relates to the anterior vertebral body , creates a device that is self - directing as to location . there is no chance of over - penetration of the device inasmuch as depth is limited by the anterior aspect of the vertebral approach . this prevents errors in placement of the type that routinely occur with the known cylindrical threaded fusion devices , such as placement which is too far lateral and , theoretically , can go beyond the cortical margin into the area of the foramen . it also removes the risk of over - drilling that can happen when a cylindrical threaded fusion device is started too far laterally on the vertebral body . moreover , it prevents the all - too - frequent complications resulting when the known device does not obtain equal purchase in each endplate . the interbody spinal fusion device of the present invention is , mechanically , a more stable construct than known prior art devices since there is a greater amount of surface area engaged against the anterior aspect of the vertebral body as well as impacting the vertebral body endplate . this allows for more aggressive removal of cartilaginous endplate and bone from the affected area . moreover , the interbody spinal fusion device of the present invention provides wide channels into which bone graft material may be packed . in addition , there large openings in the support plate provides for a large area of contact between the bone graft material and the prepared endplates of the vertebrae . although the invention has been described in terms of specific embodiments and applications , persons skilled in the art can , in light of this teaching , generate additional embodiments without exceeding the scope or departing from the spirit of the invention described herein . accordingly , it is to be understood that the drawing and description in this disclosure are proffered to facilitate comprehension of the invention , and should not be construed to limit the scope thereof .
0
fig1 is a perspective view of a first ruler member 100 which measures the length l of the wound 800 , as shown in fig4 . the first ruler member 100 is a straight strip having measurement indicia 110 . the marking indicia 110 are markings along a top surface 120 of the first ruler member 100 . the indicia 110 markings are marked at equal intervals along the left or right top edge of the top surface 120 of the first ruler member 100 . a bottom end 125 or tip of the first ruler member 100 is marked with a “ 0 ” increment marking . a top end 126 of the first ruler member 100 is marked with the largest increment , the length of the measuring area of the first ruler member 100 . a direction identifier 130 extends from the top end 126 with a marking or symbol 131 that identifies a direction the first ruler member 100 should be positioned on an object or wound 800 to be measured . the direction identifier may also feature a design or symbol to identify the brand owner or hospital or other identifier which will identify the maker or owner of the tool . the identifier is preferably circular , however , alternate shapes may be used to display the identifier or marking symbol . when the first ruler member 100 is positioned over a wound , 800 , it is used to measure the length l of the wound 800 . the wound length l is a distance from an end 125 of the first ruler member 100 to a first end of a greatest opening of the wound . the length measurement l is taken when the first ruler member is positioned over the wound or object to be measured . fig2 is a perspective member of a second ruler member 200 which measures the width w of the wound 800 . the second ruler member 200 is a straight strip having measurement indicia 110 . the marking indicia 110 are markings along a top surface 220 of the second ruler member 200 . the indicia 110 markings are marked at equal intervals along the left or right top edge of the top surface 220 of the second ruler member 200 . a bottom end 225 or tip of the second ruler member 200 is marked with a “ 0 ” increment marking . a top end 226 of the second ruler member 200 is marked with the largest increment , the length of the measuring area of the second ruler member 200 . a handle 230 extends from the top end 226 of the second ruler member 200 . the handle 230 allows the user of the second ruler member 200 to manipulate the second ruler member 200 to take measurements . the handle 230 is rectangular in shape , however , an alternate shape may be used . the handle 230 also features an area which receives the wound owner &# 39 ; s information such as name , date , etc . a label may be placed on the handle with information or it may be written directly on the handle 230 . measurement indicia are not marked on the direction indicator 130 or the handle 230 . when the second ruler member 200 is positioned over a wound or object 800 , it is used to measure the width w of the wound 800 . wound width w is a distance from an end of the connected second ruler member 225 to a second end of the greatest opening of the wound . the tip 125 of the first ruler member 100 or the tip 225 of the second ruler member measures the depth of the object or wound to be measured . the tip 125 of the first ruler member 100 or the tip 225 of the second ruler member 200 is inserted inside of the wound or object its furthest distance inside of the wound or object to a surface of the wound to determine the wound depth . the first and second ruler members 100 , 200 are preferably light grey or transparent in color . when placed over the wound 800 or object , the light color or transparency affords the measurements to easily and accurately be taken and seen as well as it affords the measurer the ability to see the wound 800 or object to be measured underneath the rulers , 100 , 200 . additional light colors may be used so long as they do not obstruct the view of the measurer or conceal the object to be measured . the markings 110 are preferably in a black or other color that can easily be seen so that an accurate measurement may be identified . markings 110 shown in fig1 and 2 are in centimeters . ruler members 100 , 200 provide measurements up to 15 cm in width and 15 centimeters in length . the markings may be shown in alternate metric units and the measurements may be increased or decreased to measure larger or shorter objects . the ruler members 100 , 200 are flexible so they can be placed on curved body surfaces as well as flat body surfaces to accurately measure . furthermore , the ruler members 100 , 200 can easily be maneuvered over irregular sized objects to be measured . the rulers are sterilized for a one - time use . it is recommended for sanitary purposes that the rulers not be reused to avoid infections , for example . open packages and unused ruler members should be discarded . fig3 a is a top side 301 of a perspective view of a connecting device 300 which secures and connects the first ruler member 100 and second ruler member 200 . the connection device 300 allows perpendicular movement of the first ruler member 100 and second ruler members 200 so that the rulers move in a sliding motion independent of each other . the connecting device 300 top side 301 features a first connector 302 . the first connector 302 features parallel first connector flanges 303 , 304 . the flanges 303 , 304 form a first channel 305 sized to receive the first ruler member 100 . the flanges &# 39 ; 303 , 304 walls contact the left and right outermost edges of the first ruler members so that the first ruler member remains secure in the connector 302 . the first ruler member 100 can movely back and forth or in and out freely through the channel . the connecting device is also a light grey or transparent color so that the markings on the ruler members remain visible . the channel has a bottom that receives and contacts a bottom side of the ruler member 100 . however , the area between the flanges 303 , 304 remains open so the markings can easily be identified and measurements can be recorded . fig3 b is a bottom side 310 of a perspective view of the connecting device 300 which secures and connects the first ruler member 100 and second ruler member 200 . the bottom side 310 of the connecting device 300 is a second connector 311 having second connector parallel flanges 312 , 313 that form a second channel 315 sized to receive the second ruler member 200 . the flanges 312 , 313 walls contacts the left and right outermost edges of the second ruler members so that the second ruler member remains secure in the connector 310 . the second ruler member 200 can movely back and forth or in and out freely through the channel 315 . the channel 315 has a bottom that receives and contacts a bottom side of the ruler member 200 . however , the area between the flanges 312 , 313 remains open so the markings can easily be identified and measurements can be recorded . the first connector 301 and second connector 310 are attached so that the first connector &# 39 ; s bottom side is secured to the second connector &# 39 ; s bottom side . however , the first connector 301 is secured so that its channel 305 receives the first ruler member in a north to south direction so that the first ruler member 100 moves through the channel 305 in an up and down direction . the second connector 310 is secured to the first connector so that its channel 315 receives the second ruler member in a east to west direction so that the second ruler member 200 moves through the channel 315 in a left to right direction . the connecting device affords the first ruler member and second ruler member the ability to move independently of each other so that when the connecting device secures the first and second ruler members , there is always a perpendicular angle between the first and second rulers . fig4 is a perspective view of the device illustrating the connected first ruler 100 member and second ruler member 200 connected by the connecting device 300 measuring a wound 800 on a body part such as a leg , for example . the connected ruler members form a measuring tool which may be used to measure the length , width and depth of a wound . the direction identifier 130 on the first ruler member identifies a direction the first ruler member 100 should be positioned on the wound 800 to be measured . the identifier is preferably an arrow , but another symbol may be used to identify which direction the ruler 100 should be positioned . the arrow should point to the wound owner &# 39 ; s head , when the first ruler member 100 is placed over the wound opening . while keeping the arrow pointed towards the wound owner &# 39 ; s head , the first ruler member 100 is adjusted so it measures the greatest expanse or opening of the wound from that direction . this is the wound length l . without moving the first ruler member 100 , the second ruler member 200 is slide through the connecting device 300 so it measures the wound expanse or opening at the point where the greatest expanse or opening can be recorded . this is the wound width w . when connected , the first and second members , 100 , 200 move perpendicular to each other . the wound length l and wound width w are recorded . also , a time - marked camera may be used to take pictures of the placement and thus the measurements of the wound . using the first ruler member tip 125 or second ruler member tip 225 where the indicator starts with “ 0 ” cm , the width depth and undermining is recorded as described above . the use of the measuring tool is contraindicated for use in measuring burns , rash or other abrasions not resulting in a puncture , cut , scrape or tear . also , the tool is contraindicated for use in measuring surgical incisions other than those experiencing dehiscence . the invention has been described in detail with particular reference to certain preferred embodiments thereof , but it will be understood that variations and modifications can be effected within the spirit and scope of the invention .
0
the present invention will now be described in detail with reference to the drawings . in the drawings , a relative dimension or size of each part or portion may be shown as somewhat different one to clarify an explanation of the present invention and the same parts or portions have the same reference numerals . reference is made to fig1 fig2 fig3 fig4 and fig5 showing a first preferred embodiment of the present invention . fig1 shows an enlarged perspective view of a cleaning head 100 in a cleaning tool 120 . fig2 shows a cross - sectional view of a cleaning apparatus . fig3 shows a light transmission passageway in cross - section of the cleaning tool 120 as shown in fig2 . fig4 shows a partially omitted enlarged cross - sectional view of the cleaning tool 120 and a light transmission passageway . and fig5 shows an enlarged cross - sectional view of a piece of brush among a group of brushes 10 in the cleaning head 100 . in fig1 fig2 fig3 and fig4 the cleaning apparatus ( or cleaning device ) 120 is roughly comprised of a cleaning tool 120 , a light source 200 and an optical fiber or an optical fiber cable 300 . the cleaning tool 120 is further comprised of a cleaning head 100 and a handle 310 with rod - like shape extending from the cleaning head 100 . the cleaning head 100 may further be comprised of a group of photocatalyst brushes ( photocatalytic brushes ) 10 and a transparent brush supporter . the group of photocatalyst brushes 10 may have multiple brushes , in which all or several brushes may include a photocatalyst . the transparent brush supporter 20 may fix ends of the photocatalyst brushes 10 and support them . it may be made of transparent material or transparent material embedding many light diffusing elements ( particles ) 22 ( as shown in fig4 ). the handle 310 may be provided with a light inlet 32 ( as shown in fig2 and fig3 ) which may be a hole , etc . in the most distant terminal of the handle 310 from the cleaning head 100 . it may be comprised of a transparent rod 30 with high refractive index and a transparent layer 31 with low refractive index . the transparent rod 30 may be coated or covered with the transparent layer 31 around the transparent rod 30 . since the transparent rod 30 is equivalent to a “ core ” of an optical fiber and the transparent layer 31 is equivalent to a “ sheath ” ( or cladding ) of the optical fiber functionally , the handle 310 is able to transmit most light rays effectively within the rod 30 with high transmission factor from the light inlet 32 to the cleaning head 100 , according to a principle of the optical fiber . alternatively , a light reflective layer such as aluminum or nickel may be used as a substitute for the transparent sheath ( layer ) 31 in order to obtain similar high transmission factor . the brush supporter 20 may be made of transparent material capable of transmitting well ultraviolet rays , such as fused quarts , crystal glass as transparent inorganic materials and acrylic resin , polycarbonate resin , epoxy resin and transparent fluoric resin as transparent organic plastic materials . for the light diffusing elements 22 in order to give the brush supporter 20 light diffusing characteristics , conventional white pigments may be used such particles as titanium oxide , aluminum , calcium carbonate and barium carbonate . a reference numeral 70 indicates an substance to be cleaned ( or a cleaned substance ) such as a floor , a carpet and a wall in a building or a house , and a reference numeral 72 indicates a dirty component , which is contacted or adhered on a surface of the cleaned substance 70 , as shown in fig2 fig3 and fig4 . the light source 200 emits or generates short wavelength rays including ultraviolet ( uv ) rays . for the light source 200 , various vacuum discharge lamps may be preferably used such as a germicidal lamp , a black light to cut visible light , a uv radiated fluorescent lamp , a halogen lamp and a conventional fluorescent lamp . a laser to emit coherent uv laser beam may also be used . the germicidal lamp is a conventional low or high pressure mercury lamp using a uv transmissible glass tube such as transparent fused quarts , which emits uv light rays with short wavelength between the range from 250 nm to 280 nm ( center wavelength ; 253 . 7 nm ) by discharge of mercury . the black light is a kind of fluorescent lamp emitting blue color and uv light rays using a vacuum uv transmissible glass tube with a black filter to cut the uv light rays , or using a vacuum uv transmissible black filter glass tube to cut only the blue color light rays , which emits uv light rays with medium wavelength between the range from 380 nm to 300 nm by discharge of mercury . the uv radiated fluorescent lamp may be used which uses a vacuum transparent glass tube without the black filter instead of the black light , which emits blue color light rays and also uv light rays with medium and long wavelength . the halogen lamp is high - pressure mercury lamp adding metal halide inside the lamp tube , which emits uv light rays with medium and long wavelength . referring again to fig2 a focus lens 40 and a reflector 42 positioned in rear of the focus lens 40 are installed . the light source 200 , the focus lens 40 and the reflector 42 are housed in a light box ( or a lamp house ) 44 . a commercial power is supplied from a power consent 48 to a light control circuit device 46 via an electric cable 47 . the light control circuit device 46 controls a lighting of the light source 200 . an optical fiber 300 may be comprised of a single number of optical fiber with a transparent core and a transparent sheath capable of transmitting uv light rays and a protective covering . instead of the optical fiber , an optical fiber cable 300 may be used , which is comprised of multiple optical fibers capable of transmitting uv light rays and a protecting covering . the optical fiber 300 has a pair of optical fiber connectors 50 and 52 in both terminals . a light connector 50 and another light connector 52 of the optical fiber 300 are connected optically with the light inlet 32 a of the handle 310 and with a light output of the lamp house 44 , respectively . the uv light rays 60 emitting from the light source 200 are collected at the focus lens 40 and are input at the light connector 52 of the optical fiber 300 . the uv light rays 60 incident to the light connector 52 are transmitting in the optical fiber 300 to the light connector 50 and are introduced to the transparent handle 30 via the light inlet 32 . for transmissible materials of short wavelength rays for the optical fiber ( core and cladding ) 300 , the handle 310 and the transparent brush supporter 20 , such transparent inorganic materials may be used as fused quarts ( including more than 99 . 9 weight % of sio 2 ), sapphire , borosilicate glass ( composing sio 2 ; 75 . 3 , b 2 o 3 ; 13 . 8 ; zno ; 1 . 4 , al 2 o 3 ; 4 . 3 , nao ; 5 . 0 weight %), etc . and also for the transmissible materials of the optical fiber , such transparent organic materials may be used as acrylic base resin such as polymethyl methacrylate ( pmma ) ( refractive index ; n ≈ 1 . 49 ), polycarbonate ( pc ) ( n ≈ 1 . 59 ) resin , polyethylene base resin such as polyethylene terephthalate ( petp ) ( n ≈ 1 . 58 ), polystyrene ( ps ) ( n ≈ 1 . 59 ) and fluoride base resin such as polytetra fluoroethylene ( ptfe ), ( n ≈ 1 . 35 ), epoxy resin ( ep ) ( n ≈ 1 . 55 - 1 . 61 ), etc . it is noted that the core of the optical fiber 300 ( or the equivalent members 30 and 20 ) must be selected from material with comparatively high refractive index , while the cladding of the optical fiber 300 ( or the equivalent members 31 ) must be selected from material with comparatively low refractive index . it is a matter of course that the core must be selected from material with high refractive index , while the sheath must be selected from material with low refractive index . the uv transmitting optical fiber or cable 300 has been put into market . such optical fiber capable of transmitting the light rays in ultraviolet region is available from famous cable manufacturers , such as mitsubishi cable industries ltd ., japan . for photocatalyst materials including in the photocatalyst brushes 10 of the cleaning head 100 , photo - activated ( i . e . photocatalytic ) semiconductors may be used such as titanium dioxide ; tio 2 ( photo activation wavelength ; not more than 388 nm ), tungsten dioxide ; wo 2 ( photo activation wavelength ; not more than 388 nm ), zinc oxide ; zno photo activation wavelength ; not more than 388 nm ), zinc sulfide ; zno photo activation wavelength ; not more than 344 nm ) and tin dioxide ; sno 2 photo activation wavelength ; not more than 326 nm ). especially the photo - activated titanium dioxide may be preferably applied for any fields , considering from that an activated power is very high , a life is long , durability is high and a safety or a harmless to a human body is certified , as it has been used for a long time safely for adding in cosmetics and foods . referring again to fig3 and fig4 as the uv transmissible handle 310 is set so that a refractive index n 1 of the uv transmissible rod 30 is higher than a refractive index n 2 of the uv transmissible sheath 31 , the uv light rays 61 and 62 are transmitted effectively to the cleaning head 100 reflecting or refracting repeatedly . the uv light rays 63 are incident light rays in which the light rays 61 and 62 are transmitting to the uv transmissible brush supporter 20 of the cleaning head 100 . as shown in fig4 ( and fig1 & amp ; fig3 ), the cleaning head 100 may have many reflective elements ( or reflective particles ) 22 which are embedded in the uv transmissible brush supporter 20 in order to give uv light diffusing characteristics . therefore , the uv light rays 63 incident to the brush supporter 20 are diffused at the reflective elements 22 to become diffusing ( scattering ) uv light rays 64 and the diffusing uv light rays 84 partially are outgoing outside from a front surface 20 a of the brush supporter 20 . the outgoing uv light rays 64 are incident to a group of brushes including photocatalyst ( photocatalyst brushes ) 10 and also incident to the dirty component 72 . the uv light rays 64 incident to the photocatalyst brushes 10 are forced to activate the photocatalyst component so that the dirty component 72 ( shown in fig2 fig3 & amp ; fig4 ) is oxidized and / or reduced by photocatalyst action , while the uv light rays 64 incident to the dirty component 72 sterilize directly the dirty component 72 by germicidal effect of the uv light rays 64 . a rear surface 20 b and a side surface 20 c of the brush supporter 20 excluding the front surface 20 a may be preferably coated with light transmissible layer with low refractive index or light reflecting layer in order to obtain more amount of uv light output to the photocatalyst brushes 10 . fig5 indicates an enlarged cross - section of a single brush or a fiber 10 a or 10 b of the group of photocatalyst brushes 10 in the cleaning head 100 , according to a preferred embodiment no . 1 . fig5 a indicates one type of the photocatalyst brush or fiber 10 . it may be comprised of a composite fiber having a core 10 a made of conventional artificial resin fiber ( or metal wire ) and a sheath including a photocatalyst 10 b . the sheath is made of conventional artificial resin or rubber , in which many photocatalyst particles are embedded . fig5 b indicates another type of the photocatalyst brush or fiber 10 which may be comprised of a composite fiber having a core 10 c made of a conventional artificial resin or rubber and many photocatalyst particles 10 d embedded in the core 10 c . in more detail , in the case of fig5 a for example , the photocatalyst brush or fiber 10 may be comprised of a conventional artificial plastic fiber 10 a ( such as polyester , acrylic and polyimide i . e . nylon ) or a conventional metal wire 10 a ( such as steel , stainless steel and titanium ) and a sheath 10 b coated around the fiber or wire 10 a having an artificial plastic compound ( such as polyamide ; pa , polyethylene ; pe , polypropylene ; pp , polystyrene ; ps , silicone rubber and chloroprene rubber ) in which many photocatalyst particles or photocatalyst coated particles are embedded . in the case of fig5 b , for example , the photocatalyst brush or fiber 10 may be comprised of a conventional artificial plastic or rubber fiber 10 c ( made of polymer or rubber such as polyester , acrylic , polyimide , polyamide ; pa , polyethylene ; pe , polypropylene ; pp , polystyrene ; ps , silicone rubber and chloroprene rubber ) in which many photocatalyst particles 10 d or photocatalyst coated particles 10 d are embedded . referring to fig2 fig3 and fig3 operation method for the cleaning apparatus of the preferred embodiment no . 1 is mentioned in sequence as follows : at first , a power consent 48 is inserted into a receptacle of a commercial power supply to operate the light control circuit device 44 and to light on the uv light source 200 ; the optical connector 52 of the optical fiber or cable 300 is optically connected with an optical inlet of the lamp house 44 and another optical connector 50 of the optical fiber or cable 300 is optically connected with an optical inlet 32 of the handle 310 in the cleaning tool 120 ; the handle 310 of the cleaning tool 120 is gripped by a human hand or hands and the brushes 10 of the cleaning head 100 is moved to sweep and make a brushing back - and / or - forth as shown as an arrow mark 74 on the surface of the cleaned substance 72 such as floors , carpets , walls and human teeth ; and the dirty component 72 as mentioned above can be easily dissolved , removed and cleaned up , because the dirty component 72 is contacted or closed to with the photocatalyst brushes 10 of the cleaning head 100 , in which the photocatalyst brushes 10 is activated by radiation of the uv light rays 63 and 64 in order to oxidize and / or reduce the dirty component 72 . simultaneously , the uv rays 63 incident to the transparent brush supporter 20 are going outside from a front surface of the brush supporter 20 and radiate or illuminate directly the dirty component 72 including such as bacteria , molds etc . on the cleaned substance 70 such as floors , carpets , walls etc ., in addition to radiation to the brushes 10 . therefore , when the germicidal lamp is preferably used for the uv light source 200 , the dirty component 72 including such as bacteria , molds etc . can be sterilized by a sterilizing effect of the uv rays 63 , 64 , because it emits the uv rays between the range from 250 nm to 280 nm ( center wavelength ; 253 . 7 nm ) exhibiting a strong sterilizing effect to bacteria , molds etc . accordingly , the dirty component 72 may be dissolved or sterilized indirectly by a photocatalyst effect according to activation of the photocatalyst and directly by the sterilizing effect according to radiation of the uv rays . in all embodiments of the present invention , the same part or the same member has the same reference numeral . therefore , in explaining various embodiments to be described below , different portions from the embodiment no . 1 already described are explained in detail and the portions already described are omitted as much as possible due to simplification of explanation . fig6 shows a second preferred embodiment of the present invention , in which a cleaning apparatus is roughly comprised of a cleaning tool 130 , a light source 200 , a light control circuit device 46 and an optical fiber 300 . the cleaning tool 130 is further comprised of a cleaning head 100 and a handle 320 . the handle 320 is formed as a pipe of hollow tube and it is extended from the cleaning head 100 or it is connected with the cleaning head 100 . a cleaning head 100 is further comprised of a group of brushes with a photocatalyst 10 ( photocatalyst brushes ) and a transparent brush supporter 20 by which the photocatalyst brushes 10 is fixed . many light diffusing elements or particles 22 ( shown in fig4 ) may preferably be embedded in the transparent brush supporter 20 . in the embodiment no . 2 , one terminal of the optical fiber 300 is connected to the cleaning head 100 by such as an optical fiber connector . the optical fiber 300 is passing inside through the handle of tube 320 and is going outside and is finally connected to a light output part of a lamp house 44 by a detachable optical or light connector 52 of the optical fiber 300 . uv light rays 60 emitting from the light source 200 are gathered by a focus lens 40 and , are input to the optical fiber 300 through the optical connector 52 and are arrived in the cleaning head 100 through the optical fiber 300 . in the embodiment no . 2 , efficient uv rays transmission is obtained with minimum transmission loss , due to use of uv transmissible optical fiber as mentioned in the embodiment no . 1 . fig7 shows a third preferred embodiment of the present invention , in which a cleaning apparatus is roughly comprised of a cleaning tool 140 , a light source 200 and a light control circuit device 46 . the cleaning tool 140 is further comprised of a cleaning head 100 , a transparent neck 100 a of a part of the cleaning head 100 and a handle 330 . the handle 330 is formed as a pipe of hollow tube and it is extended from the transparent neck 100 a , which is enlarged as taper shape in cross - section toward the handle 330 . a cleaning head 100 is further comprised of a group of brushes with a photocatalyst 10 ( photocatalyst brushes ) and a transparent brush supporter 20 by which the photocatalyst brushes 10 is fixed . many light diffusing elements or particles 22 ( shown in fig4 ) may preferably be embedded in the transparent brush supporter 20 . in the embodiment no . 3 , a cleaning tool 140 , a light source 200 , a light control circuit device 46 and a reflector 42 are housed in a hollow portion of the handle 330 . light rays emitting from the light source 200 are optically connected and mechanically fixed with the transparent neck 100 a via an optical connector 74 . the light control circuit device 46 is electrically connected with an electric cord 47 , an electric power supply is fed to the light control circuit device 46 via a power consent 48 and the light source 200 is lit on by an power output of the light control circuit device 46 . the uv light rays emitting from the light source 200 are gathered by the reflector 42 and introduced into a transparent brush supporter of the cleaning head 100 through the optical connector 74 and the transparent neck 100 a . in the embodiment no . 3 , the cleaning apparatus becomes very compact , as most components of the cleaning apparatus are accommodated in the cleaning tool 140 . fig8 and fig9 show a third preferred embodiment of the present invention . a cleaning apparatus is roughly comprised of a cleaning tool 150 , a light source 200 and a light control circuit device 46 , similar to the embodiment no . 3 . the cleaning tool 150 is further comprised of a cleaning head 100 , a transparent neck 100 a of a part of the cleaning head 100 and a handle 330 . the handle 330 is formed as a pipe of hollow tube , in which the light source 200 , the light control circuit device 46 and a reflector are accommodated inside the hollow tube . uv light rays generating from the light source 200 are collected by a reflector 42 and are incident to the transparent neck 100 a of taper shape . the light rays arrived at the he transparent neck 100 a are transmitting directly to a transparent brush support 20 of the head 100 or transmitting by repeating multiple reflection 26 to the brush support 20 . incident light rays 63 input into the brush supporter 20 are striking to at least one of many light diffusing particles 22 embedded in the brush supporter 20 and become diffusing light rays 64 . the diffusing light rays 64 radiate the photocatalyst brushes 10 by which the brushes are activated to be oxidized and / or reduced . in fig1 showing a fifth preferred embodiment of the present invention , only blush portion of a cleaning head 100 is varied from other embodiments . the cleaning head 100 is comprised of a transparent brush supporter 20 , many light diffusing particles 22 embedded in the supporter 20 and the two kinds of brushes consisting of photocatalyst brushes with photocatalyst 10 and transparent brushes without photocatalyst 12 . in the embodiment no . 5 , light diffusing rays 64 radiate directly the photocatalyst brushes 10 or radiate indirectly the photocatalyst brushes 10 through the transparent brushes without photocatalyst 12 . in fig1 showing a sixth preferred embodiment of the present invention , a cleaning head 110 is comprised of a photocatalyst brushes 10 and a brush supporter 24 and a semiconductor light source 220 having a printed wire board 220 b and a light emitting diode ( led ) or diodes 220 a capable of emitting short wavelength rays . the semiconductor light source 220 is embedded in the brush supporter 24 made of transparent resin and an electric power is supplied from lead wires 220 c to the light source 220 . in this case , very small size of cleaning apparatus is obtained for use on a tooth brushing , etc . in fig1 showing a seventh preferred embodiment of the present invention , a cleaning head 112 is comprised of photocatalyst brushes 10 and a brush supporter 25 and a semiconductor light source 230 , in which the semiconductor light source 230 is composed of a light emitting layer 230 c sandwiched by an electrode layer 230 a and a transparent electrode layer 230 a capable of emitting short wavelength rays ( the light source 230 is called as “ el ” i . e . an elector - luminescent device ). the el 230 is embedded in the brush supporter 24 made of transparent resin . the el 230 is lit on , when an electric power is supplied from lead wires 220 d . in this case , very small size of a cleaning apparatus is obtained for use on a tooth brushing , etc . referring to fig1 and fig1 , an eighth preferred embodiment of the invention is explained , in which a cleaning apparatus of the invention is applied to a vacuum cleaner . as shown in fig1 , the vacuum cleaner is roughly comprised of a cleaning tool 160 , a main cleaner body 500 , a flexible hose 330 and an optical fiber cable ( or optical fiber ) 300 . the cleaning tool 160 is further comprised of a cleaning head ( having a nozzle , a hood and a suction inlet ) 114 and a tube type handle ( or wand ) 340 . the cleaner body 500 in the body casing accommodates a motor 500 b , a fan 500 c rotating by the motor 500 b , a dust keeping means ( i . e . a dust bag , or a dust case ) 500 a , a light source 200 to emit short wavelength rays , a light control circuit device 46 and wheels ( or casters ) 500 d for the cleaner body 500 to move easily on an substance to be cleaned such as floors and carpets . the cleaning head 114 accommodates a transparent brush supporter 20 and a group of brushes 10 with photocatalyst . the flexible hose 330 is connected with a terminal of the handle ( or wand ) 340 in a terminal of the hose 330 and a vacuum inlet of the cleaner body 500 in another terminal of the hose 330 . the optical fiber cable 300 capable of transmitting short wavelength rays is connected optically with the light source 200 via an optical connector 55 at a terminal of the optical fiber cable 300 and the cleaning head 114 via another optical connector 54 at another terminal of the optical fiber cable 300 . accordingly , short wavelength rays emitted from the light source 200 housed in the cleaner body is transmitted to the transparent brush supporter 20 housed in the cleaning head 114 via the optical fiber cable 300 and radiate the photocatalyst brushes 20 to activate photocatalyst . therefore , when the fan 500 c is rotating according to rotation of the motor 500 b , an air pressure in a forward of the fan 500 c is decreased and a dirty component 72 on the floor or the carpet is forced to sucked together with an air from the cleaning head 114 and the dirty component 72 is gathered inside the dust bag or dust case 500 a through the hollow of the handle 340 , the flexible hose 330 . arrows 80 indicate airflows . in fig1 showing an enlarged detail of the cleaning head 114 , the cleaning head 114 is comprised of the head case 114 a , the transparent brush supporter 20 having the group of photocatalyst brushes 10 and a suction hole 114 b , a connecting pipe 114 c to connect the handle 340 ( shown in fig1 ) a detachable optical connector 54 a to connect between the brush supporter 20 and an optical fiber 300 a . the cleaning head 114 accommodates the brush supporter 20 with photocatalyst brushes 10 in the head case 114 a and it is constructed to keep air tightness , when the photocatalyst brushes 10 contact or approach to the floor 70 ( or carpet , etc .). the photocatalyst brushes 10 are the fibers including many photocatalyst particles 10 and they are fixed in a bottom of the brush supporter 20 as shown in fig5 . referring again to fig1 and fig1 , the optical fiber cable 300 extended from the optical fiber connector 55 in one end is connected to the optical fiber connector 54 in another end fixed at the head case 114 . the short optical fiber 300 is optically connected between the optical fiber connector 54 and the optical fiber connector 54 a . therefore , the dirty component 72 contacted or adhered on the surface of the cleaned substance 70 , for example , a floor is forced to remove from the surface by contacting ( or sweeping , brushing ) of the photocatalyst brushes 10 and moves to an upper portion of the head case 114 a via the suction inlet 114 b of the brush supporter 20 and goes out from the connecting pipe 114 c according to the airflow 80 . short wavelength rays transmitted in the cleaning head 114 are transmitted to the transparent brush supporter 20 and radiate the photocatalyst brushes 10 . since the photocatalyst brushes 10 are activated by radiation of the short wavelength rays , the dirty component 72 contacted or approached with the activated photocatalyst brushes 10 is oxidized or reduced so as to clean up . fig1 shows a ninth preferred embodiment of the invention , in which a cleaning apparatus of the invention may be applied to a dental cleaner or tooth brushing apparatus . as shown in fig1 , the dental cleaner is roughly comprised of a teeth brushing tool 170 , a light source 200 to emit short wavelength rays ( uv rays , etc . ), a light control circuit device 46 and an optical fiber 300 to transmit uv light rays . the tooth brushing tool 170 is further comprised of a cleaning head 100 having a transparent brush supporter 20 to fix brushes 10 with photocatalyst and a handle 350 having a transparent rod 30 of taper shape in cross - section to transmit uv light rays , a light reflecting sheath 31 to reflect uv light rays and a light inlet 32 . the optical fiber 300 has an optical connector 50 in an end and another optical connector 52 in another end . the optical fiber 300 is connected detachably to the light inlet 32 of the transparent rod 30 in an end via the optical connector 50 and to a light incident inlet of a lamp house 44 via the optical connector 52 . short wavelength rays 60 emitted from the light source 200 is incident to the optical fiber 300 via a lens 40 and the optical connector 52 and they are transmitting in the optical fiber 300 and they become output short wavelength rays 61 . the output rays 61 are incident to the transparent handle 30 of the tooth - brushing tool 350 via the optical connector 50 and they 61 are transmitting in the transparent handle 30 and are transmitting to the cleaning head 100 . the short wavelength rays 61 incident to the cleaning head 100 are radiating the photocatalyst brushes 10 , in which a photocatalyst component is activated . when a teeth brushing is done by using the tooth brushing tool 170 to surface of teeth , gums , and between teeth , etc . such dirty components inside a mouse are easily dissolved and removed according to photocatalyst action as residue or garbage of food , bacteria , molds , plaque , scale and nicotine / tar due to smoking . fig1 shows a tenth preferred embodiment of the invention , in which a cleaning apparatus of the invention may be applied to a dental cleaner or tooth brushing apparatus , similarly to the embodiment no . 9 previously explained . as shown in fig1 , the dental cleaner is roughly comprised of a teeth brushing tool 180 , a light source 200 to emit short wavelength rays ( uv rays , etc . ), a light control circuit device 46 and an optical fiber 300 to transmit uv light rays . the teeth brushing tool 180 is further comprised of a cleaning head 100 having a transparent brush supporter 20 to fix brushes 10 with photocatalyst and a handle 360 of tube connected or jointed to the cleaning head 100 at an end . the optical fiber 300 at an end is connected with the cleaning head 100 , it is passing through an inside of the tube 360 ( handle ), it is going outside and finally at another end it is connected with a light output inlet of a lamp house 44 by a detachable optical connector 52 . since an optical fiber cable includes multiple optical fibers , an optical cable may be used instead of an optical fiber , or vice versa in the above - mentioned embodiments . this is a division of u . s . patent application ser . no . 09 / 161 , 013 , filed on sep . 25 , 1998 , and issued on aug . 1 , 2000 as u . s . pat . no . 6 , 094 , 767 . the prior foreign application of the u . s . patent application ser . no . 09 / 161 , 013 is japanese patent application no . h08 - 103131 , filed on mar . 21 , 1996 , laid open on sep . 30 , 1997 as publication of unexamined patent application ( i . e . laying - open of application ) no . 253595 / 1997 . therefore , the u . s patent document and the publication of unexamined patent application are hereby incorporated herein by reference . while the preferred embodiments of the present invention have been disclosed , it is to be understood that various changes , modifications , combinations or equivalents will be apparent to those skilled in the related art without departing from the spirit of the present invention . therefore , the scope of the present invention is to be determined solely by the appended claims .
0
the following examples illustrate the invention &# 39 ; s applications and displays its advantages , without limiting its scope . this example describes the preparation of a catalyst according to the previous method . the metallic refractory support of the catalyst is 25 grams of alumina , which has a bet - specific surface equal to 200 m 2 / g . this alumina is made available commercially by the akzo company under the name of ck 300 . the catalyst is left overnight in nitrogen at 500 ° c . then , it is submitted to a chlorinating by a gaseous mix of chlorhydric acid and hydrogen ( ratio 80 / 20 ) at 670 ° c . for 2 hours . the catalyst is therefore an alumina chloride containing about 5 . 5 % of its mass as chloride . the catalysts , referred to from b to g , are prepared according to the following instructions : the refractory metallic support of the catalysts is the alumina used in example one . 50 grams of these supports are then impregnated by contact with a water - based solution of chloride of one of the metals from this group : lithium ; sodium , potassium , cesium , magnesium , or barium . the catalysts b , c , d , e , f , and g are respectively prepared from lithium , sodium , potassium , cesium , magnesium , and barium . different concentration levels of these metals have been studied . the water - based solution is then evaporated in a evaporation centrifuge and the catalysts thus obtained are dried at 120 ° c . then calcined at 500 ° c . for 2 hours in the oven . the chlorinating of the catalysts is performed in the way described in example one . for each catalyst thus prepared , the support contains between 5 and 6 % in chloride weight and variable metal quantities , as table 1 shows in example three . this example aims to compare the differences between catalyst a from the previous method and catalysts b - g of this invention &# 39 ; s method , prepared in examples one and two . these two types of catalysts are tested in the alkylation of isobutene by butenes reaction in the following conditions : charge : isobutene + butene - 2 - trans , with a molar ratio of isobutene to butene - 2 - trans around 14 . hourly spatial speed : expressed in p . p . h . ( weight of olefins passing on the catalyst by weight unit of the catalyst and by hour ), 0 . 25 h − 1 . before the beginning of the alkylation , the reactor is filled with nitrogen to the reaction pressure level , prior to the injection of the isobutene - butene - 2 - trans mix . after the alkylation , calculate ( for each of the catalysts a through g ) the rate of conversion of the butenes , the selectivity of c 5 + compounds obtained , the ratio of c 5 - c 7 , c 8 , c 9 + compounds obtained in the alkylate , as well as the ratio of tmp ( trimethylpentane ) compounds obtained in c 8 compounds , according to the following formulas . conversion = rate   of   butene   mass   input - rate   of   butene   mass   output rate   of   butene   mass   input c 5 +   selectivity = rate   of   c 5   mass   input rate   of   olefins   mass   input - rate   of   olefin   mass   output fraction   of   the   c 5  – c 7   in   the   c 5 + = rate   of  [ c 5 + c 6 + c 7 ]   mass   input rate   of   c 5 +   mass   input fraction   of   the   c 8   in   the   c 5 + = rate   of   c 8   mass   input rate   of   c 5 +   mass   input fraction   of   the   c 9 +   in   the   c 5 + = rate   of  [ c 9 + c 9 + ]   mass   input rate   of   c 5 +   mass   input tmp c 8 = rate   of   ( 2 , 2 , 4 - tmp + 2 , 2 , 3 - tmp + 2 , 3 , 4 - tmp + 2 , 3 , 3 - tmp )   mass rate   of   c 8   mass these results show that the invention &# 39 ; s catalysts b and g show a better quality alkylation , since the heavy c 8 compounds and especially tmp compounds are produced in greater quantity , while the conversion of butenes remains satisfactory . this example aims to compare the performances of catalyst b according to the invention and of catalyst a according to the previously used method . the alkylation reaction is performed in the same conditions as example three . the following table 2 gathers the results obtained in butene conversions and c 5 + selectivity , measured as described in example three . these results show that catalyst b of the invention presents a stability clearly superior to that of catalyst a , of the previous method . this example aims to compare the performance of catalyst c of the invention with that of catalyst a of the previous method , with regards to the reaction temperature . the alkylation is performed in the same conditions than in examples three and four . of course the temperature and pressure must be sufficient to maintain the mix of reagents in a liquid state inside the reactor . however , the reactor is filled with liquid isobutene prior to the reaction . table 3 below gathers the results obtained for the butene conversion and the c 5 + selectivity as described in example three . these results show that catalyst c from the invention permits a better conversion and a better selectivity in c 5 + no matter what the reactor temperature may be , and especially allows operation at temperature near ambient temperature .
2
the present invention relates to an automated solution for an airline to monitor online travel agency issuance of tickets and to identify abnormalities associated therewith . this is accomplished by means of the main characteristics of : detecting burst ticketing situations in a real - time environment ; managing travel agents &# 39 ; electronic sales quota ; monitoring the electronic sales of a travel agent ; and by reporting trend analysis on travel agent e - sale transactions . each of these elements will be described in greater detail below . the present invention is designed for any electronic sales environment using an electronic ticket server ( hereafter ets ) such as an ets of a validating airline ( in the environment of the airline industry ). the only requirement is that in order for the present invention to work , the system described in the present invention must have access to electronic sales data stored and / or received in a validating carrier &# 39 ; s ets . referring now to fig1 , the e - ticket quota management system will be described . a check coordination module 100 is a central part of the system performing coordination checks between other modules . the ets 102 is connected via a two way link to a number of agents 104 , 106 and 108 . these agents may be specific to a certain company or airline ( 104 ), or may be travel agents hosted in a different gds ( 106 , 108 ), assuming that the ets hosts the data of the validating carrier . the agent makes a request for an e - ticket issuance ( for example 110 ) and after processing , the ets may accept the request by means of a message 112 . after further processing ( as will be described below ) if there is an anomaly or abnormal situation the airline ets may deny the request , for example as shown by arrow 114 . similarly , this may serve merely as a message to the travel agent that sales are above the predetermined quota number or value and that action may subsequently be taken . the check coordination module 100 is connected to an airline ets 102 and on reception of an agent sale request from the ets , dispatches a request to online checks module 120 and to measurements and statistics module 122 . the check coordination module 100 collects the responses derived from the checking actions carried out by module 120 and determines the final reply to be delivered to the ets . processing rules are used to instruct the ets to reject or accept the ticket issuance and / or notify the agent and the airline . if some of the processes are down or take too long , default responses can also be defined by the rules . it should be noted that the behavior of the check coordination module is highly customizable by the rule definitions so that the whole checking process can be accurately and reactively defined by an administrator acting for a supplier or airline . the check coordination module 100 is also in regular communication with an airline business rules module 116 . the airline business rules are generated and updated by an administrator of a validating airline 118 . this module stores airline configuration parameters for the system : quota number and / or values and periods , airline notification alert types and thresholds values , electronic sales check eligibility criteria ( such as the form of payment [ e . g . cash , credit card , check , etc . ], type of sales [ e . g . all e - tickets , mco , emd etc . ], burst ticketing detection alerts [ which may define the type of alert and alert thresholds etc .). also , an immediate notification can be issued to the airline when a quota alert situation is reached ( for example , a travel agent has almost reached a quota value for the current period ) or a burst ticketing situation has been detected ( agent sales are “ out of predetermined ” limits ). in addition , the airline business rules module 116 can trigger the creation of daily trend analysis reports relating to the travel agent sales . these can be dispatched to the validating airline , either offline or online , in any appropriate manner . the present invention enables an airline to manage risk associated with delegating sales to third parties such as travel agents . the above described system enables the validating airline to be informed in real - time of any burst ticketing situation occurring in a travel agency anywhere in the world . by means of allocation of quotas ( in value and / or number ) for electronic documents ( hereafter called “ e - quotas ”) to an agent , an airline can manage allocation of tickets in a manner which presents less risk in terms of fraudulent behavior . in addition , by generation of a regular report the airline can see behavior trends for all travel agents , which may later be useful in avoiding the airline being owed large amounts of money by particular agents . this can be achieved through the setting of limits and e - quotas , as will be described in greater detail below . since june 2008 , all tickets available from travel agencies are electronic tickets . as such , there is a requirement for an airline to validate travel agencies &# 39 ; selling and issuing tickets even more closely , to avoid the risk of fraud . this is particularly the case where tickets are not paid for by a credit card form of payment ( for example cash ). when a buyer pays the sale by credit card , the associated credit card bank acts as a type of “ guarantee ” for the airline to finally collect any money due . when the buyer pays the agent with a “ non - credit card ” form of payment ( e . g . cash ), the airline has to wait for the bsp to invoice the agent for the sale , and then the bsp sends a payment to the airline . ( this process is long and in the case of fraudulent agents , the bsp sometimes has no guarantee that the agent will pay the money due ). for an electronic ticket to be issued by a travel agent , the agent connects to a gds and opens an online link with the validating airline &# 39 ; s ets . a request for a ticket issuance is received on the ets which makes a real - time decision to either issue the ticket or block the sale using a two way communication with the check module 100 . this decision is based on quota parameters stored in online checks module 120 and on the statistical data stored in module 122 , as will be described below . this is more particularly the case with regards to the remaining quota value for the travel agent in question . as a consequence , the check coordination module 100 essentially relies on the airline ets as is a central repository of all electronic transactions on behalf of an airline . these may include all travel agency sales ( so called indirect sales ), all channels ( office , websites , call centers or any other appropriate means ), all direct sales ( sales issued by an airline &# 39 ; s own agents , ato / cto , etc .). the present invention enables supplementary checks during the processing of e - tickets and their issuance , in order to avoid risk and to track risk trends more closely . referring now to fig2 , a graph of tickets issuance against day is presented for a particular agent to show how burst ticketing detection is carried out . the line 200 shows the ticket sales per day for the agent . the agent is not monitored by a quota but the validating airline has set two burst detection alerts : a first alert threshold 202 ( notification threshold ) is defined as a first percentage above the mean of a travel agent &# 39 ; s busiest days . this triggers a first airline notification . a second alert threshold 204 ( issuance threshold ) is defined as a second percentage above the mean of a travel agent &# 39 ; s busiest days , and this triggers a second airline notification which may also inhibit further sales . line 200 shows two peaks 206 and 208 . the peaks represent the busiest days for this travel agent . for example , the first alert threshold is set at 20 % above the busiest day of sales for the travel agent . if ticket sales surpass the alert threshold a first alert will be sent to the airline . the airline can then take action depending on the circumstances . if the level of sales reaches the issuance threshold , the airline is immediately notified and ticket issuance may optionally be inhibited on the basis of a decision of airline business rules and online checks modules . the measure of e - ticket issuance can be made in terms of number , value , or any other appropriate metric or criterion . in order to understand the trends of a particular travel agent , the mean ( μ ) and standard deviation ( σ ) are calculated on a predetermined period of time and recomputed on a regular basis , for example daily . the statistical values are used to rank the trends of a travel agent and build reports for the airlines . the statistical values are also used for burst ticketing detection , by comparing the level of the agent sales in real - time ( when a sales request is received at the ets ) with the statistical values described in fig3 . fig3 shows a statistical analysis of sales 300 . if the value of sales falls in the upper intervals ( i . e . greater than mean plus two sigma or three sigma ) 302 and 304 this will constitute either an alert threshold or an issuance threshold and the airline will be notified and further sales may be suppressed . the airline has the choice of possible follow - up actions : to create an emergency quota lock for the travel agent which inhibits any further sales for this agent immediately ; to let the system automatically reject the sale ; or to create an extra e - quota for this travel agent to closely monitor future activity . it may be necessary to measure agent sales data for a minimum significant period ( e . g . 30 days having non null values ) for the statistics to be reliable . the description associated with fig2 and 3 demonstrates the detection of burst ticketing situations which have led to a high level of fraudulent activity against airlines in the past . the ticketing activities for a dubious travel agent can result in losses of millions of dollars for the airline and the real - time identification of burst ticketing situations combined with immediate notification to the airline can prevent this . the present invention utilizing the above described daily calculations not only identifies burst ticketing situations , but the airline can also use daily volumes , amounts , values , criteria , etc . to determine e - quotas for new travel agents and manage those of existing agents . a validating airline can set the electronics sales quota online for a travel agent based on its iata or number ( or any other equivalent agent identifier ) for a given period and a given sales number or sales amount or value through a graphical interface , ( 118 in fig1 ). the quota can be immediately activated , for example by setting a start date . a given period is referred to as the capping period and the given number and / or value is referred to as the capping number or value . the airline may set different types of quotas which may be combined in any appropriate manner . examples of the type of quota available include a volume quota and a value quota . the volume quota is based on the number of sales ( capping number ); and the value quota is based preferably on the total sale value issued to the agent ( capping amount / value ). there may be another financial value ( commission amount , fare amount , etc .) or other criteria ( route , origin / destination , etc .) which form the basis of the quota . a capping currency is generally associated with an amount . quotas can also be defined based upon sale type ( e . g . e - ticket , emco , emd ) or the form of payment for the sale ( for example cash , credit cards etc .). the capping period can also be unspecified , so that a predetermined reference period for quota values is considered as unlimited . once quota values are reached , sales are inhibited and the airline has to update the running value of the agent quota ( remaining number / value for the current period ) to unlock further sales , and temporarily may allow the agent to issue tickets until the end of the capping period , as described below with reference to fig4 . typically , this kind of update can be performed by an airline administrator in response to an exceptional increase in activity that is justified by the agent or supplier . nevertheless , ideally the initial capping number and / or capping amount / value will remain unchanged for any subsequent periods . the airline administrator also has the ability to change initial quota parameters thereby updating the capping number , capping value ; capping period and any other capping criterion value . these changes will become effective at the beginning of the next capping period . referring now to fig4 , management of travel agency e - sale quotas will now be described . fig4 represents a graph of e - ticket issuance , either by number of tickets ( volume ) or equivalent amount ( value ) versus period . in the first period p 1 the agent sells tickets that reach the e - quota before the end of the period . at this point the travel agent will receive a warning message and the airline will be notified . since the quota is reached no more tickets will be issued on behalf of the airline by that particular agent . however , as represented by area 400 on the graph , there could be potential sales for the remainder of the period p 1 , which could indicate the requirement for a higher e - quota . in that case , the airline administrator can exceptionally increase the running value ( i . e . remaining volume / amount until the end of the capping period ) to allow further sales until the end of the current period . initial capping values ( 402 ) will reapply at the beginning of the next period . the initial e - quota set by the airline is represented by line 402 and this may be updated by an airline administrator to a level as shown at 404 . if this is the case , these new quota values will replace the initial ones for the following period . by monitoring the real - time sales of a travel agent the airline can have greater control of the ticket issuance and in guaranteeing that the agent has paid for those tickets . as previously mentioned , a predetermined limits or alert thresholds can be determined by an airline for any specific travel agent . the manner in which the alert threshold or limit - can be defined depends on the choices of the airline and the circumstances involved . several examples of predetermined limits or alert thresholds will now be described with reference to fig5 , 6 and 7 . the predetermined threshold or limit can be defined in terms of any appropriate variable and can be based on measurements , trends , statistics , or any other appropriate metric . fig5 shows the percentage of daily sales volume ( number ) or value , as determined by the airline business rules , that can be sold by a particular travel agent . based on a typical daily value for that travel agent , an alert can be sent to the airline in circumstances where the e - quota exceeds the daily value by a predetermined amount . for example , in this case when 120 % of the daily value is reached an alert will be sent to the airline . at this point the airline can then make choices as to how to proceed with this particular agent . fig6 shows an example of monitoring e - quota based on the number of days remaining before the e - quota is likely to be reached . in normal circumstances the e - quota will be reached at the end of period p 1 . however , as is shown by the line 600 in the graph , this is not the trend that is being measured . accordingly , an alert will be sent to the airline if the c - quota is likely to be reached in less than a predetermined period based on the length of p 1 . in this case the example illustrates that the e - quota will be reached in less than two days which is significantly less than period p 1 and as such the alert will be sent at point 602 . an example is shown in fig7 where a percentage of the e - quota capping value is the measure which triggers the alerts within a predetermined period . for example , if 90 % of the e - quota value has already been reached , an alert may be sent to the airline indicating that considerably more tickets are likely to be sold throughout the length of the period than would be predicted by the e - quota . the airline can take appropriate action to either curtail further sales or augment the remaining e - quota for the agent . the method steps associated with the present invention will now be described with reference to fig8 . the steps are essentially split into two separate periods , namely period 1 , 800 and period 2 , 802 . period 1 and period 2 can occur at different times from one another , or in certain circumstances may occur simultaneously . the duration of periods 1 and 2 can be any predetermined time period as required by the airline or supplier . either period can be of indefinite length . period 1 is associated with the measurement of sales and statistics associated with these measurements . during this period any sales made by an agent are registered and stored in the ets as illustrated in step 804 . step 806 computes the statistical indicators for each agent based on the measure of sales . this can occur on a regular basis , for example on a daily basis or any other appropriate basis depending on the airline or supplier needs . at step 808 , a quota is determined for each agent based on the measurements and statistical indicators . the quota is calculated so as to apply to period 2 . during period 2 a request for an agent sale is received 810 . the request is generally received at the ets which processes the request as described above , with reference to fig1 . at step 812 a comparison is made between the level of agent sales for period 2 as compared to the remaining / capping values of the quota calculated in step 808 ; and a set of predetermined business rules which are relevant to the airline or supplier . if the sale is likely to reach the quota for that particular agent ( ko , 814 ) the sale request may be rejected 816 . this can then culminate in a notification to the agent and / or supplier at step 818 . if the sale does not result in the quota being reached ( 820 ) then the sales requests can be accepted , step 822 . a subsequent check can further be made to determine whether the agent sales have reached an airline notification threshold determined by the quota and business rules , step 824 . if this is the case the supplier or airline will be notified at step 826 . if the notification threshold has been met further actions , as described above , may be made by the airline or supplier . as previously indicated , the present invention enables an airline to more carefully and directly manage electronic sales issuance performed by a travel agency ( or ato / cto ). this guarantees less likelihood of fraudulent practices going unidentified . the airline is also able to make updates online and in real - time ; to revise e - quotas based on availability ; to determine a level of confidence in agents ; to identify exceptional agent activity ; and based on many other factors . one advantage compared to existing systems is that the airline is notified in real - time and can take prompt action ( for example , to prevent further agent sales ). the prior art does not send any airline notification , and as such the airline is never aware of any possible fraud . the prior art does not provide any airline immediate access to quota determination or updates . this is handled instead through change requests to a gds and then updated manually such that the whole process can take several days , which is clearly ineffective for fraud scenario detection . whenever a travel agent registers a sale this is captured and stored in the ets . an algorithm is then applied daily to determine trends in ticket issuance in terms of volume or value , and to detect any large variations in sales based on a variation trend analysis . the daily calculations of these statistical parameters can then be used to generate a number of different reports which can be communicated to the airline and used in decision making and planning . one such report may be a general report , which identifies , for example , the top 50 highest trend variations of travel agent sales for a specific day . another example may be a list of agents which have issued a volume or value of tickets greater than a predetermined percentage ( for example , 95 % of the expected upper limit , as calculated from the travel agent &# 39 ; s busiest days ). the general report can be based on the global market or on more discreet markets selected by the airline . for each agent the following information can be provided : a reference , sales volume , sales amount , value , any other useful sale indicator , commission amount , tax amount , fee amount , etc . a further report including key data such as number and amount of key sales during a day is also provided in reports relative to a particular agent . it enables the airline to set a new e - quota if necessary . the “ top 50 ” trend variations analysis may be performed on any travel agent issuing significant volumes or values of tickets for a particular airline in a given day . the reports and alerts are used to detect any suspicious behavior by a travel agent so as to avoid the risk of substantial losses to the airline . reports can be provided using a file format or downloaded online through the interface provided by the system to the airline . it should be noted that the behavior of the check coordination module is highly customizable by the airline business rules so that the whole online checking processing can be accurately and reactively defined by an administrator acting for the supplier . in particular , the check process can be customized to take account of : the type of electronic documents ( electronic tickets , or electronic miscellaneous documents , for domestic or international itineraries , etc . ); the point of sale ( agent office registering the sale ), ( travel agent iata number , other office identifier , or corporate code level , etc . ); the form of payment used for issuance of the electronic sale ( cash only , invoices , all non - credit card types , debit cards , etc . ); the capping values ( sale number , sale amounts , commission amount , etc . ); and the airline notification trigger ( different kinds of alerts and thresholds can be determined and may coexist ). the business rules set the global behavior and also the behavior of each module and check , and depend on many criteria . for example , the validating airline , type of flights ( domestic / international ), point of sale , sale type , form of payment , currency and many others . this invention has been applied to the purchase of tickets in the travel industry environment which extends to all kinds of transportation ( train , ferry , car , etc . ), as well as hotel booking and other services that can be purchased . however , it will be appreciated that the invention may apply to other environments , for example selling other services and products such as travel and leisure packages , examples of which include the following combinations : transportation mode and hotel ( flight , hotel ; train , car , hotel ; and any other combination thereof ); furthermore , a person skilled in the art will understand that some or all of the functional entities as well as the processes themselves may be embodied in software , or one or more software - enabled modules and / or devices . process steps may also be carried out by appropriate and equivalent modules even if these are not identified herein per se . it will be appreciated that embodiments of this invention may be varied in many different ways and still remain within the intended scope and spirit of the invention .
6
the urethane polymethacrylate used in the present composition may be prepared by mixing ( 1 ) polybutadiene - based liquid rubber containing at least one , preferably two or more hydroxyl groups in its molecule , not less than 70 % of 1 , 4 - bonds and 30 % or less of 1 , 2 - bonds , ( 2 ) a polyisocyanate compound and ( 3 ) a hydroxyl group - containing methacrylate in such a ratio that the resulting mixture contains oh groups and nco groups approximately in an equivalent amount ; and then subjecting the mixture to addition - reaction according to a conventional method . since the urethane polymethacrylate thus prepared has both the urethane - bond and 1 , 4 - polybutadiene bond in its molecule , the resulting composition provides a cured product excellent in elasticity . as a polybutadiene - based liquid rubber containing hydroxyl groups in the molecule and not less than 70 % of 1 , 4 - bond may be used a butadiene homopolymer and a copolymer of butadiene with styrene or acrylonitrile both having a number average molecular weight of about 500 to 10 , 000 . the use of a liquid rubber containing less than 70 % of 1 , 4 - bond cannot provide a cured product having elasticity to satisfy the object of the present invention . as the polyisocyanate compound may be used toluylene diisocyanate , hexamethylene diisocyanate and 4 , 4 &# 39 ;- diphenylmethane diisocyanate , as well as a urethane prepolymer obtained by addition reaction of these polyisocyanates with polyhydric alcohols , and the like . the hydroxyl group - containing methacrylate is exemplified by hydroxyethyl methacrylate , hydroxypropyl methacrylate , hydroxybutyl methacrylate , polyethyleneglycol monomethacrylate , polypropyleneglycol monomethacrylate , glycerine dimethacrylate , trimethylolpropane dimethacrylate and the like . the polymerizable methacrylate to be copolymerized with the urethane polymethacrylate thus obtained includes well - known monomethacrylates and polymethacrylates . among them , a monomethacrylate having a molecular weight of 100 to 500 is preferred since it provides a cured product having an excellent elasticity upon copolymerization . a monomethacrylate with a relatively low molecular weight provides a cured product having not only excellent elasticity but also toughness . such monomethacrylates are exemplified by methoxyethyl methacrylate , ethoxyethyl methacrylate , n - butoxyethyl methacrylate , phenoxyethyl methacrylate , methoxypolyethyleneglycol methacrylate , lauryl methacrylate , stearyl methacrylate , cyclohexyl methacrylate , 2 - ethylhexyl methacrylate , hydroxyethyl methacrylate , hydroxypropyl methacrylate , hydroxybutyl methacrylate , polyethyleneglycol monomethacrylate , polypropyleneglycol monomethacrylate and the like . they may be used alone or as a mixture of two or more of them . polymethacrylates may also be used , however , in the case that they are used alone , the resulting cured product is apt to become somewhat brittle . therefore , it is preferable to use a polymethacrylate in combination with the above - mentioned monomethacrylates for the purpose of increasing chemical resistance and thermal resistance . the mixing ratio of the urethane polymethacrylate having 1 , 4 - polybutadiene bond to the polymerizable methacrylate ( a )( ii ) is 20 - 90 % by weight of the urethane polymethacrylate to 80 - 10 % by weight of the polymerizable methacrylate . outside of the range , the viscosity of the resulting polymerizable mixture will become too high or the resulting cured product will become too hard . an especially preferable range thereof is 40 - 70 % by weight of the urethane polymethacrylate to 60 - 30 % by weight of the other polymerizable methacrylate . by incorporating into 100 parts of the above - mentioned polymerizable mixture , 0 . 1 to 5 . 0 parts by weight and preferably 0 . 5 to 2 . 0 parts by weight of the salt of o - benzoic sulfimide with the amine of the general formula ( i ), there is obtained a one - part type anaerobically curable composition which produces a cured product having excellent elasticity without using an organic peroxide . the amine of the formula ( i ) is exemplified by 1 , 2 , 3 , 4 - tetrahydroquinoline , 1 , 2 , 3 , 4 ,- tetrahydroquinaldine and 6 - methyl - 1 , 2 , 3 , 4 ,- tetrahydroquinoline , and the like . the curable composition thus obtained is added with a gelling stabilizer to give a one - part type anaerobically curable composition excellent in long term storage stability . normally , a curable composition which contains a urethane polymethacrylate having 1 , 4 - polybutadiene bond was so easily gelled that it was difficult to make it a one - part type composition . indeed , it has also been difficult for the curable composition consisting of the components ( a ) and ( b ) and not containing any organic peroxide to be stabilized even if large amounts of well - known polymerization inhibitors such as hydroquinone , hydroquinone monomethyl ether and benzoquinone , or chelating agents such as acetyl acetone , o - aminophenol , salicylaldehyde , o - mercaptobenzoic acid , pyrocatechol or the sodium salt thereof , oxalic acid and maloic acid are added . the present inventors have made extensive researches on the stabilization of such curable compositions , and have found that an ammonium or amine salt of an aminopolycarboxylic acid having chelate - forming ability is very useful for this purpose even when it is added in a small amount as low as not more than 0 . 05 part by weight and that is has no adverse effect upon the performances of the resulting curable composition . the aminopolycarboxylic acid having chelate - forming ability is a chelate - forming polycarboxylic acid that has at least one amine group and a plurality of carboxylic acid groups , such as ethylenediamine tetraacetic acid , diethylenetriamine pentaacetic acid , iminodiacetic acid , cyclohexanediamine tetraacetic acid , nitrilotriacetic acid , glycoletherdiamine tetraacetic acid and the like . they are added in an amount of 0 . 0001 to 0 . 2 part by weight , to 100 parts by weight of the polymerizable mixture . the present inventors have also found that an anaerobically curable composition which has good gelling stability and rapid cure property can be obtained , by adding 0 . 0001 to 0 . 2 part by weight of an aminopolycarboxylic acid having chelate - forming ability or an alkali metal salt thereof and moreover 0 . 01 to 5 . 0 parts by weight , preferably 0 . 02 to 1 . 0 part by weight , of aqueous ammonia or a volatile organic amine having a boiling point of not higher than 250 ° c . to 100 parts by weight of the polymerizable mixture , stirring the resulting mixture at a temperature of not higher than 150 ° c ., preferably 60 ° to 100 ° c ., until the ph of the vapors of volatile components including the ammonia or the amine which are removed from the system is decreased to 9 or lower ( as measured by using a ph testing paper ), and then adding to the mixture thus obtained 0 . 1 to 5 . 0 parts by weight of the above - mentioned salt of o - benzoic sulfimide with the amine of the general formula ( i ). the mode of action of the ammonia or the amine during the stirring treatment has not been made clear . it is , however , considered that they act to increase the chelate - forming ability of the aminopolycarboxylic acid or the alkali metal salt thereof , to markedly decrease the undesirable effect of heavy metals on the storage stability of the composition and to neutralize unnecessary acid components which also adversely affect storage stability . when ammonia or amine was simply used , however , the resulting composition has strong alkalinity and was too slow in cure speed to be used as an anaerobically curable composition . in this case , the present inventors have tried to use a volatile alkali which can be readily removed from the system after stabilization , i . e ., aqueous ammonia or an organic amine having a low boiling point , and to remove the volatile components from the system at a temperature not higher than 150 ° c . under normal or reduced pressure , and thus have surprisingly found that there can be obtained an anaerobically curable composition of high performances which is very stable and , moreover , is not decreased in cure speed . as a measure for such removal , it is sufficient to remove the volatile components until the ph of said components escaped out of the system is decreased to 9 or lower by checking the ph at a constant time interval . a temperature exceeding 150 ° c . is not desired during the removal treatment since thermal polymerization of the monomers may possibly take place at such a high temperature . the volatile organic amine used in the present invention is not especially restricted as long as it has a boiling point low enough to be removed from the system ; however , it has preferably a boiling point of not higher than 250 ° c . from the viewpoint of the operation . any primary , secondary or tertiary amines may be employed . such amines are exemplified by monomethylamine , monoethylamine , n - butylamine , dimethylamine , trimethylamine , diethylamine , triethylamine , dibutylamine , tributylamine , n - hexylamine , etc . as mentioned above , the anaerobically curable composition according to the present invention , is of one - part type and is rapidly curable and excellent in long - term storage , and provides a cured product having excellent elasticity without addition of an organic peroxide . it exhibits an excellent performance in the application for prevention of leakage of liquids and gases from franges or pipe joints . that is , the composition not only has an excellent chamical - resistance but also exhibits high resistance to external change in temperature , vibrations and impacts . thus , the composition will largely contribute to the development in the fields where such properties are required . incidentally , it is possible , for the purpose of increasing the commercial value of the composition according to the present invention , to incorporate thereto suitable amounts of colorants such as dyes and the like , organic or inorganic thixotropic agents , fillers , thickening agents , plasticizers and the like . moreover , an organic perixode can be added according to circumstances in a small amount of not more than 0 . 5 part by weight to 100 parts by weight of the curable composition though it is not necessitated in the present invention . the present invention will be explained more specifically by way of the following illustrative examples , comparative examples and application examples , in which all parts are by weight . a hydroxyl - terminated polybutadiene ( known under the trade name poly bd r - 45ht , supplied by arco , u . s . a ., hydroxyl group content 0 . 804 meq / g , 1 , 4 - bond content 80 %, number average molecular weight 3000 - 4000 ), 2 , 4 - toluylene - diisocyanate and hydroxypropylmethacrylate in a molar ratio of 1 : 2 : 2 . 2 are subjected to addition reaction according to a conventional method to give a urethane polymethacrylate [ hereinafter referred to an um ( r45ht - tdi - hpm )]. to the mixture of polymerizable components consisting of 50 parts of the um ( r45ht - tdi - hpm ) and 50 parts of ethoxyethyl methyacrylate are added 300 ppm of cyclohexanediamine tetraacetic acid and 0 . 5 part of 28 % ammonia water . after stirring at room temperature for 10 minutes , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then , 1 . 5 parts of 1 , 2 , 3 , 4 - tetrahydroquinoline salt of o - benzoic sulfimide ( hereinafter referred to as sq salt ) is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the following physical properties of the resulting composition were determined . in a 100 ml polyethylene vessel was placed 50 g of the composition and the days until the composition was thickened or gelled in a oven at 50 ° c . were measured . the present inventors have confirmed that a composition will be stable at room temperature for one year or more if something unusual is not observed in the composition for 10 days or more under such conditions . m10 steel bolts and nuts degreased with trichloroethylene were bonded with each other by using a composition . the time required until the bolt and nut could not be loosened by the hands ( corresponding to a torque strength of about 10 kg - cm ) in the course of commencement of adhesion was measured and recorded as the setting time . after curing the above - mentioned bolt and nut which had been bonded with each other and subjecting to aging at 23 ° c . for 24 hours , the return torque thereof was measured by means of a torque wrench . a torque at which the bonding began to be broken was recorded as a breakloose torque , and an average of the torques at 1 / 4 , 1 / 2 , 3 / 4 and one rotations was recorded as a prevailing torque and breakloose torque / prevailing torque is shown . after a 3 / 4 &# 34 ; pf aluminum socket and a 3 / 4 &# 34 ; pt iron nipple ( pf for straight threads for pipes , and pt for taper threads for pipes ) were bonded by using a composition and aged at 23 ° c . for 24 hours , they were set in a oil pressure test fixture ( oil : turbine oil ) and subjected to an impact caused by pressure and heat by changing the pressure repeatedly from 15 to 30 kg / cm 2 every 7 seconds and the oil temperature repeatedly from 50 ° to 70 ° c . every hour . the time required until the oil began to leak from the bonded portion was measured . a cured product which is excellent in elasticity can follow the changes in pressure and heat and thus exhibits a good sealing property . the elasticity of a cured product was judged by curing a composition to give a sheet about 1 mm thick and observing cracks and restored state which appears upon folding the sheet by 180 degrees . a sheet which does not have cracks and is restored to the original state on folding is recorded as ( o ), whereas a sheet which has cracks or breaks on folding is recorded as ( x ). the results of the above - mentioned physical properties of the composition are shown in table 1 . physical properties of a sheet - like cured product of this composition were also determined to give an elongation of 123 %, a tensile strength of 38 kg / cm 2 and a shore handness of a 84 . to a mixture of polymerizable components consisting of 70 parts of um ( r45ht - tdi - hpm ) and 30 parts of cyclohexyl methacrylate are added 300 ppm of ethylenediamine tetraacetic acid and 0 . 5 part of 28 % ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 5 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were measured as in example 1 . the results thereof are shown in table 1 . the physical properties of a sheet - like cured product of the above composition were also determined to give an elongation of 115 %, a tensile strength of 101 kg / cm 2 and a shore hardness of a 96 . to a mixture of polymerizable components consisting of 50 parts of um ( r45ht - tdi - hpm ), 20 parts of hydroxypropyl methacrylate and 30 parts of methoxypolyethyleneglycol methacrylate ( known under the trade name of nk ester m - 4g , supplied by shinnakamura chemical industries co . ltd ., japan ) are added 1 . 5 parts of sq salt and 300 ppm of diammonium salt of ethylenediamine tetraacetic acid as a gelling stabilizer , and are dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . the physical properties of a sheet - like cured product of the resulting composition were also determined to give an elongation of 108 %, a tensile strength of 35 kg / cm . sup . 2 and a shore hardness of a 81 . to a mixture of polymerizable components consisting of 50 parts of um ( r45ht - tdi - hpm ), 20 parts of hydroxypropyl methacrylate and 30 parts of lauryl methacrylate are added 150 ppm of ethylenediamine tetraacetic acid and 0 . 5 part of 28 % ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 5 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . the physical properties of a sheet - like cured product of this composition were also determined to give an elongation of 100 %, a tensile strength of 43 kg / cm 2 and a shore hardness of a 86 . to a mixture of polymerizable components consisting of 50 parts of um ( r45ht - tdi - hpm ), 20 parts of hydroxyethyl methacrylate and 30 parts of ethoxyethyl methacrylate are added 300 ppm of cyclohexanediamine tetraacetic acid and 0 . 5 part of 28 % ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 5 parts of 1 , 2 , 3 , 4 - tetrahydroquinaldine salt of o - benzoic sulfimide ( hereinafter referred to as sqn salt ) is added to the mixture and is dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . the physical properties of a sheet - like product of this composition were also determined to give an elongation of 109 %, a tensile strength of 136 kg / cm 2 and a shore handness of a 97 . to a mixture of polymerizable components consisting of 50 parts of um ( r45ht - tdi - hpm ) and 50 parts of lauryl methacrylate are added 1 . 5 parts of sq salt and 300 ppm of diammonium salt of ethylenediamine tetraacetic acid as a gelling stabilizer , and are dissolved therein by heating at 80 ° c . for 10 minutes to give an anerobically curable composition . the physical properties thereof were determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable components consisting of 70 parts of um ( r45ht - tdi - hpm ) and 30 parts of hydroxypropyl methacrylate are added 300 ppm of cyclohexanediamine tetraacetic acid and 0 . 5 part of 28 % ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour , while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then , 1 . 5 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable components consisting of 50 parts of um ( r45ht - tdi - hpm ), 20 parts of hydroxyethyl methacrylate and 30 parts of methoxypolyethyleneglycol methacrylate ( known under the trade name of nk ester m - 9g , supplied by shinnakamura chemical industries co . ltd ., japan ) are added 300 ppm of nitrilo triacetic acid and 0 . 5 part of 28 % ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 5 parts of sqn salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable components consisting of 50 parts of urethane polymethacrylate which has been prepared by addition reaction of a hydroxyl - terminated polybutadiene ( known under the trade name of poly bd r - 45ht , supplied by arco , u . s . a ., hydroxyl content : 0 . 804 meq / g , 1 , 4 - bond : 80 %, number average molecular weight : 3000 - 4000 ), 2 , 4 - toluylenediisocyanate and hydroxyethyl methacrylate in a molar ratio of 1 : 2 : 2 . 2 according to a conventional method , 20 parts of hydroxypropyl methacrylate and 20 parts of lauryl methacrylate are added 300 ppm of diethylenetriamine pentaacetic acid and 0 . 45 part of ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 35 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable components consisting of 50 parts of urethane polymethacrylate which has been prepared by addition reaction of a hydroxyl - terminated polybutadiene ( known under the trade name of poly bd r - 45ht , supplied by arco , u . s . a ., hydroxyl content : 0 . 804 meq / g , 1 , 4 - bond : 80 %, number average molecular weight : 3000 - 4000 ) 4 , 4 &# 39 ;- diphenylmethane diisocyanate and hydroxyethyl methacrylate in a molar ratio of 1 : 2 : 2 according to a conventional method , 20 parts of hydroxypropyl methacrylate and 30 parts of methoxypolyethyleneglycol methacrylate ( known under the trade name of nk ester m - 9g , supplied by shinnakamura chemical industries co . ltd ., japan ) are added 1 . 5 parts of sq salt and 300 ppm of diammonium salt of ethylenediamine tetraacetic acid as a gelling stabilizer and are dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable components consisting of 50 parts of urethane polymethacrylate which has been prepared by addition reaction of a hydroxyl - terminated polybutadiene ( known under the trade name of poly bd cs - 15 , supplied by arco , u . s . a ., hydroxyl content : 0 . 645 meq / g , styrene content : 25 %, 1 , 4 - bond : 80 %, number average molecular weight : 3000 - 4000 ), 2 , 4 - toluylene diisocyanate and hydroxypropyl methacrylate in a molar ratio of 1 : 2 : 2 . 2 according to a conventional method [ hereinafter referred to as um ( cs15 - tdi - hpm )], 20 parts of hydroxypropyl methacrylate and 30 parts of cyclohexyl methacrylate are added 300 ppm of tetrasodium salt of ethylenediamine tetraacetic acid and 0 . 5 part of ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 5 parts of 6 - methyl - 1 , 2 , 3 , 4 - tetrahydroquinoline salt of o - benzoic sulfimide ( hereinafter referred to as smq salt ) is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable componets consisting of 50 parts of um ( cs15 - tdi - hpm ), 30 parts of hydroxypropyl methacrylate and 20 parts of methoxypolyethyleneglycol methacrylate ( known under the trade name of nk ester m - 9g , supplied by shinnakamura chemical industries co . ltd ., japan ) are added 300 ppm of tetrasodium salt of ethylenediamine tetraacetic acid and 0 . 5 part of 30 % aqueous solution of trimethylamine . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the trimethylamine to decrease the ph thereof to 9 or lower . then , 1 . 5 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained are determined as in example 1 . the results thereof are shown in table 1 . to a mixture of polymerizable components consisting of 50 parts of urethane polymethacrylate which has been prepared by addition reaction of hydroxyl - terminated acrylonitrilebutadiene copolymer ( known under the trade name of poly bd cn - 15 , supplied by arco , u . s . a ., hydroxyl content : 0 . 614 meq / g , acrylonitrile content : 15 %, 1 , 4 - bond : 80 %, number average molecular weight : 3000 - 4000 ), 2 , 4 - toluylenediisocyanate and hydroxypropyl methacrylate in a molar ratio of 1 : 2 : 2 according to a conventional method , 20 parts of hydroxypropyl methacrylate and 30 parts of methoxypolyethyleneglycol methacrylate ( known under the trade name of nk ester m - 4g , supplied by shinnakamura chemical industries co . ltd ., japan ) are added 300 ppm of tetrasodium salt of ethylenediamine tetraacetic acid and 0 . 5 part of 28 % ammonia water . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then , 1 . 5 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes to give an anaerobically curable composition . the physical properties of the composition thus obtained were determined as in example 1 . the results thereof are shown in table 1 . to a mixture having the composition given below , which is generally said to be flexible after curing and to have static sealing effect , were added 1 . 5 parts of sq salt , 50 ppm of tetrasodium salt of ethylenediamine tetraacetic acid and 50 ppm of oxalic acid . they were dissolved in the above mixture by heating a 80 ° c . for 10 minutes to give an anaerobically curable composition . the composition in this example corresponds to a system in which dimethacrylate of ethyleneoxide adduct of bisphenol a was used instead of urethane methacrylate in the present composition . methoxypolyethylene glycol methacrylate ( known under the trade name nk ester m - 9g , supplied by shinnakamura chemical industries co . ltd ., japan ): 50 parts the physical properties of this composition were determined as in example 1 , the results of which are shown in table 1 . the physical properties of a sheet - like cured product of the above composition were also determined to give an elongation of 10 %, a tensile strength of 58 kg / cm 2 and a shore hardness of a 96 . in comparison with compositions according to the present invention , the composition of this example is markedly low in elongation and also inferior in flexing property although it has a shore hardness approximately equivalent to that of the present composition . it is clear this composition cannot cope with dynamic changes in heat and pressure and there is a large problem as to the oil - pressure sealing property . table 1______________________________________ oil - gelling pressure flex - stability setting adhesive sealing ingat 50 ° c . time strength property pro -( day ) ( min .) ( kg - cm ) ( hr .) perty______________________________________example 1 & gt ; 10 20 97 / 44 & gt ; 24 oexample 2 &# 34 ; 80 78 / 18 &# 34 ; &# 34 ; example 3 &# 34 ; 20 89 / 35 &# 34 ; &# 34 ; example 4 &# 34 ; 35 73 / 28 &# 34 ; &# 34 ; example 5 &# 34 ; 10 110 / 58 &# 34 ; &# 34 ; example 6 &# 34 ; 50 28 / 12 &# 34 ; &# 34 ; example 7 &# 34 ; 40 86 / 23 &# 34 ; &# 34 ; example 8 &# 34 ; 45 49 / 18 &# 34 ; &# 34 ; example 9 &# 34 ; 35 56 / 25 &# 34 ; &# 34 ; example 10 &# 34 ; 30 50 / 14 &# 34 ; &# 34 ; example 11 &# 34 ; 17 115 / 68 &# 34 ; &# 34 ; example 12 &# 34 ; 35 90 / 30 &# 34 ; &# 34 ; example 13 &# 34 ; 50 65 / 25 &# 34 ; &# 34 ; compara - &# 34 ; 15 60 / 120 7 xtiveexample 1______________________________________ to a mixture of polymerizable components consisting of 50 parts of um ( ra45ht - tdi - hpm ), 20 parts of hydroxypropyl methacrylate and 30 parts of methoxypolyethylene glycol methacrylate ( known under the trade name of nk ester m - 9g , supplied by shinnakamura chemical industries co . ltd ., japan ) were added 1 . 5 parts of sq salt and a predetermined amount of a gelling stabilizer , and the resulting mixture was treated in the manner described below to give an anaerobically curable composition . gelling stability at 50 ° c ., setting time and adhesion strength of the composition were determined as in example 1 . the results thereof are shown in table 2 . a . sq salt and a gelling stabilizer are added to a mixture of polymerizable components and are dissolved therein by heating at 80 ° c . for 10 minutes . b . a gelling stabilizer and either ammonia water or a volatile organic amine are added to a mixture of polymerizable components . after stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components to decrease the ph thereof to 9 or lower . then sq salt is added to the mixture and is dissolved therein by heating at 80 ° c . for 10 minutes . c . sq salt is added to a mixture of polymerizable components and dissolved therein by heating at 80 ° c . for 10 minutes , followed by adding a gelling stabilizer and either ammonia water or a volatile organic amine and stirring for 15 minutes at room temperature . as apparent from the results shown in table 2 , good results with respect to long term storage stability and curing properties were obtained only when a gelling stabilizer added is an ammonium or amine salt of an aminopolycarboxylic acid which has chelate - forming ability , or when an aminopolycarboxylic acid having chelate - forming ability , or an alkali metal salt thereof is added together with an ammonia water or a volatile organic amine salt and then stirred while removing volatile components out of the system . table 2__________________________________________________________________________ method of gelling addition stability setting adhesion and at 50 ° c . time strengthno . type and amount of gelling stabilizer treatment ( day ) ( min .) ( kg - cm ) __________________________________________________________________________example 1 diammonium salt of edta . sup . 1 100 ppm a & gt ; 10 10 83 / 20example 2 diammonium salt of cydta . sup . 3 300 ppm &# 34 ; &# 34 ; 20 79 / 21example 3 trimethylamine salt of edta 200 ppm &# 34 ; &# 34 ; 18 75 / 28example 4 edta4na . sup . 2 159 ppm , 0 . 05 phr b &# 34 ; 10 77 / 21 28 % ammonia waterexample 5 edta4na 150 ppm , 0 . 5 phr &# 34 ; &# 34 ; 15 80 / 16 28 % ammonia waterexample 6 edta4na 150 ppm , 1 . 0 phr &# 34 ; &# 34 ; 15 71 / 15 28 % ammonia waterexample 7 edta4na 150 ppm , 0 . 5 phr &# 34 ; &# 34 ; 12 79 / 16 30 % aqueous trimethylamine solutionexample 8 edta4na 150 ppm , triethylamine 0 . 2 phr &# 34 ; &# 34 ; 15 75 / 16example 9 edta4na 150 ppm , tributylamine 0 . 2 phr &# 34 ; &# 34 ; 15 77 / 18example 10 edta 150 ppm , 28 % ammonia water 0 . 5 phr &# 34 ; &# 34 ; 13 76 / 20example 11 edta 150 ppm , diethyl amine 0 . 5 phr &# 34 ; &# 34 ; 30 80 / 16example 12 edta 150 ppm , n - butyl amine 0 . 5 phr &# 34 ; &# 34 ; 30 73 / 17example 13 cydta 150 ppm , 28 % ammonia water 0 . 5 phr &# 34 ; &# 34 ; 20 72 / 20example 14 dtpa . sup . 4 150 ppm , 28 % ammonia water 0 . 5 phr &# 34 ; &# 34 ; 24 79 / 16example 15 nta . sup . 5 300 ppm , 28 % ammonia water 0 . 5 phr &# 34 ; &# 34 ; 30 79 / 18com - p - benzoquinone 1000 ppm a 1 & gt ; 180 22 / 12parativeexample 2com - hydroquinone 3000 ppm &# 34 ; &# 34 ; 70 26 / 7parativeexample 3com - oxalic acid 150 ppm 0 . 5 phr b &# 34 ; 15 79 / 18parative 28 % ammonia waterexample 4com - edta4na 150 ppm 0 . 5 phr a &# 34 ; 8 74 / 19parativeexample 5com - edta4na 150 ppm 28 % ammonia water 0 . 05 phr c 8 10 78 / 18parativeexample 6com - edta4na 150 ppm 28 % ammonia water 0 . 5 phr &# 34 ; & gt ; 10 & gt ; 180 15 / 9parativeexample 7com - edta 150 ppm a 1 10 82 / 23parativeexample 8com - edta 150 ppm , diethyl amine 0 . 5 phr c & gt ; 10 & gt ; 180 33 / 15parativeexample 9com - cydta 150 ppm a 1 20 72 / 22parativeexample 10com - cydta 150 ppm , 28 % ammonia water 0 . 5 phr c & gt ; 10 & gt ; 180 12 / 5parativeexample 11com - dtpa 150 ppm a 1 15 73 / 18parativeexample 12com - dtpa 150 ppm , 28 % ammonia water 0 . 5 phr c & gt ; 10 & gt ; 180 9 / 5parativeexample 13com - nta 300 ppm a 1 20 74 / 18parativeexample 14com - nta 300 ppm , 28 % ammonia water 0 . 5 phr c & gt ; 10 & gt ; 180 7 / 2parativeexample 15__________________________________________________________________________ notes : . sup . 1 edta : ethylenediamine tetraacetic acid . sup . 2 edta4na : tetrasodium salt of ethylenediamine tetraacetic acid . sup . 3 cydta : cyclohexanediamine tetraacetic acid . sup . 4 dtpa : diethylenetriamine pentaacetic acid . sup . 5 nta : nitrilo triacetic acid to a mixture of polymerizable components consisting of 35 parts of um ( r45ht - tdi - hpm ), 14 parts of hydroxypropyl methacrylate and 21 parts of methoxypolyethylene glycol methacrylate ( known under the trade name of nk ester m - 9g , supplied by shinnakamura chemical industries co . ltd ., japan ) are added 300 ppm of tetrasodium salt of ethylenediamine tetraacetic acid and 0 . 42 part of 28 % ammonia water . ater stirring for 10 minutes at room temperature , the resulting mixture is further stirred at 80 ° c . in the open air for 1 hour while removing volatile components including the ammonia to decrease the ph thereof to 9 or lower . then 1 . 05 parts of sq salt is added to the mixture and dissolved therein by heating at 80 ° c . for 10 minutes , followed by adding thereto 10 parts of polyethylene powder and 20 parts of polytetrafluoroethylene powder as fillers and sufficiently mixing by agitation to produce an gascket . the physical properties of the gascket were determined as in example 1 to give a gelling stability at 50 ° c . of 10 days or more , a setting time of 22 minutes , an adhesion strength of 40 / 12 kg - cm and an oil - pressure sealing property of 24 hours or more . by using the gascket , 3 / 8 &# 34 ; pt iron socket and 3 / 8 &# 34 ; pt hexagon socket head plug ( parkerizing ) were bonded with each other and aged for 24 hours . the sealing of the bonded product was measured . there was observed no leakage under oil pressure of 200 kg / cm 2 . the flange - pressure resistance thereof was also measured according to jis k6820 to show pressure resistance of not less than 100 kg / cm 2 .
2
for the purposes of promoting an understanding of the principles of the invention , reference will now be made to the embodiment illustrated in the drawings and specific language will be used to describe the same . it will nevertheless be understood that no limitation of the scope of the invention is thereby intended , and alterations and modifications in the illustrated device , and further applications of the principles of the invention as illustrated herein are contemplated as would normally occur to one skilled in the art to which the invention relates . referring to fig1 there is shown a container and vehicle combination 10 with apparatus 11 for remotely locking and unlocking the container door 12 , in accordance with the present invention . combination 10 generally includes a vehicle 13 and a container 14 , the container &# 39 ; s dump door 12 being rear - mounted , and the apparatus 11 being remotely operable to lock and unlock door 12 in fluid tight engagement with its container 14 . the vehicle is a suitable container hoist having a main frame 17 and a tipper frame 18 hingedly connected to main frame 17 at hinge 19 . suitable hydraulic cylinders ( one shown at 20 ) connected between main frame 17 and tipper frame 18 and with the hydraulic system of vehicle 13 are operable to pivot tipper frame 18 between a reclined , container loading and transport position 23 ( fig4 - 7 ) and an inclined , dumping position 24 ( fig1 ), as is known . vehicle 13 is configured to receive and handle intermodal containers , that is , containers of a specific size and having corner blocks 25 at each of its eight corners to enable such container to be stacked for transport aboard other vessels , such as trains and ships . alternative embodiments are contemplated wherein the container 14 is of other , non - intermodal configurations , and the apparatus 11 will nevertheless operate to remotely lock and unlock the container aboard a properly equipped vehicle . referring to fig2 , vehicle 13 includes long rails 26 and 27 , numerous transverse cross - members , as at 28 and 29 , extending between long rails 26 and 27 , bolsters ( one shown at 30 , fig8 ) connected to the rear ends of and outwardly of long rails 26 and 27 , and the actuator assembly 33 of apparatus 11 , as described herein . container 14 is configured to be loaded upon vehicle 13 , resting primarily upon long rails 26 and 27 and bolster 30 , and with the locking assembly 95 of apparatus 11 ( as described herein ) positioned directly above actuator assembly 33 for operative engagement therewith . referring to fig1 and 3 , container 14 is a rectangular box container with a rear opening 34 and with its rear door 12 being hingedly mounted at the top edge thereof by hinges 35 to enable door 12 to swing open of its own accord by gravity when the locks holding it are released and tipper frame 18 is pivoted to the inclined , dumping position 24 , as shown in fig1 . container 14 includes a seal 32 ( fig4 ) held around the periphery of door opening 34 , and door 12 includes a sealing ridge 36 extending forwardly and into seal 32 when door 12 is drawn in to its closed position ( fig4 ). container 14 is provided with both bottom and side lock mechanisms 37 , 38 and 39 ( bottom ) and 41 and 42 ( side ). bottom lock mechanisms 37 , 38 and 39 are mutually identical , and only lock mechanism 38 will be fully described . likewise , side mechanisms 41 and 42 are identical , albeit mirror images of each other , and only lock mechanism 41 will be fully described . referring to fig3 and 4 , side lock mechanism 41 includes an outwardly extending door pull pin 46 , a pull pin hook 47 , a rocker link 48 and a bar link 49 . door pull pin 46 is rigidly connected to and extends laterally outwardly of door 12 . at its rear , container 13 includes two , opposing vertical box tubing members 51 and 52 , each of which defines an opening 54 and 55 , respectively , through which freely extends a corresponding door pull pin hook 47 and 56 , respectively . on opposing sides of tubing member 51 are mounted matching arrow plates 59 and 60 , which together close off the sides of opening 54 . arrow plates 59 and 60 define aligned holes for receiving a pin 61 , about which is rotatably mounted triangular rocker link 48 , as shown . rocker link 48 has three triangularly spaced mounting points , the second being at 62 where it is rotatably mounted to the forward end of door pull pin hook 47 , and the third being at 63 where it is rotatably mounted to the upper end of bar link 49 . the lower end of bar link 49 is pivotally connected to output pin 65 of locking assembly 95 , as described herein . up and down motion of bar link 49 moves pull pin hook 47 between a relaxed , unlocked position 66 ( fig6 ) and a retracted , locked position 67 ( fig4 ) wherein the upturned hook 69 at the outer end of pull pin hook 47 has moved up , under door pull pin 46 and drawn door 12 tightly against its seal 32 . at its bottom edge , door 12 is drawn and held closed by the three , identical lock mechanisms 37 - 39 . lock mechanism 38 includes an adjustable door tensioner assembly 74 and an adjustable hook 75 that moves between a lowered unlocked position 76 ( fig6 and 7 ) and a raised and retracted locking position 77 ( fig4 ). tensioner assembly 74 includes a locking plate 80 , a set screw 81 and a locking nut 82 . locking plate 80 is hingedly connected to door 12 at hinge 84 ( fig7 ) and initially lays flat against the lower frame member 83 of door 12 . when adjustable hook 75 is pulled and angled upwardly , its hook tab 85 , rigidly secured to the upturned hook end of hook 75 , bears against locking plate 80 and pulls the bottom of door 12 inwardly , against seal 32 . in the event adjustment is ever needed to draw door 12 or just one portion of door 12 in tighter ( for example , if the seal 32 wears unevenly or door 12 becomes warped ), locking nut 82 can be loosened , and set screw 81 tightened . that is , set screw 81 is threadedly advanced through a threaded hole in locking plate 80 until its forward , leading end bears against the lower frame member 83 of door 12 , which pivots locking plate 80 about its hinge 84 and away from lower frame member 83 . when hook 75 is pulled in ( forwardly ), it bears against a now more rearwardly extending locking plate 80 , and door 12 is forced more tightly against its seal 32 . locking nut 82 is re - tightened after the adjustment is complete . adjustable hook 75 is shaped as shown , and includes an arcuate camming bump 88 , whereat hook 75 rides upon a bump pin 89 . the combination of the camming bump 88 on bump pin 89 and the both curved and linear input to the forward end 90 of hook 75 provides an up and around lock engaging motion relative to tensioner assembly 74 that provides plenty of clearance for door 12 to open and close and provides a reliable and tight door locking action . referring to fig2 and 4 - 9 , the apparatus 11 for remotely locking and unlocking the container door 12 generally includes actuator assembly 33 and locking assembly 95 . actuator assembly 33 includes a push assembly 96 and a driving mechanism 97 to move push assembly 96 between an extended position 98 ( fig6 ) and a retracted position 99 ( fig4 ). push assembly 96 includes a pair of generally u - shaped , spaced apart push plates 103 and 104 that are connected together by a spanner plate 105 ( fig2 ) and a support beam 106 ( fig6 ), both extending therebetween . each push plate has a front and rear upstanding push arm 107 and 108 ( fig5 ) configured to engage with a drive input rod ( 153 and 154 ) of the locking assembly 95 . front push arm 107 has a rearward engagement surface 110 that slants up and rearwardly about 5 degrees . rear push arm 108 has a forward engagement surface 111 that slopes up and rearwardly about 5 degrees , but its top portion includes an initial locking engagement surface 112 with a forward angle of about 30 degrees . alternative embodiments are contemplated wherein the rearward and forward engagement surface angles vary to between about 3 and 8 degrees rearwardly and the initial locking engagement surface angle varies between about 20 degrees and 40 degrees . the forward bending surface portion 112 is generally straight , as are the front and rear engagement surfaces 110 and 112 , but alternative embodiments are contemplated wherein these surfaces have some degree of curvature . the initial locking engagement surface 112 fosters a smooth initial engagement with the main drive rods 153 and 154 , as described , herein , since these rods 153 and 154 may be rotated via their connector links 155 - 158 to near a state pointing almost directly to the rear . in the embodiment shown in fig7 , with hook 75 in the lowered unlocked position 76 , the radial line 159 from the pivot axis of links 155 - 158 ( that is , of main drive shaft 142 ) to their main drive rods 153 , 154 forms an angle of about 27 degrees below horizontal . in such configuration , with the force vector 160 of forward engagement surface 111 slanting up about 5 degrees , the horizontal movement of push plates 103 and 104 , upon engagement with main drive rods 153 and 154 , could bind up . the force vector 161 of forward sloping surface 112 is about 30 downward , which works to avoid such undesirable resistance by converting the initial force vector from about 5 degrees above horizontal to about 30 degrees below horizontal , as shown . driving mechanism 97 is a hydraulic cylinder 182 anchored at its forward end 183 to tipper frame 18 , and its output rod 184 is mounted to the support beam 106 of push assembly 96 . appropriate guide structure and wear plates , as at 113 and 114 are provided to maintain push assembly 96 in its intended path . referring to fig4 - 9 , and particularly 8 and 9 , locking assembly 95 is contemplated to include one , two or more sets of components , each set configured and operable , upon engagement with actuator assembly 33 , to move its adjustable hook 75 between its lowered unlocked position 76 ( fig6 and 7 ) and its raised and retracted locking position 77 ( fig4 ). as shown in fig8 and 9 , locking assembly 95 of the present invention has three hooks 75 and thus three , substantially identical locking assembly sets 115 , 116 and 117 . locking assembly set 117 is removed from fig8 for discussion of surrounding components . because locking assembly sets 115 , 116 and 117 are substantially identical , only set 116 will be described , with one notable difference discussed herein . locking assembly set 116 includes its adjustable hook 75 , the forward end of which is adjustably connected to a hook rod 121 , which is rotatably journaled to both ( 1 ) one end of a pair of bent dogbone linkages 122 and ( 2 ) one end of a pair of upper links 123 . the opposite ends of the upper links 123 are fixed to rotate with an upper locking rod 126 , which is journaled for rotation by a pair of opposing lock assembly support plates 127 and 128 , as described herein . this upper locking rod 126 generally serves no other function than to support the links and rods connected thereto . however , upper locking rods 130 and 131 of the other two locking assembly sets 115 and 117 on opposite sides thereof not only support the connected linkages , but they also extend outwardly therefrom and connect with corresponding links 132 and 133 , respectively , which in turn connect with respective bar links 50 ( fig1 ) and 49 ( fig4 ) to lock / unlock side lock mechanisms 42 and 41 . at their forward ends , the pair of bent dogbone linkages 122 define aligned holes and are rigidly connected together by a sleeve 136 which , together , form a mounting collar 137 that is disposed between and journaled to and between one end of main drive links 140 and 141 . the opposing ends of main drive links 140 and 141 are rigidly connect to and rotate as a unit with main drive shaft 142 , which is supported for rotation by all the lock assembly support plates 127 and 128 , 145 and 146 , and 147 and 148 . outside of and on opposing sides of the central pair of lock assembly support plates 127 and 128 , there are disposed main drive rods 153 and 154 , each rigidly connected via a pair of connector links 155 and 156 , and 157 and 158 , respectively , to main drive shaft 142 , as shown . forward or rearward , generally linear input to main drive rods 153 and 154 ( via rear and front upstanding push arms 108 and 107 ) causes main drive shaft 142 to rotate as a unit therewith and with main drive links 140 and 141 , which moves bent dogbone links 122 , which rotates upper links 123 and moves hook 75 . the rotation of main drive shaft 142 likewise moves hooks 75 of locking assembly sets 115 and 117 and rotates upper locking rods 130 and 131 , which moves link bars 50 and 49 via intermediate links 132 and 133 . the bend in dogbone link 122 causes collar 137 and its axis of rotation to move over center when push assembly 96 is moved to the locking position 99 . the resistance to being locked tightly against its seal 32 causes door 12 to pull dogbone linkage 122 rearwardly , but because the axis of sleeve 136 of collar 137 is above a line extending between the axis of main drive shaft 142 and the axis of rotation at the opposite end of dogbone linkage 122 ( that is , hook rod 121 ) the rearward pull on dogbone linkage 122 merely urges dogbone linkage 122 to rotate further counterclockwise about main drive shaft 142 , that is , further to the locked position . the linkages thus resist becoming unlocked without the significant input of actuator assembly 33 a variety of part sizes , angles and manners of assembly and mounting may be used , but the current configuration is believed to be preferred . locking assembly 95 is supported by the three pairs of opposing lock assembly support plates 127 and 128 , 145 and 146 , and 147 and 148 , as well as the outer lock assembly support plates 162 and 163 , as shown in fig8 . all the lock assembly support plates 127 , 128 , 144 - 148 , 162 and 163 are identical and are rigidly connected to rear and front bolsters 30 and 166 , as shown . referring to just one of the lock assembly support plates , plate 147 comprises a strong flat plate with two inverted , generally t - shaped notches 169 defined therein . at the base ( top ) of each notch is defined a semi - circular recess 170 . a complementary - shaped , removable bearing t - plate 172 has defined at its base ( top ) a mirror image semi - circular recess 174 that , with recess 170 when t - plate 172 is positioned in a complementary notch 169 , forms a bearing hole 175 for rotatably supporting a rotating rod such as main drive shaft 142 or an upper locking rod 126 , 130 or 131 . each t - plate is stitch welded to its lock assembly support plate ( i . e . 147 ) which fixedly connects t - plate and support plate together , but which enables the stitch welds to be removed by known methods , if desired , to service locking assembly 95 . assembly is also greatly facilitated as locking assembly 95 can be assembled upside down and the various linkages can be lowered into place , and the t - plates then stitch welded in place to provide a strong , secure and reliable locking assembly 95 . the entire locking assembly 95 collection is then turned over , for example as shown in fig8 , and connected to or assembled with the rest of the container , the floor of the container typically being then welded directly thereon . as assembled , when a container with locking assembly 95 is positioned atop a vehicle having actuator assembly 33 , the main drive rods 153 and 154 are each thus juxtaposed directly between the front and rear upstanding push arms 107 and 108 of a push assembly 96 . actuation of actuator assembly 33 causes push assembly 96 to engage drive rods 153 and 154 and thus move locking hooks 75 and , if the container 14 is so equipped , side pull pin hooks 47 into and out of their locking positions . container and vehicle combination 10 is further provided with one or more auxiliary locks , such as stinger locks 177 and 178 , as is known . while the invention has been illustrated and described in detail in the drawings and foregoing description , the same is to be considered as illustrative and not restrictive in character , it being understood that only the preferred embodiment has been shown and described and that all changes and modifications that come within the spirit of the invention are desired to be protected .
1
hereinafter , an electro - acoustic conversion device mount substrate , a microphone unit , and manufacturing methods of them are described in detail with reference to the drawings . fig1 is a schematic sectional view showing a structure of a microphone unit according to a first embodiment to which the present invention is applied . as shown in fig1 , a microphone unit 1 according to the first embodiment includes : a mems chip 11 ; a mike substrate 12 on which the mems chip 11 is mounted ; and a cover 13 . the microphone unit 1 according to the first embodiment functions as an omnidirectional mike . the mems chip 11 including a silicon chip is an embodiment of the electro - acoustic conversion device according to the present invention , and a small capacitor type microphone unit that is manufactured by using a semiconductor manufacturing technology . fig2 is a schematic sectional view showing a structure of the mems chip which the microphone unit according to the first embodiment includes . the mems chip 11 has a substantially rectangular parallelepiped shape in outer shape , and as shown in fig2 , includes : an insulating base substrate 111 ; a fixed electrode 112 ; an insulating intermediate substrate 113 ; and a diaphragm 114 . the base substrate 111 is provided with a through - hole 111 a having a substantially circular shape when viewed from top through its central portion . the plate - shaped fixed electrode 112 is disposed on the base substrate 111 and provided with a plurality of small - diameter ( about 10 μm in diameter ) through - holes 112 a . the intermediate substrate 113 is disposed on the fixed electrode 112 and , like the base substrate 111 , is provided with a through - hole 113 a having a substantially circular shape when viewed from top through its central portion . the diaphragm 114 disposed on the intermediate substrate 113 is a thin film which receives a sound pressure to vibrate ( i . e ., vibrate vertically in fig2 . besides , in the present embodiment , the substantially circular portion vibrates ), has electrical conductivity and forms an end of the electrode . the fixed electrode 112 and the diaphragm 114 , which are disposed to be in a substantially parallel relationship with each other across a gap gp thanks to the presence of the intermediate substrate 113 , form a capacitor . in the mems chip 11 , when a sound wave reaches and the diaphragm 114 vibrates , an inter - electrode distance between the diaphragm 114 and the fixed electrode 112 changes , accordingly , electrostatic capacity changes . as a result of this , it is possible to fetch the sound wave ( sound signal ) entering the mems chip 11 as an electric signal . here , in the mems chip 11 , thanks to the presence of the through - hole 111 a formed through the base substrate 111 , the plurality of through - holes 112 a formed through the fixed electrode 112 and the through - hole 113 a formed through the intermediate substrate 113 , a lower surface of the diaphragm 114 also is able to communicate with an outside space ( outside the mems chip 11 ). the mike substrate 12 , which is formed to have a substantially rectangular shape when viewed from top , is an embodiment of the electro - acoustic conversion device mount substrate according to the present invention , and on an upper surface 12 a of which the mems chip 11 is mounted . although skipped in fig1 , the mike substrate 12 is provided with a wiring pattern ( inclusive of a through - wiring ) that is necessary to apply a voltage to the mems chip 11 and to fetch an electric signal from the mems chip 11 . besides , the mike substrate 12 is provided with an opening 121 through the mount surface ( the upper surface ) 12 a on which the mems chip 11 is mounted , and the mems chip 11 is disposed to cover the opening 121 . the opening 121 connects to an intra - substrate space 122 that has a substantially cylindrical shape . the intra - substrate space 122 connects to only the opening 121 but does not connect to another opening . in other words , the mike substrate 12 is provided with a recess by means of the opening 121 and the intra - substrate space 122 . the intra - substrate space 122 is disposed with intention of increasing a volume of a rear chamber ( a tightly closed space that faces a lower surface of the diaphragm 114 ). if the rear chamber volume increases , the diaphragm 114 is easily displaced , and the mike sensitivity of the mems chip 11 improves . here , the mike substrate 12 may be , for example , an fr - 4 ( glass epoxy substrate ) substrate , however , may be another kind of substrate . the cover 13 , which is formed to have a substantially rectangular - parallelepiped shape in outer shape , is placed over the mike substrate 12 , thereby collaborating with the mike substrate 12 to form a housing space 14 that houses the mems chip 11 . the cover 13 is provided with a sound hole 131 that guides a sound occurring outside the microphone unit 1 to the diaphragm 114 of the mems chip 11 . here , the cover 13 is an embodiment of a cover portion of the present invention . when a sound wave input into the housing space 14 via the sound hole 131 reaches the diaphragm 114 , the diaphragm 114 vibrates , whereby as described above , a change in the electrostatic capacity occurs . the microphone unit 1 is structured to fetch the change in the electrostatic capacity as an electric signal and to output the electric signal . here , it is preferable that an electric circuit portion for fetching the change in the electrostatic capacity as an electric signal is disposed in the housing space 14 ; however , the electric circuit portion may be disposed outside the housing space 14 . besides , the electric circuit portion may be monolithically formed on a silicon substrate that forms the mems chip 11 . in the meantime , in the microphone unit 1 according to the first embodiment , a wall surface 122 a ( in the present embodiment , the entire wall surface of the intra - substrate space 122 ) of the intra - substrate 122 formed in the mike substrate 12 is covered by a coating layer cl . the covering by the coating layer cl is obtainable by , for example , a plating process , and the coating layer cl may be , for example , a metal plated layer such as a cu plated layer and the like . thanks to the covering by the coating layer cl , it is possible to reduce a likelihood that dust occurs in the intra - substrate space 122 of the mike substrate 12 . in a case where the mike substrate 12 is composed of , for example , a glass epoxy substrate ( fr - 4 substrate ), a fiber - like dust easily occurs from a machined surface ( a surface to which machining such as severing , scraping or the like is applied ) of the mike substrate 12 . in a case where the wall surface 122 a of the intra - substrate space 122 is not covered by means of the coating layer cl ( in a case different from the present embodiment ), dust easily enters the mems chip 11 that is disposed to cover the opening 121 which connects to the intra - substrate space 122 . the invasion of dust into the mems chip 11 causes malfunction of the mems chip 11 . as an example , there is a situation in which dust enters from the through - hole 112 a disposed through the fixed electrode 112 and clogs the gap gp ( see fig2 ) between the fixed electrode 112 and the diaphragm 114 . regarding this point , in the microphone unit 1 according to the first embodiment , thanks to the presence of the coating layer cl , dust is unlikely to occur from the intra - substrate space 122 , and it is possible to reduce the likelihood that the mems chip 11 malfunctions . next , methods for manufacturing the mike substrate 12 and the microphone unit 1 described above are described with chief reference to fig3 . fig3 is a sectional view for describing a manufacturing method for the mike substrate that the microphone unit according to the first embodiment includes , of which ( a ) to ( f ) show states during the manufacturing , and ( g ) shows a state in which the mike substrate is completed . when manufacturing the mike substrate 12 , first , a substrate 12 ′ ( flat - plated shape ), whose upper surface and lower surface are covered by a metal material ( electro - conductive material ) 101 such as cu or the like , is prepared ( step a ; see fig3 ( a )). the thickness of the substrate 12 ′ is 1 . 0 mm for example , and the thickness of the electro - conductive material 101 is 0 . 15 μm . at a substantially central position of the prepared substrate 12 ′, the substrate 12 ′ is dug from the upper surface to a position in a thickness direction ( the vertical direction of fig3 ). in this way , as shown in fig3 ( b ), the opening 121 having a substantially circular shape when viewed from top and the substantially cylindrical - shaped intra - substrate space 122 ( which connects to the opening 121 only but does not connect to another opening ) connecting to the opening 121 are formed ( step b ). the digging into the substrate 12 ′ is performed by using , for example , an nc ( numerical control ) apparatus that is able to perform the scrape machining of a 3d object controlling coordinate positions . the size of the intra - substrate space 122 is , for example , 0 . 6 mm in diameter and 0 . 5 mm in depth . in the meantime , here , the substrate ( a substrate provided with a recess ) which is provided with the opening 121 and the intra - substrate space 122 is obtained by using the nc apparatus ; however , this is not limiting . in other words , a first substrate ( flat - plated shape ) provided with a through - hole ( formed by a drill or a laser , for example ) and a second substrate with no through - hole are attached to each other , whereby one substrate provided with the opening 121 and the intra - substrate space 122 may be obtained . next , in the substrate 12 ′ where the opening 121 and the intra - substrate space 122 are formed , a through - hole 103 ( e . g ., 0 . 3 mm in diameter ) is formed through a portion where it is necessary to electrically connect the upper surface and the lower surface to each other as shown in fig3 ( c ) ( step c ). for the forming of the through - hole 103 , for example , a drill , a laser , an nc apparatus or the like is used . the portion where it is necessary to electrically connect the upper surface and the lower surface of the substrate 12 ′ to each other is suitably decided by how a circuit structure of the microphone unit is designed . in fig3 ( c ), three places are shown as the places where to form the through - hole 103 ; however , this is not limiting . besides , the step b and the step c may be changed with each other in order . when the through - hole 103 is formed through the substrate 12 ′, next , a plating process ( e . g ., electroless copper plating process ) is applied to the through - hole 103 to form a through - wiring 104 as shown in fig3 ( d ) ( step d ). at this time , the plating process is applied to the wall surface of the intra - substrate space 122 as well . because of this , at the same time of the forming of the through - wiring 104 , the entire wall surface of the intra - substrate space 122 is covered by a metal ( e . g ., cu ) plated layer cl ( coating layer cl ). here , the forming of the through - wiring 104 and the process of covering the wall surface of the intra - substrate space 122 by means of the coating layer cl may be performed with a method other than the plating process , for example , may be performed with a method ( burying , applying and the like ) that uses electro - conductive paste and the like . next , a portion of the upper surface and the lower surface of the substrate 12 ′ where the wiring pattern is necessary is masked by means of an etching resist 105 as shown in fig3 ( e ) ( step e ). at this time , also , the coating layer cl ( e . g ., a cu plated layer ) applied to the wall surface of the intra - substrate space 122 is masked by means of the etching resist 105 . when the masking by means of the etching resist 105 is completed , the substrate 12 ′ is dipped into an etching liquid ( step f ). in this way , of the electro - conductive material ( e . g ., cu ) disposed on the upper surface and the lower surface of the substrate 12 ′, a portion which is not covered by the etching resist 105 is removed as shown in fig3 ( f ). in the meantime , here , the unnecessary electro - conductive material is removed by the etching ; however , this is not limiting , and the unnecessary electro - conductive material may be removed by , for example , laser machining and scrape machining . when the etching is completed , the washing of the substrate 12 ′ and the removal of the etching resist 105 are performed ( step g ). in this way , as shown in fig3 ( g ), the mike substrate 12 is obtained , which includes the opening 121 and the intra - substrate space 122 whose wall surface is covered by the coating layer cl , and is provided with the wiring pattern ( inclusive of the through - wiring ). by disposing the mems chip 11 onto the upper surface 12 a of the mike substrate 12 to cover the opening 121 and further by placing the cover 13 to cover the mems chip 11 , the microphone unit 1 shown in fig1 is obtained . here , the mems chip 11 is connected to the mike substrate 12 by means of a die bonding material ( e . g ., an epoxy resin adhesive , a silicone resin adhesive or the like ) such that a sound leak does not occur and a gap is not formed between the bottom surface and the upper surface of the mike substrate 12 . besides , the cover 13 also is connected to the upper surface of the mike substrate 12 by using , for example , an adhesive or an adhesive sheet for air - tight sealing . in a case where the electric circuit portion is mounted onto the mike substrate 12 , the mems chip 11 and the electric circuit portion are connected to the mike substrate 12 , thereafter , the cover 13 is connected to the upper surface ( a mount surface of the mems chip 11 and the like ) of the mike substrate 12 . the wiring pattern formed on the lower surface of the mike substrate 12 is used as an external electrode . in the above description , the structure is described , in which the wiring pattern disposed on the mike substrate 12 is formed by means of a subtraction method that uses the etching method ; however this is not limiting . in other words , the wiring pattern disposed on the mike substrate 12 may be formed by means of an addition method that uses printing , burying and the like . fig4 is a schematic sectional view showing a structure of a microphone unit according to a second embodiment to which the present invention is applied . as shown in fig4 , a microphone unit 2 according to the second embodiment includes : a mems chip 21 ; a mike substrate 22 on which the mems chip 21 is mounted ; and a cover 23 . the microphone unit 2 according to the second embodiment functions as an omnidirectional mike . the structure of the mems chip 21 ( an embodiment of the electro - acoustic conversion device according to the present invention ), which has a fixed electrode 212 ( which has a plurality of through - holes 212 a ) and a diaphragm 214 , is the same as the structure of the mems chip 11 in the first embodiment , accordingly , a detailed description is skipped . the structure of the mike substrate 22 ( an embodiment of the electro - acoustic conversion device mount substrate according to the present invention ) is substantially the same as the structure of the mike substrate 12 in the first embodiment , but is different from the structure of the first embodiment in that an intra - substrate space 222 connecting to a first opening 221 formed through a mount surface ( upper surface ) of the mike substrate 22 connects to a second opening 223 that is formed through a rear surface ( lower surface ) 22 b opposite to the mount surface of the mike substrate 22 . in other words , the mike substrate 22 is not provided with a recess , unlike the first embodiment , but provided with a through - hole , by means of the first opening 121 , the intra - substrate space 122 and the second opening 223 , that penetrates the mike substrate 22 in a thickness direction . besides , the cover 23 ( an embodiment of the cover portion according to the present invention ) also has substantially the same structure as the cover 13 in the first embodiment , but is different from the structure of the first embodiment in that a sound hole is not disposed . here , the mike substrate 22 may be , for example , an fr - 4 ( glass epoxy substrate ) substrate , however , may be another kind of substrate . in the microphone unit 2 according to the second embodiment , the mems chip 21 is disposed to cover the first opening 221 that is formed through the mount surface 22 a of the mike substrate 22 . the through - hole formed of the first opening 221 , the intra - substrate space 222 and the second opening 223 functions as a sound hole . in other words , a sound wave occurring outside the microphone unit 2 reaches a lower surface of the diaphragm 214 via the second opening 223 , the intra - substrate space 222 and the first opening 221 . in this way , the diaphragm 214 vibrates , whereby a change in the electrostatic capacity occurs . the microphone unit 2 is structured to fetch the change in the electrostatic capacity as an electric signal and to output the electric signal . here , a caution item regarding the disposition of the electric circuit portion for fetching the change in the electrostatic capacity of the mems chip 21 as an electric signal is the same as the case of the first embodiment . the microphone unit 2 according to the second embodiment is structured to use a tightly closed space 24 ( a housing space for housing the mems chip 21 ), which is formed by the mike substrate 22 and the cover 23 , as the rear chamber ; accordingly , it is easy to enlarge the rear chamber volume . because of this , it is easy to improve the mike sensitivity . here , also in the microphone unit 2 according to the second embodiment , a wall surface 222 a ( in the present embodiment , the entire wall surface of the intra - substrate space 222 ) of the intra - substrate space 222 formed in the mike substrate 22 is covered by the coating layer cl . the covering by the coating layer cl is obtainable by , for example , a plating process , and the coating layer cl may be , for example , a metal plated layer such as a cu plated layer and the like . the effect of the covering by the coating layer cl is the same as the case of the first embodiment , and also in the microphone unit 2 according to the second embodiment , it is possible to prevent the occurrence of dust in the intra - substrate space 222 and reduce malfunction of the mems chip 21 . next , methods for manufacturing the mike substrate 22 and the microphone unit 2 described above are described with chief reference to fig5 . fig5 is a sectional view for describing a manufacturing method for the mike substrate that the microphone unit according to the second embodiment includes , of which ( a ) to ( f ) show states during the manufacturing , and ( g ) shows a state in which the mike substrate is completed . when manufacturing the mike substrate 22 , first , a substrate 22 ′ ( flat - plated shape ), whose upper surface and lower surface are covered by a metal material ( electro - conductive material ) 201 such as cu or the like , is prepared ( step a ; see fig5 ( a )). the thicknesses of the substrate 22 ′ and the electro - conductive material 201 may be the same as the first embodiment . at a substantially central position of the prepared substrate 22 ′, along a thickness direction ( the vertical direction of fig5 ) of the substrate 22 ′, a hole ( e . g ., 0 . 6 mm in diameter ), which penetrates from the upper surface to the lower surface , is opened by using , for example , a drill , a laser , an nc apparatus or the like . in this way , the first opening 221 having a substantially circular shape is formed through the upper surface of the substrate 22 ′, the intra - substrate space 222 , which has a substantially cylindrical shape and connects to the first opening 221 , is formed , and the second opening 223 , which is disposed through the lower surface of the substrate 22 ′ and connects to the intra - substrate space 222 , is formed ( step b ; see fig5 ( b )). first , a through - hole 203 is formed through a portion where it is necessary to electrically connect the upper surface and the lower surface to each other as shown in fig5 ( c ) ( step c ). here , the step b and the step c may be changed with each other in order . and , a plating process is performed to form a through - wiring 204 as shown in fig5 ( d ) ( step d ). at this time , the plating process is applied to a wall surface of the intra - substrate space 222 as well , and the entire wall surface of the intra - substrate space 222 is covered by the metal ( e . g ., cu ) plated layer cl ( coating layer cl ). here , the forming of the through - wiring 204 and the process of covering the wall surface of the intra - substrate space 222 by means of the coating layer cl may be performed with other methods , which is the same as the first embodiment . next , portions of the upper surface and the lower surface of the substrate 22 ′ where a wiring pattern is necessary are masked by means of an etching resist 205 ( step e ). at this time , the coating layer cl ( e . g ., a cu plated layer ) applied to the wall surface of the intra - substrate space 222 is also masked by means of the etching resist 105 . when the masking by means of the etching resist 205 is completed , the substrate 22 ′ is dipped into an etching liquid to remove an unnecessary electro - conductive material ( e . g ., cu ) as shown in fig5 ( f ) ( step f ), thereafter , the washing and the removal of the etching resist 205 are performed ( step g ). in this way , as shown in fig5 ( g ), the mike substrate 22 is obtained , which includes the first opening 221 , the intra - substrate space 222 covered by the coating layer cl and the second opening 223 , and is provided with the wiring pattern ( inclusive of the through - wiring ). by disposing the mems chip 21 onto the upper surface 22 a of the mike substrate 22 to cover the opening 221 and further by placing the cover 23 to cover the mems chip 21 , the microphone unit 2 shown in fig4 is obtained . the connection methods for the mems chip 21 and the cover 23 and the caution item in the case of mounting the electric circuit portion onto the mike substrate 22 are the same as the case of the first embodiment . besides , the wiring pattern disposed on the mike substrate 22 may be formed by means of the addition method instead of the subtraction method , which is also the same as the case of the first embodiment . fig6 is a schematic sectional view showing a structure of a microphone unit according to a third embodiment to which the present invention is applied . as shown in fig6 , a microphone unit 3 according to the third embodiment includes : a mems chip 31 ; a mike substrate 32 on which the mems chip 31 is mounted ; and a cover 33 . the microphone unit 3 according to the third embodiment functions as an omnidirectional mike . the structure of the mems chip 31 ( an embodiment of the electro - acoustic conversion device according to the present invention ), which has a fixed electrode 312 ( which has a plurality of through - holes 312 a ) and a diaphragm 314 , is the same as the structure of the mems chip 11 in the first embodiment , accordingly , a detailed description is skipped . besides , the structure of the cover 33 ( an embodiment of the cover portion of the present invention ) provided with a sound hole 331 is also the same as the structure of the cover 13 in the first embodiment , accordingly , a detailed description is skipped . the structure of the mike substrate 32 ( an embodiment of the electro - acoustic conversion device according to the present invention ) is different from the structure of the first embodiment . because of this , in the microphone unit 3 according to the third embodiment , the rear chamber has a structure different from the microphone unit 1 according to the first embodiment . the mike substrate 32 formed to have a substantially rectangular shape when viewed from top is composed by attaching three substrates 32 a , 32 b and 32 c to one another as shown in fig6 . although skipped in fig6 , the mike substrate 32 is provided with a wiring pattern ( inclusive of a through - wiring ) that is necessary to apply a voltage to the mems chip 31 mounted on the upper surface 32 d and to fetch an electric signal from the mems chip 31 . besides , the mike substrate 32 is provided with an opening 321 through the mount surface ( upper surface ) 32 d on which the mems chip 31 is mounted , and the mems chip 31 is disposed to cover the opening 321 . the opening 321 connects to an intra - substrate space 322 that has a substantially l shape in section . the intra - substrate space 322 connects to only the opening 321 but does not connect to another opening . as described above , the mike substrate 32 has the structure obtained by attaching the plurality of substrates , accordingly , it is easy to obtain the intra - substrate space 322 that has the substantially l shape in section . here , the mike substrate 32 may be , for example , an fr - 4 ( glass epoxy substrate ) substrate , however , may be another kind of substrate . the intra - substrate space 322 is disposed with intention of increasing a volume of the rear chamber ( a tightly closed space that faces a lower surface of the diaphragm 314 ). because of the shape ( substantially l shape in section ), it is possible to enlarge the volume of the intra - substrate space 322 in the present embodiment compared with the intra - substrate space 122 in the first embodiment . because of this , the microphone unit 3 according to the third embodiment is expected to be improved in mike sensitivity compared with the microphone unit 1 according to the first embodiment . here , to make it possible to enlarge the rear chamber volume , the intra - substrate space 322 may be structured to have a hollow space that connects to the digging in the substrate thickness direction , or is not limited to the structure of the present embodiment : for example , a substantially inverse t shape in section and the like may be used . in the microphone unit 3 according to the third embodiment , when a sound wave input into a housing space 34 ( formed by the mike substrate 32 and the cover 33 ) via the sound hole 331 of the mems chip 31 reaches the diaphragm 314 , the diaphragm 314 vibrates , whereby a change in the electrostatic capacity occurs . the microphone unit 3 is structured to fetch the change in the electrostatic capacity as an electric signal and to output the electric signal . here , the caution item regarding the disposition of the electric circuit portion for fetching the change in the electrostatic capacity of the mems chip 31 as an electric signal is the same as the case of the first embodiment . in the meantime , in the microphone unit 3 according to the third embodiment , a portion of a wall surface 322 a ( a portion except for a bottom wall of the intra - substrate space 322 ) of the intra - substrate space 322 formed in the mike substrate 32 is covered by the coating layer cl . the covering by the coating layer cl is obtainable by , for example , a plating process , and the coating layer cl may be , for example , a metal plated layer such as a cu plated layer and the like . the effect of the covering by the coating layer cl is the same as the case of the first embodiment , and also in the microphone unit 3 according to the third embodiment , it is possible to prevent occurrence of dust in the intra - substrate space 322 and reduce malfunction of the mems chip 31 . here , of course , a structure may be employed , in which also the bottom wall of the intra - substrate space 322 is covered by the coating layer cl . in the present embodiment , the structure is employed , in which the mike substrate 32 is formed by attaching the plurality of substrates 32 a to 32 c to one another , and the bottom wall of the intra - substrate space 32 is formed of an upper surface of the substrate 32 c . the upper surface of the substrate 32 c is not a surface to which machining such as severing , scraping and the like is applied , accordingly , dust is unlikely to occur . because of this , in the present embodiment , the structure is employed , in which the bottom wall of the intra - substrate space 322 is not covered by means of the coating layer cl . next , methods for manufacturing the mike substrate 32 and the microphone unit 3 described above are described with chief reference to fig7 . fig7 is a sectional view for describing a manufacturing method for the mike substrate that the microphone unit according to the third embodiment includes , of which ( a ) to ( o ) show states during the manufacturing , and ( p ) shows a state in which the mike substrate is completed . when manufacturing the mike substrate 32 , first , a first substrate 32 a ( flat - plated shape ), whose upper surface is covered by , for example , a metal material ( electro - conductive material ) 301 such as cu or the like , is prepared . and , along a thickness direction ( the vertical direction of fig7 ) of the first substrate 32 a , a first through - hole 302 having a substantially circular shape when viewed from top , which penetrates from the upper surface to the lower surface , is opened by using , for example , a drill , a laser , an nc apparatus or the like ( step a ; see fig7 ( a )). the forming position of the first through - hole 302 is a substantially central position of the first substrate 32 a . here , the thickness of the first substrate 32 a is 0 . 3 mm for example , and the thickness of the electro - conductive material 301 is 0 . 15 μm . besides , the diameter of the first through - hole 302 is 0 . 6 mm . besides , a second substrate 32 b ( flat - plated shape ), whose lower surface is covered by the metal material ( electro - conductive material ) 301 such as cu or the like , is prepared . the thicknesses of the second substrate 32 b and the electro - conductive material 301 are the same as the case of the first substrate 32 a . and , along a thickness direction ( the vertical direction of fig7 ) of the second substrate 32 b , a second through - hole 303 having a substantially circular shape when viewed from top , which penetrates from the upper surface to the lower surface , is opened by using , for example , a drill , a laser , an nc apparatus or the like ( step b ; see fig7 ( b )). the second through - hole 303 is disposed at a position that overlaps the first through - hole 302 , and is disposed larger than the first through - hole 302 in diameter . here , of course , the order of step a and step b may be reversed . next , an adhesive is applied onto at least one of the lower surface of the first substrate 32 a and the upper surface of the second substrate 32 b , and the first substrate 32 a and the second substrate 32 b are attached to each other by pressing ( step c ; see fig7 ( c )). in this way , the opening 321 of the mount surface on which the mems chip 31 is mounted is obtained , and the intra - substrate space 322 ( substantially l shape in section ) connecting to the opening 321 is obtained . here , instead of the adhesive , an adhesive sheet ( e . g ., a thermoplastic sheet having a thickness of about 50 μm ) may be used , or the first substrate 32 a and the second substrate 32 b may be attached by means of thermocompression . besides , the substrate formed by attaching the first substrate 32 a and the second substrate 32 b as shown in fig7 ( c ) may be formed of one substrate . in this case , a substrate whose upper surface and lower surface are provided with an electro - conductive material is prepared . and , a digging is formed onto the substrate from both of the upper surface and the lower surface by using an nc apparatus . if the area of the digging formed from the upper surface and the area of the digging formed from the lower surface are made different , the same substrate as shown in fig7 ( c ) is obtained . next , a third through - hole 304 ( e . g ., 0 . 3 mm in diameter ) is formed through a portion where electric connection is necessary between the upper surface of the first substrate 32 a and the lower surface of the second substrate 32 b ( step d ; see fig7 ( d )). for the forming of the through - hole 304 , for example , a drill , a laser , an nc apparatus or the like is used . next , a plating process ( e . g ., electroless copper plating process ) is applied to the third through - hole 304 to form a first through - wiring 305 as shown in fig7 ( e ) ( step e ). at this time , the plating process is applied to a wall surface as well of the intra - substrate space 322 , and the entire wall surface of the intra - substrate space 322 is covered by the metal ( e . g ., cu ) plated layer cl ( coating layer cl ). here , the forming of the first through - wiring 305 and the process of covering the wall surface of the intra - substrate space 322 by means of the coating layer cl may be performed with a method other than the plating process , for example , may be performed with a method ( burying , applying and the like ) that uses electro - conductive paste and the like . next , portions of the upper surface of the first substrate 32 a and the lower surface of the second substrate 32 b where a wiring pattern is necessary are masked by means of an etching resist 306 ( step f ; see fig7 ( f )). at this time , the coating layer cl ( e . g ., a cu plated layer ) applied to the wall surface of the intra - substrate space 322 is also masked by means of the etching resist 306 . next , the first substrate 32 a and the second substrate 32 b which are in a relationship of being attached to each other , are dipped into an etching liquid . in this way , of the electro - conductive material ( e . g ., cu ) disposed on the substrate , a portion which is not covered by the etching resist 306 is removed ( step g ; fig7 ( g )). in the meantime , here , the unnecessary electro - conductive material is removed by the etching ; however , this is not limiting , and the unnecessary electro - conductive material may be removed by , for example , laser machining and scrape machining . next , the substrate dipped in the etching liquid is washed , thereafter , the removal of the etching resist 306 is performed ( step h ; see fig7 ( h )). and , the third substrate 32 c ( an embodiment of another substrate according to the present invention ) whose lower surface is covered by the electro - conductive material 301 is attached onto the lower surface of the second substrate 32 b ( step i ; see fig7 ( i )). the thicknesses of the third substrate 32 c and the electro - conductive material are the same as the cases of the first substrate 32 a and the second substrate 32 b . the attachment of the third substrate 32 c onto the second substrate 32 b may be performed by means of the same method as the attachment of the first substrate 32 a and the second substrate 32 b . next , a protection cover 307 is mounted to cover and close tightly the entire upper surface of the first substrate 32 a ( step j ; see fig7 ( j )). in the present embodiment , the protection cover 307 has a box shape , and an outer edge portion 307 a is bonded and fixed onto the first substrate 32 a with an opening of the box facing downward . at a position other than the outer edge portion 307 a , a gap is formed between the first substrate 32 a and the protection cover 307 . here , the shape of the protection cover 307 is not limited to this , and may be a flat - plated shape . in a case where the protection cover 307 has a flat - plated shape , the entire surface may be bonded to the upper surface of the first substrate 32 a . the step of mounting the protection cover 307 is disposed for the purpose of preventing a substrate treatment liquid from invading the intra - substrate space 322 during later substrate manufacturing processes and the finally obtained electro - acoustic conversion device mount substrate 32 from being contaminated . in detail , in a case where the protection cover 307 is not present , there is a likelihood that the plating liquid and the etching liquid invade the intra - substrate space 322 during the plating , etching and washing steps and residues remain to contaminate the substrate . in this point , as in the present embodiment , by mounting the protection cover 307 , it is possible to prevent the contamination of the substrate . next , a fourth through - hole 308 having a substantially circular shape when viewed from top is opened , which extends from the lower surface of the third substrate 32 c to the lower surface of the second substrate 32 b ( step k ; see fig7 ( k )). the fourth through - hole 308 is formed by means of , for example , a laser , an nc apparatus and the like , and it is possible to form the diameter to be about 0 . 5 mm . here , the order of the step i to the step k may be changed suitably . next , a plating process ( e . g ., electroless copper plating process ) is applied to the fourth through - hole 308 to form a second through - wiring 309 as shown in fig7 ( l ) ( step l ). in this way , electric connection between the wiring pattern on the lower surface of the second substrate 32 b and the electro - conductive material 301 on the lower surface of the third substrate 32 c is performed . when performing the plating process , the etching liquid does not invade the intra - substrate space 322 thank to the presence of the protection cover 307 . here , the forming of the second through - wiring 309 may be performed by means of a method other than the plating process , for example , may be performed by means of a method ( burying , applying and the like ) that uses electro - conductive paste and the like . next , a portion of the lower surface of the third substrate 32 c where a wiring pattern is necessary is masked by means of the etching resist 306 ( step m ; see fig7 ( m )). next , the substrate ( which is formed by attaching the first substrate 32 a , the second substrate 32 b and the third substrate 32 c to one another ) is dipped into the etching liquid to remove an unnecessary electro - conductive material ( e . g ., cu ) on the lower surface of the third substrate 32 c ( step n ; see fig7 ( n )). at this time , the etching liquid does not invade the intra - substrate space 322 thanks to the presence of the protection cover 307 . in the meantime , here , the unnecessary electro - conductive material is removed by the etching ; however , this is not limiting , and the unnecessary electro - conductive material may be removed by , for example , laser machining and scrape machining . when the etching is completed , the substrate washing is performed , and further , the removal of the etching resist 306 is performed ( step o ; see fig7 ( o )). and , finally , as shown in fig7 ( p ), the bonded portion of the protection cover 307 is demounted to separate the protection cover 307 ( step p ). in this way , the mike substrate 32 is obtained , which includes the opening 321 and the intra - substrate space 322 whose wall surface is partially covered by the coating layer cl , and is provided with the wiring pattern ( inclusive of the through - wiring ). by disposing the mems chip 31 onto the upper surface 32 d of the mike substrate 32 to cover the opening 321 and further by placing the cover 33 to cover the mems chip 31 , the microphone unit 3 shown in fig6 is obtained . the connection methods of the mems chip 31 and the cover 33 and the caution item in the case of mounting the electric circuit portion onto the mike substrate 32 are the same as the case of the first embodiment . besides , the wiring pattern disposed on the mike substrate 32 may be formed by means of the addition method instead of the subtraction method , which is also the same as the case of the first embodiment . fig8 is a schematic sectional view showing a structure of a microphone unit according to a fourth embodiment to which the present invention is applied . as shown in fig8 , a microphone unit 4 according to the fourth embodiment includes : a mems chip 41 ; a mike substrate 42 on which the mems chip 41 is mounted ; and a cover 43 . the microphone unit 4 according to the fourth embodiment functions as a bidirectional differential mike . the structure of the mems chip 41 ( an embodiment of the electro - acoustic conversion device according to the present invention ), which has a fixed electrode 412 ( which has a plurality of through - holes 412 a ) and a diaphragm 414 , is the same as the structure of the mems chip 11 according to the first embodiment , accordingly , detailed description is skipped . the structure of the mike substrate 42 ( an embodiment of the electro - acoustic conversion device according to the present invention ) is different from the structures of the first , second and third embodiments . the mike substrate 42 formed to have a substantially rectangular shape when viewed from top is composed by attaching three substrates 42 a , 42 b and 42 c to one another as shown in fig8 . although skipped in fig8 , the mike substrate 42 is provided with a wiring pattern ( inclusive of a through - wiring ) that is necessary to apply a voltage to the mems chip 41 mounted on the upper surface 42 d and to fetch an electric signal from the mems chip 41 . besides , the mike substrate 42 is provided with a first opening 421 near a center of the mount surface ( upper surface ) 42 d on which the mems chip 11 is mounted , and the mems chip 41 is disposed to cover the first opening 421 . the first opening 421 connects to an intra - substrate space 422 that has a substantially u shape in section . the intra - substrate space 422 connects to not only the first opening 421 but also to a second opening 423 that is formed through the mount surface 42 d of the mike substrate 42 . as described above , the mike substrate 42 has the structure obtained by attaching the plurality of substrates , accordingly , it is easy to obtain the intra - substrate space 422 that has the first opening 421 , the intra - substrate space 422 and the second opening 423 . here , the mike substrate 42 may be , for example , an fr - 4 ( glass epoxy substrate ) substrate , however , may be another kind of substrate . the cover 43 , which is formed to have a substantially rectangular - parallelepiped shape , is placed over the mike substrate 42 , thereby collaborating with the mike substrate 42 to form a housing space 44 that houses the mems chip 41 . the cover 43 is provided with a first sound hole 431 that communicates with the housing space 44 . besides , the cover 33 is provided with a second sound hole 432 that communicates with the intra - substrate space 422 via the second opening 423 . here , the cover 43 is an embodiment of the cover portion of the present invention . in the microphone unit 4 according to the fourth embodiment , a sound wave input into the housing space 44 via the first sound hole 431 reaches an upper surface of the diaphragm 414 . besides , a sound wave input into the intra - substrate space 422 via the second sound hole 432 reaches a lower surface of the diaphragm 414 . because of this , when a sound occurs outside the microphone unit 4 , the diaphragm 414 vibrates thanks to a difference between a sound pressure acting on the upper surface and a sound pressure acting on the lower surface . a sound pressure ( amplitude of a sound wave ) of a sound wave is inversely proportional to the distance from a sound source . and , the sound pressure attenuates sharply at a position near the sound source , and attenuate more slowly at a position that is more distant from the sound source . because of this , in a case where a distance from the sound source to the upper surface of the diaphragm 414 and a distance from the sound source to the lower surface of the diaphragm 414 are different from each other , a user voice , which occurs near the microphone unit 4 and enters from the upper surface and the lower surface of the diaphragm 414 , generates a large sound pressure difference between the upper surface and the lower surface of the diaphragm 414 to vibrate the diaphragm . on the other hand , noises from distant places , which enter from the upper surface and the lower surface of the diaphragm 414 have substantially the same sound pressures , accordingly , they cancel out each other and hardly vibrate the diaphragm . accordingly , the electric signal fetched by means of the vibration of the diaphragm 414 is regardable as an electric signal from which the noise is removed and which indicates the user voice . in other words , the microphone unit 4 according to the present embodiment is suitable for a close - talking mike that is required to alleviate a distant noise and collect a near sound . here , the electric circuit portion for fetching the change in the electrostatic capacity of the mems chip 41 as an electric signal may be disposed , for example , in the housing space 44 , or outside the microphone unit . besides , the electric circuit portion may be monolithically formed on the silicon substrate that forms the mems chip 41 . in the meantime , in the microphone unit 4 according to the fourth embodiment , a portion of a wall surface 422 a of the intra - substrate space 422 formed in the mike substrate 42 is covered by the coating layer cl . the covering by the coating layer cl is obtainable by , for example , a plating process , and the coating layer cl may be , for example , a metal plated layer such as a cu plated layer and the like . the effect of the covering by the coating layer cl is the same as the case of the first embodiment , and also in the microphone unit 4 according to the fourth embodiment , it is possible to prevent the occurrence of dust in the intra - substrate space 422 and reduce malfunction of the mems chip 41 . here , of course , a structure may be employed , in which the entire wall surface that forms the intra - substrate space 422 is covered by the coating layer cl . in the present embodiment , the structure is employed , in which the mike substrate 42 is formed by attaching the plurality of substrates 42 a to 42 c to one another . a portion ( wall surface ) where the coating layer cl of the intra - substrate space 422 is not disposed is formed of an upper surface of the third substrate 42 c . this portion is not a surface to which machining such as severing , scraping and the like is applied , accordingly , dust is unlikely to occur . because of this , in the present embodiment , the structure is employed , in which a portion of the wall surface of the intra - substrate space 422 is not covered by means of the coating layer cl . next , methods for manufacturing the mike substrate 42 and the microphone unit 4 described above are described with chief reference to fig9 . fig9 is a sectional view for describing a manufacturing method for the mike substrate that the microphone unit according to the fourth embodiment includes , of which ( a ) to ( o ) show states during the manufacturing , and ( p ) shows a state in which the mike substrate is completed . when manufacturing the mike substrate 42 , first , a first substrate 42 a ( flat - plated shape ), whose upper surface is covered by , for example , a metal material ( electro - conductive material ) 401 such as cu or the like , is prepared . and , along a thickness direction ( the vertical direction of fig9 ) of the first substrate 42 a , a first through - hole 402 and a second through - hole 403 having a substantially circular shape , which penetrate from the upper surface to the lower surface , are opened by using , for example , a drill , a laser , an nc apparatus or the like ( step a ; see fig9 ( a )). here , the thickness of the first substrate 42 a is 0 . 3 mm for example , and the thickness of the electro - conductive material 401 is 0 . 15 μm . besides , the diameters of the first through - hole 402 and the second through - hole 403 are 0 . 6 mm . here , the shapes of the first through - hole 420 and the second through - hole 403 are the same as each other , however , may have different shapes . besides , a second substrate 42 b ( flat - plated shape ), whose lower surface is covered by the metal material ( electro - conductive material ) 401 such as cu or the like , is prepared . the thicknesses of the second substrate 42 b and the electro - conductive material 401 are the same as the case of the first substrate 42 a . and , along a thickness direction ( the vertical direction of fig9 ) of the second substrate 42 b , a third through - hole 404 having a substantially rectangular shape when viewed from top , which penetrates from the upper surface to the lower surface , is opened by using , for example , a drill , a laser , an nc apparatus or the like ( step b ; see fig9 ( b )). the third through - hole 404 is disposed to overlap the first through - hole 402 and the second through - hole 403 . here , in the present embodiment , a right end of the third through - hole 404 is formed to be situated at the same position of a right end of the first through - hole 402 , while a left end of the third through - hole 404 is formed to be situated at the same position of a left end of the second through - hole 403 ; however , this structure is not limiting . for example , a structure may be employed , in which the left and right ends of the third through - hole 404 are more widened to the left and right than the present embodiment . besides , also the shape of the third through - hole 404 is not limited to the shape ( substantially rectangular shape when viewed from top ) of the present embodiment , and is suitably modifiable . here , of course , the order of the step a and the step b may be reversed . next , the lower surface of the first substrate 42 a and the upper surface of the second substrate 42 b are attached to each other ( step c ; see fig9 ( c )). in this way , the first opening 421 of the mount surface on which the mems chip 41 is mounted is obtained , the intra - substrate space 422 ( a substantially u shape in section ) connecting to the first opening 421 is obtained , and the second opening 423 is obtained which is disposed , independent of the first opening 421 , on the mount surface on which the mems chip 41 is mounted and connects to the intra - substrate space 422 . here , the attachment of the first substrate 42 a and the second substrate 42 b may be performed in the same way as the attachment of the first substrate 32 a and the second substrate 32 b in the third embodiment . besides , in the same way as the case of the third embodiment , the substrate ( the board formed by attaching the first substrate 42 a and the second substrate 42 b ) having the structure shown in fig9 ( c ) may be formed of one substrate . hereinafter , although there is a difference in the substrate shape , the manufacturing of the mike substrate 42 is performed in a procedure similar to the case of the third embodiment . points overlapping the third embodiment are skipped or described briefly . a fourth through - hole 405 ( e . g ., 0 . 3 mm in diameter ) is formed through a portion where electric connection is necessary between the upper surface of the first substrate 42 a and the lower surface of the second substrate 42 b by using , for example , a drill , a laser , an nc apparatus or the like ( step d ; see fig9 ( d )). next , by applying a plating process ( e . g ., electroless copper plating process ) onto the fourth through - hole 405 , a first through - wiring 406 shown in fig9 ( e ) is formed ( step e ). at this time , the plating process is also applied to a wall surface of the intra - substrate space 422 , and the entire wall surface of the intra - substrate space 422 is covered by the metal plated layer cl ( coating layer cl ). here , the forming of the through - wiring 406 and the process of covering the wall surface of the intra - substrate space 422 by means of the coating layer cl may be performed with a method other than the plating process , which is the same as the case of the third embodiment . next , portions of the upper surface of the first substrate 42 a and the lower surface of the second substrate 42 b where a wiring pattern is necessary to be formed are masked by means of an etching resist 407 ( step f ; see fig9 ( f )). at this time , the coating layer cl applied to the wall surface of the intra - substrate space 422 is also masked by means of the etching resist 407 . and , the removal of the unnecessary electro - conductive material 401 is performed by means of the etching liquid ( step g ; see fig9 ( g )), and after the etching , the washing and the removal of the etching resist 407 are performed ( step h ; see fig9 ( h )). in the meantime , here , the unnecessary electro - conductive material is removed by the etching ; however , this is not limiting , and the unnecessary electro - conductive material may be removed by , for example , laser machining and scrape machining . next , the third substrate 42 c ( an embodiment of another substrate according to the present invention ) whose lower surface is covered by the electro - conductive material 401 is attached onto the lower surface of the second substrate 42 b ( step i ; see fig9 ( i )). next , a protection cover 408 is mounted to cover and close tightly the entire upper surface of the first substrate 42 a ( step j ; see fig9 ( j )). the shape and the mounting method of the protection cover 408 and the reason for using the protection cover 408 are the same as the case of the third embodiment . next , a fifth through - hole 409 having a substantially circular shape when viewed from top is opened by using , for example , a laser , an nc apparatus or the like , which extends from the lower surface of the third substrate 42 c to the lower surface of the second substrate 42 b ( step k ; see fig9 ( k )). here , the order of the step i to the step k may be changed suitably . next , a plating process ( e . g ., electroless copper plating process ) is applied to the fourth through - hole 409 to form a second through - wiring 410 as shown in fig9 ( l ) ( step l ). in this way , electric connection between the wiring pattern on the lower surface of the second substrate 42 b and the electro - conductive material 401 on the lower surface of the third substrate 42 c is performed . when performing the plating process , the etching liquid does not invade the intra - substrate space 422 thank to the presence of the protection cover 408 . here , the forming of the second through - wiring 410 may be performed by means of a method other than the plating process , which is the same as the third embodiment . next , a portion of the lower surface of the third substrate 42 c where a wiring pattern is necessary is masked by means of an etching resist 407 ( step m ; see fig9 ( m )); the substrate ( which is formed by attaching three substrates of the first substrate 42 a to the third substrate 42 c to one another ) is dipped into the etching liquid to remove an unnecessary electro - conductive material ( e . g ., cu ) on the lower surface of the third substrate 42 c ( step n ; see fig9 ( n )). at this time , the etching liquid does not invade the intra - substrate space 422 thank to the presence of the protection cover 408 . in the meantime , here , the unnecessary electro - conductive material is removed by the etching ; however , this is not limiting , and the unnecessary electro - conductive material may be removed by , for example , laser machining and scrape machining . when the etching is completed , the substrate washing is performed , and further , the removal of the etching resist 407 is performed ( step o ; see fig9 ( o )). and , finally , as shown in fig9 ( p ), the bonded portion of the protection cover 408 is demounted to separate the protection cover 408 ( step p ). in this way , the mike substrate 42 is obtained , which includes the first opening 421 , the second opening 423 , and the intra - substrate space 422 whose wall surface is partially covered by the coating layer cl , and is provided with the wiring pattern ( inclusive of the through - wiring ). by disposing the mems chip 41 onto the upper surface 42 d of the mike substrate 42 to cover the first opening 421 and further by placing the cover 43 such that the second sound hole 432 overlies the second opening 423 , the microphone unit 4 shown in fig8 is obtained . the connection methods of the mems chip 41 and cover 43 and the caution item in the case of mounting the electric circuit portion onto the mike substrate 42 are the same as the case of the first embodiment . besides , the wiring pattern disposed on the mike substrate 42 may be formed by means of the addition method instead of the subtraction method , which is also the same as the case of the first embodiment . the microphone units 1 to 4 , the electro - acoustic conversion device mount substrates ( e . g ., the mike substrates ) 12 , 22 , 32 , 42 , and the manufacturing methods of them according to the embodiments described above are mere examples of the present invention , and the application scope of the present invention is not limited to the embodiments described above . in other words , it is possible to add various modifications to the embodiments described above without departing the object of the present invention . for example , in the embodiments described above , the structure is employed , in which the electro - acoustic conversion device is the mems chip that is formed by using a semiconductor manufacturing technology ; however , the structure is not limiting . the electro - acoustic conversion device formed of the mems chip is especially weak for dust , accordingly , the present invention is preferably applied ; however , the present invention is applicable to a case where an electro - acoustic conversion device other than the mems chip is used . besides , in the above embodiments , the case is described , in which the electro - acoustic conversion device is a so - called capacitor type microphone ; however , the present invention is applicable to a case where the electro - acoustic conversion device is a microphone ( e . g ., a moving conductor ( dynamic ) microphone , an electromagnetic ( magnetic ) microphone , a piezo - electric microphone and the like ) which has a structure other than the capacitor type microphone . besides , in the above embodiments , the case is described , in which the coating layer disposed in the intra - substrate space of the electro - acoustic conversion device mount substrate is a metal layer such as a plated layer and the like ; however , this is not limiting . in short , the coating layer disposed in the intra - substrate space may be a layer other than the metal layer if the layer has the function to alleviate dust that has a likelihood of occurring in the intra - substrate space . in addition , the shapes of the electro - acoustic conversion device and the microphone unit ( inclusive of the opening , the intra - substrate space and the like that are disposed in them ) are not limited to the shapes according to the embodiments , and of course , modifiable into various shapes . the present invention is suitable for a microphone unit that is included in voice input apparatuses such as , for example , a mobile phone and the like . 11 , 21 , 31 , 41 mems chips ( electro - acoustic conversion devices ) 12 , 22 , 32 , 42 mike substrates ( electro - acoustic conversion device mount substrates ) 103 , 203 , 304 , 308 , 405 , 409 through - holes for through - wiring 122 a , 222 a , 322 a , 422 a walls surfaces of intra - substrate spaces
8
the feedstream to the present process generally comprises alkylaromatic hydrocarbons of the general formula c 6 h ( 6 - n ) r n , where n is an integer from 0 to 5 and each r may be ch 3 , c 2 h 5 , c 3 h 7 , or c 4 h 9 , in any combination . the aromatics - rich feed stream to the process of the invention may be derived from a variety of sources , including without limitation catalytic reforming , steam pyrolysis of naphtha , distillates or other hydrocarbons to yield light olefins and heavier aromatics - rich byproducts ( including gasoline - range material often referred to as “ pygas ”), and catalytic or thermal cracking of distillates and heavy oils to yield products in the gasoline range . products from pyrolysis or other cracking operations generally will be hydrotreated according to processes well known in the industry before being charged to the complex in order to remove sulfur , olefins and other compounds which would affect product quality and / or damage catalysts or adsorbents employed therein . light cycle oil from catalytic cracking also may be beneficially hydrotreated and / or hydrocracked according to known technology to yield products in the gasoline range ; the hydrotreating preferably also includes catalytic reforming to yield the aromatics - rich feed stream . if the feed stream is catalytic reformate , the reformer preferably is operated at high severity to achieve high aromatics yield with a low concentration of nonaromatics in the product . fig1 is a simplified flow diagram of a typical aromatics - processing complex of the known art directed to the production of at least one xylene isomer . the complex may process an aromatics - rich feed which has been derived , for example , from catalytic reforming . usually such a stream will have been treated to remove olefinic compounds and light ends , e . g ., butanes and lighter hydrocarbons and preferably pentanes ; such removal , however , is not essential to the practice of the broad aspects of this invention . the aromatics - containing feed stream contains benzene , toluene and c 8 aromatics and typically contains higher aromatics and aliphatic hydrocarbons including naphthenes . the feed stream is passed via conduit 10 via a heat exchanger 12 to reformate splitter 14 and distilled to separate a stream comprising c 8 and heavier aromatics , withdrawn as a bottoms stream in conduit 16 , from toluene and lighter hydrocarbons recovered overhead via conduit 18 . the toluene and lighter hydrocarbons are sent to extractive distillation process unit 20 which separates a largely aliphatic raffinate in conduit 21 from a benzene - toluene aromatics stream in conduit 22 . the aromatics stream in conduit 22 is separated , along with stripped transalkylation product in conduit 45 and overhead from para - xylene finishing column in conduit 57 , in benzene column 23 into a benzene stream in conduit 24 and a toluene - and - heavier aromatics stream in conduit 25 which is sent to a toluene column 26 . toluene is recovered overhead from this column in conduit 27 and may be sent partially or totally to a transalkylation unit 40 as shown and discussed hereinafter . a bottoms stream from the toluene column 26 is passed via conduit 28 , along with bottoms from the reformate splitter in conduit 16 , after treating via clay treater 17 , and recycle c 8 aromatics in conduit 65 , to fractionator 30 . the fractionator 30 separates concentrated c 8 aromatics as overhead in conduit 31 from a high - boiling stream comprising c 9 , c 10 and heavier aromatics as a bottoms stream in conduit 32 . this bottoms stream is passed in conduit 32 to heavies column 70 . the heavy - aromatics column provides an overhead stream in conduit 71 containing c 9 and at least some of the c 10 aromatics , with higher boiling compounds , primarily c 11 and higher alkylaromatics , being withdrawn as a bottoms stream via conduit 72 . the c 9 + aromatics from heavies column in conduit 71 is combined with the toluene - containing overhead contained in conduit 27 as feed to transalkylation reactor 40 , which contains a transalkylation catalyst as known in the art to produce a transalkylation product comprising benzene through c 11 + aromatics with xylenes as the focus . the transalkylation product in conduit 41 is stripped in stripper 42 to remove gases in conduit 43 and c 6 and lighter hydrocarbons which are returned via conduit 44 to extractive distillation 20 for recovery of light aromatics and purification of benzene . bottoms from the stripper are sent in conduit 45 to benzene column 23 to recover benzene product and unconverted toluene . the c 8 - aromatics overhead provided by fractionator 30 contains para - xylene , meta - xylene , ortho - xylene and ethylbenzene and passes via conduit 31 to para - xylene separation process 50 . the separation process operates , preferably via adsorption employing a desorbent , to provide a mixture of para - xylene and desorbent via conduit 51 to extract column 52 , which separates para - xylene via conduit 53 from returned desorbent in conduit 54 ; the para - xylene is purified in finishing column 55 , yielding a para - xylene product via conduit 56 and light material which is returned to benzene column 23 via conduit 57 . a non - equilibrium mixture of c 8 - aromatics raffinate and desorbent from separation process 50 is sent via conduit 58 to raffinate column 59 , which separates a raffinate for isomerization in conduit 60 from returned desorbent in conduit 61 . the raffinate , comprising a non - equilibrium mixture of xylene isomers and ethylbenzene , is sent via conduit 60 to isomerization reactor 62 . the raffinate is isomerized in reactor 62 , which contains an isomerization catalyst to provide a product approaching equilibrium concentrations of c 8 - aromatic isomers . the product is passed via conduit 63 to deheptanizer 64 , which removes c 7 and lighter hydrocarbons with bottoms passing via conduit 65 to xylene column 30 to separate c 9 and heavier materials from the isomerized c 8 - aromatics . overhead liquid from deheptanizer 64 is sent to stripper 66 , which removes light materials overhead in conduit 67 from c 6 and c 7 materials which are sent via conduit 68 to the extractive distillation unit 20 for recovery of benzene and toluene values . there are many possible variations of this scheme within the known art , as the skilled routineer will recognize . for example , the entire c 6 - c 8 reformate or only the benzene - containing portion may be subjected to extraction . para - xylene may be recovered from a c 8 - aromatic mixture by crystallization rather than adsorption . meta - xylene as well as para - xylene may be recovered from a c 8 - aromatic mixture by adsorption , and ortho - xylene may be recovered by fractionation . alternatively , the c 9 - and heavier stream or the heavy - aromatics stream is processed using solvent extraction or solvent distillation with a polar solvent or stripping with steam or other media to separate highly condensed aromatics as a residual stream from c 9 + recycle to transalkylation . in some cases , the entire heavy - aromatic stream may be processed directly in the transalkylation unit . the present invention is useful in these and other variants of an aromatics - processing scheme , aspects of which are described in u . s . pat . no . 6 , 740 , 788 which is incorporated herein by reference . the separation of c 8 aromatics from heavy aromatics in fractionator 30 is a situation in which the distillation process of the invention generally is effective . a distillation process of the present invention is represented by two or more xylene columns each effecting substantially the same separation between c 8 and c 9 + aromatics contained in two or more internal or external - feed streams of the aromatics complex designated respectively as a first and a second feed streams . preferably the two streams comprise a first feed stream which is higher - boiling and a second feed stream which is lower - boiling , wherein the higher - boiling first feed stream has a higher content of c 9 + hydrocarbons than the second feed stream . the invention comprises distilling the first feed stream in at least one first fractionation column at a low pressure to separate a first c 8 - aromatics stream from a first c 9 - and - heavier aromatics stream , distilling the second feed stream in a second fractionation column at an elevated pressure to separate a second c 8 - aromatics stream from a second c 9 - and - heavier aromatics stream , and circulating an overhead stream from the second column to provide heat to a reboiler of the first column . the low pressure typically is between 100 and 800 kpa and the elevated pressure is chosen to enable heat transfer from the first column to the second and typically is at least about 400 kpa above the low pressure . this concept of different pressures in parallel columns is particularly valuable when the heavy components present in the higher - boiling feed stream are subject to degradation at reboiler temperatures needed to separate the light and heavy components . the second fractionation column processes a second feed stream with a lower concentration of heavy materials subject to decomposition than the feed to the first column , and the pressure thus may be raised higher in order to effect energy savings through heat exchange between the first and second columns without loss of product yield or risk of equipment fouling . this feed preferably comprises most or all of the isomerized c 8 aromatics from the isomerization reactor following deheptanization , but may also comprise other c 8 - aromatic streams with low concentrations of heavy aromatics . this stream to the second column typically contains less than about 10 weight -% c 9 + aromatics , more often less than about 5 weight -% c 9 + aromatics , and frequently less than about 2 weight -% c 9 + aromatics . effectively , the process comprises operating the second column at a pressure that would enable the overhead to provide heat to a reboiler of the first column and , preferably , a reboiler of at least one other column and / or steam generator in an associated processing complex . in another embodiment , the process comprises operating the second fractionation column at a pressure that would enable the overhead to provide heat to generate steam useful in an associated processing complex . further , the c 8 - aromatics fractionator may comprise three or more columns comprising additional heat exchange between overheads and reboilers in an analogous manner to the above description . fig2 is an energy - efficient aromatics complex employing a number of concepts of the invention . for ease of reference , a parallel numbering system is employed to those of fig1 and 2 . the feed stream is passed via conduit 110 via heat exchangers 112 and 113 , which raise the temperature of the feed stream , to reformate splitter 114 . the heat exchange is supplied via conduits 213 and 214 respectively from the net para - xylene product and the recovered para - xylene separation process recovered desorbent as discussed later in this section . as in fig1 , c 8 and heavier aromatics are withdrawn as a bottoms stream in conduit 116 while toluene and lighter hydrocarbons recovered overhead via conduit 118 are sent to extractive distillation process unit 120 which separates a largely aliphatic raffinate in conduit 121 from a benzene - toluene aromatics stream in conduit 122 . the aromatics stream in conduit 122 is separated , along with stripped transalkylation product in conduit 144 and overhead from para - xylene finishing column in conduit 157 , in fractionator 123 into a benzene stream in conduit 124 and a toluene - and - heavier aromatics stream in conduit 125 which is sent to a toluene column 126 . toluene is recovered overhead from this column in conduit 127 and may be sent partially or totally to a transalkylation unit 140 as shown and discussed hereinafter . a bottoms stream from the toluene column 126 is passed via conduit 128 , along with bottoms from the reformate splitter in conduit 116 , after treating via clay treater 117 , and recycle c 8 aromatics in conduit 148 , to low - pressure xylene column 130 . other c8 - aromatics streams having significant contents of c9 and heavier aromatics , including streams obtained from sources outside the complex , also may be processed in this column ; a portion of deheptanizer bottoms in stream 165 also may be included depending on overall energy balances . the low - pressure xylene column separates concentrated c 8 aromatics as overhead in conduit 131 from a high - boiling stream comprising c 9 , c 10 and heavier aromatics as a bottoms stream in conduit 132 . simultaneously , an isomerized c 8 - aromatics stream is passed via conduit 165 to a high - pressure second xylene column 133 . this is characterized as a lower - boiling feed stream which contains a lower concentration of heavy materials subject to decomposition than the feed to column 130 , and the column pressure thus can be increased in order to effect energy savings . other c 8 - aromatics - containing streams having similarly low contents of c 9 - and - heavier aromatics , including streams obtained from sources outside the complex , also may be contained in the feed stream to this column . the second xylene column separates a second c 8 - aromatics stream as overhead in conduit 134 from a second c 9 - and - heavier stream in conduit 132 . at least a portion of overhead vapor from the high - pressure xylene column in conduit 134 preferably is employed to reboil low - pressure xylene column 130 in reboiler 135 , leaving as a condensed liquid to the xylene - separation process 150 in conduit 136 as well as reflux ( not shown ) to column 133 . in addition , the overhead in conduit 134 preferably is used to provide energy to the reboiler of extract column 152 as well as other such services which are described later or will be apparent to the skilled routineer . the c 9 + bottoms stream passing to reboiler 137 may provide energy via one or both of the stream before the reboiler in conduit 270 and the heated stream from the reboiler in conduit 259 for reboiling respectively one or both of heavy - aromatics column 170 and raffinate column 159 ; the bottoms stream after heat exchange would be sent to the heavy - aromatics column 170 . other similar heat - exchange services will be apparent to the skilled routineer . the net bottoms stream in conduit 138 usually is passed through column 130 or may be in conduit 139 combined directly with the stream in conduit 132 to heavies column 170 . the heavies column provides an overhead a stream in conduit 171 containing c 9 and at least some of the c 10 aromatics , with higher boiling compounds , primarily c 11 and higher alkylaromatics , being withdrawn as a bottoms stream via conduit 172 . this column may be reboiled by xylene column bottoms in conduit 270 , as discussed above . overhead vapor from columns 130 and 170 also may generate steam respectively via conduits 230 and 271 as indicated , with condensed liquids either serving as reflux to each column or as net overhead respectively in streams 131 or 171 . the c 9 + aromatics from heavies column in conduit 171 is combined with the toluene - containing overhead contained in conduit 127 as feed to transalkylation reactor 140 to produce a transalkylation product containing xylenes . the transalkylation product in conduit 141 is stripped in stripper 142 to remove gases in conduit 143 and c 7 and lighter liquids which are returned via conduit 144 to extractive distillation 120 for recovery of light aromatics following stabilization in isomerate stripper 166 . bottoms from the stripper are sent in conduit 145 to benzene column 123 to recover benzene product and unconverted toluene . the first and second c 8 - aromatics streams provided by xylene columns 130 and 133 , containing para - xylene , meta - xylene , ortho - xylene and ethylbenzene , pass via conduit 131 and 136 to xylene - isomer separation process 150 . the description herein may be applicable to the recovery of one or more xylene isomers other than para - xylene ; however , the description is presented for para - xylene for ease of understanding . the separation process operates via a moving - bed adsorption process to provide a first mixture of para - xylene and desorbent via conduit 151 to extract column 152 , which separates para - xylene via conduit 153 from returned desorbent in conduit 154 . extract column 152 preferably is operated at an elevated pressure , at least about 300 kpa and more preferably about 500 kpa or higher , such that the overhead from the column is at sufficient temperature to reboil finishing column 155 via conduit 256 or deheptanizer 164 via conduit 265 . heat supplied for reboiling duty via conduits 256 and 265 results in the condensation of the extract in these streams which is either or both refluxed to column 152 ( not shown ) or sent as a net stream in conduit 153 to finishing column 155 . the para - xylene is purified in finishing column 155 , yielding a para - xylene product via conduit 156 and light material which is returned to benzene column 123 via conduit 157 . a second mixture of raffinate , as a non - equilibrium blend of c 8 aromatics , and desorbent from separation process 150 is sent via conduit 158 to raffinate column 159 , which separates a raffinate to isomerization in conduit 160 from returned desorbent in conduit 161 . the raffinate column may be operated at higher pressure to generate steam via conduit 260 or to exchange heat in other areas of the complex ; condensed liquids from such heat exchange either serve as reflux to the raffinate column or as net overhead in conduit 160 . recovered desorbent in conduits 154 and 161 and net finishing column bottoms may heat the incoming feed stream in conduit 110 via conduits 213 and 212 , respectively . energy savings are attainable through tailoring the equipment and operations around the raffinate column 159 , as illustrated in fig2 a and 2b . these drawings illustrate modifications to selective portions of fig2 . fig2 a illustrates energy savings through pressurization of the raffinate column with provisions to avoid decomposition of the desorbent in the reboiler of the column . a pressurized raffinate column operating usually at more than about 400 kpa , and preferably approximately 500 kpa or higher , permits an overhead stream from the column to generate steam and / or exchange useful energy with other streams in an aromatics complex ; however , such pressurizations results in a temperature in the bottom of the column which could result in significant decomposition of the desorbent . fig2 a shows the section of the complex of fig2 pertaining to the lower section of high - pressure xylene column 133 and to the raffinate column 159 . here , at least a portion of the effluent from reboiler 237 is directed to a drum 240 which separates a vapor in conduit 242 from a liquid in conduit 241 which is returned to column 133 along with any remaining portion of the reboiler effluent in conduit 238 . the vapor in conduit 242 provides heat to reboiler 243 , maintaining peak film temperature below decomposition limits preferably using exchangers having enhanced nucleate boiling surface as discussed below . the overhead condenser preferably operates at a temperature to produce medium - pressure steam , yielding net non - equilibrium mixed xylenes in conduit 160 . fig2 b illustrates an alternative energy - saving method , focusing on the area of the raffinate column 159 of fig2 . the feed mixture of raffinate and desorbent in conduit 158 passes to a prefractionator 258 , which recovers overhead via condenser 261 a portion of the net mixed xylene stream via conduit 262 . the remaining xylenes plus desorbent pass via conduit 264 to a pressurized raffinate column 159 . overhead is at least partially condensed via conduit 265 in prefractionator reboiler 263 , returning via conduit 266 to the top of the raffinate column with the remainder of the mixed xylenes being recovered via conduit 160 . as in fig2 , the column is reboiled with overhead from the high - pressure xylene column in conduit 259 with net desorbent being returned to adsorption via conduit 161 as before . the raffinate , comprising a non - equilibrium blend of xylene isomers and ethylbenzene , is sent via conduit 160 to isomerization reactor 162 . in the isomerization reactor 162 , raffinate is isomerized to provide a product approaching equilibrium concentrations of c 8 - aromatic isomers . the product is passed via conduit 163 to deheptanizer 164 , which removes c 7 and lighter hydrocarbons and preferably is reboiled using overhead in conduit 265 from extract column 152 . bottoms from the deheptanizer passes via conduit 165 to xylene column 133 to separate c 9 and heavier materials from the isomerized c 8 - aromatics . overhead liquid from deheptanizer 164 is sent to stripper 166 , which separates light materials overhead in conduit 167 from c 6 and c 7 materials which are sent via conduit 168 to the extractive distillation unit 120 for recovery and purification of benzene and toluene values . pressures of deheptanizer 164 and stripper 166 are selected to exchange heat or generate steam in a manner analogous to the xylene columns discussed elsewhere in this specification . fig3 shows in more detail the heat exchange of the invention between parallel xylene distillation columns 130 and 133 . feed to the low - pressure xylene column 130 comprises bottoms from the toluene column via conduit 128 , clay - treated bottoms from the reformate splitter in conduit 116 , and purge c 8 aromatics in conduit 138 and may comprise other c 8 - aromatics - containing streams not suitable for processing in the high - pressure xylene column as well as a portion of the deheptanized stream 165 if appropriate for energy balances . the combined feeds of heavy reformate and toluene - column bottoms may contain heavy aromatics which are susceptible to degradation at high temperatures , and operating at a pressure lower than 800 kpa permits temperatures to be maintained in the bottom of the column and reboiler which avoid such decomposition . the low - pressure xylene column separates concentrated c 8 aromatics as overhead in conduit 131 from a high - boiling stream comprising c 9 , c 10 and heavier aromatics as a bottoms stream in conduit 132 . the overhead stream from column 130 may be used at least partially via conduit 230 of fig2 to generate steam or reboil other columns as discussed previously and thus be condensed to provide reflux to the column as well as the net overhead to xylene separation in conduit 131 . simultaneously , an isomerized c 8 - aromatics stream is passed via conduit 165 to high - pressure xylene column 133 ; this stream contains a lower concentration of heavy materials subject to decomposition than the feed to column 130 ; the column pressure is elevated with respect to that of the low - pressure xylene column according to the invention , as discussed previously , in order to effect energy savings through concomitantly higher temperatures which may be employed to exchange heat at useful levels . the temperature of the overhead vapor from the high - pressure xylene column 133 therefore is sufficient to provide useful energy to other services in an aromatics complex . as shown , the temperature of the overhead vapor is sufficient to reboil the low - pressure xylene column 130 in reboiler 135 , providing reflux to column 133 and a net stream in conduit 136 . a small net bottoms stream in conduit 138 preferably is sent to low - pressure column 130 for recovery of remaining c 8 aromatics . alternatively or in addition , the temperature of overhead vapor from high - pressure xylene column 133 is sufficient to generate steam useful for heating services or to reboil columns in other processing units . such steam is generated usually at a pressure of in excess of about 300 kpa , preferably at least about 500 kpa , and most preferably about 1000 kpa or higher . the overhead stream may be indirectly heat exchanged with a water circuit which feeds a steam drum . most usually , boiler feed water is heated in heat exchangers decoupled from the steam drum . multiple water circuits serving different exchangers are arranged in parallel with each other and feed a single steam drum to provide a steam product of a desired pressure for which only one set of instrumentation is needed . such steam systems are well known , and details can be added through such teachings as found in u . s . pat . no . 7 , 730 , 854 which is incorporated herein by reference . energy recovery according to the present invention , often involving close temperature approaches between process fluids , is improved through the use of exchangers having enhanced nucleate boiling surface . such enhanced boiling surface can be effected in a variety of ways as described , for example , in u . s . pat . no . 3 , 384 , 154 ; u . s . pat . no . 3 , 821 , 018 ; u . s . pat . no . 4 , 064 , 914 ; u . s . pat . no . 4 , 060 , 125 ; u . s . pat . no . 3 , 906 , 604 ; u . s . pat . no . 4 , 216 , 826 ; u . s . pat . no . 3 , 454 , 081 ; u . s . pat . no . 4 , 769 , 511 and u . s . pat . no . 5 , 091 , 075 ; all of which are incorporated herein by reference . such high - flux tubing is particularly suitable for the exchange of heat between the overhead of the second high - pressure xylene column and the reboiler of the first low - pressure xylene column or for the generation of steam from the xylene - column overhead . typically , these enhanced nucleate boiling surfaces are incorporated on the tubes of a shell - and - tube type heat exchanger . these enhanced tubes are made in a variety of different ways which are well known to those skilled in the art . for example , such tubes may comprise annular or spiral cavities extending along the tube surface made by mechanical working of the tube . alternately , fins may be provided on the surface . in addition the tubes may be scored to provide ribs , grooves , a porous layer and the like . generally , the more efficient enhanced tubes are those having a porous layer on the boiling side of the tube . the porous layer can be provided in a number of different ways well known to those skilled in the art . the most efficient of these porous surfaces have what are termed reentrant cavities that trap vapors in cavities of the layer through restricted cavity openings . in one such method , as described in u . s . pat . no . 4 , 064 , 914 , the porous boiling layer is bonded to one side of a thermically conductive wall . an essential characteristic of the porous surface layer is the interconnected pores of capillary size , some of which communicate with the outer surface . liquid to be boiled enters the subsurface cavities through the outer pores and subsurface interconnecting pores , and is heated by the metal forming the walls of the cavities . at least part of the liquid is vaporized within the cavity and resulting bubbles grow against the cavity walls . a part thereof eventually emerges from the cavity through the outer pores and then rises through the liquid film over the porous layer for disengagement into the gas space over the liquid film . additional liquid flows into the cavity from the interconnecting pores and the mechanism is continuously repeated . such an enhanced tube containing a porous boiling layer is commercially available under the trade name high flux tubing made by uop , des plaines , ill . fig4 illustrates examples of specific units within an aromatics complex in which direct heat exchange of overhead from one or more higher - temperature columns to reboilers of one or more lower - temperature columns could achieve energy savings , using numerical designations of processes from fig2 . overhead in conduit 134 from the high - pressure xylene column 133 has a temperature sufficient to provide energy to reboil extract column 152 via reboiler 235 , condensing the xylene overhead in conduit 236 for return to 133 as reflux or net overhead . the extract column may be pressurized such that overhead in conduit 256 has a sufficient temperature to reboil finishing column 155 , which preferably operates at vacuum pressure , via reboiler 257 , condensing extract column overhead in conduit 258 . as before , the product para - xylene is recovered in conduit 156 . fig5 summarizes a number , not exhaustive or exclusive , of direct heat - exchange possibilities related to fig2 . high - pressure xylene column 133 may provide heat to reboil one or more of low - pressure xylene column 130 , extract column 152 , and raffinate column 159 . the low - pressure xylene column 130 may provide heat to reboil extractive distillation column 120 . a pressurized extract column 152 may provide heat to reboil one or more of benzene column 123 and finishing column 155 . a pressurized raffinate column 159 may provide heat to reboil one or more of reformate splitter 114 , toluene column 126 , and deheptanizer 164 . fig6 summarizes nonexhaustive examples of indirect heat - exchange possibilities through the generation of medium - pressure steam . overhead streams 230 ( fig2 ) from the low - pressure xylene column 130 and 260 ( fig2 ) from the pressurized raffinate column 159 may generate medium - pressure steam in header 100 at 0 . 6 to 2 mpa , and preferably 0 . 7 to 1 . 5 mpa , which can be used to reboil one or more of reformate splitter 114 , extractive distillation column 120 and toluene column 126 with the added potential of exporting steam to other units . such generation and usage of steam can be considered as a supplement or substitute for other energy savings such as those described in fig5 . for example , the high - pressure xylene column 133 may provide heat to reboil the low - pressure xylene column 130 and extract column 152 , which in turn reboils the benzene column 123 and finishing column 155 . the combination of steam generation and direct heat exchange described above in fig6 was evaluated in terms of payback on investment . the base case is the facility described in fig1 and the case of the invention is the fig6 case as applied to the flow scheme in fig3 . the relative key parameters for the production of para - xylene are as follows :
2
to understand the structural features and benefits of the dental appliance or mouthguard 70 of the present invention , some anatomy will first be described . referring to fig1 and 1a , the user or athlete has a mouth 10 generally comprised of a rigid upper jaw 12 and a movable lower jaw 42 which are movably connected at the temporomandibular joint ( tmj ) 32 and 50 . more specifically , the rigid upper jaw 12 has gum tissue 14 within mouth 10 . gum tissue 14 , as well as the bone thereunder , supports anterior teeth ( incisors and canines ) 18 which have incisal or biting surfaces 19 . the gum tissues 14 and the bone thereunder also support posterior teeth ( molars and bicuspids ) 22 which have cusps or biting surfaces 26 . referring to one side of the human head , the temporal bone 28 is located upwardly and rearwardly of the upper jaw 12 and is in the range of { fraction ( 1 / 16 )} th to { fraction ( 1 / 32 )} nd inch thick . the articular eminence 30 forms the beginning of the fossae 32 or the socket of the temporomandibular joint 32 and 50 . rearwardly and posteriorly to the articular eminence 30 is located cartilage 34 . through the temporomandibular joint 32 and 50 pass the ariculo - temporalis nerve 36 and supra - temporo artery 38 . posteriorly to this structure is located the inner ear 40 . within the mouth is located tongue 39 and the roof or hard palate 41 , which terminates rearwardly into the soft palate and forwardly into the anterior palate or ruggae 43 . the ruggae 43 has a rib surface which is identifiable by the fingers or tongue 39 . the tongue touches the ruggae 43 during speech . the movable jaw or mandible 42 supports a bone covered by gum tissue 44 which further supports anterior teeth ( incisors and canines ) 46 with incisal or biting surfaces 47 and posterior teeth ( molars and bicuspids ) 48 with occlusal biting surfaces 49 . the condyle 50 of the lower jaw 42 forms the ball of the temporormandibular joint 32 and 50 . the anatomical structure is the same for both sides of the head . repeated impacts , collisions , blows , stress or forces exerted on the movable lower jaw 42 results in excessive wearing forced upon the condyle 50 and the cartilage , meniscus , or disc 34 — typically resulting in bone deterioration on the head of the condyle or slippage and compressive damage of the cartilage 34 . thereafter , the lower jaw 42 may be subject to irregular movement , pain , loss of comfortable range of movement , and clicking of the joint 32 and 50 . the ariculo - temporatis nerve 36 relates to both sensory and motor activity of the body . any impingement or pinching of this nerve 36 can result in health problems as previously mentioned . this supra - temporal artery 38 is important in that it provides blood circulation to portions of the head . impingement , pinching , rupture or blockage of this artery 38 will result in possible loss of consciousness and reduced physical ability and endurance due to the restriction of blood flow to portions of the brain . thus , it is extremely important to assure that the condyle 50 does not impinge upon the ariculo - temporalis nerve 36 or the supra - temporal artery 38 . it is also important to note that the temporal bone 28 is not too thick in the area of the glenoid fossae . medical science has shown that a sharp shock , stress or concussive force applied to the lower jaw 42 possibly could result in the condyle 50 pertruding through the glenoid fossae of the temporal bone 28 thereby causing death . this is a suture line ( growth and development seam ) in the glenoid fossae , resulting in a possible weakness in the fossae in many humans . this incident rarely , but sometimes , occurs with respect to boxing athletes . the mouthguard of the present invention is shown in the figures as reference number 70 . mouthguard 70 is generally u - shaped and is comprised of labial wall 72 , lingual wall 74 , which are upstanding from base 76 , and channel 78 is formed by this arrangement . specifically referring to fig2 - 4 , the mouthguard 70 generally comprises three layers of distinct materials 86 , 114 and 136 . the framework 86 is of a non - softenable , flexible material to assist in maintaining the shape of the heated mouthguard 70 and to permit the sizing of the mouthguard by way of twisting , expansion and contraction for variously configured mouths . the bite plate wedge 92 is part of the framework and permits displacement of the condyle and proper positioning of the lower jaw 42 . the traction pads 114 are elastomeric and therefore rubbery and grippable . the anterior impact brace or internal protective bumper 122 extends from the traction pads 114 while the external protective bumper 126 extends from the internal protective bumper 122 . the encapsulating material 136 is softenable and forms walls 72 and 74 and channel 78 . this portion of the mouthguard 70 softens when heated and permits custom fitting of the mouthguard 70 in a particular mouth configuration . the first shot of the mouthguard 70 is comprised of the non - softenable , flexible framework 86 which is suitably made of high - density polyethylene which exhibits a rigid character in that it holds its shape and can handle hot water because its melting point is 270 ° farenheit . the material also has excellent bonding qualities with other copolymers and is fda compliant . the polyethylene part number appropriate for the framework 86 is hd - 6706 from exxonmobil chemical company , p . o . box 3272 , houston , tex . 77253 - 3272 . the framework 86 suitably may have a connecting belvedere bridge 88 which spans across the anterior portion of the labial wall 72 . the bridge 88 then connects to cross - cantilever connectors 90 which connect to the occlusal pad plates or wedges 92 in various places to assure the relative stability of the framework 86 . the occlusal pad plates 92 shown in fig3 are shown to be thicker posteriorly than anteriorly . the pad plates or wedges 93 in fig4 are shown to be thicker anteriorly than posteriorly . the particular choice of plates or wedges 92 or 93 are dependent upon the physiology of the wearer of the mouthguard 70 suitably determined by medical assistance . the plates or wedges 92 have index openings 94 therethrough . the next injection molding shot is that of traction pads 114 , internal protective bumper 122 , protruding tab 124 , and external protective bumper 126 . the traction pads 114 contact and grip the occlusal biting surfaces 49 of the posterior teeth 48 of the lower jaw and must be composed of a durable , resilient material which deforms somewhat when the jaws are closed and cushion teeth 48 of the lower jaw 42 . the durable resilient material of this layer or second shot comprises a thermoplastic elastomer . the material may be dynaflex ®, part no . g2780 - 0001 from gls corporation , 833 ridgeview drive , mchenry , ill . 60050 . this material is suitable in that the teeth can interdigitate on the pads 114 and the material is chemically and bondably compatible , as well as being fda compliant and approved for mouthguards . the traction pads 114 have projecting interlocking knob or projections 116 which resemble a christmas tree . the bucket lip or retaining lid 120 and interlocking knobs 116 assure that the pads 114 are interlocked with the bite plate wedges 92 . forward of the traction pads 114 extend an anterior impact brace or internal protective elastomeric bumper 122 from which extends protruding tab 124 in an anterior fashion . a transverse external protective elastomeric bumper 126 is connected to tab 124 as they are all integrally molded . connectors for the tethers may be left port 128 or right port 130 . because the tether is meant to be securely and permanently fastened , nylon inserts 132 with an annular locking rib 134 are placed in the mold for their interlocking position within the external protective bumper 126 shown in detailed cross section in fig7 . the external bumper 126 also suitably supports an artistic logo 135 . the nylon material suitably may be part number n6650l from michael day enterprises , 960 seville road , wadsworth , ohio 44281 . the nylon material does not begin to melt until approximately 500 ° farenheit . the durable resilient material of the traction pads 114 and bumpers 122 and 126 may include in another embodiment a styrene block copolymer and ethylene vinyl acetate ( eva ). eva is available from a number of sources , such as elvax ® resins from dupont packaging and industrial polymers , 1007 market street , wilmington , del . 19398 . it is desirable that the durable resilient material have a shore “ a ” hardness of approximately 82 , which is very durable , yet rubbery . in another embodiment , the traction pads may have the styrene block copolymer mixed with polyolefin elastomer , which is a copolymer of ethylene and octene - 1 . a suitable copolymer is available under the trademark engage ® from dupont canada , inc ., p . o . box 2200 , streetsville , mississauga , ontario l5m 2h3 . another embodiment of the pads and bumpers may be a mixture of thermoplastic rubber and a polyolefin elastomer as described above . suitably thermoplastic rubbers are santoprene ® from advanced elastomer systems , l . p ., 388 south main street , akron , ohio 44311 and kraton ® thermoplastic rubber from shell oil company , houston , tex . kraton ® is composed of a styrene - ethylene - butylene - styrene block copolymer and other ingredients . the exact composition of santoprene ® is a trade secret . the third shot of the mouthguard 70 comprises an encapsulation material 136 which is suitably softenable and forms the walls 70 and 74 and channel 78 , as well as base 76 of the mouthguard 70 . thus , the softenable material does not encapsulate the traction pads 114 or bumpers 122 and 126 , but does encapsulate the entire framework 86 . the softenable outer fitting material 136 suitably comprises a mixture of exact ®, which is a plastomer , part no . 4023 from exxonmobil chemical company , p . o . box 3272 , houston , tex . 77253 - 3272 . the exact ® material is suitably blended 3 : 1 with a hydrocarbon resin called regalrez ®, part no . 1128 from eastman chemical company , 200 south wilcox , kingsport , tenn . 37660 . these materials exhibit low melting points , good density and chemically and bondably compatible with other materials , as well as being fda compliant for mouthguards . another combination of the softenable material 136 suitably comprises a mixture of eva and polycaprolactone . a suitable polycaprolactone is tone ®, part no . polymer p - 767 from union carbide corporation , 39 old ridgebury road , danbury , conn . 06817 - 0001 . the softenable material may consist of polycaprolactone alone as the possibility of ethylene vinyl acetate alone may be utilized . another embodiment of the softenable outer material 136 may be a mixture of polycaprolactone and polyolefin elastomer . preferably , the polyolefin elastomer is a copolymer of ethylene and octene - 1 . a suitable copolymer is available as engage ® from dupont canada , inc ., p . o . box 2200 , streetsville , mississauga , ontario l5m 2h3 . it is well known that illnesses , infection , tooth decay and / or periodontal disease is caused by bacteria , fungus , yeast and viruses . these microbials can grow and multiply on dental appliances when the appliances are being stored between uses , as well as when the appliance is being worn or used . an antimicrobial substance such as angion ® from angion technologies llc , 60 autobon road , wakefield , mass . 01880 may be blended with the framework 86 , traction pads 114 and bumpers 122 and 126 , along with the softenable material 136 . other antimicrobial substances which are non - toxic and free of heavy metal for resisting the growth of microbials may include chlorinated phenol ( e . g . 5 - chloro - 2 -( 2 ,- 4 - dichlorophenoxy ) phenol ), polyhexamethylene biguanide hydrochloride ( phmb ), doxycycline , hlorhexidine , metronidazole , thymol , eucalypol and methyl salycilate . triclosan ® from siba giegy of switzerland is also available . mouthguard 70 incorporating the antimicrobial agent during the manufacture of the mouthguard is achieved by incorporating the agent into the synthetic polymer master batch . the antimicrobial agent is suitably placed into the batch in a concentration as high as 10 % which will permit a let - down ratio resulting in final concentration of the antimicrobial agent and the dental appliance of about 0 . 005 to about 2 % by weight . the antimicrobial agent will survive molten temperatures of approximately 350 ° farenheit and thus the antimicrobial agent loses none of its biocidal properties in the formation of the mouthguard . to fit the mouthguard 70 to the user &# 39 ; s mouth , the mouthguard is placed in hot water at 211 ° farenheit ( i . e . water that has been brought to a boil and taken off the heat ) for about fifteen seconds . the mouthguard is then removed from hot water , and it will be very soft , but the framework 86 will hold the mouthguard in its general shape . excess water is allowed to drain off the mouthguard 70 by holding it with a spoon or a fitting tool . next , the wearer carefully places the mouthguard in the mouth so that the interior portion of the appliance 70 touches and covers the eye teeth and extends backwards towards the molars . next , the wearer bites down firmly on the appliance and pushes the tongue against the roof of the mouth . the cross - cantilever connectors guide the upper molars 22 in position on plates 92 . with a strong sucking motion , the wearer draws out all of the air and water from the mouthguard 70 . the projections or knobs 116 of the traction pads 114 will index to the cusps 26 of the molars 22 . with the thumb , the wearer presses the bridge 88 and lingual wall 74 tight against the mouth and then uses his hands and figures to press the outside of the cheeks against the appliance as the labial wall 72 moves to custom form the lingual and buccal or labial walls 72 and 74 , respectively . because there are no rigid lingual or labial walls in the appliance 70 , the mouthguard 70 will fit any width of molar 22 or mouth . the wearer retains the mouthguard in the mouth for at least one minute and , with the mouthguard still in the mouth , takes a drink of cold water . next , the wearer removes the mouthguard from the mouth and places it in cold water for about thirty seconds . next , referring to the tether 150 and anchor various arrangements , fig5 through 13 should be considered . tether 150 suitably may include an internal wire 152 with a plastic 154 outer casing . the ends of the tether 150 may have over - molded connectors 156 with a locking plug 158 and a lip 160 suitably of a christmas tree design . the locking plug 158 will almost permanently lock with the nylon insert 132 and its locking rib 134 , as shown in fig7 . attempts to remove the tether from either the left or right ports 128 or 130 will likely result in some destruction of the tether or external protective bumper 126 . the over - molded connector 156 suitably may be made of a thermoplastic polyurethane elastomer ( polyether ) marketed under the name pellethane ®, part no . 2363 - 55d , by ashland distribution company , 5200 blazer parkway , dublin , ohio 43017 . this material must be rigid and durable to secure to connection ports 128 and 130 in a permanent fashion once the user determines whether tethering should be on the left or right side of mouthguard 70 . football helmet 162 is shown in fig8 having a face mask 164 and chin strap catches , fasteners or male snap connectors or buckles 166 . face mask tether snap anchor 170 suitably secures to the buckle snaps 166 and has a port 172 with an internal annular locking rib 174 . the catch or buckle snap 176 may be utilized for helmets that do not have buckles 166 therein , such as a hockey helmet face shield 180 . catch 176 is secured to the face shield 180 with double - sided adhesive tape 178 shown in fig9 . in another embodiment , face mask tether clamp anchor 182 is shown in fig1 suitably having a port 184 with an annular locking rib internally to receive the over - molded connectors 156 of tether 150 . face mask tether cinch anchor 190 is another variation shown in fig1 having a port 192 with an internal annular locking rib . anchors 170 , 182 and 190 are suitably made of thermoplastic resin or ethylene / methacrylic acid copolymer such as surlyn ® 8150 from dupont . referring to fig1 and 13 , the lighted mouthguard tether and anchor assembly 200 is shown . the face mask tether snap anchor 202 has a logo lens 204 therein with a light 206 or suitably an led there below . a battery 208 sits within door switch 210 much like a hearing aid . upon closing the door switch 210 , the circuit is closed and the led lights the logo lens 204 . tether 212 may have internal fiberoptics 214 which will carry the light to the mouthguard logo lens 216 in the external bumper 126 . the present invention may be embodied in other specific forms without departing from the spirit or central attributes thereof ; therefore , the illustrated embodiments should be considered in all respects as illustrative and not restrictive , reference being made to the appended claims rather than to the foregoing description to indicate the scope of the invention .
0
referring to fig1 , and 3 , the invention , an attachment and reinforcement member for molded construction forms , comprises a piece of expanded mesh 10 with a central web portion 12 and extensions 14 bent at an angle 16 and extending in the same or opposite direction at a distance determined by the application of the invention with attachment members 18 of solid galvanized steel bent snugly on either side of the extensions 14 as shown in fig2 . it is to be understood that while the preferred embodiment of the present invention uses an expanded metal mesh , preferably steel , as the expanded mesh , other metals , such as aluminum , or even nonmetallic substances which provide high tensile strength may also be used as the expanded mesh 10 of the invention . likewise , the preferred embodiment of the invention uses solid metal , and most preferably , solid galvanized steel of a lighter gage than the expanded mesh 10 , as the attachment member 18 , but other materials with a solid surface , an appropriate thickness , and with sufficient strength characteristics may be incorporated into the present invention . initially , the dimensions of the flattened piece of expanded mesh 10 are nine inches by thirteen inches . the extensions 14 of the expanded mesh 10 are bent at angles 16 , leaving approximately one inch at the bent extensions , and a central web portion 12 of the invention as a rectangle of approximately nine inches by eleven inches . the dimensions of the attachment members 18 are approximately ten inches by two inches . the attachment members 18 are then folded along the longitudinal axis with one inch extending from either side of the center fold and applied to the extensions 14 of the expanded mesh 10 thus covering the mesh of the extensions 14 as shown in fig2 . care must be taken during the manufacture of the invention to ensure that the overall depth of the finished construction form 20 , shown in fig4 minus the overall dimension of the central web portion 12 , the bent extensions 14 , and the attachment members 18 covering the extensions 14 is between one thirty - second and one - eighth of an inch . this difference in dimensions must be slight for two reasons . if this difference does not fall within the aforementioned specifications , the metal or substance from which the expanded mesh 10 is composed , may scratch or otherwise mar the delicately machined aluminum molds when the invention is placed in the mold during the manufacture of the construction form , especially if the expanded mesh is expanded steel . the critical dimension of the invention , moreover , allows the attachment members 18 to extend to and lie within the plane of the outer surfaces 26 of the construction form 20 , and are thus easily visible . while it should be noted that the preferred embodiment of the present invention is incorporated into the molded polystyrene concrete form 20 , the dimensions of the invention can be altered to accommodate its use with other types and sizes of molded construction forms . for example , for a smaller polystyrene mold the initial expanded mesh 10 may be of the dimensions nine inches by eleven inches , such that when the extensions 14 are bent at angles 16 , a central web portion 12 would be a square of approximately nine inches by nine inches . furthermore , the extensions 14 bent at angles 16 to the expanded mesh 10 may be greater than or less than one inch , and correspondingly the dimensions of the attachment members 18 may be greater or less to accommodate the changes in dimensions of the extensions 14 , thereby creating a larger or a smaller attachment surface 18 on the outer surface 26 of the construction form 20 . thus , it is intended that the dimensions given are not limitations of the present invention , but rather merely provide an example of its application . the central web portion 12 , as shown in fig1 is an open mesh structure , preferably provided by the expanded metal technique , well known in the art , wherein longitudinal slits are perforated in sheet metal and the metal is stretched laterally to expand the slits resulting in a uniform pattern of staggered diamond shaped longitudinal openings 30 having a longer or major axis , and a shorter or minor axis . upon expansion of the metal , the longitudinal openings 30 are angularly configured , i . e ., the side of each diamond shaped longitudinal opening along the major axis is situated above the plane of the other side . this angular arrangement of the steel mesh is common in the building industry and is suitable for the application of plaster to the steel mesh . it is also common to the specialty steel sheet industry and is generically referred to as expanded metal . the expanded metal is then preferably flattened to form the expanded mesh portion 10 of the invention . the expanded mesh portion 10 , however , need not be flattened . the invention as embodied herein may accommodate the angular configuration of the central web portion 12 if the slots in the aluminum mold are sufficiently wide enough to allow for that additional depth or if replaceable inserts are placed in the mold to prevent the scratching and marring of the aluminum mold that may otherwise occur . the advantages presented by using the expanded metal technique eliminates the additional labor associated with punching the holes in the steel , and the waste resulting from the punching arcuate or polygonal holes as taught in the prior art . furthermore , the expanded metal is readily available . the expanded mesh 10 of the central web portion 12 also facilitates the flow of the construction material which can be quite viscous , such as concrete , within the cavities 22 of the molded construction form 20 more efficiently than the flow of wet concrete through the polygonal or arcuate holes embodied in the prior art . as mentioned , it is preferred that the attachment members 18 are constructed from a solid piece of a lighter gage of steel than is required for the central expanded steel mesh portion 10 of the invention . this arrangement is advantageous because the lighter gage steel is less expensive than the heavier gage steel used in the prior art , and the lighter gage steel is readily available in the building industry . the heavier steel construction of these devices taught in the prior art , moreover , makes penetration of the steel more difficult and , of course , more time consuming for the construction worker . the present invention overcomes this disadvantage of the prior art by providing a lighter gage steel surface for attachment making it easier to screw or otherwise apply materials to the finished form . the lighter gage steel of the attachment members , moreover , provides sufficient strength to function as a load bearing unit to support the finishing materials . the attachment members 18 , shown in fig2 and 3 , are folded over the extensions 14 , rather than integrally attached to the extensions 14 . this means of attachment presents several advantages over the prior art in which the attachment flanges are integrally connected with the a heavier steel and are manufactured from steel of the same gage . first , by merely folding the attachment members 18 , one does not have to spot weld or otherwise go through a time consuming and costly process required for integral construction . another advantage of the present invention addresses the orientation of the diamond - shaped longitudinal openings 30 within the central web portions 12 resulting from avoiding the integral construction of the cross members and attachment flanges presented in the prior art . in fig1 note that the major axis of the diamond - shaped longitudinal openings 30 are parallel to the line a -- a &# 39 ; and are perpendicular to the line b -- b &# 39 ;. if the invention were to use an integral construction technique whereby the interior portion of a solid piece of steel were slit and then expanded leaving extensions 14 , the orientation of the diamond - shaped longitudinal openings 30 would be rotated , and the major axis of the openings would be parallel to the line b - b &# 39 ;. additional strength is obtained by orientation of the major axis of the diamond - shaped longitudinal openings 30 along a - a &# 39 ; because the expanded mesh 10 has greater resistance to forces applied normally along b - b &# 39 ; than along a - a &# 39 ;. note that when the invention is embedded in the construction form 20 , as shown in fig4 the orientation of the major axis of the diamond - shaped longitudinal openings 30 is perpendicular to the plane of the outer surfaces 26 of the form 20 . when the construction forms 20 are stacked one upon the other for storage or shipping , stresses are applied along the line b - b &# 39 ; which provides greater resistance to compression and other forces than if the diamond - shaped longitudinal openings 30 were along axis a - a &# 39 ;. fig4 illustrates the incorporation of the invention into a construction form 20 . during manufacture of the construction form 20 , the invention comprising the central web portion 12 , with the extensions 14 of expanded mesh 10 bent away from the central web portion 12 and covered by the folded attachment members 18 of solid galvanized steel are placed in the grooves of the mold of the construction form 20 . in the preferred case of using an expanded polystyrene concrete form , the molds are closed and polystyrene beads are injected . the polystyrene beads expand around the invention and embed the present invention within the finished construction form 20 , as shown in fig4 , 6 , and 7 . the attachment members 18 extend to the outer surfaces 26 of the molded construction form 20 . as can be seen in fig4 and 6 , the attachment surfaces presented by the embedded attachment members 18 are easily visible . a template or otherwise marking the finished construction forms 20 to locate the attachment surfaces as taught in the prior art becomes unnecessary , and the present invention eliminates the costs of the required template and the labor associated with its use or otherwise locating the attachment surfaces . the attachment members 18 also visually define vertically where the concrete posts are located in the finished structure because the center of the concrete posts are located in the form cavity midway between each of the attachment members 18 , shown at 22 in fig4 , and 7 . this allows for a simplified means of locating where wall or adjoining floor members may be anchored into the concrete posts . most preferably , the present invention is inserted in five positions of the molded polystyrene concrete mold 20 , i . e ., at each end 28 of the form and at each of the three interior ribs 24 within the molded polystyrene concrete form 20 shown in fig4 and 5 . this placement of the invention provides increased reinforcement and added strength of the form 20 , especially at the ends 28 of the form which are the weakest parts of the structure . the use of the attachment and reinforcement member in the five placement positions strengthens the construction form 20 to withstand the strain and stress that occur during the pouring , settling , and curing of wet concrete . the construction form 20 incorporating the present invention is at least two times as strong as any other form presented by the prior art . the attachment members 18 , moreover , are conveniently located at the ends 28 and are placed in the center of each rib 24 , at intervals of the building standard of twelve inch centers per construction form 20 . each of the attachment members 18 offers an attachment surface area , as shown in fig4 . the use of the present invention provides one hundred and fifty percent more attachment surfaces for finishing materials to the construction form 20 than as taught in the prior art . as shown in fig5 the attachment members 18 all project towards the left side of the drawing , except for the unit placed at the far right end 28 of the form 20 . at these ends 28 , where the tongue of the form 20 extends to mate with the groove of the adjacent form 20 , the invention projects to the right in the drawing . when the forms 20 are fit together , as shown in fig6 by matching the tongues of one form with the grooves of the adjacent form , an effective attachment surface of two inch width is provided at the matching ends 28 by reversing the projection of this last unit . the figures , fig2 , and 7 , depict the extensions 14 in a channel configuration . one extension 14 , however , may be bent in an opposite direction from the other extension 14 , such that the angle 16 at which one extension 14 is bent will be substantially ninety degrees relative to the central web portion 12 , while the angle 16 of the extension 14 at the opposing end will be substantially two hundred seventy degrees relative to the central web portion 12 , in an essentially z - shaped configuration . the projection of each attachment member 18 , as shown in fig5 moreover , need not all be in the same direction . thus , any one or more of the attachment surfaces 18 may project in any direction and may be channel - or z - shaped so long as the attachment member 18 does not interfere with the tongue and groove arrangement of the construction forms 20 . it is important to note that there are five such units used in the polystyrene molded concrete form 20 because that is the number of grooves in the premanufactured molds of this particular construction form 20 . the invention may be adapted for use with any construction molds , and the number and dimension of the units is determined by the number of grooves in the molds , by the preferred building interval , and the number required to hold the construction form 20 together . thus , if only three units of the present invention were placed in the polystyrene molds , one on each end 28 and one at the center rib 24 , the attachment and bracing surfaces would be located at twenty - four inch centers . some molds allow for sixteen inch building centers . european and foreign construction forms have standard building increments based upon the metric system . thus , the design of the mold and the resulting construction form 20 will determine the number and dimension of the present invention used and incorporated into the form 20 . during construction of a building structure , the forms 20 are placed in a staggered and layered arrangement shown in fig6 . it is preferred that the form 20 that is placed above the underlying form 20 be offset at a distance of at least one integral number of the attachment and reinforcement member . in this fashion , the attachment members 18 are right above or below the attachment member 18 of the adjacent form 20 , as along line c - c &# 39 ; shown in fig6 . this placement not only permits alignment of the attachment members 18 along the building increments , but more importantly , allows alignment of the concrete cavities 22 , which is essential to the structural strength of the concrete structure being built . wet concrete is then poured into the cavities 22 of the forms 20 , directly from a concrete truck or more conveniently with a hose from a concrete pump for better control . after a sufficient length of time while the concrete is allowed to set up , another tier of construction forms 20 is built upon the previous and concrete is again poured . it is necessary to provide a bracing means , usually straps , wires or a rigid material , to maintain the construction forms 20 plumb , level , and straight while the concrete is poured into the forms 20 and while the concrete sets up . the attachment members 18 provide an easily locatable and a strong surface to attach the bracing means to the construction forms 20 while the concrete is poured and sets up . fig7 is an enlarged view of a construction form 20 incorporating the present invention . in this view , finishing material 32 has been applied to the outer surfaces 26 of the construction form 20 through the attachment member 18 by a screw or other penetrating device 34 . the steel web cross member 12 reinforces the construction form 20 at each rib 24 and at the ends 28 of the form 20 . the extensions 14 of the invention are shown covered with the attachment members 18 which extend to the outer surfaces 26 of the form 20 . a penetrating device 34 , such as a screw or nail , is shown , and penetrates and extends through the finishing material 32 and both sides of the folded piece of galvanized steel comprising the attachment member 18 . if necessary , more than one penetrating device 34 can be applied to each attachment member 18 . those skilled in the art will appreciate the ease with which these attachment members 18 can be located , and because , in the preferred embodiment of the invention , the attachment members 18 are of a lighter gage steel than the central web portion 12 , the ease with which the penetrating device 34 can be applied .
4
the present invention is broadly concerned with a novel method for treatment of an infection comprising administering to a host or subject in need thereof an effective amount of certain compounds represented by formula ( i ) ## str2 ## in which r 1 can be an h , oh , or 5 , nh 2 , nhr 6 or nr 6 r 7 ; r 2 and r 3 may be the same or different and can be an h , oh or or 5 ; r 4 can be conh 2 , conhr 6 , conr 6 r 7 , ch 2 nh 2 , ch 2 nhr 6 , ch 2 nr 6 r 7 , co 2 -- y -- nh 2 , co 2 -- y -- nhr 6 , or co 2 -- y -- nr 6 r 7 ; r 5 is a protected or unprotected glycosyl moiety comprising 1 - 10 monosaccharide units in which the glycosidic linkage at the anomeric carbon atom of each monosaccharide unit is independently alpha or beta ; nh 2 , nhr 6 , and nr 6 r 7 represent an unsubstituted amino group , monosubstituted amino groups , and a disubstituted amino group , respectively , in which r 6 and r 7 may be the same or different and represent a linear , branched or cyclic hydrocarbon group ( e . g ., an aliphatic group , a cyclic aliphatic group , an aromatic group or combinations of same ) comprising 1 - 15 carbon atoms optionally substituted with one or more unsubstituted , monosubstituted or disubstituted amino groups ; y represents a linear or branched alkylene group comprising 1 - 10 carbon atoms ; n is an integer from 0 - 10 , preferably 0 - 3 ; or its salts . the degree of substitution of the amino group is determined by the number of bonds to hydrogen emanating from the amino group . thus , an unsubstituted amino group has two n -- h bonds ( e . g ., -- ch 2 -- ch 2 -- nh 2 ). a monosubstituted amino group has one n -- h bond ( e . g ., -- ch 2 -- nh -- ch 2 -- or -- ch ═ nh ). a disubstituted amino group has none ( e . g ., ═ ch -- nr -- ch 2 -- or -- ch ═ n -- ch ═). by &# 34 ; substituted with one or more unsubstituted , monosubstituted or disubstituted amino groups &# 34 ; is meant that the hydrocarbon group comprising 1 - 15 carbon atoms contains at least one amino group either within the hydrocarbon backbone ( e . g ., -- ch 2 -- nh -- ch 2 --, -- ch 2 -- nr -- ch 2 --, -- ch ═ n -- ch 2 , -- ch ═ n -- ch ═, and the like ) or coming off the backbone ( e . g ., a primary amine , a secondary amine , a tertiary amine , an imine or the like , such as -- ch 2 -- ch 2 -- nh 2 , -- ch 2 -- ch (-- nh 2 )-- ch 2 --, -- ch 2 -- cr ( nh 2 )-- ch 2 --, -- ch ═ nh or -- cr ═ nh ). accordingly , such amino groups are capable of accommodating a charge , for example , in protic media ( e . g ., -- ch 2 -- nh 2 . sup .⊕ -- ch 2 -- or -- ch 2 -- ch 2 -- nh 3 . sup .⊕) or on formation of a quaternary ammonium salt ( e . g ., -- ch 2 -- ch 2 -- nme 3 . sup .⊕, wherein me stands for methyl ). the preferred compounds of the present invention include those that are able to accommodate two or more positive charges . yet others can accommodate three , four or even more positive charges . additional examples of selected amino group - containing moieties , that may be used as r 6 and / or r 7 , can be found in fig1 and 2 . as stated above , the group r 5 can be a protected or unprotected glycosyl moiety , which , in turn , may comprise 1 - 10 monosaccharide units ( e . g ., a monosaccharide , a disaccharide , a trisaccharide , etc .). in the present case , the term &# 34 ; monosaccharide &# 34 ; is any sugar residue or derivative thereof . the monosaccharide may , for example , be a hexose ( e . g ., d - allose , l - allose , d - altrose , l - altrose , d - fucose , l - fucose , d - glucose , l - glucose , d - mannose , l - mannose , d - gulose , l - gulose , d - idose , l - idose , d - galactose , l - galactose , d - rhamnose , l - rhamnose , d - talose , l - talose , and the like , or any deoxy form thereof , e . g ., a 2 - deoxyhexose , or any amino - substituted derivative thereof , e . g ., an aminosugar , such as d - glucosamine , l - glucosamine , d - galactosamine , l - galactosamine , etc .). puranoses , deoxyfuranoses , amino - substituted furanoses , and the like are also suitable , such as d - ribose , l - ribose , d - arabinose , l - arabinose , d - xylose , l - xylose , d - lyxose , l - lyxose , etc . furthermore , the protecting groups for the hydroxyl groups ( or amino groups , as the case may be ) can be chosen from a wide variety of protecting groups appropriate for a given set of conditions . these protecting groups , the choice of which will be apparent to one skilled in the art , may include , but are not limited to , benzyl , pentenyl , pivaloyl , trimethylsilyl , tert - butyldimethylsilyl , tert - butyldiphenylsilyl , triisopropylsilyl , acetyl , tetrahydropyranyl , benzoyl , c 1 - c 3 alkyl , isopropylidene , benzylidene , trifluoroacetyl , ( 2 - methoxyethoxy ) methyl , succinyl , orthoester , paramethoxybenzyl , allyl , and the like . the term &# 34 ; salt &# 34 ;, as used herein , denotes acidic and / or basic salts , formed with inorganic or organic acids and / or bases , preferably basic salts . while pharmaceutically acceptable salts are preferred , particularly when employing the compounds of the invention as medicaments , other salts find utility , for example , in processing these compounds , or where non - medicament - type uses are contemplated . salts of these compounds may be prepared by art - recognized techniques . examples of such pharmaceutically acceptable salts include , but are not limited to , inorganic and organic addition salts , such as hydrochloride , sulphates , nitrates or phosphates and acetates , trifluoroacetates , propionates , succinates , benzoates , citrates , tartrates , fumarates , maleates , methane - sulfonates , isothionates , theophylline acetates , salicylates , respectively , or the like . lower alkyl quaternary ammonium salts and the like are suitable , as well . in a specific embodiment , the group r 1 has the configuration beta . in another , the group r 1 has the configuration alpha . in a particular embodiment , at least one of r 1 , r 2 , and r 3 represents oh . in another embodiment , at least two of r 1 , r 2 , and r 3 represent oh , and in still another embodiment , all three of r 1 , r 2 , and r 3 represent oh . the present invention contemplates all other combinations of the various groups , including , but not limited to , embodiments in which r 1 and r 2 represent or 5 , and r 3 represents oh ; r 1 and r 3 represent or 5 , and r 2 represents oh ; or r 2 and r 3 represent or 5 , and r 1 represents oh . furthermore , a method is disclosed wherein r 6 together with the nitrogen atom to which it is attached derives from a polyamine . suitable polyamines include , but are not limited to , alkylene diamines , such as 1 , 3 - diaminopropane , and 1 , 12 - diaminododecane , and biogenic polyamines ( that is , those found in nature ), such as 1 , 4 - diaminobutane ( putrescine ), 1 , 5 - diaminopentane ( cadaverine ), n -( 4 - aminobutyl )- 1 , 3 - diaminopropane ( spermidine , an alkylene triamine ), and n -[ n -( 3 - aminopropyl )- 4 - aminobutyl ]- 1 , 3 - diaminopropane ( spermine , an alkylene tetraamine ). other polyamines are also suitable , including but not limited to , tetraethylenepentamine (&# 34 ; pentamine &# 34 ;), pentaethylenehexamine (&# 34 ; hexamine &# 34 ;) and the like , including branched aliphatic polyamines . with unsymmetrical polyamines , the present invention contemplates all other possible points of attachment of the polyamine to the steroid nucleus . for example , in spermidine , any of the three amino groups may be attached to the side chain or at the c - 3 position of the steroid nucleus . in selected embodiments of the present invention , the group r 1 or r 4 is neither an amino acid nor a peptide . in especially preferred embodiments of the present invention , the compound is selected from the group wherein n = 2 and , r 1 = α - oh , r 2 = h , r 3 = oh and r 4 = co - spermine ; r 1 = α - oh , r 2 = oh , r 3 = oh and r 4 = co - spermine ; r 1 = α - oh , r 2 = α - d - glc , r 3 = α - d - glc and r 4 = co - spermine ; r 1 = α - oh , r 2 = h , r 3 = α - d - glc and r 4 = co - spermine ; r 1 = α - oh , r 2 α - d - glc , r 3 = h and r 4 = co - spermine ; r 1 = α - oh , r 2 h , r 3 = oh and r 4 = co - pentamine ; r 1 = α - oh , r 2 = h , r 3 = oh and r 4 = co - hexamine ; r 1 = α - oh , r 2 = oh , r 3 = h and r 4 = co - spermine ; r 1 = α - oh , r 2 = oh , r 3 = h and r 4 = co - pentamine ; r 1 = α - oh , r 2 = oh , r 3 = oh and r 4 = co - pentamine ; r 1 = α - oh , r 2 = oh , r 3 = oh and r 4 = co - hexamine ; r 1 = α - oh , r 2 = α - d - glc , r 3 = α - d - glc and r 4 = co - hexamine ; r 1 = α - oh , r 2 = α - d - glc , r 3 α - d - glc and r 4 = co - pentamine ; and r 1 = α - oh , r 2 = h , r 3 = h and r 4 = co - hexamine . particularly preferred compounds include 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( compound a ); 3α , 7α , 12α - trihydroxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( compound b ); 3α - hydroxy - 7α , 12α - di ( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( compound c ); 3α - hydroxy - 7 - deoxy - 12α -( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( compound d ); 3α - hydroxy - 12 - deoxy - 7α -( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( compound e ); 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 - triaza - 11 - aminoundecyl ) amide ( compound f ); 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ( compound g ); 3α , 7α - dihydroxy - 12 - deoxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( compound h ); 3α , 7α - dihydroxy - 12 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 - triaza - 11 - aminoundecyl ) amide ( compound i ); 3α , 7α , 12α - trihydroxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 - triaza - 11 - aminoundecyl ) amide ( compound j ); 3α , 7α , 12α - trihydroxy - 12 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ( compound k ); 3α - hydroxy - 7α , 12α - di ( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ( compound l ); 3α - hydroxy - 7α , 12α - di ( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 - triaza - 11 - aminoundecyl ) amide ( compound m ); and 3α - hydroxy - 7 , 12 - dideoxy - 5β - cholan - 24 - oic acid ( or lithocholic acid ), n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ( compound n ). it is of course preferred that the compounds have a degree of purity such that they are suitable for use as an anti - infective . further , the pure or substantially pure compounds are preferably employed in the methods of the present invention . it is understood that one or more compound ( s ) of the present invention may be employed in any of the methods described herein . the compounds represented by formula ( i ) are useful as anti - infective agents , having utility in inhibiting the growth of , including killing , microorganisms . the compounds are particularly useful as broad spectrum antibacterial agents , having activity against both gram - positive and gram - negative bacteria , and as antifungal agents , having activity against yeast , mold , or other types of fungi . thus , the compounds represented by formula ( i ) may be employed in utilities suitable for such antimicrobial or antifungal agents . the compounds represented by formula ( i ) may , for example , be used in treating a host infected with a bacterium or fungus , or in preventing infection of said host by said bacterium or fungus , comprising the step of administering to the host one or more compounds represented by formula ( i ) or a pharmaceutically acceptable salt thereof in an amount effective for prevention or treatment . treatment of such infections according to the present invention includes both mitigation as well as elimination thereof . hosts administered the compounds represented by formula ( i ) may be plants or animals , particularly animals such as dogs , cats and other domestic mammals and , especially humans . the dosage form and mode of administration , as well as the dosage amount , may be selected by one of ordinary skill in the art . the dosage amount will vary with the severity of the infection , and with the size and species of the host . exemplary daily dosages for an adult human are those within the range of from about 0 . 001 mg to about 1 , 000 mg / day , preferably about 0 . 01 mg to about 500 mg / day , most preferably about 0 . 1 mg to about 200 mg / day . in certain instances , the preferred ranges may be about 0 . 5 mg to about 100 mg / day , more preferrably about 1 mg to about 25 mg / day , and most preferably , about 1 mg to about 10 mg / day . in order to use a compound represented by formula ( i ) in the method for the therapeutic treatment of mammals including humans , in particular in treating infection , it is normally formulated in accordance with standard pharmaceutical practice as a pharmaceutical composition . the compounds represented by formula ( i ) may be administered in standard manner for the disease condition that one desires to treat . administration to a mammalian host may , for example , be oral , topical , rectal or parenteral . administration to a plant host may be accomplished by , for example , application to seed , foliage or other part of the plant , or to the soil . it may also be sprayed over surfaces and over a wide area to be treated . for these purposes the compounds of this invention may be formulated by means known in the art into the form of , for example , tablets ( including lozenges and granules ), dragees , pills , ampoules , capsules , aqueous or oily solutions or suspensions , emulsions , dispersible powders , suppositories and sterile injectable aqueous or oily solutions or suspensions . &# 34 ; pharmaceutical composition &# 34 ; means physically discrete coherent portions suitable for medical administration . &# 34 ; pharmaceutical composition in dosage unit form &# 34 ; means physically discrete coherent units suitable for medical administration , each containing a daily dose or a multiple ( up to four times ) or a sub - multiple ( down to a fortieth ) of a daily dose of the active compound in association with a carrier and / or enclosed within an envelope . whether the composition contains a daily dose , or for example , a half , a third or a quarter of a daily dose , will depend on whether the pharmaceutical composition is to be administered once or , for example , twice , three times or four times a day , respectively . advantageously , the compositions are formulated as dosage units , each unit being adapted to supply a fixed dose of active ingredients . tablets , coated tablets , capsules , ampoules and suppositories are examples of preferred dosage forms according to the invention . it is only necessary that the active ingredient constitute an effective amount , i . e ., such that a suitable effective dosage will be consistent with the dosage form employed in single or multiple unit doses . the exact individual dosages , as well as daily dosages , are determined according to standard medical principles under the direction of a physician or veterinarian . it should be understood that an effective dose of the compound useful in the present method may vary depending on whether the compound is being administered alone or in combination with a second compound . generally , the effective dose can decrease if the second compound of a combination also exhibits anti - infective activity , especially those anti - infective agents whose activity is augmented in the presence of the compounds disclosed for use in the invention . the active agents can also be administered as suspensions , solutions and emulsions of the active compound in aqueous or non - aqueous diluents , syrups , granulates or powders . diluents that can be used in pharmaceutical compositions ( e . g ., granulates ) containing the active compound adapted to be formed into tablets , dragees , capsules and pills include the following : ( a ) fillers and extenders , e . g ., starch , sugars , mannitol and silicic acid ; ( b ) binding agents , e . g ., carboxymethyl cellulose and other cellulose derivatives , alginates , gelatine and polyvinyl pyrrolidone ; ( c ) moisturizing agents , e . g ., glycerol ; ( d ) disintegrating agents , e . g ., agar - agar , calcium carbonate and sodium bicarbonate ; ( e ) agents for retarding dissolution , e . g ., paraffin ; ( f ) resorption accelerators , e . g ., quaternary ammonium compounds ; ( g ) surface active agents , e . g ., cetyl alcohol , glycerol monostearate ; ( h ) adsorptive carriers , e . g ., kaolin and bentonite ; ( i ) lubricants , e . g ., talc , calcium and magnesium stearate and solid polyethylene glycols . the tablets , dragees , capsules and pills comprising the active agent can have the customary coatings , envelopes and protective matrices , which may contain opacifiers . they can be so constituted that they release the active ingredient only or preferably in a particular part of the intestinal tract , possibly over a period of time . the coatings , envelopes and protective matrices may be made , for example , from polymeric substances or waxes . the active ingredient can also be made up in microencapsulated form together , with one or several of the above - mentioned diluents . the diluents to be used in pharmaceutical compositions adapted to be formed into suppositories can , for example , be the usual water - soluble diluents , such as polyethylene glycols and fats ( e . g ., cocoa oil and high esters , ( e . g ., c 14 - alcohol with c 16 - fatty acid ]) or mixtures of these diluents . the pharmaceutical compositions which are solutions and emulsions can , for example , contain the customary diluents ( with , of course , the above - mentioned exclusion of solvents having a molecular weight below 200 , in the presence of a surface - active agent ), such as diluents , dissolving agents and emulsifiers . specific non - limiting examples of such diluents are water , ethyl alcohol , isopropyl alcohol , ethyl carbonate , ethyl acetate , benzyl alcohol , benzyl benzoate , propylene glycol , 1 , 3 - butylene glycol , dimethylformamide , oils ( for example , ground nut oil ), glycerol , tetrahydrofurfuryl alcohol , polyethylene glycols and fatty acid esters of sorbitol or mixtures thereof . for parenteral administration , solutions and suspensions should be sterile , e . g ., water or arachis oil contained in ampoules and , if appropriate , blood - isotonic . the pharmaceutical compositions which are suspensions can contain the usual diluents , such as liquid diluents , e . g ., water , ethyl alcohol , propylene glycol , surface active agents ( e . g ., ethoxylated isostearyl alcohols , polyoxyethylene sorbitols and sorbitan esters ), polycrystalline cellulose , aluminum methahydroxide , agar - agar and tragacanth , or mixtures thereof . the pharmaceutical compositions can also contain bulking agents and preservatives , as well as perfumes and flavoring additions ( e . g ., peppermint oil and eucalyptus oil ), and sweetening agents , ( e . g ., saccharin and aspartame ). the pharmaceutical compositions will generally contain from about 0 . 0001 to 90 wt . %, preferably about 0 . 01 to 10 wt . % of the active ingredient by weight of the total composition . in addition to the active agent , the pharmaceutical compositions and medicaments can also contain other pharmaceutically active compounds . any diluent in the pharmaceutical compositions of the present invention may be any of those mentioned above in relation to the pharmaceutical compositions . such compositions may include solvents of varying molecular weight as the sole diluent . the active compound is administered perorally , parenterally ( for example , intramuscularly , intraperitoneally , subcutaneously , transdermally or intravenously ), rectally or locally , preferably orally or parenterally , especially perlingually , or intravenously . the dosage rate , e . g ., 0 . 001 to 200 mg / kg of body weight , will be a function of the nature and body weight of the human or animal subject to be treated , the individual reaction of this subject to the treatment , type of formulation in which the active ingredient is administered , the mode in which the administration is carried out and the point in the progress of the infection or interval at which it is to be administered . thus , it may in some case suffice to use less than a minimum dosage rate , while other cases an upper limit must be exceeded to achieve the desired results . where larger amounts are administered , it may be advisable to divide these into several individual administrations over the course of the day . in addition to the compounds of the present invention , the pharmaceutical composition of this invention may also contain , or be co - administered with , one or more known drugs selected from other clinically useful anti - infective agents . examples of such anti - infective agents include , for example , amikacin , bacitracin , candicidin , capreomycin , cephalosporins ( cefazolin , cephaloglycine , cephaloridine , cephalothin , cephapirin sodium , cephradine ), chloramphenicol , colistin ( polymyxin ), cycloserine , dactinomycin , erythromycin , fusidic acid , gentamicin , gramicidin , kanamycin , lincomycins ( clindamycin , lincomycin ), neomycin , oleandomycins ( oleandomycin , troleandomycin ), paromomycin , penicillins ( amoxicillin , ampicillin , carbenicillin , carbenicillin , indanyl ester , cloxacillin , dicloxacillin , hetacillin , methacillin , nafcillin , oxacillin , penicillin g ( benzylpenicillin ), penicillin v ( phenoxymetholpenicillin ), phenethicillin ), rifampin , spectinomycin , staphylomycin , streptomycins ( dihydrostreptomycin , streptomycin ), tetracyclines ( chlortetracycline , demeclocycline , deoxycycline , methacycline , minocycline , oxytetracycline , tetracycline ), tyrothricin , vancomycin , and viomycin . preferred anti - infective agents are those that exhibit augmented or enhanced activity in the presence of the compounds of the present invention , such as erythromycin . the anti - infective compounds provide action against specific organisms susceptible to them . examples of microorganisms that the compounds represented by formula ( i ) are believed to be active against include , but are not limited to alpha - streptococci , beta - streptococci , diplococcus pneumoniae , staphylococcus species , bacillus anthracis , clostridia spp ., corynebacterium xerose , haemophilus ducreyi , haemophilus influenzae , escherichia coli , klebsiella - enterococcus species , neisseria species , proteus mirabilis , salmonella typhosa , pseudomonas aeruginosa , histoplasma capsulatum , coccidioides immitis , candida species , blastomyces dermatitidis , rhondototorula , cryptococcus neoformans , sporothrix schenckii , mucor mucedo and aspergillus fumigatus . examples of infections , which may respond to treatment or which may be prevented by administration of the compounds represented by formula ( i ) include , but are not limited to , skin and soft tissue infections , genitourinary - tract infections , gastrointestinal infections , gonorrhea , respiratory infections , meningitis , aspergillosis , cryptococcosis ( torulosis ), north american blastomycosis , systemic candidiasis , coccidioidomycosis , histoplasmosis , zygomycosis and subacute bacterial endocarditis . the appropriate solid or liquid vehicle or diluent may be selected , and the compositions prepared , by methods known to one of ordinary skill in the art . prevention or treatment of simultaneous infections by more than one bacterium or fungus , or combinations thereof is , of course , contemplated . the compounds represented by formula ( i ) may also be employed as antimicrobial agents useful in inhibiting the growth of , including killing , microorganisms present on a surface or in a medium outside a living host . the present invention therefore provides a method for inhibiting the growth of at least one bacterium or fungus present on a surface or in a medium , comprising the step of contacting the surface or medium with one or more compounds represented by formula ( i ), or a salt thereof , in an amount effective for the inhibition . thus , the inventive compounds may be employed , for example , as disinfectants for surface treatments , such as disinfection of surgical instruments , or as preservatives for a variety of solid and liquid media susceptible to microbial growth . suitable amounts of the compounds may be determined by methods known to one of ordinary skill in the art . compositions comprising at least one compound represented by formula ( i ), or a salt thereof in an amount effective for inhibiting the growth of at least one bacterium or fungus , and a vehicle or diluent , are also provided by the present invention . the following examples further illustrate the invention , and are not intended to in any way limit the present claims . methyl - α - d - glucopyranose ( 100 g , 0 . 516 mol ) is suspended in benzyl chloride ( 400 ml , 3 . 5 mol ) with koh pellets ( 336 g , 6 mol ), and the mixture is stirred using a mechanical stirrer at 120 - 130 ° c . for 3 h . the reaction mixture is cooled and water ( 800 ml ) is added to dissolve the crystalline mass , which is extracted with ether ( 2 × 200 ml ). the combined organic layer is washed with water ( 2 × 500 ml ) and dried ( na 2 so 4 ). the solvents are removed by vacuum distillation to give the crude methyl 2 , 3 , 4 , 6 - tetra - o - benzyl - α - d - glucopyranoside for the next reaction . to a stirred solution of above crude compound in glacial acetic acid ( 700 ml ) at 110 ° c . is added 3n sulfuric acid ( 120 ml ) dropwise during 15 min . after 3 h the reaction mixture is cooled to room temperature and left over night for crystallization of product . the crystals are filtered , washed consecutively with water ( 4 × 500 ml ) and methanol ( 2 × 250 ml ), and air dried to afford 2 , 3 , 4 , 6 - tetra - o - benzyl - α - d - glucopyranose ( 115 g , 41 % overall two steps ) as a white powder ( mp 150 - 51 ° c ., lit . 151 - 152 ° c . ; see , perrine , t . d . et al . j . org . chem . ( 1967 ) 32 : 664 ). tlc ( etoac : hexane 3 : 7 ) r f 0 . 2 . ir ( kbr ): 3362 , 3030 , 2911 , 2863 , 1454 , 1357 , 1146 , 1088 cm - 1 . 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 38 - 7 . 10 ( m , 20h ), 5 . 21 ( d , j = 3 . 3 hz , 1h ), 4 . 98 - 4 . 44 ( m , 9h ), 4 . 25 ( m , 1h ), 3 . 72 - 3 . 50 ( m , 4h ). anal . calc . for c 34 h 36 o 6 : c , 75 . 53 ; h , 6 . 71 . found : c , 75 . 68 ; h , 6 . 80 . to a stirred solution of 2 , 3 , 4 , 6 - tetra - o - benzyl - α - d - glycopyranose ( 108 g , 0 . 2 mol ) and phenyl disulfide ( 53 g , 0 . 24 mol ) in dichloromethane ( 500 ml ) is added tri - n - butylphosphine ( 60 ml , 90 %, 0 . 22 mol ). after allowing the reaction mixture to stir at room temperature for 15 h , it is poured into a solution of saturated aqueous sodium bicarbonate ( 600 ml ) and stirred for 10 min . the organic layer is separated , washed with water ( 2 × 500 ml ), dried ( na 2 so 4 ) and concentrated . the oily residue is dissolved in hexane ( 500 ml ) and chilled to 0 ° c . to give phenyl 2 , 3 , 4 , 6 - tetra - o - benzyl - 1 - thio - d - glucopyranoside ( 75 g , 60 %) as a white solid ( mp 85 - 86 ° c ., lit . 84 - 85 ° c . for β - thio compound ; see , ferrier , r . j . et al . carbohyd . res . ( 1973 ) 27 : 55 ). tlc ( etoac : hexane 1 : 3 ) r f 0 . 6 . ir ( kbr ): 3061 , 3030 , 2900 , 2865 , 1584 , 1494 , 1453 , 1358 , 1125 , 1085 , 1070 , 1029 cm - 1 . 1 h nmr ( 300 mhz , cdcl 3 ): δ 7 . 70 - 7 . 00 ( m , 25h ), 4 . 90 - 4 . 40 ( m , 9h ), 3 . 80 - 3 . 40 ( m , 6h ). anal . calc . for c 40 h 40 o 5 s : c , 75 . 92 ; h , 6 . 38 , s , 5 . 06 . found : c , 75 . 99 ; h , 6 . 39 ; s , 5 . 12 . to a stirred cooled (- 78 ° c .) solution of phenyl 2 , 3 , 4 , 5 - tetra - o - benzyl - 1 - thio - d - glucopyranoside ( 130 g , 0 . 2 mol ) in dichloromethane ( 400 ml ) is added dropwise over a period of 20 min a solution of mcpba ( 74 %, 58 . 31 g , 0 . 25 mol ) in dichloromethane ( 300 ml ) the mixture is stirred and allowed to warm up to - 30 ° c . the mixture is then filtered . the filtrate is washed with saturated aqueous sodium bisulfite ( 2 × 300 ml ), sodium bicarbonate ( 2 × 400 ml ), brine ( 400 ml ) and water ( 2 × 400 ml ). the organic layer is dried ( na 2 so 4 ) and concentrated . flash chromatography ( ch 2 cl 2 : etoac 9 : 1 ) of the residue furnishes the above - referenced sulfoxide mixture ( 127 g , 95 %) as a white solid ( mp 120 - 122 ° c .) tlc ( etoh : ch 2 cl 2 1 : 9 ) r f 0 . 3 . ir ( kbr ): 3060 , 3030 , 2910 , 2867 , 1495 , 1450 , 1360 , 1210 , 1136 , 1092 , 1049 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 72 - 7 . 14 ( m , 25h ), 5 . 12 - 4 . 42 ( m , 9h ), 4 . 40 - 3 . 30 ( m , 6h ). anal . calc . for c 40 h 40 o 6 s : c , 74 . 04 ; h , 6 . 22 ; s , 4 . 93 . found : c , 74 . 10 ; h , 6 . 26 ; s , 4 . 99 . to a solution of methyl cholate ( 42 . 2 g , 0 . 1 mol ), p - anisoyl chloride ( 20 ml , 0 . 133 mol ) and dmap ( 1 g ) in pyridine ( 500 ml ) is stirred and refluxed for 8 h . additional p - anisoyl chloride ( 10 ml , 0 . 67 mol ) is added and stirred 12 h . the reaction mixture is concentrated , and the residue is dissolved in dichloromethane ( 600 ml ). the solution is washed consecutively with 1n hcl ( 2 × 500 ml ) and water ( 3 × 500 ml ), dried ( na 2 so 4 ) and the solvent allowed to evaporate . crystallization of the residue from etoac / hexane ( 1 : 1 ) furnishes the desired acid ester ( 40 g , 72 %) as a white solid ( mp 179 - 180 ° c .). tlc ( etoac : hexane 7 : 3 ) r f 0 . 7 . triflic anhydride ( 30 ml , 0 . 178 mol ) is added to cooled toluene ( 300 ml , - 78 ° c .) and stirred for 5 min . to this solution , the dried ( by azeotropic distillation from toluene ) sulfoxide from 1 . 3 ( 97 g , 0 . 1495 mol ) dissolved in toluene ( 300 ml ) is added dropwise . after 15 min of stirring , a solution of dried ( by azeotropic distillation with toluene ) 2 , 6 - di - ter - butyl - 4 - methyl - pyridine ( 30 . 8 g , 0 . 150 mol ) in toluene ( 100 ml ) is added to the reaction mixture and stirred for 10 min at - 78 ° c . to this reaction mixture , dried ( by azeotropic distillation with toluene ) acid ester from 1 . 4 ( 33 . 36 g , 0 . 06 mol ) in ch 2 cl 2 and toluene ( 1 : 1 , 200 ml ) is added dropwise . the reaction progress is monitored by tlc . the temperature of the reaction mixture is slowly brought to - 50 ° c . ( during 45 min ) and during this time the spot of acid ester from 1 . 4 on the tlc disappeared completely . the reaction mixture is poured into a saturated aqueous solution of sodium bicarbonate ( 1000 ml ) and stirred for 10 min . the organic layer is separated , and the aqueous layer is extracted with dichloromethane ( 2 × 100 ml ). the combined organic layers is washed with water ( 3 × 500 ml ), dried ( na 2 so 4 ) and concentrated . the residue purified by flash chromatography ( etoac : hexane = 1 : 9 to 1 : 4 ) to furnish the desired bis ( glycosylated ) acid ester ( 84 g , 87 %) as a white foam ( mp 46 - 48 ° c .). tlc ( etoac : hexane 1 : 3 ) r f 0 . 3 . ir ( kbr ): 3084 , 3062 , 3028 , 2936 , 2867 , 1735 , 1707 , 1605 , 1496 , 1453 , 1360 , 1321 , 1275 , 1254 , 1210 , 1165 , 1097 , 1073 , 1030 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 60 - 6 . 70 ( m , 43h ), 5 . 95 ( d , 1h , j = 9 hz ), 4 . 99 ( d , 1h , j = 3 . 6 hz ), 4 . 93 ( d , 1h , j = 6 hz ), 4 . 88 - 3 . 29 ( m , 31h ), 2 . 68 - 0 . 65 ( m , 37h ). fab ms : 1624 ( m + na ) + . anal . calc . for c 101 h 116 o 17 : c , 75 . 71 ; h , 7 . 30 . found , c , 75 . 59 ; h , 7 . 31 . to a stirred solution of the product from 1 . 5 ( 24 g , 15 mmol ) in thf ( 150 ml ), naoh ( 10 g , 250 mmol ) in 95 % ethanol ( 200 ml ) is added and refluxed for 48 h . the reaction mixture is then concentrated , and the residue is dissolved in ethyl acetate ( 300 ml ), washed with water ( 2 × 250 ml ), saturated aqueous sodium bicarbonate ( 2 × 300 ml ), brine ( 300 ml ) and dried ( na 2 so 4 ). solvent is evaporated and the resulting desired compound ( 18 . 5 g , 85 %) is used for the next step without further purification . tlc ( etoac : hexane 1 : 3 ) r f 0 . 4 . a cooled (- 10 ° c .) solution of diazomethane in ether ( 100 ml , generated from 5 . 35 g of diazalid , 25 mmol ) is added to a cooled (- 10 ° c .) solution of the product from 1 . 6 ( 18 . 5 g , 12 . 74 mmol ) in ether ( 100 ml ). after 1 h , excess diazomethane is destroyed by adding glacial acetic acid ( 2 ml ). the reaction mixture is washed consecutively with saturated aqueous sodium bicarbonate ( 2 × 400 ml ), brine ( 300 ml ), and water ( 300 ml ), dried ( na 2 so 4 ) and concentrated . the residue is purified by flash chromatography ( etoac : hexane 3 : 17 ) to furnish the desired ester ( 13 g , 70 %) as a gum . tlc ( etoac : hexane 1 : 3 ) r f 0 . 6 . ir ( neat ): 3450 , 2925 , 2866 , 1736 , 1453 , 1362 , 1158 , 1071 , 1030 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 50 ( m , 40h ), 5 . 10 - 3 . 40 ( m , 33h ), 2 . 40 - 0 . 71 ( m , 38h ). anal . calc . for c 93 h 110 o 15 : c , 76 . 08 ; h , 7 . 56 . found : c , 74 . 79 ; h , 7 . 50 . to a cooled ( 0 ° c .) solution of methyl bis ( glucosyl ) cholate from 1 . 7 ( 13 g , 8 . 87 mmol ) and pyridine ( 2 . 5 ml , 31 mmol ) in dichloromethane ( 50 ml ), triflic anhydride is added and allowed to stir for 20 min . to this mixture , a solution of sodium azide ( 2 . 6 g , 40 mmol ) in dmf / dmpu ( 1 : 1 , 250 ml ) is then added at - 20 ° c . the reaction mixture is allowed to warm up to room temperature , where it is stirred overnight . the solvents are evaporated , and the residue is dissolved in dichloromethane ( 200 ml ), washed with water ( 3 × 200 ml ), dried ( na 2 so 4 ), and concentrated . flash chromatography of the residue on silica ( etoac : hexane 3 : 17 ) furnished 10 g ( 75 %) of azide compound as a white solid ( mp 112 - 114 ° c .). tlc ( etoac : hexane 1 : 4 ) r f 0 . 6 . ir ( kbr ): 3085 , 3061 , 3029 , 2921 , 2867 , 2097 , 1735 , 1603 , 1495 , 1452 , 1360 , 1256 , 1207 , 1160 , 1091 , 1071 , 1031 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 37 - 6 . 84 ( m , 40h ), 5 . 15 ( d , 1h , j = 4 hz ), 4 . 95 ( d , 1h , j = 4 hz ), 4 . 86 - 4 . 26 ( m , 15h ), 4 . 08 - 3 . 40 ( m , 16h ), 3 . 62 ( s , 3h ), 2 . 60 - 0 . 71 ( m , 37h ), 1 . 02 ( d , 3h ), 0 . 89 ( s , 3h ) and 0 . 63 ( s , 3h ). fab ms : 1515 ( m + na ) + . anal . calc . for c 93 h 110 o 14 n 3 : c , 74 . 76 ; h , 7 . 43 ; n , 2 . 81 . found : c , 74 . 84 ; h , 7 . 40 ; n , 2 . 79 . a solution of compound azide of 1 . 8 ( 11 g , 7 . 38 mmol ) and ph 3 p ( 5 . 76 g , 22 mmol ) in 90 % aqueous thf ( 100 ml ) is stirred and refluxed for 48 h . the reaction mixture is concentrated , and the residue is purified by flash chromatograph ( ch 2 cl 2 and then ch 2 cl 2 : etoh = 98 : 2 to 9 : 1 ) to give the desired 3 - amino compound ( 6 g , 56 %) as a white solid ( mp 43 - 45 ° c .). tlc ( etoh : ch 2 cl 2 1 : 19 ) r f 0 . 15 . ir ( kbr ): 3418 , 2922 , 2868 , 1736 , 1496 , 1453 , 1362 , 1161 , 1071 , 1032 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 38 - 6 . 84 ( m , 40h ), 5 . 10 - 3 . 48 ( m , 33h ), 2 . 62 - 0 . 70 ( m , 37h ). anal . calc . for c 93 h 112 o 14 n : c , 76 . 08 ; h , 7 . 70 ; n , 0 . 95 . found : c , 75 . 82 ; h , 7 . 71 ; n . 0 . 89 . to a solution of the 3 - amino compound of 1 . 9 ( 14 . 65 g , 10 mmol ) in toluene ( 50 ml ) and ethanol ( 200 ml ) is added formic acid ( 15 ml ) and palladium hydroxide ( 20 %) on carbon ( 15 g ). the resulting mixture is stirred for 24 h under a hydrogen atmosphere at 40 psi . tlc indicated incomplete hydrogenolysis . additional formic acid ( 4 ml ) and catalyst ( 4 g ) is then added , and the hydrogenation reaction allowed to proceed for another 24 h . the reaction mixture is then filtered through sand over a membrane filter and concentrated . the filtrate is then mixed with ethyl acetate to form a precipitate . ( in some instances , the methanol solvent from the hydrogenation reaction may need to be removed .) the filtered precipitate is then dissolved in 25 ml deionized water and freeze - dried . flash chromatography gave 2 . 82 g ( 38 %) of the deprotected amino cholate ester as white foam ( mp 170 - 172 ° c ., decomp .). tlc ( meoh : ch 2 cl 2 : isopropylamine 2 : 2 : 1 ) r f 0 . 15 . ir ( kbr ): 3450 , 2932 , 1736 , 1595 , 1451 , 1381 , 1151 , 1023 cm - 1 . 1 h nmr ( cdcl 3 ): δ 5 . 05 ( d , 1h ), 4 . 80 ( d , 1h ), 3 . 91 - 3 . 10 ( m , 15h ), 2 . 50 - 0 . 58 ( m , 37h ). ms ( fab ): 746 ( m + h ) + . anal . calc . for c 37 h 63 o 14 n : c , 59 . 56 ; h , 8 . 52 ; n , 1 . 88 . found : c , 54 . 60 ; h , 8 . 47 ; n , 2 . 49 . the corresponding 3α - amino compound can be obtained from the 3β - hydroxy starting material similarly . the 3β - hydroxy starting material can be obtained , for example , by treatment of methyl cholate with diethyl azidodicarboxylate in the presence of formic acid and triphenyl phosphine with inversion of stereochemistry to provide the methyl 3β - o - formylcholate , which , subsequently , can be hydrolyzed or manipulated , as needed . to a solution of the acid ester of 1 . 5 ( 10 mmol ; see , above ) in toluene ( 50 ml ) and ethanol ( 200 ml ) is added formic acid ( 15 ml ) and palladium hydroxide ( 20 %) on carbon ( 15 g ). the resulting mixture is stirred for 24 h under a hydrogen atmosphere at 40 psi . ( additional formic acid and catalyst can be added , if desired , if tlc analysis reveals that the reaction is incomplete after the initial 24 h reaction period . a second 24 h reaction period can then be initiated .) the reaction mixture is then filtered through sand over a membrane filter and concentrated . the filtrate is then mixed with ethyl acetate to form a precipitate . ( some of the methanol solvent from the hydrogenation reaction may need to be removed .) the filtered precipitate is then dissolved in 25 ml deionized water and freeze - dried . subjecting the residue to flash column chromatography gave the title compound in ca . 38 % yield . 1 h nmr ( cd 3 od ): δ 0 . 71 ( s , 3h , 18 - h ), 0 . 90 ( d , 3h , 21 - h , j = 6 . 6 hz ), 0 . 93 ( s , 3h , 19 - h ), 1 . 0 - 2 . 6 ( m ), 3 . 2 - 3 . 4 ( m , 2h ), 3 . 55 ( s , 3h , co 2 ch 3 ), 3 . 65 ( m ), 3 . 76 ( s , 3h , anisoyl - 4 - methyl ), 4 . 83 ( d , 1h , anomeric h ), 5 . 02 ( d , 1h , anomeric h ), 6 . 87 ( d , 2h , anisoyl aromatic , j = 9 hz ), 7 . 92 ( d , 2h , anisoyl aromatic , j = 9 hz ). triethylamine ( 10 ml , 71 . 2 mmol ) is added to a stirred solution of the sodium salt of deoxycholic acid ( 15 g , 34 . 7 mmol ), n - hydroxysuccinimide ( 7 . 5 g , 65 . 2 mmol ) and 1 -( 3 - dimethylaminopropyl )- 3 - ethylcarbodiimide ( 13 . 2 g , 69 . 3 mmol , edc ) in dichloromethane . the mixture is stirred for 12 h . the reaction mixture is then diluted with water ( 150 ml ) and extracted twice with dichloromethane . the organic layers are combined , dried over mgso 4 , filtered , and concentrated under reduced pressure to provide a solid residue . the residue is recrystallized from ethyl acetate - petroleum ether to give 5 . 5 g ( 30 %) of product . selected 1 h resonances : ( 270 mhz , cdcl 3 ): δ 4 . 00 ( br s , 1h , c12 ), 3 . 6 ( m , 1h , c3 ), 1 . 03 ( d , 3h , c21 ), 0 . 9 and 0 . 68 ( s , 3h each , angular methyls of steroid ). 4 . synthesis of the deoxycholic acid - spermine conjugate ( comp . a of table 1 ) spermine ( 0 . 3 g , 1 . 18 mmol ) is added to a stirred solution of the activated ester of deoxycholate from example 3 ( 0 . 15 g , 0 . 28 mmol ) and triethylamine ( 0 . 1 ml , 0 . 71 mmol ) in dichloromethane . the mixture is stirred for 0 . 5 h and a precipitate is observed . the solids are filtered through a buchner funnel . the filtrate is washed with water ( 10 ml ). the organic layer is concentrated to give a residue ( 0 . 18 g ). the residue is acidified with methanolic trifluoroacetic acid . the resulting solution is purified by reverse phase chromatography to give 0 . 14 9 ( 80 %) of the steroid - polyamine conjugate . selected 1 h resonances : ( 270 mhz , cd 3 od ): δ 3 . 98 ( br s , 1h , c12 ), 3 . 55 ( m , 1h , c3 ), 3 . 4 ( br t , 2h , spermine methylenes next to amide linkage ), 3 . 0 ( br s , 10h , spermine methylenes except those next to amide ), 1 . 03 ( d , 3h , c21 ), 0 . 9 and 0 . 68 ( s , 3h each , angular methyls of steroid ). high resolution mass spectrometry confirmed the proper molecular weight . in the same fashion , other non - glycosylated amphiphatic steroidal compounds , including but not limited to cholic acid or chenodeoxycholic acid , may be conjugated to a polyamine molecule , including but not limited to ethylene diamine , diethylene triamine , spermidine , other polyalkylenepolyamines , and the like . to a stirred solution of the methylcholate product of example 2 , above , ( 15 mmol ) in thf ( 150 ml ) is added naoh ( 10 g , 250 mmol ) in 95 % ethanol ( 200 ml ). the reaction mixture is refluxed for 48 h . the reaction mixture is then concentrated , acidified with dilute hcl and the residue is dissolved in ethyl acetate ( 300 ml ), washed with water ( 2 × 250 ml ), saturated aqueous sodium bicarbonate ( 2 × 300 ml ), brine ( 300 ml ) and dried ( na 2 so 4 ). solvent is evaporated to provide the 7 , 12 - bis - α - perbenzylglucosylcholic acid product in 80 % yield . ( see , fig6 .) activation of the carboxylic acid group is carried out as follows . 6 . synthesis of the bis ( glycosylated ) cholic acid - spermine conjugate ( comp . c of table 1 ) via the activated acid triethylamine ( 120 μl , 0 . 8 mmol ) is added to a stirred solution of the cholic acid product of example 5 ( 0 . 3 g , 0 . 2 mmol ), n - hydroxysuccinimide ( 72 mg , 0 . 6 mmol ) and 1 -( 3 - dimethylaminopropyl )- 3 - ethylcarbodiimide ( 160 mg , 0 . 8 mmol ) in dichloromethane . the mixture is stirred for 12 h . after this time , the reaction mixture is diluted with water ( 50 ml ) and extracted twice with dichloromethane . the organic layers are combined , dried over mgso 4 , filtered , and concentrated under reduced pressure to provide a solid residue 0 . 33 g ( 96 %) of the activated ester . ( see , comp . 5 of fig6 .) to a stirred solution of the activated ester ( 0 . 15 g , 0 . 089 mmol ) and triethylamine ( 50 ml , 0 . 35 mmol ) in dichloromethane is added spermine ( 0 . 3 g , 0 . 61 mmol ). the mixture is stirred for 0 . 5 h and a precipitate is observed . the solids are filtered over a buchner funnel . the filtrate is washed with water ( 10 ml ). the organic layer is concentrated to give a residue ( 0 . 18 g ). the residue is acidified with methanolic trifluoroacetic acid . the resulting solution is purified by reverse phase chromatography to give 0 . 14 g ( 85 %) of the protected bis ( glycosylated ) cholic acid - spermine conjugate . in the same fashion , other glycosylated amphiphatic steroidal compounds , including but not limited to the mono -, di -, or triglycosylated forms ( as appropriate ) of cholic acid , 7 - deoxycholic acid , or chenodeoxycholic acid , may be conjugated to a polyamine molecule , including but not limited to ethylene diamine , diethylene triamine , spermine , spermidine , other polyalkylenepolyamines , and the like . a hydrogenation flask is charged with a solution of the protected bis ( glycosylated ) cholic acid - spermine conjugate ( 0 . 11 g , 0 . 06 mmol ; see , above ) in a mixture of methanol ( 20 ml ) and benzene ( 4 ml ) or thf , followed by pd ( oh ) 2 catalyst and formic acid ( 1 ml ) or hydrochloric acid . the reaction mixture is shaken under a hydrogen atmosphere at 50 psi for 40 h . the catalyst is filtered off with celite ®, and the solvent is removed by evaporation under reduced pressure . the product is purified over sephadex - lh - 20 gel , eluting with meoh , to give the desired bisglycosteroid - spermine conjugate ( comp . c ). 8 . synthesis of the 12α -( o - glucosyl ) deoxycholic acid - spermine conjugate ( comp . d of table 1 and comp . 6 of fig3 ) 8 . 1 . preparation of 3α - o - cbz - deoxycholic acid , methyl ester ( comp . 1 of fig3 ) a mixture of methyldeoxycholate ( 25 g , 61 mmol ), benzylchloroformate ( 17 . 0 g , 14 ml , 100 mmol ), dimethylaminopyridine ( 1 . 22 g , 10 mmol ), pyridine ( 30 ml ) and dioxane ( 150 ml ) are stirred at room temperature 3h , the additional amounts of the benzylchloroformate ( 12 . 0 g , 10 ml ) are added two times in 2 h to complete reaction . total amount of the benzylchloroformate is 41 . 0 g ( 34 ml ). the reaction mixture is poured into a separatory funnel , water ( 500 ml ) and ethyl acetate ( 300 ml ) are added . the organic layer is washed with water ( 500 ml × 2 ), dried over sodium sulfate , concentrated to give an oil . the product is purified on flash chromatography over silica gel ( ea - hexane 1 : 1 ) providing 24 . 0 g ( 73 % yield ) of comp . 1 as a thick oil . tlc ( ea : hexane 2 : 5 ) r f 0 . 65 . ir ( neat ): 3553 ( oh ), 2943 , 2869 ( ch ), 1742 ( c ═ o ), 1453 , 1389 , 1263 ( arom . ), 944 , 911 , 789 , 747 , 696 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 38 ( s , 5h ), 5 . 15 ( s , 2h ), 3 . 6 ( s , 3h ), 2 . 0 - 1 . 0 ( m , 24h ), 0 . 96 ( d , 3h , j = 6 hz ), 0 . 86 ( s , 3h ), 0 . 65 ( s , 3h ). 8 . 2 . preparation of 3α - o - cbz - 12α -( tetra - o - benzyl - o - glucosyl ) deoxycholic acid , methyl ester ( comp . 2 of fig3 ) triflic anhydride ( 2 . 08 g , 1 . 26 ml , 7 . 4 mmol ) is added to dry toluene ( 100 ml ), chilled to - 75 ° c . with acetone - dry ice bath , then phenylsulphenyl tetra - o - benzylglucopyranoside ( glucosulfoxide ) ( 5 . 06 g , 7 . 4 mmol ) is added dropwise , and in 10 minutes the 2 , 6 - tert - butyl - 4 - methyl - pyridine , and then 3 - o - cbz - deoxymethyl cholate 1 is added dropwise . when tlc showed the reaction is finished , it is quenched by sodium bicarbonate ( saturated solution , 200 ml ) at - 25 to - 30 ° c . the organic layer is dried over sodium sulfate , concentrated in vacuum at + 50 to + 60 ° c . the residue on flash chromatography ( ea - hexane , 20 % of ea ) afforded 2 ( 1 . 8 g , 29 %), as thick colorless oil . tlc ( ea - hexane 2 : 5 ) r f 0 . 70 . 1 h nmr ( cdcl 3 ): δ 7 . 3 ( m , 24h ), 4 . 4 - 5 . 0 ( m , 10h ), 3 . 6 ( s , 3h ), 3 . 4 - 4 . 0 ( m , 7h ), 1 . 0 - 1 . 95 ( m , 40h ), 0 . 92 ( d , 3h ), 0 . 82 ( s , 3h ), 0 . 56 ( s , 3h ). 8 . 3 . preparation of 12α -( o - glucosyl ) deoxycholic acid , methyl ester ( comp . 3 of fig3 ) the comp . 2 ( 1 . 6 g , 1 . 47 mmol ) is dissolved in ethyl acetate ( 15 ml ) and ethanol ( 50 ml ) together with catalyst pd ( oh ) 2 / c ( 500 mg ). using a parr shaker , the reaction mixture is pressurized under hydrogen at 50 psi for 24 h . the catalyst is filtered off , and the filtrate is evaporated to give a crystalline residue . the residue is purified by flash chromatography ( etoh - dcm 2 : 8 ) to afford comp . 3 ( 0 . 65 g , yield 72 %) as white crystals , m . p . 186 - 188 ° c . tlc ( etoh - dcm 2 : 8 ) r f 0 . 5 . ir ( neat ): 3510 , 2943 , 2585 , 1690 , 1452 , 1376 , 1148 , 1090 , 1050 cm - 1 . 1 h nmr : δ 5 . 05 ( d , 1h , j = 3 hz ), 3 . 9 ( s , 1h ), 3 . 7 - 3 . 8 ( m , 3h ), 3 . 6 ( s , 3h ), 2 . 2 - 1 . 4 ( m , 40h ), 0 . 95 ( d , 3h ), 0 . 90 ( s , 3h ), 0 . 72 ( s , 3h ). the methyl ester 3 ( 0 . 6 g , 1 . 1 mmol ) is refluxed in 5 ml of etoh - hydrazine hydrate ( 10 : 1 ) for 3 h . the solvent is evaporated , water ( 50 ml ) added , then distilled off to remove excess of hydrazine hydrate . the residue is azeotroped with toluene to afford a colorless crystalline hydrazide 4 ( 0 . 50 g , yield 81 %, m . p . 180 - 182 ° c .). tlc ( etoh - dcm 2 : 5 ) r f 0 . 15 . anal . calc . for c 30 h 52 n 2 o 8 : n 5 . 0 . found : n 4 . 81 . ir ( kbr ) 3393 , 2907 , 2863 , 1633 , 1543 , 1452 , 1372 , 1144 , 1016 , 704 cm - 1 . hydrazide 4 ( 0 . 5 g , 0 . 88 mmol ) is dissolved in 5 ml of 10 % hcl at + 1 to + 3 ° c . to give a clear solution . then nano 2 ( 0 . 14 g , 2 . 0 mmol ) in 5 ml of water is added dropwise at + 1 to + 5 ° c . to the reaction mixture to afford a precipitate of the azide 5 . this azide is unstable and could not be isolated in pure form . ir ( kbr ): 3485 - 3290 , 2928 , 2866 , 2270 , and 2134 ( con 3 ), 1690 , 1651 , 1451 , 1376 , 1147 , 1031 cm - 1 . tlc ( etoh - dcm 2 : 5 ) r f 0 . 35 . the precipitate of azide 5 is fast filtered off through a glass filter with porosity 40 - 60 μm and washed with ice water ( 10 ml ). while still wet , the precipitate of azide 5 is immediately transferred into a solution of spermine ( 0 . 5 g , 2 . 5 mmol ) and triethylamine ( 0 . 5 ml ) in 10 ml of water . the resulting mixture is stirred for 30 min , then heated up to 60 ° c . for 10 min , chilled to room temperature , and treated with acetic acid to a ph 4 . 5 - 5 . 0 . the clear solution of spermine derivative d is purified by flash chromatography using a reverse - phase column chp 20 in meoh - water . the spermine derivative d is eluted with a solvent gradient ranging from 50 - 100 % of meoh . the water - methanol fractions are combined and concentrated . the ph is adjusted to 3 . 5 - 3 . 0 with hcl . the clear solution is lyophilized to afford white , highly hygroscopic , crystalline spermine derivative d ( 0 . 37 g , yield 42 % based on hydrazide 4 , 180 ° c . sinks , 200 ° c . decomposition ). tlc ( meoh - dcm 2 : 8 ) r f 0 . 1 ; ( meoh - isopropylamine - dcm 2 : 2 : 6 ) r f 0 . 55 . ir ( kbr ): 3450 , 2943 , 1690 , 1452 , 1376 , 1148 , 1091 , 950 cm - 1 . 1 h nmr ( d 2 o ): δ 4 . 95 ( d , 1h , j = 3 hz ), 3 . 9 ( s , 1h ), 3 . 65 ( m , 3h ), 3 . 4 ( m , 3h ), 3 . 0 ( m , 3h ), 1 . 0 - 2 . 4 ( m , 60h ), 0 . 95 ( d , 3h ), 0 . 90 ( s , 3h ), 0 . 62 ( s , 3h ). anal . calc . for c 40 h 74 n 4 o 8 . 3hcl . 10h 2 o : c 46 . 7 , h 8 . 91 , n 5 . 45 , cl 10 . 2 . found : c 56 . 02 , h 8 . 91 , n 5 . 66 , c 9 . 47 . f . w . 739 . 5 . found : m + na + = 763 . 9 . synthesis of the 7α -( o - glucosyl ) chenodeoxycholic acid - spermine conjugate ( comp . e of table 1 or comp . 6 of fig4 ) 9 . 1 . preparation of 3α -( o - anisoyl ) chenodeoxycholic acid , methyl ester ( comp . 1 of fig4 ) a mixture of methyl chenodeoxycholate ( 5 . 0 g , 12 . 3 mmol ), anisoyl chloride ( 2 . 3 g , 2 . 0 ml , 13 . 5 mmol ), dimethylaminopyridine ( 0 . 8 g , 6 . 5 mmol ) in pyridine ( 15 ml ) is heated at 100 ° c . for 3 h . reaction mixture is poured into a separatory funnel , water ( 200 ml ) and ethyl acetate ( 300 ml ) is added . the organic layer is washed with 5 % hcl ( 100 ml ), water ( 200 ml ), sodium bicarbonate , and dried over sodium sulfate . sometimes a precipitate of the product appeared between layers . this precipitate may be filtered off and combined with the product that is obtained after evaporation of ethyl acetate . total amount is 5 . 2 g ( yield 78 %, m . p . 188 - 190 ° c . from etoh ). tlc ( ea - hexane 2 : 5 ) r f 0 . 6 . ir ( kbr ): 3513 ( oh ), 2938 , 2851 , 1730 ( cooch 3 ), 1712 ( anis - co ), 1607 , 1579 , 1509 , 1451 , 1279 , 1165 , 1100 , 963 , 770 cm - 1 . 1 h nmr ( cdcl 3 ): δ 8 . 03 ( d , 2h ), 7 . 96 ( d , 2h ), 4 . 85 ( s , 1h ), 3 . 85 ( s , 3h ), 3 . 65 ( s , 3h ), 2 . 0 - 1 . 0 ( m , 24h ), 0 . 96 ( d , 3h ), 0 . 90 ( s , 3h ), 0 . 66 ( s , 3h ). 9 . 2 . preparation of 3α -( o - anisoyl )- 7α -( tetra - o - benzyl - o - glucosyl ) chenodeoxycholic acid , methyl ester ( comp . 2 of fig4 ) triflic anhydride ( 2 . 1 g , 1 . 27 ml , 7 . 4 mmol ) is added to dry toluene ( 100 ml ), chilled up to - 72 to - 75 ° c . with acetone - dry ice bath . phenylsulphenyl glucoside ( 5 . 1 g , 7 . 4 mmol ) in 20 ml of dry toluene is added dropwise , then in 10 mins the 2 , 6 - di - tert - butyl - 4 - methyl - pyridine ( 1 . 52 g , 7 . 4 mmol ) in toluene ( 15 ml ) is added , and in 5 min the anisoyl derivate 1 ( 3 . 2 g , 5 . 9 mmol in 30 ml of dry toluene ) is added dropwise . when tlc showed the starting material disappeared , saturated solution of the sodium bicarbonate ( 150 ml ) is poured , and the mixture is transferred into a separatory funnel . the organic layer is washed with water ( 20 ml ), brine ( 50 ml ), dried over sodium sulfate , and concentrated to give a thick oil . it is purified by flash chromatography ( ea - hexane ); the product is eluted with 20 % ethyl acetate . the product ( 4 . 0 g , yield 62 %) is obtained as a thick colorless oil . tlc ( ea - hexane 2 : 5 ) r f 0 . 65 . ir ( neat ): 2950 , 2870 , 1690 , 1745 , 1610 , 1450 , 1275 , 1160 , 1050 , 970 , 775 cm - 1 . 9 . 3 . preparation of 3α -( anisoyl )- 7α -( o - glucosyl ) chenodeoxycholic acid , methyl ester ( comp . 3 of fig4 ) the above obtained oil ( 4 . 0 g , 3 . 7 mmol ) is dissolved in ethyl acetate ( 15 ml ) and ethanol ( 75 ml ), together with catalyst ( pd ( oh ) 2 / c , 2 . 0 g ). formic acid ( 2 . 0 ml ) is added to the mixture . the mixture is set up for hydrogenation in an 0 . 5 l parr &# 39 ; s apparatus at 50 psi for 24 h . the catalyst is filtered off , and the filtrate is evaporated to give a crystalline residue of 3 ( 1 . 8 g , yield 69 %), m . p . 258 - 260 ° c . ( from etoh ), no decomposition . tlc ( meoh - dcm 1 : 9 ) r f 0 . 35 . ir ( kbr ): 3439 ( oh ), 2863 , 1742 ( cooch 3 ), 1684 ( anis . co ), 1606 , 1284 , 1260 , 1022 , 967 , 773 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 9 ( d , 2h , j = 6 hz ), 6 . 8 ( d , 2h , j = 6 hz ), 4 . 95 ( d , 1h , j = 3 hz ), 4 . 75 ( s , 1h ), 3 . 80 ( s , 3h ), 3 . 58 ( s , 3h ), 3 . 3 - 3 . 5 ( m , 4h ), 2 . 0 - 1 . 1 ( m , 30h ), 0 . 92 ( s , 3h ), 0 . 88 ( d , 3h ), 0 . 62 ( s , 3h ). 9 . 4 . preparation of 7α -( o - glucosyl ) chenodeoxycholic acid , hydrazide ( comp . 4 of fig4 ) the methyl ester 3 ( 1 . 7 g , 3 . 0 mmol ) is refluxed in mixture etoh - hydrazide hydrate ( 20 ml + 6 ml ) for 2 h . the crystals of hydrazide 4 ( 0 . 45 g , m . p . 238 - 40 ° c .) that form are separated from solution at room temperature and filtered off . the mother liquid is concentrated , to afford an additional amount of hydrazide 4 ( 0 . 65 g ). total yield 1 . 1 g ( 70 %). tlc ( meoh - dcm , 2 : 8 ) r f 0 . 05 . ir ( kbr ): 3378 ( nh , oh ), 2927 , 1697 ( conh ), 1601 , 1260 , 1020 , 980 , 770 cm - 1 . hydrazide 4 ( 0 . 8 g , 1 . 4 mmol ) is dissolved in 10 ml 10 % hcl , chilled to + 3 to + 5 ° c ., then nano 2 ( 0 . 21 g , 3 mmol ) in 5 . 0 ml of water is added dropwise affording a precipitate of azide 5 . this compound is unstable and cannot be isolated as a pure substance . tlc ( etoh - dcm 2 : 8 ) r f 0 . 45 . ir ( kbr ): 3490 - 3300 , 2930 , 2850 , 2260 and 2133 ( con 3 ), 1700 , 1640 , 1450 , 1366 , 1147 , 1050 cm - 1 . the precipitate of azide 5 is fast filtered through a glass filter ( porosity 40 - 60 μm ) washed with ice water ( 5 ml ), and while wet is immediately transferred into a solution of spermine ( 0 . 5 g , 2 . 5 mmol ) and triethylamine ( 0 . 5 ml ) in 10 ml of water . the mixture is stirred for 30 min , then is heated up to 60 ° c . for 10 min , then is chilled to room temperature . the ph is adjusted to 4 . 5 - 5 . 0 using acetic acid . the insoluble impurities are filtered off , and the clear filtrate of spermide e is purified by flash chromatography using a reverse - phase column chp - 20 . the spermide e is eluted with a solvent gradient ranging from 40 - 100 % of meoh . the water - methanol fractions are combined , evaporated to dryness . water ( 10 ml ) and concentrated hcl ( 0 . 2 ml ) is added , and the clear solution is lyophilized to afford white , highly hygroscopic , crystalline spermide e ( 0 . 50 g , yield 42 % based on hydrazide 4 , m . p . 162 - 164 ° c . with decomp .). tlc ( meoh - i - proh - dcm 2 : 2 : 6 ) r f 0 . 6 . ir ( kbr ): 3447 , 2934 , 2865 , 1652 ( conh ), 1457 , 1379 , 1256 , 1026 , 772 cm - 1 . 1 h nmr ( d 2 o ): δ 4 . 85 ( d , 1h , j = 3 hz ), 3 . 5 - 3 . 8 ( m , 8h ), 3 . 5 ( m , 6h ), 3 . 1 ( m , 2h ), 2 . 9 - 3 . 0 ( m , 10h ), 2 . 1 - 1 . 0 ( m , 40h ), 0 . 796 ( m , 6h ), 0 . 551 ( s , 3h ). anal . calc . for c 40 h 74 n 4 o 8 . 3hcl . 10h 2 o : c 46 . 7 , h9 . 44 , n 5 . 45 , cl 10 . 37 . found : c 60 . 8 , h 8 . 97 , n 4 . 60 , cl 6 . 09 . f . w . 847 . 5 . mass - spectrum fab . m - hcl + h + = 815 . found : 815 . a mixture of dry cholic acid ( 8 . 16 g , 20 mmol ), dicyclohexeylcarbodimide ( 4 . 33 g , 21 mmol ) and n - hydroxysuccinimide ( 2 . 417 g , 21 mmol ) is stirred in dry methylene chloride ( 200 ml ) at room temperature for 6 h . the reaction mixture is filtered , and the filtrate concentrated . the residue is purified by flash chromatography through florosil ( etoh : ch 2 cl 2 1 : 19 ) giving 8 g ( 79 % yield ) of compound 1 as a white foam ( mp 92 - 95 ° c ). tlc ( etoh : ch 2 cl 2 1 : 19 ) r f 0 . 6 . ir ( kbr ): 3385 ( br ), 2933 , 2861 , 2118 , 1814 , 1783 , 1738 , 1376 , 1208 , 1073 cm - 1 . 1 h nmr ( cdcl 3 ): δ 3 . 94 ( s , 1h ), 3 . 81 ( s , 1h ), 3 . 42 ( m , 1h ), 2 . 82 ( br , 4h ), 2 . 30 - 1 . 00 ( m , 24h ), 0 . 99 ( d , 1h , j = 5 . 7 hz ), 0 . 862 ( s , 3h ), 0 . 67 ( s , 3h ). fab ms : 528 ( m + na ) + . 10 . 1 . preparation of 3α , 7α , 12α - trihydroxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( comp . b of table 1 or comp . 2 of fig5 ) to a stirred solution of spermine ( 303 mg , 1 . 5 mmol ) and triethylamine ( 1 ml ) in anhydrous methylene chloride ( 20 ml ), n - oxysuccinimidocholate 1 ( 505 mg , 1 mmol ) in anhydrous methylene chloride ( 20 ml ) is added dropwise during a 10 min period . the solution is then stirred for 3 h at room temperature . the reaction mixture is filtered and filtrate concentrated . the residue is purified by flash chromatography using chp - 20 reverse - phase resin ( water and then 75 % aqueous meoh ), affording 2 ( 360 mg , 52 % yield ) as a white foam ( mp 140 - 145 ° c .). tlc ( meoh : ch 2 cl 2 : isopropylamine 4 . 5 : 4 . 5 : 1 ) r f 0 . 4 . ir ( kbr ): 3350 ( br ), 2934 , 2859 , 1685 , 1644 , 1547 , 1449 , 1377 , 1234 , 1207 , 1078 , 1046 cm - 1 . 1 h nmr ( dmso - d 6 and 2 drops of d 2 o ): δ 3 . 78 ( s , 1h ), 3 . 61 ( s , 1h ), 3 . 40 - 2 . 80 ( m , 9h ), 2 . 42 - 0 . 77 ( m , 42h ), 0 . 55 ( s , 3h ). fab ms : 615 ( m + na ) + . a mixture of dry deoxycholic acid ( 2 . 356 g , 6 mmol ), dicyclohexeylcarbodimide ( 1 . 444 g , 7 mmol ) and n - hydroxy - succinimide ( 0 . 806 g , 7 mmol ) are stirred in dry methylene chloride ( 200 ml ) at room temperature for 6 h . the reaction mixture is filtered , and the filtrate concentrated . the residue is purified by flash chromatography through florosil ( etoh : ch 2 cl 2 1 : 19 ), affording 1 . 764 g ( 60 % yield ) of the title compound as a white foam ( mp 75 - 80 ° c .). tlc ( etoh : ch 2 cl 2 1 : 9 ) r f 0 . 5 . ir ( kbr ): 3364 ( br ), 2934 , 2862 , 1814 , 1783 , 1738 , 1655 , 1627 , 1449 , 1376 , 1208 , 1068 cm - 1 . 1 h nmr ( cdcl 3 ): δ 3 . 97 ( s , 1h ), 3 . 62 ( m , 1h ), 2 . 82 ( br , 4h ), 2 . 70 - 0 . 83 ( m , 30h ), 0 . 67 ( s , 3h ). fab ms : 512 ( m + na ) + . to a stirred solution of dodecan - 1 , 12 - diamine ( 600 mg , 3 mmol ) and triethylamine ( 1 ml ) in anhydrous methylene chloride ( 25 ml ), n - oxysuccinimidodeoxycholate ( 980 mg , 2 mmol ) in anhydrous methylene chloride ( 25 ml ) is added dropwise during 10 minute period . the contents are stirred for 14 h at room temperature . the reaction mixture is filtered , and the filtrate concentrated . the residue is purified by flash chromatography using chp - 20 reverse - phase resin ( 20 %, 40 %, 60 %, 80 % aqueous meoh and then meoh ) to give the title compound ( 575 mg , 50 % yield ) as a white foam ( mp 118 - 120 ° c .). tlc ( meoh : ch 2 cl 2 : isopropylamine 4 . 5 : 4 . 5 : 1 ) rf 0 . 8 . ir ( kbr ): 3365 ( br ), 2928 , 2857 , 1654 , 1647 , 1534 , 1449 , 1376 , 1044 cm - 1 . 1 h nmr ( cdcl 3 ): δ 3 . 97 ( s , 1h ), 3 . 62 ( m , 1h ), 3 . 21 ( q , 1h , j = 6 . 6 hz ), 2 . 70 - 1 . 00 ( m , 48h ), 0 . 98 ( d , 1h , j = 6 . 0 hz ), 0 . 90 ( d , 1h ), 0 . 67 ( s , 3h ). fab ms : 622 ( m + 2na ) + . 12 . preparation of bis ( glycosylated ) cholic acid - spermine conjugate ( comp . c of table 1 or comp . 7 of fig6 ) 12 . 1 . synthesis of 3α - hydroxy - 7α , 12α - di ( 2 &# 39 ;, 3 &# 39 ;, 4 &# 39 ;, 6 &# 39 ;- tetra - o - benzyl - 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n - oxysuccinimide ( comp . 5 of fig6 ) a solution of dry 7α , 12α - di -( 2 &# 39 ;, 3 &# 39 ;, 4 &# 39 ;, 6 &# 39 ;- tetra - o - benzyl - 1 &# 39 ; α - glucosyl )- 5 . beta .- cholan - 24 oic acid ( 1 . 452 g , 1 mmol ), n - hydroxysuccinimide ( 126 mg , 1 . 1 mmol ) and dcc ( 226 mg , 1 . 1 mmol ) in dry methylene chloride is stirred at room temperature for 3 h . the reaction mixture is filtered , and the filtrate concentrated . the residue is purified by flash chromatography through a column of florosil ( etoh : ch 2 cl 2 1 : 19 ) to give 1 . 40 g ( 90 % yield ) of comp . 5 as a white foam ( mp 63 - 65 ° c .). tlc ( etoh : ch 2 cl 2 1 : 19 ) r f 0 . 5 . ir ( kbr ): 3062 , 3030 , 2928 , 2863 , 2117 , 1813 , 1784 , 1740 , 1685 , 1496 , 1453 , 1363 , 1206 , 1070 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 90 ( m , 40h ), 5 . 10 - 3 . 10 ( m , 33h ), 2 . 80 ( br s , 4h ), 2 . 62 - 0 . 84 ( m , 30h ), 0 . 73 ( s , 3h ). fab ms : 1572 ( m + na ) + . 12 . 2 . preparation of 3α - hydroxy - 7α , 12α - di ( 2 &# 39 ;, 3 &# 39 ;, 4 &# 39 ;, 6 &# 39 ;- tetra - o - benzyl - 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( comp . 6 of fig6 ) to a stirred solution spermine ( 0 . 808 g , 4 mmol ) and triethylamine ( 3 ml ) in dry methylene chloride ( 50 ml ), comp . 5 ( 5 . 16 g , 3 . 33 mmol ) in methylene chloride ( 50 ml ) is added and stirred for 4 h . the reaction mixture is filtered , and the filtrate is washed with water ( 2 × 50 ml ), dried ( na 2 so 4 ), and concentrated . the residue is purified by flash chromatography through a column of chp - 20 reverse - phase resin ( water , then methanol ) to afford comp . 6 ( 4 . 9 g , 85 % yield ) as a white foam ( mp 58 - 60 ° c .). tlc ( meoh : ch 2 cl 2 : isopropylamine 4 . 5 : 4 . 5 : 1 ) r f 0 . 2 . ir ( kbr ): 3063 , 3030 , 2928 , 2863 , 1655 , 1628 , 1496 , 1452 , 1362 , 1208 , 1147 , 1070 , 1028 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 90 ( m , 40h ), 6 . 62 ( br s , 1h ), 5 . 03 - 3 . 20 ( m , 33h ), 3 . 00 - 0 . 86 ( m , 55h ), 0 . 72 ( s , 3h ). fab ms : 1659 ( m + na ) + . anal . calc . for c 102 h 132 o 14 n 4 . h 2 o : c , 74 . 16 ; h , 8 . 19 ; n , 3 . 35 . found : c , 73 . 53 ; h , 8 . 24 ; n , 3 . 72 . to a solution of comp . 6 ( 2 . 455 g , 1 . 5 mmol ) and 1n aqueous hcl ( 25 ml ) in thf ( 50 ml ), 20 % palladium hydroxide on carbon ( 2 g , perlman &# 39 ; s catalyst ) is added . the mixture is subjected to hydrogenalysis at 50 psi for 6 h . the reaction mixture is filtered through sand and membrane filter and concentrated . the residue is dissolved in water ( 5 ml ) and filtered . the filtrate is purified by flash chromatography through a column of chp - 20 reverse - phase column ( water , followed by meoh : water 1 : 9 ) to give 1 . 078 g ( 70 % yield ) of c as a white foam ( mp 83 - 85 ° c .). tlc ( trifluoroacetic acid : water 1 : 9 ) r f 0 . 35 . ir ( kbr ): 3365 ( br ), 2938 , 2867 , 1638 , 1629 , 1561 , 1545 , 1459 , 1150 , 1075 , 1048 , 1025 cm - 1 . 1 h nmr ( d 2 o ): δ 5 . 06 ( d , 1h , j = 3 . 6 hz ), 4 . 85 ( d , 1h , j = 3 . 6 hz ), 3 . 95 ( br s , 1h ), 3 . 78 - 2 . 88 ( m , 21h ), 2 . 28 - 0 . 76 ( m , 46h ), 0 . 64 ( s , 3h ). fab ms : 940 ( m + na ) + . anal . calc . for c 36 h 84 o 14 n 4 . 3hcl . 5h 2 o : c , 49 . 66 ; h , 8 . 52 ; n , 5 . 04 ; cl , 9 . 44 . found : c , 49 . 68 ; h , 8 . 60 ; n , 5 . 06 ; cl , 9 . 65 . to a solution of tetraethylenepentamine ( 0 . 378 g , 2 . 5 mmol ) and triethylamine ( 0 . 3 ml ) in dmf ( 5 ml ) is added dropwise over 10 min the n - oxysuccinimidodeoxycholate ( 1 . 0 g , 2 mmol ) in 5 ml of dmf . the solution is stirred overnight at room temperature , poured into water ( 20 ml ). the precipitate obtained is washed with cold water ( 50 ml ), dissolved in 10 ml of 2 % hcl , and filtered . the solution is poured over a chp - 20 reverse phase column and eluted using a 40 - 80 % meoh in water solvent gradient system to afford 1 . 1 g ( 72 % yield ) of the trihydrochloride , pentahydrate form of the title compound , as a white powder after lyophilization ( m . p . 130 - 132 ° c .). tlc ( meoh : i - prnh 2 : dcm 2 : 2 : 6 ) r f 0 . 6 . ir ( kbr ): 3419 , 2934 , 1642 ( conh --), 1553 , 1454 , 1038 cm - 1 . 1 h nmr ( d 2 o ): δ 3 . 88 ( s , 1h ), 2 . 9 - 3 . 3 ( m , 16h ), 1 . 2 - 2 . 4 ( m , 42h ), 0 . 88 ( d , 3h ), 0 . 78 ( s , 3h ), 0 . 55 ( s , 3h ). fab ms : 696 ( base . 3hcl + na + ). anal . calc . for c 32 h 61 n 5 o 3 . 3hcl . 5h 2 o : c 50 . 3 ; h 9 . 69 ; n 9 . 17 ; cl 13 . 95 . found : c 51 . 5 ; h 9 . 04 ; n 10 . 1 ; cl 10 . 9 . 13 . 2 . preparation of 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ( comp . g of table 1 ) to a solution of pentaethylenehexamine ( 0 . 58 g , 2 . 5 mmol ) and triethylamine ( 0 . 3 ml ) in dmf ( 5 ml ) is added dropwise over 10 min the n - oxysuccinimidedeoxycholate ( 1 . 0 g , 2 mmol ) in 5 ml of dmf . the solution is stirred overnight at room temperature , then poured into water ( 50 ml ) to give a precipitate . the liquid phase is decanted . the semi - solid precipitate is washed successively with cold 5 % naoh ( 10 ml × 2 ) and water ( 10 ml ), dissolved in 10 ml of 10 % acetic acid , and purified by flash chromatography through a chp - 20 reverse - phase column using a 40 - 100 % meoh in water solvent gradient system . the fractions containing product are combined , evaporated at reduced pressure , dissolved in 2 % aqueous hcl solution , and lyophilized to afford 0 . 75 g ( 42 % yield ) of the title compound as a white powder ( m . p . 140 - 142 ° c .). tlc ( meoh : i - prnh 2 : dcm 2 : 2 : 6 ) r f 0 . 65 . ir ( kbr ): 3425 , 2932 , 1770 ( cooh ), 1643 ( conh ), 1552 ( coo - ), 1454 , 1032 cm - 1 . 1 h nmr ( d 2 o ) δ 3 . 92 ( s , 1h ), 2 . 6 - 3 . 6 ( m , 20h ), 1 . 0 - 1 . 6 ( m , 30h ), 0 . 83 ( d , 3h ), 0 . 75 ( s , 3h ), 0 . 55 ( s , 3h ). fab ms : 863 ( m + h + ). anal . calc . for c 34 h 66 n 6 o 3 . 2hcl . 3acoh : c 55 . 8 ; h 9 . 28 ; n 9 . 70 ; cl 8 . 2 . found : c 59 . 0 ; h 9 . 40 ; n 8 . 3 ; cl 6 . 6 . to a solution of spermine ( 0 . 8 g , 2 mmol ) and triethylamine ( 0 . 3 ml ) in 5 ml of dmf is added dropwise the n - oxysuccinimidechenodeoxycholate ( 1 . 0 g , 2 mmol ) in 5 ml of dmf . the mixture is stirred overnight at room temperature , then poured into dcm ( 100 ml ). the precipitate of the hydroxysuccinimide is filtered , and the filtrate is evaporated to give a liquid phase , which is poured into water ( 100 ml ). the precipitate of the product is obtained . it is dissolved in meoh ( 5 ml ) and passed through a chp - 20 reverse - phase column . a 30 % meoh in water solvent system is used to elute the product . the solvent is removed by evaporation , and the residue is dissolved in 1 ml of trifluoroacetic acid . the resulting solution is diluted up to 10 ml with water , filtered , and the filtrate subsequently lyophilized to afford 0 . 9 g ( 50 % yield ) of a solid ( m . p . 96 - 100 ° c .). the product is soluble in water . a 5 % solution of the trifluoroacetate salt of the chenodeoxycholic acid - spermine conjugate is stable at room temperature over about 12 - 24 h , after which a precipitate of the base separates as a slurry . tlc ( meoh : i - prnh 2 : dcm 1 : 1 : 2 ) r f 0 . 7 . ir ( kbr ): 3406 , 2939 , 2869 , 1778 ( cooh ), 1680 ( conh --), 1553 , 1458 , 1196 , 834 , 722 cm - 1 . 1 h nmr ( d 2 o ): δ 3 . 75 ( s , 1h ), 3 . 4 ( s , 1h ), 2 . 8 - 3 . 15 ( m , 12h ), 2 . 2 - 1 . 2 ( m , 39h ), 0 . 9 ( d , 3h ), 0 . 86 ( s , 3h ), 0 . 55 ( s , 3h ). fab ms : ( m + na + )= 598 . anal . calc . for c 34 h 64 n 4 o 3 . 3cf 3 cooh : c 52 . 5 ; h 7 . 29 ; n 6 . 09 . found : c 53 . 5 ; h 7 . 20 ; n 4 . 95 . to a solution of the tetraethylenepentaamine base ( 1 . 90 g , 10 mmol ) and triethylamine ( 1 . 0 g , 10 mmol ) in 100 ml of dcm , n - oxysuccinimidechenodeoxycholate ( 2 . 46 g , 5 mmol ) in dcm ( 50 ml ) is added and the solution is stirred 48 h at room temperature . the reaction mixture is diluted with 100 ml of dcm , washed with water ( 2 × 100 ml ), dried over sodium sulfate and evaporated to dryness . the residue is dissolved in 25 ml of 10 % acetic acid , filtered and the clear filtrate is purified on chp - 20 column in meoh - water . at 40 %- 80 % of meoh the product is eluted . the combined fractions are acidified by 10 % hcl ( 5 ml ) and the methanol is distilled off under vacuum . the rest of the water solution is removed by lyophilization to give 2 . 84 g ( 77 % yield , m . p . 200 - 203 ° c . decomp .) of the pentaaminotetraethyleneamide of the chenodeoxycholic acid . tlc ( meoh : i - prnh 2 : dcm ) r f 9 . 8 . ir ( kbr ): 3350 , 2974 , 1665 , 1635 , 1551 , 1539 , 1460 , 1470 , 1377 , 1077 , 978 , 766 cm - 1 . 1 h nmr ( d 2 o )= δ 3 . 378 ( s , 1h ), 2 . 9 - 3 . 4 ( m , 16h ), 1 . 8 - 1 . 2 ( m , 39h ), 0 . 85 ( d , 3h ), 0 . 76 ( s , 3h ), 0 . 55 ( s , 3h ). fab ms : ( m + h + )= 564 . anal . calc . for c 32 h 61 n 5 o 3 . 4hcl . 2h 2 o : c 51 . 54 ; h 9 . 26 ; n 9 . 39 ; cl 19 . 06 . found : c 50 . 48 ; h 8 . 84 ; n 8 . 86 ; cl 19 . 7 . to a solution of the tetraethylenepentamine ( 0 . 8 g , 5 mmol ) and tea ( 0 . 3 g , 3 mmol ) in dcm ( 25 ml ) the n - oxysuccinimidecholate ( 1 . 0 g , 2 . 0 mmol ) is added . a clear solution is stirred at room temperature for 48 h , the reaction mixture is diluted with dcm ( 100 ml ), washed with cold water ( 20 ml ), dried over sodium sulfate and evaporated to dryness . the residue is dissolved in 20 ml of 5 % acoh . a purification is carried out on a chp - 20 reverse phase column in meoh - water . the product runs at 40 %- 80 % of meoh . the fractions containing target compound are combined , methanol is distilled off , and 10 ml of 10 % hcl is added . lyophilization gives 0 . 70 g ( 50 % yield ) of the pure substance , m . p . 135 - 140 ° c . tlc ( meoh : i - prnh 2 : dcm - 1 : 1 : 3 ) r f 0 . 8 . ir ( kbr ): 3406 , 2937 , 1640 ( c ═ o ), 1556 , 1453 , 1376 , 1023 cm - 1 . 1 h nmr ( d 2 o ): δ 3 . 8 ( s , 1h ), 3 . 65 ( s , 1h ), 3 . 0 - 3 . 3 ( m , 16h ), 2 . 0 - 1 . 1 ( m , 26h ), 0 . 78 ( d , 3h ), 0 . 72 ( s , 3h ), 0 . 48 ( s , 3h ). fab ms : ( m + h + ) 580 . anal . calc . for c 32 h 61 n 5 o 4 . 5hcl : c 50 . 4 ; h 8 . 66 ; n 9 . 18 ; cl 23 . 29 . found : c 47 . 27 ; h 8 . 31 ; n 8 . 57 ; cl 25 . 63 . 13 . 6 . preparation of 3α , 7α , 12α - trihydroxy - 12 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ( comp . k of table 1 ) to a solution of the pentaethylenehexamine ( 0 . 9 g , 5 . 5 mmol ) and triethylamine ( 0 . 3 g , 3 mmol ) in dcm ( 10 ml ) the neat n - oxysuccinimidecholate ( 1 . 0 g , 2 . 0 mmol ) is added with stirring at room temperature . the reaction mixture is stirred at room temperature for 48 h . at the end of this period , the reaction mixture turns into a semisolid , which is diluted with 150 ml of dcm , washed with cold water ( 2 × 50 ml ), dried and distilled to dryness , dissolved in 10 ml of 10 % acoh , filtered from insoluble material , and purified on a reverse - phase column chp - 20 with methanol - water . the product runs at 40 %- 70 % of methanol . the combined fractions containing product is distilled from methanol . afterwards , 10 % hcl ( 5 ml ) is added . after lyophilization , 0 . 96 g ( 55 % yield ) is obtained ( m . p . 230 ° c ., decomp .). tlc ( dcm : meoh : iprnh 2 - 5 : 1 : 1 ) r f 0 . 85 . ir ( kbr ): 3393 , 2937 , 1646 ( c ═ o ), 1550 , 1483 , 1376 , 1072 , 1028 , 774 cm - 1 . 1 h nmr ( d 2 o ): δ 3 . 83 ( s . 1h ), 3 . 67 ( s . 1h ), 3 . 1 - 3 . 5 ( m . 21h ), 2 . 0 - 1 . 4 ( m . 26h ), 0 . 78 ( d . 3h ), 0 . 68 ( s . 3h ), 0 . 48 ( s . 3h ). fab ms : ( m + h + ): 623 . anal . calc . for c 32 h 61 n 5 o 4 . 5hcl : c 50 . 4 ; h 8 . 66 ; n 9 . 18 ; cl 23 . 29 . found : c 47 . 27 ; h 8 . 31 ; n 8 . 57 ; cl 25 . 63 . to a stirred solution of pentaethylenehexamine ( 367 mg , 1 . 5 mmol ) and triethylamine ( 2 ml ) in dry methylenechloride ( 50 ml ), n - oxysuccinimide - 7α , 12α - di ( perbenzylglucosyl ) cholate ( 1 . 549 g , 1 mmol ) in methylene chloride ( 50 ml ) is added dropwise and stirred for 48 h . the reaction mixture is filtered , and the filtrate is concentrated . the residue is purified on flash chromatography over chp - 20 reverse phase resin ( eluants , water and then gradually increasing to 90 % methanol ; product is obtained from 90 % methanol in water fractions ) affords the title compound ( 950 mg , 57 % yield ) as a white foam ( m . p . 78 - 80 ° c .). tlc ( solvent - meoh : ch 2 cl 2 : isopropylamine 4 : 4 : 2 ) r f 0 . 1 . ir ( kbr ): 3500 ( br ), 3086 , 3061 , 3030 , 2929 , 2864 , 1699 , 1652 , 1453 , 1363 , 1155 , 1071 , 1028 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 90 ( m , 40h ), 5 . 03 - 3 . 10 ( m , 33h ), 2 . 90 - 0 . 66 ( m , 65h ). fab ms : 1674 ( m + na ) + . to a solution of the compound from above ( 333 mg , 0 . 2 mmol ) and 1n aqueous hcl ( 3 ml , 3 mmol ) in thf and water ( 2 : 1 , 30 ml ), 20 % palladium hydroxide on carbon ( 300 mg , perlman &# 39 ; s catalyst ) is added and the mixture is subjected to hydrogenolysis at 50 psi for 15 h . the reaction mixture is filtered through sand and membrane filter and then concentrated . the residue is dissolved in water ( 5 ml ) and filtered . the filtrate is purified on flash chromatography over chp - 20 reverse phase column ( water , followed by meoh : water = 1 : 19 , 1 : 4 and 2 : 3 ; product is found in 20 % methanol in water fractions ) to give 110 mg ( 40 % yield ) of the desired compound as a white foam ( mp 180 - 82 ° c .). tlc ( solvent - trifluoroacetic acid : water 1 : 9 ) r f 0 . 3 . ir ( kbr ): 3394 , 2934 , 2867 , 1652 , 1647 , 1636 , 1558 , 1541 , 1027 cm - 1 . 1 h nmr ( d 2 o ): δ 5 . 09 ( d , 1h , j = 3 . 6 hz ), 4 . 86 ( d , 1h , jjjj - 3 . 6 hz ), 3 . 95 ( brs , 1h ), 3 . 80 - 255 ( m , 15h ), 2 . 30 - 0 . 65 ( m , 56h ). fab ms : 970 ( m + na ) + . anal . calc . for c 46 h 86 o 14 n 6 . 4hcl : c 50 . 55 ; h 8 . 30 ; n 7 . 69 ; cl 12 . 97 . found : c 50 . 67 ; h 8 . 71 ; n 6 . 70 ; cl 11 . 65 . to a stirred solution of tetraethylenepentamine ( 285 mg , 1 . 5 mmol ) and triethylamine ( 2 ml ) in dry methylene chloride ( 50 ml ), n - oxysuccinimide - 7α , 12α - di ( perbenzylglucosyl ) cholate ( 1 . 549 g , 1 mmol ) in methylene chloride ( 50 ml ) is added dropwise and stirred for 48 h . the reaction mixture is filtered , and the filtrate is concentrated . the residue is purified on flash chromatography over chp - 20 reverse phase resin ( eluants , water and then gradually increasing to 90 % methanol ; product is obtained from 90 % methanol in water fractions ) to afford the title compound ( 1 g , 63 . 8 % yield ) as a white foam ( mp 74 - 76 ° c .). tlc ( solvent - meoh : ch 2 cl 2 : isopropylamine 4 : 4 : 2 ) r f 0 . 1 . ir ( kbr ): 3365 , 3086 , 3061 , 3029 , 2925 , 2864 , 1699 , 1653 , 1496 , 1453 , 1155 , 1070 , 1028 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 95 ( m , 40h ), 5 . 10 - 3 . 20 ( m , 33h ), 2 . 82 - 0 . 82 ( m , 57h ), 0 . 72 ( s , 3h ). fab ms : 1651 ( m + na ) + . to a solution of the above compound ( 486 mg , 0 . 3 mmol ) and 1n aqueous hcl ( 4 ml , 3 mmol ) in thf and water ( 2 : 1 , 30 ml ), 20 % palladium hydroxide on carbon ( 400 mg , perlman &# 39 ; s catalyst ) is added and the mixture is subjected to hydrogenolysis at 50 psi for 15 h . the reaction mixture is filtered through sand and membrane filter and concentrated . the residue is dissolved in water ( 5 ml ) and filtered . the filtrate is purified on flash chromatography over chp - 20 reverse phase column ( water followed by meoh : water = 1 : 19 , 1 : 4 and 2 : 3 ; product is found in 20 % methanol in water fractions ) to give 160 mg ( 50 % yield ) of the desired compound as white foam ( m . p . 151 - 53 ° c .). tlc ( solvent - trifluoroacetic acid : water 1 : 9 ) r f 0 . 3 . ir ( kbr ): 3390 , 2938 , 2869 , 1652 , 1647 , 1636 , 1541 , 1457 , 1251 , 1150 , 1073 , 1026 cm - 1 . 1 h nmr ( d 2 o ): δ 5 . 09 ( br s , 1h ), 4 . 86 ( br s , 1h ), 4 . 00 ( m , 2h ), 3 . 85 - 2 . 60 ( m , 16h ), 2 . 30 - 0 . 75 ( m , 49h ) and 0 . 66 ( s , 3h ). fab ms : 927 ( m + na ) + . anal . calc . for c 44 h 81 o 14 n 5 . 3hcl : c 52 . 14 ; h 8 . 35 ; n 6 . 91 ; cl 10 . 49 . found : c 52 . 41 ; h 8 . 75 ; n 5 . 21 ; cl 9 . 49 . 13 . 9 . preparation of 3α - hydroxy - 7 , 12 - dideoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetrodecyl ) amide ( comp . n of table 1 ) n - oxysuccinimidelithocholate ( 1 . 0 g , 2 . 1 mmol ) is added to pentaethylenehexamine ( 0 . 73 g , 3 . 2 mmol ) and triethylamine ( 0 . 21 g , 2 . 1 mmol ) in dcm ( 50 ml ). the reaction mixture is stirred at room temperature for 48 h , diluted with dcm ( 100 ml ), washed with water ( 2 × 100 ml ), dried , and the solvent evaporated . the residue is dissolved in 50 ml of 10 % acoh over 5 h with vigorous stirring . the cloudy solution is purified on a reverse phase column in meoh - water . after lyophilization , 1 . 1 g ( 60 % yield ) of the product is obtained ( m . p . 94 ° c .). tlc ( dcm : meoh : iprnh 2 5 : 1 : 1 ) r f 0 . 65 . ir ( kbr ): 3390 , 2933 , 2862 , 1648 ( c ═ o ), 1555 , 1402 , 1075 , 656 cm - 1 . 1 h nmr ( d 2 o ): δ 3 . 2 - 2 . 6 ( m , 19h ), 1 . 7 - 1 . 0 ( m , 29h ), 0 . 70 ( s , 6h ), 0 . 42 ( s , 3h ). fab ms : ( 597 ). anal . calc . for c 34 h 66 n 6 o 2 . 5acoh : c 59 . 3 ; h 9 . 66 ; n 9 . 44 . found . c 58 . 2 ; h 9 . 51 ; n 10 . 9 . a solution of dry 3 - β - azido - 7α , 12α - di -( 2 &# 39 ;, 3 &# 39 ;, 4 &# 39 ;, 6 &# 39 ;- tetra - o - benzyl - 1α - glucosyl )- 5β - cholan - 24 - oic acid ( 4 . 443 g , 3 mmol ), n - hydroxysuccinimide ( 406 mg , 3 . 5 mmol ) and dcc ( 722 mg , 3 . 5 mmol ) in dry methylene chloride is stirred at room temperature for 3 h . the reaction mixture is filtered , and the filtrate concentrated . the residue is purified by flash chromatography through a florosil column ( etoac : hexane 1 : 3 ) to give 4 g ( 80 % yield ) of the activated cholate ester as a white foam ( m . p . 64 - 66 ° c .). tlc ( etoac : hexane 3 : 7 ) r f 0 . 3 . ir ( kbr ): 3325 , 3088 , 3062 , 3030 , 2924 , 2867 , 2099 , 1815 , 1785 , 1742 , 1206 , 1070 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 90 ( m , 40h ), 5 . 02 ( q , 2h , j = 3 . 6 hz ), 4 . 90 - 3 . 42 ( m , 31h ), 2 . 80 ( br s , 4h ), 2 . 62 - 0 . 90 ( m , 30h ), 0 . 75 ( s , 3h ). to a stirred solution of spermine ( 0 . 303 g , 1 . 5 mmol ) and triethylamine ( 3 ml ) in dry methylene chloride ( 75 ml ), compound from 14 . 1 ( 1 . 579 g , 1 mmol ) in methylene chloride ( 75 ml ) is added and stirred for 4 h . the reaction mixture is filtered , and the filtrate is washed with water ( 2 × 50 ml ), dried ( na 2 so 4 ), and concentrated . the residue is purified by flash chromatography through a chp - 20 reverse - phase resin ( eluant : water and then methanol ) to afford the title compound ( 1 . 46 g , 86 % yield ) as a white foam ( m . p . 60 - 62 ° c .). tlc ( meoh : ch 2 cl 2 : isopropylamine 4 . 5 : 4 . 5 : 1 ) r f 0 . 5 . ir ( kbr ): 3432 ( br ), 3087 , 3062 , 3030 , 2925 , 2865 , 2098 , 1670 , 1663 , 1656 , 1640 , 1630 , 1496 , 1452 , 1364 , 1071 , 1028 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 90 ( m , 40h ), 6 . 30 - 6 . 10 ( m , 1h ), 5 . 04 - 3 . 10 ( m , 33h ), 2 . 80 - 0 . 83 ( m , 55h ), 0 . 73 ( s , 3h ). to a stirred mixture of the compound of 14 . 2 ( 0 . 999 g , 0 . 6 mmol ) and raney ni ( 500 mg ) in ethanol ( 10 ml ) is added dropwise over 10 min a hydrazine hydrate ( 0 . 2 ml , 4 mmol ) in ethanol ( 10 ml ). the mixture is stirred for 2 h , after which it is filtered . the filtrate is concentrated under vacuum ( aspirator pump ). the residue is washed with water ( 3 × 50 ml ) and dried under vacuum to give the desired 3 - amino compound ( 920 mg , 94 %) as a white foam ( m . p . 55 - 57 ° c .). tlc ( meoh : ch 2 cl 2 : isopropylamine 4 . 5 : 4 . 5 : 1 ) r f 0 . 5 . ir ( kbr ): 3415 ( br ), 3087 , 3062 , 3029 , 2925 , 2864 , 1669 , 1662 , 1654 , 1647 , 1630 , 1496 , 1453 , 1362 , 1086 , 1070 , 1028 cm - 1 . 1 h nmr ( cdcl 3 ): δ 7 . 40 - 6 . 90 ( m , 40h ), 6 . 30 - 6 . 10 ( m , 1h ), 5 . 00 - 3 . 00 ( m , 33h ), 2 . 80 - 0 . 78 ( m , 55h ), 0 . 66 ( s , 3h ). to a solution of compound of 14 . 3 ( 0 . 91 g , 0 . 56 mmol ) and 1n aqueous hcl ( 8 ml , 8 mmol ) in thf ( 25 ml ) and water ( 10 ml ) is added 20 % palladium hydroxide on carbon ( 0 . 9 g , perlman &# 39 ; s catalyst ), and the mixture is subjected to hydrogenolysis at 50 psi for 14 h . the reaction mixture is filtered through sand and a membrane filter , then concentrated . the residue is dissolved in water ( 5 ml ) and filtered . the filtrate is purified by flash chromatography through a chp - 20 reverse - phase column ( eluant : water , followed by 2 % meoh in water ) to give 260 mg ( 44 % yield ) of the title compound as a white powder ( m . p . 125 - 127 ° c .). tlc ( trifluoroacetic acid : water 1 : 9 ) r f 0 . 3 . ir ( kbr ): 3395 ( br ), 2940 , 1640 , 1630 , 1450 , 1150 , 1075 , 1047 , 1023 cm - 1 . 1 h nmr ( d 2 o ): δ 5 . 09 ( br s , 1h ), 4 . 87 ( br s , 1h ), 3 . 98 ( br s , 1h ), 3 . 78 - 2 . 88 ( m , 21h ), 2 . 60 - 1 . 00 ( m , 40h ), 0 . 91 ( s , 3h ), 0 . 82 ( d , 3h , j = 5 . 1 hz ), 0 . 66 ( s , 3h ). hence , the present invention also contemplates various compounds selected from non - glycosylated , monoglycosylated , and bis ( glycosylated ) bile acid - poly ( aminoalkylene ) or aminoarylene conjugates , including , in particular , 3α , 12α - dihydroxy - 7 - deoxy - 5α - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( deoxycholic acid - spermine conjugate ); 3α - hydroxy - 7α , 12α - di ( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( bis ( glycosylated ) cholic acid - spermine conjugate ); 3α - hydroxy - 12α -( 1 &# 39 ; α - glucosyl )- 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( 12α -( o - glucosyl ) deoxycholic acid - spermine conjugate ); 3α - hydroxy - 7α -( 1 &# 39 ; α - glucosyl )- 12 - deoxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ( 7α -( o - glucosyl ) chenodeoxycholic acid - spermine conjugate ); 3α , 7α , 12α - trihydroxy - 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ; 3α , 12α - dihydroxy - 7α - deoxy - 5β - cholan - 24 - oic acid , n -( 12 - aminododecyl ) amide ( deoxycholic acid - 1 , 12 - diaminododecane conjugate ); 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 12 - aminododecyl ) amide ; 3α - hydroxy - 7α , 12α - di ( 2 &# 39 ;, 3 &# 39 ;, 4 &# 39 ;, 6 &# 39 ;- tetra - o - benzyl - 1 &# 39 ;. alpha .- glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ; 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 - triaza - 11 - aminoundecyl ) amide ; 3α , 12α - dihydroxy - 7 - deoxy - 5β - cholan - 24 - oic acid , n -( 3 , 6 , 9 , 12 - tetraaza - 14 - aminotetradecyl ) amide ; 3α , 7α - dihydroxy - 12 - deoxy - 5 - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ; 3β - and 3α - amino - 7α , 12α - di ( 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide ; 3β - and 3α - amino - 7α , 12α - di ( 2 &# 39 ;, 3 &# 39 ;, 4 &# 39 ;, 6 &# 39 ;- tetra - o - benzyl - 1 &# 39 ; α - glucosyl )- 5β - cholan - 24 - oic acid , n -( 4 , 9 - diaza - 12 - aminododecyl ) amide , intermediates in their syntheses described herein , and their pharmaceutically acceptable salts . the results shown in table 1 demonstrate that the compounds of the present invention exhibit activity useful in the treatment or prevention of infections . the biological activity of the present compounds is demonstrated as follows . to demonstrate their anti - infective properties , the minimum inhibitory concentration ( mic ) for many of the novel compounds is obtained against a variety of antibiotic indicator strains of bacteria . antibiotic indicator strains escherichia coli strain 25922 , enterococcus faecalis 29212 , pseudomonas aeruginosa 27853 , and staphylococcus aureus 29213 are obtained from the american type tissue culture collection ( atcc ) in rockville , md . the cystic fibrosis isolate , pseudomonas aeruginosa 39324 , is also obtained from atcc . bacteria are routinely cultivated in cation - supplemented mueller - hinton broth ( camhb ) or agar at 37 ° c . the minimum inhibitory concentration ( mic ) of glycosylated and non - glycosylated steroidal polyamines for antibiotic indicator strains is determined by dissolving the test compounds in deionized water to a final concentration of 1 mg per ml . those compounds that are poorly soluble in water are dissolved in acetic acid , dried in a stream of nitrogen gas , and dissolved in deionized water to a final concentration of 1 mg per ml . these solutions are sterilized by filtration through 0 . 22 micron syringe filters . stock solutions of individual compounds are serially diluted ( two - fold ) in sterile camhb in 96 - well tissue culture dishes ( falcon ) and inoculated with antibiotic indicator strains that are prepared as described below . all compounds are tested in duplicate at concentrations that ranged from 1 . 56 to 200 μg per ml . antibiotic indicator strains are grown in 5 ml of camhb for 3 - 4 h at 37 ° c . with shaking ( 200 rpm ) on a new brunswick rotary shaker . bacteria are adjusted to a turbidity that matched a 0 . 5 mcfarland standard ( ca . 10 8 cfu per ml ) in sterile 0 . 85 % saline . these bacterial suspensions are diluted 1 : 20 in sterile 0 . 85 % saline and 10 μl ( ca . 5 × 10 5 cfu ) of each suspension is used to inoculate individual wells of a 96 well plate that contained different concentrations of the test compounds . following inoculation , the plates are sealed with plastic tape , incubated for 24 h at 37 ° c . and visually inspected for bacterial growth . camhb inoculated with each of the antibiotic test strains and uninoculated cambh plus each of the test compounds served as positive and negative controls . the mic is defined as the lowest concentration of a compound that completely inhibited visual evidence of bacterial growth . table 1__________________________________________________________________________anti - infective properties of compounds ## str3 ## mic ( μg / ml ) e . p . e . s . p . cmpd coli aeurginosa faecalis aureus aeruginosano . r . sup . 1 r . sup . 2 r . sup . 3 side chain 25922 27853 29212 29213 39324__________________________________________________________________________a α - oh h oh spermine 12 . 5 3 . 12 12 . 5 6 . 25 25b α - oh oh oh spermine 200 100 - 200 200 50 100c α - oh α - d - glc α - d - glc spermine 200 200 & gt ; 200 200 -- d α - oh h α - d - gln spermine 100 100 - 200 200 50 - 100 -- e α - oh α - d - glc h spermine 12 . 5 12 . 5 25 25 12 . 5f α - oh h oh pentamine 100 100 100 25 100g α - oh h oh hexamine 100 50 100 25 50 - 100h α - oh oh h spermine 25 12 . 5 3 . 12 6 . 25 50 - 100i α - oh oh h pentamine 25 50 25 12 . 5 50j α - oh oh oh pentamine 75 75 18 . 7 37 . 5 37 . 5k α - oh oh oh hexamine 75 75 18 . 7 37 . 5 75l α - oh α - d - glc α - d - glc hexamine & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 150m α - oh α - d - glc α - d - glc pentamine & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 150n α - oh h h hexamine & gt ; 200 200 200 50 200pentaethylene - -- -- -- -- & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 150hexaminespermine -- -- -- -- & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 150tetraethylene - -- -- -- -- & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 150pentaminecholic acid -- -- -- -- & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200sodium saltdeoxycholic -- -- -- -- & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200 & gt ; 200acid sodiumsalt__________________________________________________________________________ the nomenclature of compounds a to n has been provided earlier in this sepcification . the effect of the present compounds on the mic of erythromycin , gentamicin and vancomycin for antibiotic indicator strains is determined , as described below . stock solutions 1 - 2 mg / ml of test compounds are prepared in distilled water , filter - sterilized through a 0 . 22 μm filter and diluted in camhb to the desired starting concentration . aliquots of each test compound ( 0 . 1 ml ), at 2 × the final concentration , are added to the first rows of 96 well plates . the remaining wells of these plates are charged with 0 . 1 ml aliquots of each test compound at the desired final concentration . subsequently , 0 . 1 ml of solutions of erythromycin , gentamicin , or vancomycin , prepared in camhb , are added to the first rows of these plates and serailly diluted . the wells are inoculated in duplicate with each of four antibiotic indicator strains prepared as described previously above . the final concentrations of antibiotics tested in these experiments range from 0 . 185 - 250 μg per ml . plates containing each of the antibiotics serially diluted in camhb alone are also inoculated with antibiotic indicator strains to determine the mic of erythromycin , gentamicin and vancomycin in the absence of the compounds of the invention . the plates are sealed with plastic tape , incubated in for 24 h at 37 ° c ., visually inspected for bacterial growth . the mic of erythromycin , gentamicin and vancomycin for each of the indicator strains in the presence or absence of test compound is subsequently determined . the results observed are listed in table 2 below . table 2______________________________________augmentation of the antibacterial activityof erythromycin mic ( μg / ml ) erthromycin p . aeruginosa p . aeruginosaplus : e . coli 25922 27853 39324______________________________________no compound 125 & gt ; 250 & gt ; 250compound b . sup . a & lt ; 0 . 19 3 . 12 3 . 12compound d 0 . 39 0 . 39 6 . 25compound h & lt ; 0 . 39 3 . 12 6 . 25compound j 0 . 39 0 . 78 12 . 5compound n 0 . 78 6 . 25 25______________________________________ . sup . a all compounds tested at 25 μg / ml , except compound h , which is tested at 6 . 25 μg / ml . bacteria grow in camhb supplemented with each test compound at the indicated concentrations . fig8 a , 8b , 9a , 9b , 10a and 10b present selected results of the above - described augmentation experiments in the form of histograms . as shown in these figures , significant reductions in the mic ( μg / ml ) of erythromycin are obtained with the co - administration of this conventional anti - infective agent with selected compounds of the formula . comparable results are shown or expected for the other compounds of the formula . the purpose of the above description and examples is to illustrate some embodiments of the present invention without implying any limitation . it will be apparent to those of skill in the art that various modifications and variations may be made to the composition and method of the present invention without departing from the spirit or scope of the invention . all patents and publications cited herein are incorporated by reference in their entireties .
0
referring now to the drawings , and more particularly to fig1 ( a ), there is depicted a novel resistive structure 10 according to a first embodiment of the invention . in this embodiment , the resistive structure 10 is formed in a trough 11 , for example , formed in a substrate ( not shown ) having a layer of dielectric material conforming to the base and sidewalls . the trough structure 11 comprises a bottom portion of dielectric material 12 a and two parallel sidewall formations 12 b , 12 c of dielectric material . examples of insulative dielectric materials for the portions 12 a - 12 c include , but are not limited to : low - k materials , silk ®, an oxide , nitride , oxynitride or any combination thereof including multilayers , porous or non - porous inorganic and / or organic dielectrics formed by a deposition process such as cvd , pecvd , chemical solution deposition , atomic layer deposition and other like deposition processes . thus , the dielectric material may be comprised of sin , sio 2 , a polyimide polymer , a siloxane polymer , a silsesquioxane polymer , diamond - like carbon materials , fluorinated diamond - like carbon materials and the like including combinations and multilayers thereof . in the embodiment depicted in fig1 ( a ), resistive elements are formed within the trough structure 11 by utilizing a deposition process such as , for example , sputtering , plating , evaporation , chemical vapor deposition ( cvd ), plasma enhanced chemical vapor deposition ( pecvd ), chemical solution deposition , atomic layer deposition and other like deposition processes . the first resistor material 15 typically has a thickness , after deposition , of from about 50 to about 1000 å , with a thickness of from about 50 to about 500 å being more preferred and includes an outer conductor portion including lateral conductive film 115 a and two parallel vertical formations 15 b , 15 c of conductive material . the resistive structure further comprises an inner conductive portion 16 . the outer and inner conductor portions 15 a , 15 b , 15 c and 16 preferably comprise a resistive material including but not limited to : ta , tan , ti , tin , w , wn . in this structure , refractory metal films are ideal because of the high melting temperature , however , the material chosen may also be chosen for the tcr values . the conductive material forming outer conductor portions 15 a , 15 b , 15 c has a first sheet resistance value and a first tcr value and , the conductive material forming inner conductor portions 16 may have a second sheet resistance value and a second tcr value . the tcr values may be positive or negative depending on the type of resistor material used , and the sheet resistance is also dependent on the type of material used as well as its length and area . as shown in fig1 , the resistive structure 10 may be formed as part of an interlevel circuit or comprise part of an interconnect structure as shown connected to another wire level 19 by a conducting via 18 . as shown in fig1 ( a ), the via connects all conductive materials of the resistive element 10 . with respect to the embodiment depicted in fig1 ( b ), the thin film resistor 20 includes alternating conductive and insulating films in a trough configuration by repeating resistor material deposition and insulating material formation steps . in the structure depicted in fig1 ( b ), a plurality of alternating refractory metal films 25 a , b , c in trough configuration having lateral and vertical formations and alternating insulator films 22 a , b , c formed between the conductive layers is shown . as mentioned , this resistive element may be formed as part of an interlevel circuit or comprise part of an interconnect structure as shown connected to another wire level 29 by a conducting via 28 which is electrically connected to each of the conductor layers 25 a , b , c . it is understood that the via may alternately connect some or all of the conductors in the achievement of a desired design parameter , e . g ., resistance . in this structure , the plurality of film types may be chosen to have different thicknesses and widths to provide a desired matching of current carrying capability and tcr values . the insulator films and materials can also be chosen to provide the adhesion , thermal and mechanical desired features . in an alternate embodiment , a resistive structure 30 depicted in the cross - section view of fig1 ( c ) includes a structure similar to that depicted in fig1 ( b ) comprising alternating conductive and insulative films in a trough configuration . in the embodiment depicted in fig1 ( c ), the conductor layers 35 a , b , c having lateral and vertical formations each comprise a different material , e . g ., having different tcr values , and designed to achieve a net tcr value , e . g ., zero . in the resistive structure of fig1 ( c ), alternating insulator films 32 a , b , c are formed between the conductive layers with each layer being the same material including , but not limited to : an oxide , nitride , oxynitride or any combination thereof including multilayers , porous or non - porous inorganic and / or organic dielectrics formed by a deposition process , including low - k materials and silk ®. the alternating conductive layers include a resistive material including but not limited to : ta , tan , ti , tin , w , wn or other refractory metal films . as mentioned , this resistive element may be formed as part of an interlevel circuit or comprise part of an interconnect structure as shown connected to another wire level 39 by a conducting via 38 which is electrically connected to each of the conductor layers 35 a , b , c . it is understood that the via may alternately connect some or all of the conductor layers of the trough to the adjacent wire level in the achievement of a desired design parameter , e . g ., resistance . in another alternate embodiment , a resistive structure 40 depicted in the cross - section view of fig1 ( d ) includes a structure similar to that depicted in fig1 ( b ) comprising alternating conductive and insulative films in a trough configuration . in the embodiment depicted in fig1 ( d ), the conductor layers 45 a , b , c having lateral and vertical formations with each layer comprising a different material , e . g ., having different tcr values capable of being designed to achieve a desired net tcr value , e . g ., zero . in the resistive structure of fig1 ( d ), alternating insulator films 42 a , b , c are formed between the conductive layers with each layer comprising a different material including , but not limited to : an oxide , nitride , oxynitride or any combination thereof including multilayers , porous or non - porous inorganic and / or organic dielectrics formed by a deposition process . the alternating conductive layers include a resistive material including but not limited to : ta , tan , ti , tin , w , wn or other refractory metal films . as mentioned , this resistive element may be formed as part of an interlevel circuit or comprise part of an interconnect structure as shown connected to another wire level 49 by a conducting via 48 which is electrically connected to each of the conductor layers 45 a , b , c . it is understood that the via may alternately connect some or all of the conductor layers of the trough to the adjacent wire level in the achievement of a desired design parameter , e . g ., resistance . a methodology 100 for forming the resistive structures depicted in fig1 ( a )- 1 ( d ) is shown in fig3 which includes a first step 102 of depositing a first interlevel dielectric layer , and , a further step 105 of implementing a conventional photolithographic technique for etching ( e . g ., reactive ion etching ) the trough structure , as depicted , and cleaning it . then , as next depicted at step 110 , a resistor film may then be deposited using an atomic layer deposition technique known in the art . additionally , alternate dielectric levels may be deposited with alternating resistor films within the trough structure . then , as depicted at step 120 , a chemical mechanical polish ( cmp ) technique is used to planarize and clean the structure . as shown in further step 125 , a top metal wire structure is deposited and etched . known single or dual damascene techniques may be employed . it should be understood that , in each of the resistive structures depicted in fig1 ( b )- 1 ( d ), due to the resistive nature of many of the refractory metals , a resistor film thickness may be chosen to provide lateral resistor ballasting across the resistor film . the lateral resistor ballasting is established if the material exhibits a lateral resistance of greater than 10 to 50 ohms . lateral ballasting can provide lower peak current and distributes the current and thermal stress at the insulator sidewalls . at high frequencies , the skin depth alters the current distribution . however , using thin films that are resistive and wide prevents redistribution of current . vertical ballasting is additionally provided by the presence of insulator films between the conductive films . the vertical ballasting is achieved since the current does not flow between the films . to avoid skin effect vertical redistribution , the insulators serve as a means of preventing vertical current redistribution . by using resistive materials of different tcr values , the tcr value of the net resistor element can be tuned . the magnitude of the different contributions is preferably balanced by both material and width or thickness contributions to the net resistor element . to control the temperature rise in the resistor , various materials can be used to influence the thermal resistance and thermal capacitance . the net temperature rise is a function of the distance from the substrate ( what metal level the resistor is on ), the insulating layer type and thickness . in another embodiment of the invention , depicted in the cross - section view of fig2 ( a ), there is shown a resistive structure 50 including multiple alternating conductive and insulating layers . in this embodiment , the resistive structure 50 is a planar stack of conductive layers 55 a , b , c and insulating layers 52 a , b , c , d , for example . in the resistive structure 50 of fig2 ( a ), the alternating conductive films are of the same material and may comprise a resistive material including but not limited to : ta , tan , ti , tin , w , wn or other refractory metal films . further , the alternating insulating films are of the same material and may comprise a dielectric material including , but not limited to : an oxide , nitride , oxynitride or any combination thereof including multilayers , porous or non - porous inorganic and / or organic dielectrics formed by a deposition process . the resistive element may be formed as part of an interlevel circuit or comprise part of an interconnect structure as shown connected to another wire level 59 by one or more conducting vias 58 a , b , c which electrically connects each conductor layer 55 a , b , c to the adjacent wire level . it is understood that the vias may alternately connect some or all of the conductor layers of the multi - layer planar resistive structure 50 to the adjacent wire level 59 in the achievement of a desired design parameter . in another embodiment depicted in the cross - section view of fig2 ( b ), there is shown a resistive structure 60 including multiple alternating conductive and insulating layers . in this embodiment , the resistive structure 60 is a planar stack of conductive layers 65 a , b , c and insulating layers 62 a , b , c , d , for example . in the resistive structure 60 of fig2 ( b ), the alternating conductive films each comprise a different conductive material and each alternating insulating film may comprise the same dielectric material . as in the other embodiments depicted herein , vias 68 a , b , c , may alternately connect some or all of the conductor layers of the multi - layer planar resistive structure 60 to the adjacent wire level 69 in the achievement of a desired design parameter . in another embodiment depicted in the cross - section view of fig2 ( c ), there is shown a resistive structure 70 including multiple alternating conductive and insulating layers . in this embodiment , the resistive structure 70 is a planar stack of conductive layers 75 a , b , c and insulating layers 72 a , b , c , d , for example . in the resistive structure 70 of fig2 ( c ), the alternating conductive films each comprise a same conductive material and each alternating insulating film may comprise a different dielectric material . the vias 78 a , b , c may connect some or all of the conductor layers of the multi - layer planar resistive structure 70 to an adjacent wire level 79 in the achievement of a desired design parameter . a methodology 200 for forming the resistive structures depicted in fig2 ( a )- 2 ( c ) include a first step 202 of depositing a first interlevel dielectric layer , and , a further step 205 of implementing an atomic layer deposition technique known in the art depositing a resistor film . next at step 210 , using convention photolithographic techniques , the resistor layer is then etched and stripped at designed locations to accommodate the formed via structures . then , as depicted at step 220 , a further interlevel dielectric level may be deposited with alternating resistor films within the trough structure . these steps may be repeated to form the alternating conductive and insulating structures with the formed via structures . then , as depicted at step 230 , a chemical mechanical polish ( cmp ) technique is used to planarize and clean the structure . as shown in further step 235 , a top metal wire structure is deposited and etched with via fill . known single or dual damascene techniques may be employed . it should be understood that , in each of the resistive structures depicted in fig2 ( a )- 2 ( c ), the lateral resistor ballasting is established if the conductive materials exhibit a lateral resistance of greater than 10 to 50 ohms . lateral ballasting can provide lower peak current and distributes the current and thermal stress at the insulator sidewalls . at high frequencies , the skin depth alters the current distribution . however , using thin films that are resistive and wide prevents redistribution of current . vertical ballasting is additionally provided by the presence of insulator films between the conductive films . the vertical ballasting is achieved since the current does not flow between the films . to avoid skin effect vertical redistribution , the insulators serve as a means of preventing vertical current redistribution , i . e ., serves as a means for limiting current flow perpendicular to the insulator film surfaces . further , by using resistive materials of different tcr values , the tcr value of the net resistor element can be tuned . the magnitude of the different contributions is preferably balanced by both material and width or thickness contributions to the net resistor element . moreover , to control the temperature rise in the resistor , various materials can be used to influence the thermal resistance and thermal capacitance . the net temperature rise is a function of the distance from the substrate ( what metal level the resistor is on ), the insulating layer type and thickness . for instance , it is desired that the insulator film layers are thinner than the adjacent conductive layers so that the thermal conductivity difference and temperature gradient , from one conductor to another , is reduced or neglible . this is desirable because the more uniform the temperature is across the physical structure the less temperature gradient and hence , less thermal stress which can cause cracking . by making thin dielectric layers , the thermal gradient is very small laterally thus maintaining temperature uniformity because of the self - ballasting of the film . furthermore , it is desired that the insulator layers are uniform is undesirable because , difference in thickness may contribute to bad modeling in the modeling techniques described hereinafter . the present invention additionally provides for a computer aided design ( cad ) methodology and structure for providing design , verification and checking of high current characteristics and esd robustness of a resistor element in an analog , digital , and rf circuits , system - on - a - chip environment in a design environment which utilizes parameterized cells . that is , a cad strategy is implemented that provides design flexibility , rf characterization and esd robustness of the resistor element . this resistor element may be constructed in a primitive or hierarchical “ parameterized ” cell , hereinafter referred to as a “ p - cell ”, which may be constructed into a higher level resistor element . this resistor element may further be integrated into a hierarchical structure that includes other elements which do not necessarily include resistor elements , and becomes a component within the hierarchical structure of the network . these resistor elements may be the lowest order p - cells and capable of rf and dc characterization . high current analysis , esd verification , dc characterization , schematics and lvs ( logical verification to schematic ) are completed on the resistor element . elements that may be integrated into a hierarchical network may comprise diode , bipolar and mosfet hierarchical cells . the parameterized cells , or “ p - cells ”, may be constructed in a commercially available cad software environment such as cadence ®-( cadence design systems , inc ., san jose , calif . ), e . g ., in the form of a kit . fig5 illustrates a cad design tool concept whereby a computer 300 is implemented that interacts with graphical generator and schematic generator processing sub - systems 305 , 310 , respectively . these graphical and schematic generator sub - systems interact with each other to aid in the generation of resistor p - cells , e . g ., including the resistor structures as described herein . for instance , the graphical generator 305 generates a physical layout of a resistor structure and the schematic generator 310 will generate a schematic view of the structure that is suitable for specification in a designed circuit . all designs generated by the system are subject to a verification checking sub - system 320 to verify design integrity and ensure no technology rules are violated . thus , for instance , as shown in detail in fig6 , via a user interface , a resistor p - cell 325 is designed via the graphical and schematic design sub - systems 305 , 310 and the design system and the verification checking sub - system 320 will implement design checking rules , e . g ., check the physical layout of the p - cell and ensure that it conforms to physical layout rules or violates any technology rules , for example . fig7 depicts an implementation of the design system of the present invention implemented in cadence . via the graphical user interface ( gui ) 330 of computer device 300 , create generator module 340 and placement generator module 345 are implemented for designing the resistor p - cell elements and generating circuits employing the resistor p - cells , respectively . in the design of the resistor p - cell element , several views are possible including a layout ( graphical ) view , a schematic view and / or a symbol view which enables generation of a symbol , for instance , having associated stored physical information . fig8 ( a ) depicts conceptually , the p - cell graphical design system 350 according to the invention . as shown in fig8 ( a ), functionality provided via graphical generator 305 is invoked to design graphic p - cells , e . g ., a resistor p - cell 350 . p - cell elements 351 , 352 may be combined and merged by a compile function to generate a hierarchical graphical p - cell 360 , or a higher order element . thus , for instance , a second order resistor element may be generated inheriting parameters of a lower p - cell ( e . g . a single order ) resistor element . the same analysis is applicable for the schematic generation sub - system . fig8 ( b ) depicts conceptually , the p - cell schematic design system 370 according to the invention . as shown in fig8 ( b ), functionality provided via schematic generator 310 is invoked to design schematic p - cells , e . g ., a resistor circuit element p - cell 370 . circuit p - cell elements 371 , 372 may be combined and merged by the compile function 355 to generate a hierarchical schematic p - cell , or a higher order circuit element 365 . the p - cells 360 , 365 are hierarchical and built from device primitives which have been rf characterized and modeled . without the need for additional rf characterization , the design kit development cycle is compressed . auto - generation also allows for drc ( design rule checking ) correct layouts and lvs correct circuits . thus , as exemplified in fig8 ( a ) and 8 ( b ), resistor p - cells are “ growable ” elements such that they can form repetition groups of an underlying p - cell element to accommodate the design parameters . that is , they can be changed in physical size based on the criteria autogenerated . the p - cells fix some variables , and pass some variables to higher order p - cell circuits through inheritance . for example , from a base resistor p - cell 350 , there can be constructed a plurality of p - cells 351 , 352 where each conductive layer is a p - cell and the composite resistor element 360 is a hierarchical p - cell comprising of the plurality of conductive films such as described herein with respect to fig1 and 2 . the plurality of films can be constructed within a given primitive p - cell . as an example of the schematic methodology , fig9 ( a ) depicts an exemplary schematic editing graphical unit interface ( gui ) 330 , invoking functionality for constructing a transistor p - cell 331 , a capacitor p - cell 332 , or a resistor p - cell 335 or , for invoking an ams ( analog mixed signal ) utility choice 336 . for example , upon selection of the resistor p - cell 335 , a resistor pull - down menu 380 is displayed providing design options including : create a resistor element choice 381 , create and place a resistor element choice 382 , place an existing resistor element choice 383 , and place a resistor schematic choice 384 . in the cad design system aspect of the invention , the schematic p - cell is generated by the input variables to account for the inherited parameters input values . to retain resistor circuit variability , a design flow has been built around the schematic p - cell . as an example , the selection of “ create a resistor element ” function 381 initiates creation of a schematic for a parameterized resistor cell ( resistor p - cell ). to generate the electrical schematic , via the pull - down menu 390 depicted in fig9 ( b ), the design panel requests the designer to input parameters , such as : tcr 391 , ballasting 392 , esd protection 393 and a net resistance value 394 . other parameters of interest or desired features that may be entered via the gui include , but are not limited to : the width , the length , the net total resistance , the maximum mechanical stress integrity value , the maximum peak temperature thermal integrity value , the mechanical or thermal strain limit , the resistance , the worst case capacitance , the worst case inductance , the q ( quality factor ), the worst case tcr , the high current limit , the worst case esd robustness level ( e . g ., human body model ( hbm )), machine model ( mm ), charged device model ( cdm ), transmission line pulse current ( tlp )), and other design parameters . this implementation and definition is performed via input from the gui to define the parameters . it is understood that other resistor parameters may additionally be integrated with the design system . these input parameters are passed into a procedure that will build a resistor p - cell with the schematic p - cell built according to the input parameters and placed in the designated resistor cell . an instance of the resistor layout p - cell will also be placed in the designated resistor cell . for example , fig9 ( c ) illustrates an example resistor p - cell gui panel showing a built resistor p - cell having attributes including : a resistor cell type 396 , a type of technology 397 , a library name 398 , a resistor value ( e . g . 50 ohms ), a tcr value ( e . g ., 1 %) and an esd value ( e . g ., 4000 v ). in the computer aided design ( cad ) system and methodology , a parameterized cell ( p - cell ) is thus constructed as a primary cell or a hierarchical cell consisting of a plurality of primitive cells to generate the resistor element . the resistor element parameters can be chosen from electrical circuit values , and / or rf features desired . from the electrical schematic , a symbol function can be created representing and containing all the information of the resistor p - cell . in the case of the resistor p - cell , the hierarchical p - cell information is included in a “ translation box ” 400 such as shown in fig1 that include a plurality of input connections 402 and output connections 404 that may be later specified for connection in a circuit to achieve a certain performance or parameter value , e . g ., a resistance or esd robustness value , when included in a circuit application . for instance , a symbol view 400 , representing the built resistor , may be specified for connection in an rf circuit 500 such as shown in fig1 , for example , by selecting a “ place an resistor circuit ” option ( not shown ) via the gui . generation of the graphical implementation is achievable using the translation box that generates the graphical implementation of the resistor element . the graphical implementation will have the information stored in the translation box and may reconstruct the multi - film resistor design implementing the variable information stored constraints contained in the translation box . the cad design kit of the present invention further enables the automated building of a resistor library by creating and storing both schematic , layout , and symbol views of the p - cell element including associated specified input parameters and physical models . for instance , as electrical and thermal characteristics of a design are additionally influenced by the surrounding insulator films , and “ fill shapes ” placed around the film , in the implementation of the invention , the physical model for evaluation of the electrical and thermal characteristics include algorithms or physical models that characterize the physical structure . these can also be obtained from experimental work and a “ look - up table ” that may be placed in the design system as a gui to assist the user in choosing the parameters of interest . for example , the smith - littau model is used to determine the maximum current and voltage across a resistor element as a function of an applied pulse width or energy . as known to skilled artisans , various models exist that allow quantification of the electrical and thermal failure of the structure . the p - cell may be a gui that allows generation of the fill - shapes to modify the thermal characteristics of the resistor film . the gui may be used also to choose whether the surrounding interlevel dielectric films are high - k or low - k materials . the resistor element design may further allow for “ cheesing ” which is a process where holes are placed in a film to establish mechanical stability of the element . if the user desires the resistor element may be auto - cheesed . this will allow thermal and mechanical stability wherein the design would auto - adjust to the correct size to achieve the other desired parameters . the design system further provides a tunable thermal resistance feature that attempts to satisfy the desired characteristic by material changes , widths , dielectric film spacing , and material types . additionally , it can change the thermal impedance , thermal resistance and thermal capacitance as well as quality factor ( qf ) or q of the resistor by adjusting the electrical capacitance , inductance and other parasitic features . further , according to the invention , a methodology is provided that allows for the auto - generation of the schematic circuit to be placed directly into the design . this procedure is available with a “ place a resistor schematic ” option ( not shown ) via the user gui that enables the designer to auto - generate the circuit and place it in the schematic . since these cells are hierarchical , the primitive devices and auto - wiring are placed by creating an instance of the schematic p - cell and then flattening the element . to maintain the hierarchy during the layout phase of the design , an instance box is placed in the schematic retaining the input parameters and device names and characteristics as properties and the elements are recognized and the primitives are replaced with the hierarchical p - cell . to produce multiple implementations using different inherited parameter variable inputs , different embodiments of the same circuit type may be created by the methodology of the invention . in this process , the schematic is renamed to be able to produce multiple implementations in a common chip or design ; the renaming process allows for the design system to distinguish multiple cell views to be present in a common design . when the inherited parameters are defined , the circuit schematic is generated according to the selected variables . for example , substrate , ground and pin connections are established for the system to identify the connectivity of the circuit . the design system may additionally auto - generate the layout from the electrical schematic which will appear as equivalent to the previously discussed graphical implementation . the physical layout of the resistors circuits is implemented with p - cells using existing primitives in the reference library . the circuit topology is formed within the p - cell including wiring such that all parasitics may be accounted for . it should be understood that the design system and methodology permits for change of circuit topology as well as structure size of the resistor structure in an automated fashion . layout and circuit schematics are auto - generated with the user varying the number of elements in the circuit . the circuit topology automation allows for the customer to auto - generate new resistor elements without additional design work . interconnects and wiring to and between the resistor elements are also auto - generated . the resistor elements described herein with respect to fig1 and 2 and embodied as a hierarchical parameterized cell designed via the cad tool kit of the invention , may thus be designed with the following achievable design objectives including , but not limited to : 1 ) verification of the connection between a first and second element by verifying and checking electrical connectivity wherein the first element is a p - cell and the second element is a p - cell ; 2 ) verification of the width requirements to maintain high current and esd robustness to a minimum level ; 3 ) verify that based on the high current or esd robustness of the esd network that the resistor width and via number is such to avoid electrical interconnect failure prior to the esd network failure ; 4 ) allow for parallel resistors whose cross section can be maintained and evaluated as a set of parallel resistors ; 5 ) allow for “ resistor ballasting ” by dividing into a plurality or array of resistors ; 6 ) allow for calculation of the high current robustness of the resistor based on pulse width , surrounding insulator materials ( e . g . sio 2 or low k materials ), metal level and distance from the substrate ( thermal resistance based on the metal level or underlying structures ; 7 ) account for surrounding fill shapes around the resistor p - cell ; and , 8 ) account and adjust for “ cheesing ” ( removal of interconnect material inside the interconnect ) of the resistor element . various modifications may be made to the structures of the invention as set forth above without departing from the spirit and scope of the invention as described and claimed . various aspects of the embodiments described above may be combined and / or modified . while the invention has been particularly shown and described with respect to illustrative and preferred embodiments thereof , it will be understood by those skilled in the art that the foregoing and other changes in form and details may be made therein without departing from the spirit and scope of the invention that should be limited only by the scope of the appended claims .
7
fig1 is a sectional view of a first embodiment of a solid state image sensor of the invention . in fig1 as in fig6 only one unit cell of the interline transfer type ccd solid state image sensor using a pn junction photo diode as the photo detector , is shown . in fig1 the parts which substantially have the same function as the conventional ccd solid state image sensor shown in fig6 are identified with the same reference numerals , and a detailed explanation thereof is omitted . as is evident from a the comparison between fig1 and fig6 in fig1 a p - type region 11 is formed by injecting or diffusing a p - type impurity in the surface portion of the n - type region 5 forming the photo diode . one edge of the p - type region 11 is located at a position remote from one edge of the polycrystalline silicon electrode 8 by distance l 1 , while the other edge of the p - type region 11 is connected to the p - type channel stop region 3 . therefore , the p - type region 11 is connected to the ground potential through the channel stop region 3 . in this embodiment , the junction depth of the p - type region 11 is 0 . 5 μm and the surface impurity concentration is 2 × 10 18 / cm 3 . several causes are considered regarding the generation of dark current , but as a result of experiments by the present inventors , it has been discovered that the depleted region formed in the interface between the silicon substrate and the silicon dioxide film is a principal source of dark current . also , from the fact , as stated above , that the dark current increases when the photo diode of the complete depletion type is used to improve the image lag characteristic , it is observed that the depleted region in the interface of the substrate and silicon dioxide film is a dominant factor in the generation of dark current . that is , in the conventional ccd solid state image sensor shown in fig6 a depleted region is formed in the interface of the p - type well 2 and n - type region 5 , and a depleted region is also formed in the interface of the n - type region 5 and silicon dioxide film 7 . of these , the depleted region formed in the interface of the n - type region 5 and silicon dioxide film 7 , in other words , interface traps existing at the interface , makes it easier to generate electrons . the current generated by these electrons becomes a main component of the dark current . still more , as a result of damage or electrostatic breakdown in the plasma processing or ion processing steps during the semiconductor processing , the quantity of the interface traps increases . further , the quantity of interface traps increases exponentially with a rise in temperature , so that the dark current increases as a matter of course . accordingly , in the first embodiment of the invention shown in fig1 the p - type region 11 is formed in the portion where the interface traps are generated , that is , in the interface of the n - type region 5 and the silicon dioxide film 7 . this p - type region 11 is connected to the ground potential through the p - type channel stop region 3 . fig2 ( a ) shows a potential profile along line a -- a in fig1 . immediately beneath the silicon dioxide film 7 , an interface traps 12 is generated as schematically indicated by the x &# 39 ; s shown in fig2 ( a ). on the other hand , fig2 ( b ) shows a potential profile along line a - a shown in fig6 . in the conventional structure shown in fig6 since the n - type region 5 is formed immediately beneath the silicon dioxide film 7 , the potential profile continues flatly from the n - type region 5 to the interface with the silicon dioxide film 7 as shown by reference numeral 13 in fig2 ( b ). therefore , the electrons generated from the interface traps flow into the n - type region 5 , which causes the dark current . by contrast , in the structure of the first embodiment of the invention as shown in fig1 the p - type region 11 is buried in the surface portion of the n - type region 5 , and this p - type region 11 is connected to the grounding potential . accordingly , the potential profile is fixed at ov in the p - type region 11 as shown in fig2 ( a ). as a result , the electrons generated at the interface traps disappear by re - combining with holes through the p - type region 11 . therefore , the electrons generated at the interface trap do not flow into the n - type region 5 , and hence the dark current is notably suppressed . to suppress the dark current , meanwhile , it is desired to bury the p - type region 11 in the entire surface of the n - type region 5 . thus , the affects of the interface trap in the region indicated by l 1 in fig1 may be also suppressed . however , when l 1 is set at about 0 . 5 μm , that is , at about the depth of the p - type region 11 , the p - type impurity is diffused nearly to the lower part of the polycrystalline silicon electrode 8 , which may affect the potential profile reading of the signal electric charge . hence , an image lag due to imperfect pickup of the signal electric charge may be likely to occur . therefore , the value of l 1 must be determined considering the shape of photo diode and the impurity profile of the n - type region 5 , etc . in the embodiment shown in fig1 setting l 1 at 0 . 8 μm , the p - type region 11 was formed in about 80 percent of the surface area of the n - type region 5 . at this time , the dark current was decreased to about 25 % of the conventional level . in the embodiment shown in fig1 the impurity concentration of the p - type region 11 is 2 × 10 18 / cm 3 . according to experiments by the present inventors , when the impurity concentration of the p - type region was on the order of 10 17 , the stability was poor . when the impurity concentration was on the order of 10 18 or more , depletion of the interface during ordinary operation could be prevented , and the dark current could be stably suppressed . meanwhile , in the first embodiment of the invention shown in fig1 the structure of the reading gate parts of the ccd , that is , the n - type region 6 , polycrystalline silicon electrode 8 and other parts may be same as in the conventional structure . therefore , the characteristics relating to the function of reading signals are not at all changed . therefore , it is not required to modify the external circuits connected to the ccd solid state image sensor . in the embodiment shown in fig1 , it is intended to suppress the dark current itself , but actually the amplitude of dark current components is often different among multiple unit cells , and such fluctuation of the amplitude of dark current may lead to increasing noise , narrowing of dynamic range , and a rough image of the entire picture as if seen through a ground glass at low illumination or high temperature . additionally , as stated in relation to the embodiment shown in fig1 when the distance l 1 between the polycrystalline silicon electrode 8 and p - type region 11 is narrowed , the dark current decreases , but the potential profile in the overlap area of the polycrystalline silicone electrode 8 and n - type region 5 becomes higher due to the effect of the p - type region 11 . accordingly , an image lag is likely to occur due to the imperfect pickup of the signal electric charge during the reading operation . in order to suppress such a fluctuation in the amplitude of dark current and to improve the image lag characteristic , it is extremely important to control the position of the p - type region 11 accurately with respect to the polycrystalline silicon electrode 8 . fig3 ( a ) to ( d ), which relate to a second embodiment of the invention , sequentially show sectional views of manufacturing steps of a solid state image sensor capable of controlling the position of the p - type region 11 accurately with respect to the polycrystalline silicon electrode 8 , and fig4 is a sectional view showing its completed state . both fig3 and fig4 as fig1 show only the unit cell portion of the interline transfer type ccd solid state image sensor using a pn junction photo diode as the photo detector , and the substantially same parts as shown in fig1 are identified with the same reference numerals . hereinafter , the manufacturing method is explained while referring to fig3 ( a ) to ( d ). first of all , as shown in fig3 ( a ), a polycrystalline silicon electrode 8 is formed on a silicon dioxide film 7 . thereafter , the polycrystalline silicon electrode 8 is oxidized , and the silicon dioxide film 7 of about 2500 å in thickness is formed on the surface and side face of the polycrystalline silicon electrode 8 [ fig3 ( b )]. next , as shown in fig3 ( c ), boron ions ( b + ) are injected from the surface of the silicon dioxide film 7 toward the substrate surface . in fig3 ( c ), boron ions are injected through the silicon dioxide film 7 , and at this time the silicon dioxide film 7 at the side face of the polycrystalline silicon electrode 8 is relatively thick , and therefore the polycrystalline silicon electrode 8 and the silicon dioxide film 7 at its side face function as masks when injecting ions . accordingly , boron ions are injected into the region remote from the edge of the polycrystalline silicon electrode 8 . the gap between the edge of the polycrystalline silicon electrode 8 and the boron injection region is determined by the film thickness of the silicon dioxide film 7 at the side face of the polycrystalline silicon electrode 8 grown in fig3 ( b ). thereafter , by the heat treatment for about 1 hour at 900 ° c ., the impurities of boron ions are diffused toward the polycrystalline silicon electrode 8 , thereby forming a p - type region 11 which partly overlaps with the polycrystalline silicon electrode 8 [ fig3 ( d )]. thereafter , by forming an aluminum film 9 for cutting off light on the surface of the silicon dioxide film 7 , the unit cell portion as shown in fig4 is completed . in this manufacturing process , especially in the thermal diffusion step shown in fig3 ( d ), when diffusing the boron ion impurities toward the polycrystalline silicon electrode 8 , it is important to optimize the process conditions in order to suppress to the extend possible the dark current and the image lag during reading of signal electric charges . when such process conditions are optimized , the dark current may be sufficiently suppressed and the image lag characteristic may be satisfactorily maintained without having to maintain a distance of l 1 between the p - type region 11 and the polycrystalline silicon electrode 8 as in the first embodiment of the invention shown in fig1 . according to the experiment by the present inventors , even if the gap l 2 in fig4 ( the overlapping width of polycrystalline silicon electrode 8 and n - type region 5 ) is set at 1 . 0 μm , longer than the junction depth 0 . 5 μm of the p - type region 11 , and the p - type region 11 is diffused up to a point beneath the polycrystalline silicon electrode 8 , the boron concentration profile beneath the polycrystalline silicon electrode 8 can be accurately controlled by optimizing the film thickness of the silicon dioxide film 7 at the side face of the polycrystalline silicon electrode 8 shown in fig3 ( c ) and the thermal diffusion conditions in fig3 ( d ), and as a result the dark current characteristic and image lag characteristic can be improved at the same time . thus , the feature of the second embodiment of the invention as discussed with reference fig3 is that the position or the area of the p - type region 11 is accurately controlled by self - alignment on the basis of the end portion of the polycrystalline silicon electrode 8 . that is , as shown in fig3 ( b ), the film thickness of the silicon dioxide film 7 at the side face of the polycrystalline silicon electrode 8 can be accurately controlled . additionally , as shown in fig3 ( c ), since boron ions are injected by using the polycrystalline silicon electrode 8 and silicon dioxide film 7 as masks , the shape of the p - type region 11 can be accurately controlled . moreover , when the heat treatment condition in fig3 ( d ) is optimized , the boron concentration profile beneath the polycrystalline silicon electrode 8 may be also controlled accurately . thus , according to the second embodiment shown in fig3 , since the shape of the p - type region 11 and the impurity concentration beneath the polycrystalline silicon electrode 8 can be accurately controlled , fluctuations in the amplitude of the dark current among multiple unit cells may be suppressed . as a result , noise , dynamic range and image lag characteristics are greatly improved . incidentally , in the first and second embodiments shown in fig1 and fig4 the aluminum film 9 for cutting off light is formed within the top area of the polycrystalline silicon electrode 8 or in a size slightly projecting from the end portion of the polycrystalline silicon electrode 8 . accordingly , the light obliquely entering the photo diode ( pd ) from upper right to the lower left corner of the drawings may pass near the end portion of the polycrystalline silicon electrode 8 to directly enter the ccd part . when the ccd directly receives oblique incident light in this way , the signal electric charges due to the oblique incident light may be added to the original transfer electric charges during the ccd reading operation , and it may create a kind of false signal to make the image become unclear , which is known as the smear phenomenon . fig5 shows a third embodiment capable of solving such a problem . fig5 also shows , as in the first and second embodiments , only the unit cell portion of the interline transfer type ccd solid state image sensor using a pn junction photo diode as the photo detector . in fig5 the parts which are substantially same in function as those shown in fig1 are identified with the same reference numerals , and a detailed explanation thereof is omitted . on the surface of a silicon dioxide film 7 , an aluminum film 14 for cutting off light is formed in the portion excluding the region of the photo diode ( pd ). as is evident from fig5 the end portion of the aluminum film 14 is formed so as to cover the surface of the silicon dioxide film 7 at both sides of the polycrystalline silicon electrode 8 . in this way , as shown in fig5 the aluminum film 14 is extended to the photo diode ( pd ) by the total dimension of the film thickness l 3 of the silicon dioxide film 7 and the film thickness l 4 of the aluminum film 14 . as a result , the oblique light entering the ccd part may be securely blocked at the end portion of the aluminum film 14 , so that generation of the smear phenomenon may be notably suppressed . in the foregoing embodiments , meanwhile , the p - type well 2 is used as the substrate . by using the epitaxilaly grown p - type well 2 as the substrate , blooming and the smear phenomena can be suppressed , and it is also effective to bring the spectral response closer to the response of the human eye . additionally , in the foregoing embodiments , the excess electric charge is designed to overflow into the n - type silicon substrate 1 , but a similar effect is obtained in a method of sweeping out the excess electric charge into the drain formed in the substrate surface portion . furthermore , in all of the embodiments herein , the n - type silicon substrate 1 is used , but it may also be possible , needless to say , to use a p - type silicon substrate . further , similar effects are also obtained when this invention is applied to a solid state image sensor of types other than the ccd type .
7
claus sulfur recovery systems are widely utilized to recover sulfur from acid gas streams produced in natural gas purification and in petroleum refineries , primarily from amine sweetening . in refineries , the hydrogen sulfide is in the crude oil and is contained in hydrocarbon desulfurization unit off gases and fluidized catalytic cracker unit off gases . often times , gas streams produced in the amine unit are quite rich in hydrogen sulfide , particularly in petroleum refineries , where it may be in the range of 80 - 95 mole % hydrogen sulfide . in many refineries , the claus plant units are either fully loaded or subject to becoming fully loaded ( capacity limited ) due to the processing of heavy crude oils , which contain relatively large amounts of sulfur compounds . with the dwindling known reserves of refinable sweet hydrocarbons and crude oils , less attractive known sour oil reserves are now being processed , which less attractive oil reserves typically have high sulfur content . a trend in refining such high sulfur containing feeds will increase in the future . therefore , a method for increasing the capacity of claus plants to process sulfur , while maintaining the temperature limitations of the materials of the claus plant is needed . as claus sulfur recovery unit feed rates are increased above capacity , several problems develop . at increased flow , the pressure dropped through the claus plant and tailgas cleanup unit increases , and the back pressure increases require hydrogen sulfide and air feed inlet pressures beyond what is available from the equipment that supplies the hydrogen sulfide feed and the air blower that provides feed air . the increased flow also increases the space velocity in the reaction furnace and the catalytic reactor stages . this increase in space velocity , reduces sulfur conversion and increases emissions to the tailgas clean up unit . the increase flow to the tailgas clean up unit increases its pressure drop and further lowers tailgas sulfur recover to give increased and usually unacceptable sulfur emissions from the overall systems . the increased back pressures made in some claus plants pose the risk of blowing the liquid sulfur drain seals which would release noxious , toxic hydrogen sulfide into the area of the plant . while booster blowers for the hydrogen sulfide and air feeds and higher pressure sulfur drain seals can provide some increase in capacity , the reduced sulfur conversion and increase sulfur emissions remain a problem . one method which may be used to increase the capacity of an existing claus plant is the use of oxygen to enrich the air stream to the reaction furnace of the plant from 21 mole % oxygen which is the content of air up to 70 - 90 mole % oxygen or higher , such as 100 mole % oxygen ( wherein no air is introduced into the claus plant ). any increase in oxygen content of the air stream effectively reduces the nitrogen content of gases passing through the claus plant and increases its throughput capacity for sulfur by diminishing the gas flow of inerts , namely nitrogen which must also be passed through the equipment . typically , the capacity of a claus plant which is handling 80 - 90 mol % hydrogen sulfide with a typical concentration of hydrocarbons can be increased 10 to 15 % by enriching the air with oxygen . any further addition of oxygen will cause the flame temperature limitations of the firebrick and refractory in the reaction furnace to be exceeded . if the acid gas stream contains 90 mole % hydrogen sulfide and the claus plant is performing a typical burn of only one third of the hydrogen sulfide ( one third of the fully stoichiometric air requirements ) and the burner is receiving air ( 21 mole % oxygen ), then the calculated theoretical adiabatic flame temperature should be about 2400 ° f . if the air stream is enriched with oxygen to 40 mole % oxygen , the calculated adiabatic theoretical flame temperatures should increase to about 3150 ° f . again if the air stream is enriched with oxygen , by this time to 70 mole % oxygen , the calculated theoretical adiabatic flame temperature should increase to about 3750 ° f . however , most better quality fire brick and refractory material installed in claus plant reaction furnaces are good for a maximum continuous operating temperature of only 2700 ° to 2800 ° f ., if they have an alumina content of 85 - 90 wt % or greater . therefore , it may be seen from the above calculations that only limited oxygen enrichment , 30 - 32 mole % oxygen of the air stream can be used and still hold the temperature below a maximum of 2800 ° f . with the small reduction of nitrogen input when increasing the air stream oxygen content from 21 up to 32 mole % oxygen , only a slight increase in claus plant capacity is realized , approximately 12 - 15 % capacity . the present invention however permits increasing the oxygen - enrichment to above 32 mole % to increase capacity of an existing claus sulfur recovery unit further by injecting water into the reaction furnace to moderate the oxygen - enriched flame temperatures . in practice , the injection rate of water would be set to provide dilution and cooling to control the reaction furnace temperature in the 2400 ° to 2800 ° f . with this technique , hydrogen sulfide feed and sulfur recovery capacity can be increased by 50 - 100 % by enriching the air stream to 70 mole % oxygen when handling 90 mole % hydrogen sulfide acid gas feed . by injecting a liquid water stream under atomized or well dispersed conditions into the reaction furnace or preferably the oxygen inlet to the reaction furnace , the flame temperatures associated with very high oxygen - enrichment necessary to effect significant throughput increases are moderated by the relatively cool and inert injected water . additionally , the water has a very high heat sink capacity . although , liquid water is preferred in order to take advantage of its heat of vaporization , it is contemplated that steam may be used with a less dramatic temperature moderating effect . it should be understood that the use of the term water herein shall include steam . optimally , the water injection is made in the oxygen inlet to the burner 20 . it is contemplated that the water can be added in a jacketed oxygen lance wherein the water cools the lance apparatus to avoid combustion of the same by the rich oxygen atmosphere . alternately , the water injection could be made in the hydrogen sulfide feed to the reaction furnace , the air feed to the reaction furnace or an independent feed to the reaction furnace . the combination of oxygen - enrichment and water injection provides an unexpected potential enhancement of capacity or throughput for a claus plant . such a process configuration can be provided as a retrofit to a capacity limited existing claus plant system or could be provided in a smaller size new installation taking into account the increased capacity freedom provided by the oxygen - enrichment and water injection attributes . at first glance , it may appear that the increased flow from the introduction of water into the process will increase the claus plant system pressure drop and reintroduce the pressure drop limitation which oxygen - enrichment alleviated . this is not correct , as is apparent from a comparison of the deleted nitrogen in contrast to the added water . for the case of pure oxygen with a 92 . 4 % hydrogen sulfide feed , every mole of nitrogen removed from the system by the use of oxygen - enrichment , only 0 . 44 moles of liquid water are necessary to alleviate the flame temperature increases above the maximum allowable flame temperature . further , by introducing water into the system in the form of a dispersion or atomization of liquid water , rather than as steam , the heat capacity of the water is increased by the heat absorbed as the water changes from its liquid state to its vapor state . this provides an unexpected freedom for moderating temperature without increasing pressure drop through the system as one would expect to have occurred by the addition of an additional ingredient into the process , i . e . adding water as a moderant . in examining the claus process , the combustion of hydrogen sulfide by ## str1 ## is irreversible . all of the oxygen is reacted . the reaction is reversible . increasing the water and is partial pressure will tend to reverse this reaction . it therefore appears that water injection would greatly decrease equilibrium conversion . but this is not so . water injection greatly decreases the nitrogen partial pressure . this , in turn , increases the hydrogen sulfide and sulfur dioxide partial pressure , which drives the reaction to the right . the net effect is that there is little or no direction in sulfur conversion . going from a case 1 bottlenecked air operation and a case 2 oxygen enriched operation at 32 mole % oxygen enrichment to case 3 and 4 oxygen - enrichment with water moderation that a substantial increase in sulfur processing capacity is achieved without any significant loss in sulfur recovery wt %. this capacity increase is equal to or greater than any other known arrangement for accomplishing a claus plant capacity increase . __________________________________________________________________________ relative sulfur processing sulfurcase description mol % o . sub . 2 capacity recovery wt % __________________________________________________________________________1 air only 21 1 . 00 97 . 72 o . sub . 2 enriched air 32 1 . 15 98 . 03 o . sub . 2 enriched air 70 1 . 75 97 . 0 water injection4 oxygen 100 1 . 85 97 . 0 water injection__________________________________________________________________________ the present invention will now be described in greater detail with reference to a preferred embodiment which is illustrated in the figure . an acid gas feed stream is introduced into the claus system in line 10 having a hydrogen sulfide content of 92 . 4 mole %. the feed is at a temperature of 100 ° f . and a pressure of 25 psia . the acid gas stream is introduced into a burner 20 of the reaction furnace 22 to be combusted with , potentially , air in line 14 which is pressurized through compressor 16 , as well as oxygen in line 12 , also introduced into the burner for the downstream combustion reaction . the oxygen can be of any desired purity although preferably commercially pure oxygen is introduced into the system . it is understood that depending upon the total oxygen - enrichment required it may be chosen to delete some or all of the air introduced into the burner 20 . in order to moderate the temperature of the oxygen - enriched combustion of the acid gas feed , water is introduced in line 18 into the burner 20 and , most preferably , the water is introduced into the oxygen stream 12 prior to the burner . however , it is contemplated that the water addition could be directly into the burner or alternately into the air feed or acid gas feed to the burner . preferably , the water / oxygen mixture is introduced into the air feed ( if used ) prior to the burner . preferably , the water is dispersed in an atomized manner . the amount of water added is in the range of up to 2 . 4 moles per moles of enriching oxygen fed to the system . preferably the range of water addition is up to 1 . 68 moles of water per mole of enriching oxygen . in order to atomize the water it is usually necessary to send a pressurized water stream through a small orifice and in dealing with a small orifice it will be preferable to use demineralized water . although the source of the water may be a fresh water supply , it is also contemplated that recycle water from the water of reaction from the downstream process system could be treated and recycled for introduction at the burner 20 of the reaction furnace 22 . the reactants are combusted in burner 20 and evolved into the reaction furnace 22 where the reactions of the claus process occur . specifically in the burner , hydrogen sulfide and oxygen combine to produce sulfur dioxide and water , wherein 1 / 3 of the reaction feed is initially combusted and the remaining 2 / 3 react with the sulfur dioxide produced to result in sulfur and water according to the following formulaes : the reactor furnace effluent then passes through a circuitous heat exchange zone or waste heat boiler 24 wherein the combustion effluents are cooled against boiler feed water in line 26 , which then produces steam in line 28 . in the waste heat boiler 24 the reaction effluents are converted from one form of sulfur species to another ranging from s 3 to s 8 . the major sulfur species are formed according to the following equations : the cooled effluent from the waste heat boiler in line 30 is still at high temperature and at a pressure only slightly below the pressure of the feeds to the burner . the effluent is then introduced into the first condenser 32 , wherein the effluent is again heat exchanged to cool the effluent against boiler feed water in line 34 which produces steam in line 36 . liquid sulfur is condensed out in line 38 and the gaseous combustion effluent stream is removed in line 42 . the effluent stream in line 42 is then reheated in a reheater heat exchanger 48 against process steam . the reheated stream now in line 50 has been reheated to a temperature sufficient for further reaction of the sulfur contained therein . this stream is then introduced into a catalytic converter reactor 52 wherein additional quantities of hydrogen sulfide and sulfur dioxide are reacted to produce sulfur ( primarily s 6 and s 8 ) and water according to the following equations : the reacted stream now in line 54 is introduced into a second condenser 56 which again cools the effluent stream against boiler feed water in line 58 to produce additional steam in line 60 . additional elemental sulfur is recovered in line 62 wherein the sulfur species produced in the catalytic reaction are converted to high molecular weight sulfur species and are then condensed to elemental sulfur ( primarily from s 6 and s 8 ) according to the following reactions : the stream in line 64 is at a reduced temperature , which is below that desired for additional catalytic reaction . therefore , the stream is introduced into reheater heat exchanger 66 and heated against processs steam to produce a feed stream in line 68 at a temperature sufficient for catalytic claus reaction . this stream is introduced into a second catalytic converter 70 wherein a similar catalytic reaction between hydrogen sulfide and sulfur dioxide occurs with the catalytic effluent in line 72 going to yet another condenser 74 , which is cooled with boiler feed water 76 to produce steam in line 78 . an additional quantity of liquid elemental sulfur is removed in line 80 . the effluent stream in line 82 is further reheated in reheater heat exchanger 84 against process steam to produce a stream in line 86 at high temperatures sufficient for a catalytic claus reaction . this stream is introduced into the third and final catalytic reactor 88 to react substantially the remaining hydrogen sulfide and sulfur dioxide to produce sulfur species which are removed in line 90 . that stream is introduced into a condenser 92 and cooled by boiler feed water in line 94 producing steam in line 96 . further elemental sulfur in liquid form is removed in line 98 , while a final effluent is recovered in line 100 comprising predominantly steam , nitrogen , carbon dioxide , hydrogen and residual hydrogen sulfide and sulfur compounds . the stream in line 100 is introduced into a tailgas coalescer 102 wherein additional sulfur is removed in line 104 . the residual stream in line 106 can be sent to a tailgas clean up unit 109 through line 107 or sent directly to an incinerator 114 by opening of valve 113 . if the stream in line 106 is directed into the tailgas clean up unit 109 it can be further processed for the removal of sulfur and the resulting effluent in line 111 can be recycled to the front end of the system to the acid gas feed in line 10 . the cleaned up inert gas stream can then be cycled through line 115 into an incinerator for venting to the atmosphere . the incinerator 114 is operated with a burner 112 supplied with air 108 and fuel such as natural gas in line 110 to combust any residual amounts of sulfur from the tailgas unit or alternately from the coalescer 102 . the resulting stream in line 116 should be environmentally acceptable and can be vented to atmosphere . the present invention as described above is exemplary of only one embodiment of the invention which incorporates oxygen - enrichment with a moderating water injection stream to provide : ( a ) an unlimited degree of freedom in oxygen - enrichment levels , ( b ) an increase in throughput of a claus plant to very high levels , ( c ) a decrease in overall pressure drop through the claus plant system , ( d ) reduction effluent flow to and through the tailgas process unit , ( e ) an equivalent or heightened percent recovery of sulfur from the feed gas stream , ( f ) a negligible effect by water addition on the claus reaction equilibrium , ( g ) an improved and easier separation of the inerts from the sulfur to the tailgas clean up unit wherein the water being the predominant inert is easily phase separated from the residual gas stream , and ( h ) increased residence time in the reaction furnace over that wherein other inerts moderating streams are utilized or nitrogen from air is present , due to the decreased volume of gases passing through the reaction furnace with water injection which results from the superior heat capacity of liquid water as a moderant and the absence of any large quantities of nitrogen , which results from the use of oxygen - enrichment . the present invention has been described with regard to one preferred embodiment , but those skilled in the art will be capable of contemplating other variants which are deemed to be within the scope of the invention , which scope should be ascertained from the claims which follow .
2
in the fluoroalkyloxyalkyl containing diorganopolysiloxanes represented by the above formula , r 1 may be 1 , 1 , 2 , 2 - tetrafluoroethoxyethyl , 1 , 1 , 2 , 2 - tetrafluoroethoxypropyl , 1 , 1 , 2 , 2 - tetrafluoroethoxybutyl , ( 2 - hydro - hexafluoropropyl )- oxyethyl , ( 2 - hydro - hexafluoropropyl )- oxypropyl , ( 2 - hydro - hexafluoropropyl ) oxybutyl , ( 2 - hydro - octafluorobutyl )- oxyethyl , ( 2 - hydro - octafluorobutyl )- oxypropyl , ( 2 - hydro - octafluorobutyl )- oxybutyl , ( 2 - hydro - decafluoropentyl )- oxyethyl , ( 2 - hydro - decafluoropentyl ) oxypropyl , ( 2 - hydro - decafluoropentyl )- oxybutyl , ( 2 - hydro - dodecafluorohexyl )- oxyethyl , ( 2 - hydro - dodecafluorohexyl )- oxypropyl , and ( 2 - hydro - dodecafluorohexyl )- oxybutyl . examples of r 2 , r 4 , r 5 and r 6 groups are hydrogen and alkyl radicals such as the methyl , ethyl , propyl , n - butyl , n - pentyl , n - hexyl , n - heptyl , n - octyl ; aminoalkyl radicals such as aminomethyl , aminoethyl , aminopropyl and aminopentyl radicals ; thiol groups such as mercaptomethyl and mercaptoethyl groups ; alkenyl groups such as vinyl and allyl radicals and aryl groups such as the phenyl , tolyl and xylyl radicals . examples of groups represented by r 3 are ( trifluoromethyl - ethyl ), ( trifluoromethyl - propyl ), ( trifluoromethyl - butyl ), perfluoroethyl - ethyl ), ( perfluoroethyl - propyl ), ( perfluoroethylbutyl ), ( perfluorooctyl - ethyl ), ( perfluorooctyl - propyl ), ( perfluoropropyl - butyl ), ( perfluorobutyl - ethyl ), ( perfluorobutylpropyl - ethyl ), ( perfluorobutyl - butyl ), ( perfluorodecyl - ethyl ), ( perfluorodecyl - propyl ), ( perfluorodecyl - butyl ), ( perfluorohexylethyl ), ( perfluorohexyl - propyl ), ( perfluorohexyl - butyl ), [( w - chloro - dodecafluorohexyl )- ethyl ], [( w - bromo - dodecafluorohexyl )- ethyl ], ( perfluorododecyl - ethyl ), ( perfluoroquatordecyl - ethyl ), ( perfluorohexadecyl - ethyl ) and ( perfluorooctadecyl - ethyl ). examples of terminal groups represented by x and y are trimethylsiloxy and triethylsiloxy groups ; condensable groups , such as hydrogen and the oh group ; alkyloxy groups having from 1 to 5 carbon atoms , especially the methoxy , ethoxy , propyloxy , n - butyloxy , n - pentyloxy , as well as alkoxyalkyl groups such as the ethoxymethyleneoxy group . preferred examples of the r 1 groups are 1 , 1 , 2 , 2 - tetrafluoroethyoxypropyl and ( 2 - hydro - hexafluoropropyl )- oxypropyl groups . the methyl group is the preferred example for the r 2 , r 4 and r 5 radicals . the perfluorohexyl - ethyl group is the preferred radical for the r 3 group . the organopolysiloxanes of this invention are prepared by the hydrolysis or the co - hydrolysis of the silanes and the subsequent condensation or equilibration of the resultant hydrolysates . generally , the process of this invention is carried out by hydrolyzing silanes having the formula r 1 r 2 sicl 2 , r 5 r 6 sicl 2 and optionally r 3 r 4 sicl 2 in an aqueous system , preferably in 3 to 30 percent by weight of sodium hydroxide . the silane is preferably added to the aqueous system . in principle , the silanes can be hydrolyzed separately or together as a silane mixture and in the desired molar ratio . occassionally the socalled &# 34 ; gradient hydrolysis &# 34 ; process is used , in which a hydrolysate of a silane or a silane mixture is co - hydrolyzed in a second hydrolysis stage together with at least one additional silane . hydrolysis reactions are customarily performed at temperatures between 20 ° and 80 ° c . and under atmospheric pressure . the hydrolysates are isolated by separating the aqueous phase and by purifying the hydrolysate by neutralization , extraction , vacuum drying or by other techniques known in the art . the condensation or equilibration of the hydrolysate or hydrolysates is generally achieved in the absence of a solvent and in the presence of condensation or equilibration catalysts . examples of suitable catalysts are phosphoronitrile chlorides , quaternary ammonium salts and quaternary ammonium hydroxides such as tetramethylammonium hydroxide , benzyltrimethylammonium hydroxide and similar compounds . the catalysts are generally employed in an amount of from 10 to 300 ppm by weight , based on the total weight of the components of the reaction . the reaction temperatures are generally between 80 ° and 120 ° c . it is preferred that the process be carried out under reduced pressure , for example , in the range of from 0 . 5 to 15 torr . the condensation or equilibration reactions take place with practically quantitative results , so that the proportion of the individual reactive substances employed is reflected by the molar ratio of the individually desired structural units in the resultant condensate or equilibrated product . after the desired degree of condensation or equilibration has been achieved , the reactions are terminated by deactivating the catalyst . the catalyst may be deactivated by the addition of amines , for example , triisononylamine , or by heating to temperatures between 130 ° and 150 ° c ., especially when quaternary ammonium hydroxides are used as the equilibration catalysts . often , &# 34 ; monofunctional &# 34 ; silanes such as trialkylchlorosilanes are added to terminate the condensation or equilibration reactions . the fluoroalkoxyalkyl containing organopolysiloxanes of this invention may consist of block copolymers , i . e ., the individual structural elements are present as contiguous blocks , or they may be present in the form of copolymers wherein the individual structural elements are randomly distributed . a random distribution is preferred . furthermore , the organopolysiloxanes of this invention may also contain such structural elements as are obtained by the equilibration of small amounts , for example 1 to 2 percent by weight based on the total weight of the organopolysiloxane of phenols , such as tertiary butyl and tertiary octylphenol . the organopolysiloxanes of this invention generally have viscosities in the range of from 30 to 100 , 000 mm 2 / s and preferably from 100 to 10 , 000 mm 2 / s . when they contain reactive groups , they may be used in preparing elastomers and resins . the organopolysiloxanes of this invention may be used as hydrophobization agents , as oleophobization agents , as textile adjuvants , and especially as lubricants and antifoaming agents . when the organopolysiloxanes are used as lubricants , they can be subjected to elevated mechanical and thermal stress . elastomers prepared from the organopolysiloxanes of this invention can for example be used as sealing and coating compositions . the following examples will further illustrate the invention ; however , they should not be construed as limiting the scope of the invention which is delineated in the claims . ( a ) about 687 gm of a 15 percent by weight aqueous sodium hydroxide solution were placed in a 2 liter three - necked flask equipped with a stirrer , dropping funnel and a reflux condenser . over a period of one hour , a mixture consisting of 115 gm of ( n - perfluorohexyl - ethyl )- methyldichlorosilane , 136 . 5 gm of ( 1 , 1 , 2 , 2 - tetrafluoroethyl - oxypropyl )- methyldichlorosilane and 64 . 5 gm of dimethyldichlorosilane was added dropwise . the temperature of the reaction mixture increased to 80 ° c . after stirring for an additional 15 minutes , the phases were separated . the final product was then neutralized by washing with water and dried at 70 ° c . and at 1 torr . about 216 gm ( 85 percent of theory ) of a cohydrolysate containing an oh group in each of its terminal units were obtained . viscosity : 170 mm 2 / sec . ( b ) about 217 gm of the cohydrolysate prepared in ( a ) above and 9 gm of a silicone oil which was end - blocked with trimethlsiloxy groups and which contained 10 dimethylsiloxy groups , were mixed with 0 . 136 ml of a 25 percent by weight solution of ( pncl 2 ) x in methylene chloride and stirred for 3 hours at 100 ° c . and at a pressure of 1 torr . the mixture was then removed , mixed with 0 . 271 ml of triisononylamine and heated for 15 minutes to 130 ° c . at 1 torr in order to remove the volatile constituents . a 95 percent yield of clear oil was obtained . viscosity : 5 , 000 mm 2 / sec . refractive index n d 20 1 . 3730 . the product showed a random distribution of the individual structural elements , with 40 mol percent being dimethylsiloxy units , 20 mol percent of ( perfluorohexyl - ethyl )- methylsiloxy units and 40 mol percent of ( 1 , 1 , 2 , 2 - tetrafluoroethyloxypropyl )- methylsiloxy units . ( a ) about 533 gm of a 15 percent by weight aqueous sodium hydroxide solution were placed in a 3 - necked flask similar to that used in example 1 ( a ) above and then 273 gm of ( 1 , 1 , 2 , 2 - tetrafluoroethyl - oxypropyl ) - methyldichlorosilane were added dropwise over a period of 20 minutes . after stirring for an additional 15 minutes , the phases were separated and the desired product was neutralized by washing with water . the product was subsequently dried at 100 ° c . and at a pressure of 1 torr . about 246 gm of hydrolysate was obtained ( 90 percent yield ) which contained an oh group in each of its terminal units and which had a viscosity of 200 mm 2 / sec . ( b ) about 218 gm of the hydrolysate obtained in accordance with 2 ( a ) above , 74 gm of a dimethylpolysiloxane having an oh group in each of its terminal units and having a viscosity of 100 mm 2 / sec . and 3 gm of a trimethylsiloxy end - blocked dimethylpolysiloxane having a viscosity of 20 mm 2 / sec . were equilibrated in a vacuum sealed mixer at 100 ° c . and at a pressure of 1 torr , in the presence of 0 . 1 ml of a 40 percent by weight methanol solution of benzyltrimethylammonium hydroxide . three hours later 0 . 2 ml of trimethylchlorosilane was added to the reaction mixture . after mixing for an additional 15 minutes , the product was maintained under a pressure of 1 torr and at a temperature of 130 ° c . for an additional 2 hours . an equilibrated product having a viscosity of 5000 mm 2 / sec . and having a refractive index of n d 20 = 1 . 3920 was obtained at a yield of 98 percent . the product had a random distribution of 50 mol percent of ( 1 , 1 , 2 , 2 - tetrafluoroethyloxypropyl )- methylsiloxy groups and 50 mol percent of dimethylsiloxy groups . ( a ) the procedure described in example 1 ( b ) above was repeated to prepare a cohydrolysate consisting of 185 gm of ( nperfluorohexylethyl )- methyldichlorosilane , 109 gm of ( 1 , 1 , 2 , 2 - tetrafluoroethyl - oxyethyl )- methyldichlorosilane and 52 gm of dimethyldichlorosilane . the yield was 270 gm ( 96 percent of theory ). viscosity : 200 mm 2 / sec . refractive index n d 20 = 1 . 3640 . ( b ) about 210 gm of the cohydrolysate prepared in example 3 ( a ) above , were equilibrated with 9 gm of a silicone oil which was end - blocked with trimethylsiloxy groups and which contained 10 dimethylsiloxy groups , in the presence of 0 . 073 ml of a 26 percent by weight solution of ( pncl 2 ) x in methylene chloride , in accordance with the procedure described in example 1 ( b ) above . the equilibrated product which was obtained in a 95 percent yield , was then mixed with 2 . 2 gm of tert - octylphenol and 0 . 073 ml of a 25 weight percent solution of ( pncl 2 ) x in methylene chloride and stirred for 2 hours at 150 ° c . and at a pressure of 1 bar . the equilibration catalyst was then deactivated by the addition of 0 . 29 ml triisononylamine and then the volatile constituents were removed by stirring at 130 ° c . under a pressure of 1 torr for an additional 15 minutes . the final product consisted of a clear oil having a viscosity of 5 , 000 mm 2 / sec . and a refractive index of n d 20 1 . 3650 . the product has a 1 : 1 : 1 random distribution of the individual structural elements consisting of dimethylsiloxy groups , ( 1 , 1 , 2 , 2 - tetrafluoroethyloxypropyl )- methylsiloxy groups and ( n - perfluorohexyl - ethyl ) methylsiloxy groups . the product was then examined for its thermostability and volatility by adding 3 gm samples of the product to pans whose dimensions were such that the specimens had a surface area of 20 cm 2 and then heated to a temperature of 200 ° c . after 240 hours , the weight loss of the samples was only 2 . 2 percent by weight . even after 1000 hours of this treatment , there was no indication of gel formation . ( a ) about 166 gm of a 15 percent by weight aqueous sodiumhydroxide solution were placed in a 3 - necked flask equipped with a stirrer , dropping funnel and reflux condenser , and then 100 gm of ( 1 , 1 , 2 , 2 - tetrafluoroethyl - oxypropyl )- methyldichlorosilane were added dropwise with constant agitation . the hydrolysate was isolated in accordance with the procedure described in example 1 ( a ) above . the product consisted of 90 gm of a hydrolysate consisting of an oh group in each of its terminal units . viscosity : 200 mm 2 / sec . ( b ) the method described in example 4 ( a ) above , was repeated except that 506 gm of ( n - perfluorohexyl - ethyl )- methyldichlorosilane were hydrolyzed and isolated . viscosity : 600 mm 2 / sec . ( c ) about 185 gm of a dimethylpolysiloxane having an oh group in each of its terminal units and having a viscosity of 100 mm 2 / sec ., 406 gm of the hydrolysate described in example 4 ( b ) above , 68 gm of the hydrolysate described in example 4 ( a ) above , 19 gm of a trimethylsiloxy end - blocked dimethylpolysiloxane having a viscosity of 5 mm 2 / sec ., and 0 . 51 ml of a 40 percent by weight methanol solution of benzyltrimethylammonium hydroxide were stirred for 3 hours at a temperature of 100 ° c . and at a pressure of 1 torr . the mixture was then removed and 1 . 16 ml of trimethylchlorosilane were added . after stirring for an additional 15 minutes , the reaction mixture was maintained for 2 hours at a temperature of 130 ° c . and at a pressure of 1 torr . the final product was obtained at a yield of 96 percent and consisted of an oil having a viscosity of 1000 mm 2 / sec . and a refractive index of n d 20 1 . 3640 . the equilibrated product consisted of 66 mol percent of dimethylsiloxy units , 8 mol percent ( n - perfluorohexyl - ethyl ) methylsiloxy units and 26 mol percent ( 1 , 1 , 2 , 2 - tetrafluoroethyloxypropyl )- methylsiloxy units . about 33 gm of the hydrolysate described in example 4 ( a ) above ( viscosity 200 mm 2 / sec . ), 61 gm of the hydrolysate described in example 4 ( b ) above ( viscosity 600 mm 2 / sec . ), 178 gm of a dimethylpolysiloxane having an oh group in each of its terminal units and having a viscosity of 100 mm 2 / sec ., 0 . 3 gm of a trimethylsiloxy end - blocked dimethylpolysiloxane having a vinylmethylsiloxy group in each fourth unit and having a viscosity of 30 mm 2 / sec ., 0 . 1 gm of a vinyldimethylsiloxy terminated dimethylpolysiloxane having a viscosity of 100 mm 2 / sec ., and 0 . 1 ml of a 40 percent by weight methanol solution of benzyltrimethylammonium hydroxide were mixed in a laboratory kneader for 3 hours at a temperature of 100 ° c . and at a pressure of 1 torr . the mixture was subsequently removed and 0 . 2 ml of vinyldimethylchlorosilane was added . the reactive mixture was maintained at a temperature of 130 ° c . and at a pressure of 1 torr for an additional 2 hours . a solid polymer having a viscosity of 15 , 000 , 000 mm 2 / sec . was obtained . in the following examples the antifoaming properties and the lubricating properties of products obtained in accordance with examples 1 through 4 were determined . in the following examples the product of example 1 is identified as &# 34 ; a &# 34 ;; the product of example 2 is identified as &# 34 ; b &# 34 ;; the product of example 3 is identified as &# 34 ; c &# 34 ;; and the product of example 4 is identified as &# 34 ; d &# 34 ;. a commercially available fluorosilicone oil containing 90 mol percent of 1 , 1 , 1 - trifluoropropyl - methylsiloxy units and 10 mol percent of dimethylsiloxy units ( viscosity 1000 mm 2 / sec .) is identified as &# 34 ; v &# 34 ;. the solubility of the organopolysiloxanes prepared in accordance with examples 1 through 4 was determined by mixing the products with each of the solvents listed in table i below so that each sample contained a 5 percent by weight solution of the product . table i______________________________________solvent v a b c d______________________________________ethylene glycol - - - - - methylethylketone + + ± + ± methylisobutylketone + + ± + ± benzene - - ± - + frigen 113 - + + + + isopropanol - - - - - perchloroethylene ± - ± ± ± ethylglycol acetate + ± + ± - acetic acid ethylester + + ± - - ______________________________________ + = soluble ± = dispersible or partially soluble - = insoluble the antifoaming properties of the organopolysiloxanes prepared in accordance with examples 1 through 4 were determined by adding 100 ml of a 2 . 5 weight percent solution of a trimethylsiloxy end - blocked dimethylpolysiloxane having a viscosity of 1000 mm 2 / sec . in perchloroethylene to a 250 ml cylinder equipped with a ground glass stopper . in each case these solutions were mixed with 0 . 25 ml of a 10 percent solution of the samples whose antifoaming properties were to be tested , in a 1 : 1 mixture consisting of acetic acid ethylester and frigen 113 . the fluorosilicone oil whose antifoaming properties were to be tested was present in an amount of 0 . 01 percent by weight . each of the test mixtures obtained was vigorously agitated 10 times in a vertical direction and subsequently the height of the foam and the time required for the foam to collapse were recorded . table ii______________________________________ foam height foam collapseadditive after agitation in sec . ______________________________________none ( control ) 180 60v 120 15a 106 11b 105 5c 110 7d 112 10______________________________________ the antifoaming properties at the boiling temperatures of the oils prepared in accordance with examples 1 through 4 were tested by heating 250 ml of test solutions obtained in accordance with example 7 , using a one - liter flask equipped with a distillation unit . in each case , 3 boiling stones were used and the mixture was heated to a vigorous boil . the foam formation of the solution under boiling conditions was then evaluated . the results are shown in table iii . table iii______________________________________additive foam level / observations______________________________________none ( control ) immediate excessive foaming at boilingv 16 mm of foam at boiling , slight decrease in foam level as distillation progressesa 10 mm of foam at boiling , then relatively large bubbles that burst quicklyb up to 8 mm of foam at boiling , then quick decrease with 2 to 3 mm of foam remainingc a few separate bubbles at boiling , then practically no foam during distillationd up to 13 mm of foam at boiling , then decrease in foam formation______________________________________ a shell - 4 - ball apparatus was used to determine the lubricating properties of the products prepared in accordance with examples 1 through 4 . table iv shows the maximal load as the vak welding power ( according to german industrial standard din 51350 ), at which the test balls were welded in the apparatus . table iv______________________________________vak welding power ( n ) ______________________________________v less than 2 , 000 na 3 , 600 - 3 , 800 nb 3 , 200 - 3 , 400 nc 3 , 400 - 3 , 600 nd 2 , 600 - 2 , 800 n______________________________________ the lubricating properties of the organopolysiloxanes prepared in accordance with examples 1 to 4 were tested with the aid of the almen - wieland oil test apparatus . a friction bearing , consisting of two separate bushings and a steel shaft which operated in a bath of the lubricant to be tested , was subjected to a given load and then the friction between the bushings and the shaft was measured . the maximum load applied was 20 , 000 n and the maximum potential friction was 3 , 500 n . in table v , the lubricating effect is indicated as the friction factor at the maximal load ( ratio of frictional force : contact pressure ). the lower the factor , the better the lubricating properties . table v______________________________________ friction index frictional contact underlubricant force pressure maximum load______________________________________v 1 , 000 2 , 000 0 . 500a 3 , 500 8 , 500 0 . 411b 3 , 500 16 , 000 0 . 184c 3 , 400 20 , 000 0 . 170d 3 , 500 20 , 000 0 . 368______________________________________ the swelling properties of oils obtained in accordance with examples 1 and 2 were compared with a sealing composition obtained from a diorganopolysiloxane which had been cross - linked at a high temperature and which had a shore hardness of 70 . the silicone rubber was in the form a a 2 mm thick o - ring gasket with a diameter of 16 mm . the gasket was kept in the test compositions for 100 hours at a temperature of 160 ° c . the test compositions had been formulated as oils , using lithium stearate to impart consistency . the formulations were selected so that the oils had a consistency of 270 [ 1 / 10 mm ] as measured pursuant to din 51804 . following the heat treatment , the gaskets were examined in order to determine any increase in their weight and volume . the results are shown in table vi . table vi______________________________________lithium stearate weight increase volume increasebased lubricant in percent by weight in percent______________________________________ + v 0 . 45 2 . 75 + a 0 . 39 2 . 25 + b 0 . 33 1 . 93______________________________________
2
the preferred form of the invention is shown in fig1 - 3 . as seen in fig1 and 2 , the stoplog 2 generally comprises an upper u - shaped channel member 4 , a middle u - shaped channel member 6 , a lower u - shaped channel member 8 , and a lower end cap channel member 10 . channel members 4 , 6 , 8 and 10 are all preferably formed of extruded aluminum stock . upper channel member 4 is joined to middle channel member 6 by a pair of continuous welds 12 , middle channel member 6 is joined to lower channel member 8 by a pair of continuous welds 14 , and lower channel member 8 is joined to lower end cap channel member 10 by a pair of continuous welds 16 . in this way channel members 4 , 6 , 8 and 10 reinforce one another so as to form a single rigid body of substantially rectangular cross - section which contains a plurality of horizontal interior cavities 18 . at least one , and preferably both , of the two vertical faces 17 of the single rigid body formed from the welded channel members 4 , 6 , 8 and 10 are substantially impervious to water . channel members 4 , 6 , 8 and 10 are all formed of substantially identical lengths , except as will hereinafter be pointed out in detail , and are sized so that they are all slightly shorter in length than the distance extending between the opposing vertical groove liners 20 which are set into the opposing concrete walls 22 of a water flow channel 24 . at the same time , channel members 4 , 6 , 8 and 10 are formed with substantially identical widths , and are sized so that they are all slightly less in width than the widths of the grooves 26 which are defined by the vertical groove liners 20 . formed in the top surface of upper channel member 4 is a lifting hook channel 28 . channel 28 runs the length of upper channel member 4 and serves to slidably constrain a pair of lifting hooks 30 . lifting hooks 30 are preferably formed of a cast aluminum alloy and serve to receive chains or other lifting apparatus ( not shown ) which are used to manipulate the stoplog into or out of the stoplog gate . lifting hooks 30 are intended to be introduced into lifting hook channel 28 at either of the two ends of upper channel member 4 , and are slid along channel 28 until they are properly positioned intermediate the two ends of upper channel member 4 , e . g ., as shown in fig1 . once lifting hooks 30 are deemed to be in their proper position along channel 28 , the hooks 30 are welded into place with spot or continuous welds 32 . lower end cap channel member 10 is provided with four support extensions 34 . extensions 34 run the length of lower end cap member 10 and , together with other portions of lower end cap member 10 , define a pair of grooves 35 on the bottom end of stoplog 2 . as shown in fig2 one of the grooves 35 is set on the upstream side of stoplog 2 and the other of the grooves 35 is set on the downstream side of stoplog 2 . the direction of water flow is indicated by the arrow in fig3 . disposed in the downstream groove 35 is a seal 36 . seal 36 is sized to run the length of lower end cap member 10 and serves to assure a substantially watertight fit between the stoplog and whatever structure resides immediately below the stoplog . seal 36 is preferably formed of neoprene and is intended to be fixed in groove 35 by means of a suitable cement , although a simple friction fit may also be utilized to hold seal 36 in place . disposed in the upstream groove 35 are a pair of feet 37 . feet 37 serve to assure that stoplog 2 will remain vertically upright when its seal 36 makes contact with whatever structure resides immediately below the stoplog . to this end each of the feet 37 is sized so that it has the same cross - sectional dimensions as seal 36 . however , since feet 37 serve simply as support for the stoplog , and not as sealing means as is the case with seal 36 , feet 37 do not extend along the entire length of lower end cap member 10 . in the embodiment shown in fig1 - 3 , feet 37 are sized much shorter in length than seal 36 and are disposed at opposite ends of cap member 10 . preferably each foot 37 is spaced from the end edge of cap member 10 . if desired three or more feet 37 may be installed in the upstream groove 36 at spaced locations . thus , it will be seen that , in the case where the stoplog 2 is the bottommost one in the stoplog gate ( see fig1 ), the stoplog will rest on its seal 36 and feet 37 on the concrete bottom section 38 of the channel 24 , and seal 36 will form a substantially watertight seal with the concrete bottom of the channel . in the alternative situation where the stoplog is not the bottommost one in the stoplog gate , but rather seats itself on its seal 36 and feet 37 on a lower stoplog ( see fig2 ), seal 36 and feet 37 will rest on the upper channel member 4a of the next - lower stoplog 2a so that seal 36 forms a substantially watertight fit with the uppermost surface of the upper channel member 4a of that next - lower stoplog . in the latter case , in order that the lifting hooks 30 will not interfere with a proper mounting of seal 36 and feet 37 onto the upper channel member 4 of the next - lower stoplog , each lower end cap member 10 is also provided with a recess 40 which preferably runs the length of cap member 10 . recess 40 is sized and located relative to the lifting hooks 30 such that when one stoplog is located adjacent to and above another stoplog , the lifting hooks 30a from the lower stoplog will be received in the recess 40 and seal 36 and feet 37 from the upper stoplog will seat properly on the upper channel member 4a of the lower stoplog ( see fig2 ). in this respect it will be readily appreciated that since the recess 40 runs the length of each lower end cap member 10 , recess 40 will adequately receive the lifting hooks 30a regardless of where hooks 30a are positioned along the lifting hook channel 28a . the two vertical ends of the single rigid stoplog body which is formed by the united channel members 4 , 6 , 8 and 10 are each fitted with a side end cap 42 ( see fig1 and 3 ). side end caps 42 are sized slightly wider than the widths of channel members 4 , 6 , 8 and 10 , but are still sized slightly narrower in dimension than the width of vertical grooves 26 . each side end cap 42 is attached to channel members 4 , 6 , 8 and 10 by means of the two continuous welds 43 . each side end cap 42 is provided with a seal support extension 44 . each extension 44 runs the length of end cap 42 and , in conjunction with other portions of end cap 42 , defines a vertical groove 45 on the downstream side of the stoplog . each groove 45 serves to receive and support a seal 46 . seals 46 serve to assure a substantially watertight fit between the stoplog and liners 20 which define vertical grooves 26 , in a manner which will hereinafter be discussed . seals 46 are preferably formed of neoprene and are intended to be fixed in grooves 45 by means of a suitable cement . alternatively , a simple friction fit may be used to hold seals 46 in place within grooves 45 . as shown in fig1 side end caps 42 run from the top surface of upper channel member 4 to a point approximately equal in height to the top end of seal 36 . at the same time , seals 46 are sized somewhat greater in length than the vertical height of side end caps 42 , in order that the bottom ends of seals 46 may lie flush with the bottom surface of seal 36 and the top ends of seals 46 may lie flush with the top end surface of upper channel member 4 . seal 36 is sized such that it can properly abut with and form a watertight fit with seals 46 in order that no water can pass between seal 36 and seals 46 . seals 46 are sized relative to side end caps 42 and vertical groove liners 20 such that seals 46 can form a substantially watertight seal with the liners 20 when the stoplog 2 is placed in position within the stoplog gate and the stoplog is forced in a downstream direction by the flow of water within channel 24 . at the same time , however , seals 46 are sufficiently sized relative to side end caps 42 and groove liners 20 so that a stoplog 2 can be easily moved up and down within the vertical grooves 26 of the stoplog gate . each side end cap 42 also coordinates with channel members 4 , 6 , 8 and 10 so as to provide a vertical interior cavity 48 ( see fig3 ). vertical interior cavities 48 communicate with horizontal interior cavities 18 . vertical cavities 48 allow the horizontal cavities 18 to be flooded with water during installation , in order that the stoplog may be more easily seated in the gate . in addition , cavities 48 allow the horizontal cavities 18 to drain during withdrawal of the stoplog , thus lightening the weight of the stoplog . thus it will be apparent to one skilled in the art that when a first stoplog 2 , made in accordance with the preferred embodiment , is lowered into the stoplog gate &# 39 ; s vertical grooves 26 , the stoplog will drop to the bottom of the grooves so that its seal 36 and feet 37 and the bottom ends of seals 46 seat securely on the bottom section 38 of the channel 24 and form a watertight seal therewith . at the same time , seals 46 will form a watertight seal with vertical groove liners 20 as the flow of water in channel 24 forces the stoplog toward the downstream sides of liners 20 . in this way no water will be able to pass by the stoplog 2 so long as the level of the water in channel 24 is below the uppermost surface of upper channel member 4 . if the height of the water in channel 24 is greater than the height of a single stoplog 2 , and one desires to stop the flow of water within the channel , additional stoplogs can be added to the stoplog gate in the manner previously described . as pointed out above , such additional stoplogs will mate to one another so as to provide a substantially watertight barrier to the water . it will be readily appreciated by one skilled in the art that various modifications may be made to the preferred embodiment without departing from the scope of the present invention . thus , for example , one might choose to form channel members 4 , 6 and 8 in a shape other than u - shaped , e . g . as square or rectangular box sections . alternatively , one might elect to use more or fewer extruded channel members than the four used in the preferred embodiment . also contemplated are seals which have other cross - sectional shapes yet have substantially flat surfaces engaging the sides of the grooves in the channel members and the confronting surfaces of the groove liners 20 . by way of example the seals 46 may be t - shaped in cross - section , with the head of the t engaging the adjacent liner 20 . the stoplogs also may be made of a material other than aluminum , e . g ., steel . it is also contemplated that one might use a means other than welding , e . g . cementing , to secure the extruded channel members to one another . still another modification could involve disposing another seal 46 in the vertical groove 49 formed in each side end cap 42 . by appropriately dimensioning these additional seals 46 one could assure that each stoplog gate would be snugly held in grooves 26 in liners 20 regardless of the presence of a downstream flow in channel 24 . these and other changes of their type are foreseen as obvious to one skilled in the art , and within the scope of the present invention . in any event , the stoplogs offer the advantage of high strength , ease of manufacture and use , relatively light weight , durability , low cost replaceable seals , and water tight association with one another .
4
since an inventive concept of the present invention depends upon a control of elastic properties of a component of an article of footwear , in particular , an outersole , through intelligent design of the component &# 39 ; s shape , it will not be inappropriate to give a brief , qualitative , overview of aspects of solid elasticity or strength of materials which are especially relevant to this invention . a modulus of elasticity , or stiffness , may be understood generically in an engineering sense as a stress , or force per unit area , divided by a strain , or displacement per unit length . this means qualitatively , that for a test piece of given dimensions and a given mode of deformation ( such as bending ), a stiffer material , i . e . one with a higher modulus , will require a greater amount of force to achieve a given deformation or bending , or , conversely , will bend or deform less for a given application of force than a less stiff material . even given a simple elastomeric material , such as injection molded - rubber , it is still possible , and indeed , inevitable , to acquire non - directionally uniform elastic properties , or stiffnesses , in a finished article or component , based on a shape of the component . it will become clear through a consideration of the remaining specification and drawings that a novel design of an outersole of a shoe confers upon the outersole an advantageous set of elastic behaviors or moduli in response to forces encountered in use . in fig1 a a cross section of a block 50 of generic elastic material is shown , subject to a moment , represented by curved arrows 52 , 54 , tending to bend the block around an axis ( not shown ) perpendicular to a plane of the paper and lying above an upper surface 51 . in this context , it should be noted that “ elastic ” calls our attention to the idea that we are regarding the block as a uniform piece of material with respect to the laws of elasticity , rather than as a member of any particular class of materials , such as the elastomers . in the present invention , however , an elastomeric , or rubber - like , compound will be used for fabrication of an outersole 120 ( fig3 ); in particular , a composition of thermo plastic rubber ( tpr ) or ( natural ) rubber . as is well known , in a block subject to such a bending , a compressive stress , indicated by double - tailed arrow 56 and a tensile stress , indicated by double - headed arrow 58 , are set up in regions approximately bisected by a central plane 60 , as further shown in fig1 a . any modification to block 50 tending to reduce stresses represented by arrows 56 , 58 will result in a larger deflection ( not shown ) of the block in response to a given bending moment , and hence in a lower stiffness or enhanced flexibility . a modification to an elastic block as adumbrated above is shown in fig1 b . a series of stress - relief notches or grooves 64 , 64 ′ et alia are cut into a surface 66 of block 62 ; a remaining surface of block 62 is thereby partitioned into a plurality of lands ( not separately designated ) or treads . it can be appreciated for purposes of application of block 62 as an outersole of a shoe ( not shown ), whereby surface 66 serves as a bottom or exterior surface of an outersole , that an ability of block 62 to absorb and redistribute stresses resulting from contact with irregularities , such as pebbles , 68 , 70 protruding from a ground surface g , is either not substantially reduced or in fact increased by introduction of grooves 64 , 64 ′ et alia . irregularity 68 for example lying under a land or tread surface ( not designated ) meets an unimpaired thickness d of , in the present context , an elastomeric material , which thickness is indeed better able to deform into surrounding grooves than an equivalent volume in a monolithic material . irregularity 70 on the other hand lying within a groove ( not designated ) is seen to cause no deformation of block 62 . generally , only an obstacle or irregularity intersecting a wall 72 or floor ( ceiling ) 74 ( fig1 b ) of a groove may cause a larger deformation of an upper surface 76 of a grooved block 62 than would be caused in solid block 50 by an equivalent irregularity . grooves 64 , 64 ′ et alia do on the other hand clearly relieve tensile stresses of a nature indicated by double - headed arrow 58 , and increase flexibility in response to bending moments of a nature represented by arrows 52 , 54 in fig1 a , as illustrated in fig1 d . the following points will be seen to plausibly arise from an elementary consideration of elasticity , or the strength of materials , in connection with structures similar to those of the present invention ( reference may be made to fig2 ): a ) given a first sequence of parallel grooves 102 , 102 ′, 102 ″ cut into an elastic slab 100 , a stiffness in bending about an adjacent parallel axis 104 will increase as axis 104 is displaced towards increasing spacing of the first sequence of grooves ( i . e ., in a direction x ); similarly b ) given a second sequence of parallel grooves 106 , 106 ′, 106 ″ cut into elastic slab 100 , perpendicular to first sequence , a stiffness in bending about an adjacent parallel axis 108 will increase as axis 108 is displaced towards increasing spacing of the second sequence of grooves ; and c ) for small displacements , a bending about an oblique axis 110 , lying in a plane spanned by axes 104 and 108 , may be approximately decomposed into bendings about axes parallel to axis 104 and axis 108 , and a material response be predicted from a local stiffness as a function of an adjacent spacing of grooves parallel to axis 104 and grooves parallel axis 108 . in other words , it is asserted , a local stiffness or modulus resisting bending about an axis parallel to a surface of an elastic , or more particularly , an elastomeric slab , may approximately controlled in two independent directions by a spacing or linear density of locally perpendicular stress - relief grooves . reference will now be made to fig3 in comprehending application of these principles to the present invention . a shoe outersole 120 composed of an elastormeric , or rubber - like , material . sets of grooves 122 , 123 , 124 , 125 and 126 , 127 , 128 , 129 start at opposite lateral edges e , f respectively of outersole 120 . it may be observed that sets 122 - 125 and 126 - 129 maintain substantially parallel , and slightly converging , orientations , terminating on a rear or heelmost element of an opposing set of indentations , so that grooves 122 et alia terminate on groove 129 , while grooves 126 et alia terminate on groove 125 ; generally the grooves are curvilinear or arcuate in form , and particular families of curves of smoothly varying curvature , such as paraboli or hyperboli , for ease in achieving a simple and aesthetic product design . heel - most grooves 125 , 129 together form a substantially v - shaped groove or indentation , having an apex , as may be understood from consultation of fig3 . this apical rearmost groove demarks a boundary of a foresole region a of outersole 120 , simultaneously comprising a forward boundary of a bridge or metatarsal support 134 , which support includes a v - shaped cutout , receiving the apex . the bridge element or support , in one embodiment , also extends into a heel 142 of outersole 120 , which arrangement increases strength of the outersole , by eliminating a joint which might otherwise open up at a forward boundary 143 of the heel , relieving stress by simultaneously moving a frontal surface 145 of a heel - support joint ( not separately designated ) to a less flexible , central , portion of the heel , and extending the joint with lateral faces 147 , 149 . outersole lands ( not separately designated ) formed in interstices of grooves 122 , 126 et alia are decorated or finished with surface patterns or micro - treads 130 , 132 et alia ( not shown ) in order to improve sole traction , and give the product a finished and aesthetically pleasing appearance . foresole a further comprises a forward , or toe region , aa , and a rearward grooved or grid region ab , while the metatarsal support spans an arch region b of the outersole . a final rearward or heel region c completes a gross geography of the outersole . it will be appreciated in light of discussion accompanying fig2 that a curvilinear diamond or grid pattern 140 formed by grooves sets 122 - 125 and 126 - 129 in the foresole region , together with extensions of either groove set to lateral edges e , f , results in significant variations in stiffness with varying position in the forsole , these variations having substantially independent components about two major axes of bending . it is believed that the particular two - component / two - dimensional variation achieved confers a novel utility on the present invention . in particular , extensions of grooves 122 et alia and 126 et alia to the lateral edges confer a first added flexibility about a frontal axis 136 in proximity to the edges . however , it will be apparent from the above discussion that in a region of the diamond pattern 140 an added flexibility about axis 136 is taken up equally by grooves at approximately a 45 degree angle to the axis , so that the first added flexibility in maintained essentially constant from edge to edge in a region of the diamond pattern and a lateral extension ( not separately designated ) thereof . however , it will likewise be apparent that a second added flexibility about a longitudinal or sagittal axis 138 is created in the same region of the diamond pattern , and that this second flexibility is confined largely to a centroid ( not separately designated ) of the foresole . it may thus be appreciated that an advantageous flexibility is maintained corresponding to a phalangeal movement , or upward flexure of the toes , and to pronating and supinating movements , or rolling of a sole of the foot inwardly and outwardly about longitudinal axis 138 respectively , but , that this flexibility is confined to a centroid of the foresole , avoiding an edge rolling or bending flexure parallel to and in a vicinity of the lateral edges of the outersole . by these considerations a normal and necessary degree of pronation and supination is facilitated , while an excessive and generally deleterious degree of these motions is restrained . a relative depth of grooves 122 , 126 et alia and outersole 120 is also a substantive feature of the present invention . as shown schematically in fig1 b , an outersole has a total thickness d , and a groove depth g & lt ; d . in one embodiment of the present invention , in a ball region , or vicinity of axis 136 , the outersole has a thickness d = 7 mm and a groove depth g = 5 mm . thus a remaining , uncut , thickness of outersole amount to only 2 mm . thus , in light of discussion surrounding fig1 a - 1d , it may be appreciated that a flexibility or stiffness of the outersole to bending about axis 126 is governed by a dimensions of 2 mm , while a cushioning and distribution of stress from irregularities in a ground surface is governed by a material dimension of d = 7 mm . it may be readily apprehended that a degree of flexibility about frontal axis 136 and parallel translations thereof in a ( drawing ) plane of fig3 decreases in a heelward direction as bridge 134 , also known as a shank support , is encountered , and further as heel 142 is met , as will be appreciated from an inspection of fig5 a . in prior art , a steel shank support ( not shown ) will be utilized internal to a composite sole construction , rather than external elastomeric support or bridge 134 . the internal steel shank support will result in a sharper fall of flexibility in a shank or metatarsal region of the shoe , as shown by a dashed curve 147 in fig5 a . external support 134 thus provides more gradual variation and better design control of elastic properties of an outersole over a length of longitudinal axis 138 , then is allowed by prior art . fig5 a shows a schematic graph of flexibility or degree of deformation for a fixed system of applied forces ( not illustrated ) about a frontal axis 136 as varying along a longitudinal axis 138 for outersole 142 . flexibility , or inverse stiffness , is a measure of degree of deformation of a structure in response to a given system of forces , in this case , a system tending to bend outersole 120 around frontal axis 136 and parallel displacements thereof ; flexibility is shown increasing along a vertical graph axis 144 in fig5 a . it will be appreciated that a moderate degree of flexibility in a toe region aa , or foremost section of foresole a , reaches a maximum at a point p , corresponding roughly to a position of axis 136 , in a rearward or grid region ab of the foresole , as shown along a horizontal graph axis 145 . in arch region b an increasing thickness of metatarsal support 134 , in particular in taper region 144 , results in a decrease in flexibility , passing through a point q corresponding towards a low plateau value in heel region c . flexibility about longitudinal axis 138 in a vicinity of frontal axes 136 and 136 ′ is graphed in fig5 b and 5c respectively . as shown in fig5 b , longitudinal flexibility , measured along frontal axis 136 and shown increasing along a vertical graph axis 146 , is at a relative minimum at lateral edges e and f , passes through a maximum at a point r , corresponding roughly to a center line or longitudinal axis 138 . in contrast , longitudinal flexibility as varying across frontal axis 136 , passing through bridge or metatarsal support 134 , is at a relative maximum at points corresponding to lateral edges e and f , and passes through a minimum at a point s , approximately corresponding to a location of center line or longitudinal axis 138 . fig4 shows a schematic perspective view of the outersole of fig3 showing a conformation of grooves 122 , 126 et alia , and a taper or wedge region 144 of bridge 134 , and permitting a general comprehension of features of the outersole . it may also be added that a principal embodiment of the invention utilizes tpr giving a hardness of 50 - 55 degrees in a forepart , or regions a and b , of the outersole , softer than a typical standard of greater than 55 degrees hardness in the industry , as will be understood by those schooled in the art . fig6 a illustrates a flat blank 150 , which is cut from a sheet of thermo plastic rubber ( tpr ), for use in making an upper portion of a shoe . blank 150 has a first or outer edge 152 , a second or inner edge 154 , and rear - seam edges 156 , 158 , as well as an outer surface 155 and an inner surface 165 . in a first forming operation ( not illustrated ) blank 150 is manufactured into a first - stage preform 162 by means of a special use sewing machine , known in the art as a cap beat crease machine ( not shown ). the crease machine , in the control of a skilled operator , creates a series of small creases or crimps 160 , 160 ′, 160 ″ et alia , tending to contract or draw together outer edge 152 of blank 150 . blank 150 is thereby distorted into partially convex preform 162 , as illustrated in fig6 b . in order to complete formation of an upper , a second special use sewing machine ( not illustrated ), known in the art as a disc feed overseaming machine ( not shown ), is employed to join a non - woven fabric midsole or insole to the first - stage preform by stitching , in order to form a second - stage preform 170 , an item shown in fig6 c . contemporaneously with this stage of processing a rear seam 168 is sewn , joining rear - seam edges , and the preform is mounted on a rigid thermoplastic form 172 , or last . the last is shown in isolation in fig7 illustrating that a similarity in form to a human foot , and an inclusion of a post or mounting hole 174 , to facilitate handling of the second - stage preform . preform 170 is now essentially a fully formed upper , but must be subjected to further processing to relieve stresses and imbue the upper with a permanent shape of a finished shoe . in a first step of a thermal processing stage , the preform is subjected to a 100 to 110 degree centigrade vulcanizing treatment , which removes residual stresses , or a “ shape - memory ” of a prior flat form of blank 150 . subsequently to the vulcanizing treatment material of the preform or new upper is subjected to a controlled chilling in a second step of thermal processing . the controlled chilling sets the material in a new shape or conformation of a shoe upper . following the second step of thermal processing , preform , now upper , 170 , is ready for final affixement to outersole 120 in a bonding operation . a substantially uniform layer of adhesive is interposed between upper 170 and outersole 120 , the upper and outersole subsequently joined and held together until a curing of the adhesive . a layer of open weave or net fabric ( not shown ) may be interposed between upper 170 and outersole 120 to improve adhesion and reinforce cured adhesive via a fiber reinforcing principle . the bonding operation substantially completes structural assembly of the shoe , leaving only non - structural items such as an innersole , or insert , and ornamentation such as buckles or straps , which do not significantly alter structural characteristics of the footwear .
0
this application incorporates by reference the subject matter of u . s . application ser . no . 12 / 631 , 497 ( apparatus and method for searing , branding , and cooking , filed dec . 4 , 2009 ) and ser . no . 12 / 836 , 886 ( method , continuous apparatus , and burner for producing a surface - roasted product , filed jul . 15 , 2010 ). a pasteurization system and process made according to this invention preferably makes use of a flame pasteurizer . a continuous flame grill or roaster such as the unitherm ® flame grill ™ ( see fig2 ) or tunnel of fire ™ roaster ( see fig3 ) ( unitherm food systems , inc ., bristow , okla .) or its equivalent is a preferred flame pasteurizer . the flame pasteurizer should heat the surface of the root vegetable or product to a temperature sufficient to kill pathogens on the surface ( at least 145 ° f . or about 62 . 8 ° c . ), and the product should remain in the flame pasteurizer for a sufficient time to achieve at least a 1 log reduction listeria monocytogenes and alternate pathogens such as salmonella , e . coli , and other bacteria . preferably , the residence time for onions should be at least 30 seconds and no greater than 90 seconds ; with 45 to 60 seconds being ideal . some variance may occur based on onion size and temperature . the flame should make contact on the surface of the product and engulf a minimum of at least 65 percent of the total surface area . ideally , 100 percent of the surface area should be contacted and engulfed by the flame . preferably , the flame pasteurizer should have the ability to change the angle of flame from burner - to - burner to ensure heat - treatment of all exposed surfaces . for example , the burner could be arranged at an angle in the range of 5 ° to 60 ° from vertical . a first burner could be arranged at − x ° from vertical and a second burner could be arranged at + y ° from vertical , where x and y are the angle from vertical ( see fig2 ). preferably , x and y are the same magnitude . the surface of the product ( e . g ., an onion &# 39 ; s outer layer , a carrot &# 39 ; s or potato &# 39 ; s skin ) should be completely burned up to at least the outermost layer and controlled by time to leave the membrane under the first layer intact or mostly intact ( see e . g ., fig1 ). once the product is pasteurized , the membrane can then be removed mechanically or manually to leave a product that does not appear to have been flame pasteurized . once the product exits the flame pasteurizer it can be transferred as part of a continuous process without human intervention . this limits the possibly of re - contamination . at the discharge opening or exit of the flame pasteurizer , the surface of the product can be rinsed by spraying , deluging or submerging with clean , bacteria - free water to inhibit further heat transfer to the core , control the burn , and end the pasteurization process . product that is not subjected to water at the end of the flaming process can continue to burn . the core temperature of the product should be unaffected between the entrance point to the flame pasteurizer and the exit point from the water application . for example , product entering with a core temperature of 50 ° f . ( 10 ° c .) would exit from the water application with that same core temperature . in order for this process to work , and using onions as an example , the onions must be individually separated or have space around them ( e . g ., 10 or 20 onions evenly spaced across a belt , one - level deep ) as the onions pass through a ribbon flame or burner arrangement like that disclosed in the above patent applications . a continuous ribbon burner that encircles the cook belt is a preferred burner . in other embodiments of the invention , a gas infrared system that operates at surface temperatures of 1 , 000 ° f . or higher can ignite the skin of the onion for a similar effect . however , systems in the above patent applications are preferred because each makes use of a ribbon flame which fully engulfs the outer layer , ignites it , and burns the circumference sufficiently to achieve lethality . while infrared would work on a single - lane , the shadowing for multiple lanes could leave cold spots on which pathogens survive . as mentioned above , a product pasteurized by this system and process typically requires a quick wash to ready it for further processing . shrinkage is reduced relative to peeling processes . in tests conducted by the inventor , shrinkage was in the range of about 3 to 5 % by weight . 1 . in a gas flame - fired grill at unitherm food systems , inc . ( bristow , okla .) (“ unitherm ”) for microbial testing of process effectiveness on indigenous microorganisms ( aerobic plate count , yeast and mold ). 2 . in a gas flame - fired grill at unitherm for microbial testing of process effectiveness on non - pathogenic listeria innocua - inoculated onions . 3 . in a pilot - plant scale oven at the robert m . kerr food & amp ; agricultural products center ( stillwater , okla .) (“ fapc ”) to mimic the commercial process and test its effectiveness against listeria monocytogenes . indigenous bacteria on the surface of onions were plated on nonselective tryptic soy agar ( tsa ). a non - pathogenic , antibiotic resistant strain of listeria innocua will also be used to inoculate onions ( 24 - hrs in advance of use ) for processing through commercial ovens at unitherm food systems manufacturing facility . for processing in the pathogen - processing lab at the robert m . kerr food & amp ; ag products center ( stillwater , okla . ), four strains of pathogenic l . monocytogenes ( scott a - 2 , serotype 4b , clinical isolate ; v7 - 2 , serotype 1 / 2a , clinical isolate ; 39 - 2 retail hotdog isolate ; 383 - 2 ground beef isolate ) were used for inoculation of whole onions for processing on pilot plant scale equipment that mimics the commercial process . the listeria strains are all resistant to streptomycin ( 100 μg / ml ) and rifamycin s / v ( 10 μg / ml ). samples were plated on general - purpose agar ( tsa ) containing these antibiotics for selective enumeration of our inoculum on non - sterile product ( i . e ., this precludes the enumeration of other contaminating bacteria ). natural , whole onions ( with their indigenous microflora ) as well as surface - inoculated onions were inoculated with either listeria innocua ( at unitherm ) or a 4 - strain cocktail of l . monocytogenes ( at fapc ). plating was performed on potato dextrose agar for enumeration of yeast and mold . the process was evaluated by microbial enumeration of pre - process and postprocess levels of organisms . processing included preliminary trials to determine approximate processing times that would be used for microbial process testing . a gas - fired flame oven at unitherm was used for testing for lethality on indigenous organisms on onions and onions inoculated with nonpathogenic listeria innocua . testing of onions in a mimic system at the food pathogen processing lab at fapc was performed on indigenous organisms ( for comparison of processes ) as well as pathogen - inoculated onions using 4 - strain cocktail of listeria monocytogenes . data from the microbial recovery trials at different processing times were analyzed by one - way analysis of variance using the holm - sidak test for pairwise comparisons for significant difference in comparison with unprocessed onions . onions ( see fig5 ) were obtained locally ( sunset brand , white onions , # 4663 ) and were approximately 0 . 6 - 0 . 7 lbs / each ). they were held at room temperature prior to processing . a flame oven with continuously moving conveyor belt transported onions through the gas flame grill ( see fig4 & amp ; 6 ). a clean - in - place system was in place but not used . workers wore nitrile laboratory gloves to place onions on the grill ; other workers removed onions and placed them two - to - a - bag for microbial processing ( see fig9 & amp ; 11 ). one additional set of onions were rinsed by hose / water spray to remove the black ash prior to microbial sampling ( see fig1 ). a 50 - ml rinse was added to each bag of two onions , hand massaged for 3 - 5 min , and then approximately a 10 - ml sample was removed for microbial testing ; the sample was placed on ice and transported to fapc for microbial sampling later the same day . an additional set of onions were inoculated by rolling the onion in a white plastic tray lined with absorbant paper towels to which 60 mls of non - pathogenic listeria innocua ( 10 ml test tube of l . innocua + 50 ml 0 . 1 % bpw diluent ) was added ; this was replaced with a fresh inoculum solution after processing 4 onions ( see fig1 ). the inoculated onions were placed on the conveyor belt and processed in a similar fashion as the prior onions . the equipment was sanitized by a hypochlorite bleach solution . the flame grill does an effective job at ‘ burning off ’ the outer paper - like layer of the onions without damaging the onion ‘ meaty ’ layers ( see fig7 - 9 ). this will very likely reduce waste and increase yield of the process compared to mechanical peelers that remove a considerable amount of the onion “ meat .” the process achieved a nearly 5 - log reduction of indigenous bacterial contamination , 4 - log reduction of yeast and mold ( below level of detection after processing ), and a 6 - log reduction of inoculated listeria innocua ( see fig1 ). although some residual contamination was obtained after heating . this could be due to non - aseptic handling by gloved workers and by the ‘ hairy root ’ region of the onion which may be more difficult to eliminate indigenous / inoculated organisms .
0
[ 0015 ] fig1 illustrates a typical rear loading refuse collection truck of the type having a pair of sidewalls 20 , a top wall 22 , and bottom wall ( not shown ) forming a refuse collection body , generally at 24 . a rear load hopper assembly , generally at 26 , is mounted at the back of the collection body and includes sidewalls 28 and a curved bottom hopper wall 30 . the bottom hopper wall slopes upwardly toward a rearward sill or sill edge 32 , over which refuse is dumped into the collection hopper . for convenience , the directions corresponding to the front and rear of the truck will be the same as those used for the present invention . although the present invention is illustrated on a refuse collection vehicle , its utility is not limited to that application and it may be mounted on stationary or portable refuse collection stations or the like . the collection truck illustrated in fig1 is adapted for dumping residential style containers ( as shown for example in fig2 ). for dumping the residential style containers , the refuse collection truck in fig1 has two lifters 40 embodying the present invention mounted at the rear , although only one could also be used . also , the lifter of the present invention is not limited to rear mounting , but may also be side mounted or mounted directly on larger refuse collection containers that are either stationary or movable , for example , by refuse collection vehicle . before turning to a more detailed description of the lifter 40 , reference is made to fig2 which shows a typical residential roll out refuse collection container or cart 42 for which the present lifter is intended . the typical container 42 is made of rigid plastic construction , with a body 44 and a hinged lid 46 . a pair of wheels 48 allow the container to be conveniently moved curbside or to another pickup location . the front side of the container includes a generally recessed area 50 to accommodate lifter units on the refuse collection vehicle . for cooperation with such lifters , a pair of parallel , spaced - apart lift bars 52 are firmly secured in the container body in the recessed area 50 and provide upper and lower engagement surfaces ( upper and lower lift bars ) for engagement by a lifter . lid 46 is hingedly connected to the body , so that the lid is naturally opened by gravity when the container is inverted for dumping . it should be understood that refuse collection containers of the type shown , are available in a variety of styles and designs , and the present invention is not limited to any particular type style or design of refuse collection container . for example , some refuse carts have molded - in lift surfaces or areas instead of lift bars , and the lifter 40 is suited for those carts as well . turning to fig3 each lifter 40 attached to the back of the truck has the same basic construction . each lifter 40 includes a base or base plate 100 for attachment to the truck , container or lift station . a rotary hydraulic actuator 102 is welded , bolted or otherwise attached to the base , and includes a rotary output shaft 104 extending from at least one and preferably both ends . when mounted on the truck or container , the output shaft extends generally horizontally and has opposed ends that extend through each end of the cylindrical rotary actuator housing . a rotary hydraulic actuator of the type sold by helac corporation of enumclaw , wash ., usa , is preferred , although other types of rotary or other actuators may be used with the present invention . a lift or drive arm 106 is fixedly attached , as by a splined connection , to each end of the output shaft 104 , so as to rotate or pivot about the output shaft axis 132 as the output shaft is rotated . there is at least one , and preferably two , lift arms having first and second ends , the first end being attached to the output shaft 104 and the terminal or second ends of the lift arms being connected by a cross member 108 . the cross member mounts a saddle or hook 110 of engaging and lifting the upper bar or lift surface 52 of the refuse container or cart 40 . for capturing the cart and holding it when inverted , the lifter 40 includes a lower hook actuation assembly , generally at 112 , for moving a lower hook 114 to a position over the lower bar or engagement area 52 . this actuation assembly includes at least a first actuator arm 116 ( and preferably two such arms ), that is pivotally attached at a first end to the lift arm 106 at a location intermediate the ends of the lift arm , and a second actuator arm 118 that is pivotally attached at a first end to the base 100 by way of brackets 119 . an identical actuator arm pair is employed on each side of the lifter , and description of one pair will suffice for the other as well . more specifically , the first actuator arm is preferably pivotally attached to the lift arm , as seen in fig4 between the first end and the mid - point of the lift arm , and near or in the proximity to the first end or to the output shaft 104 . the other or second ends of the actuator arms are cooperatively attached to an extension assembly , such as a telescoping arrangement , having first and second relatively movable members , such as inner and outer members of a telescoping assembly , generally at 120 . the extension assembly is operable to move the lower hook downwardly , in a direction away from the upper hook , as the lifter rotates from the lower retracted position to the raised and inverted dumping position . more specifically , in the illustrated embodiment , the second end of the first actuator arm is fixed , as by welding or the like , to a steel rod 122 that forms the inner member of the relatively slidable or telescoping arrangement , generally at 120 . the other or second end of the second actuator arm 118 is pivotally fixed to a hollow steel cylinder or sleeve 124 that forms the outer member of the relatively slidable or telescoping arrangement , and slidably receives the steel rod 122 within the bore of the cylinder . as shown more clearly in fig5 and one or more of the applications incorporated by reference above , the sleeve 124 is slotted to receive the first actuator arm as the rod moves into the sleeve . these parts could , of course , be reversed without departing from the present invention . as illustrated , cross member 126 extends between and is attached to each of the cylinders or sleeves 124 . the cross member mounts the lower hook 114 for capturing the lower bar or engagement area 52 of the container 42 . the hook may be spring biased and is flanked by a pair of rollers 128 for protecting the side of the cart or container against damage from the lower hook . in operation , the elongated lift arms 106 , which rotate with the output shaft of the actuator , form a fixed radius of rotation for the upper hook . in the retracted position , as seen in fig4 the elongated lift arms hang nearly vertically downwardly , and the upper hook is located at the bottom end of the lift arms in proximity to the lower hook . this lower location allows the upper hook to sweep upwardly from a very low position and catch beneath the upper bar 52 or engagement surface of a container , as the lifter is rotated to a raised and inverted position . this is particularly advantageous because it allows to lifter to be mounted at different heights , depending on the particular vehicle or location where mounted , and still be very effective in lifting and dumping containers . as seen , for example in fig6 and 7 , the lifter may be mounted at very different heights and still function effectively in lifting and dumping containers , due the very low position of the upper hook when the lifter is in the retracted position . the movement of the lower hook is effected by the actuator arms 116 and 118 and the extension or telescoping assembly 120 . the second actuator arms are pivotally attached to the base 100 at a pivot axis 130 spaced above and slightly rearward of the pivot axis 132 of the rotary hydraulic actuator 102 . as a result of the relative spacing of the axes , when the lifter moves rearwardly and upwardly , second actuator arm effectively pushes the sleeve or cylinder 124 and the first actuator arm effectively pulls on the inner rod 122 , such that the second cylinder or sleeve 124 slides downwardly or outwardly along the steel rod 122 , telescoping apart and increasing the distance between the upper and lower hooks 110 and 114 to capture the container or cart by capturing the lower bar or engagement surface 52 under the lower hook 114 . the reverse movement takes place during retraction of the lifter . the lift arm are rotated clockwise ( as seen in fig6 and 7 ), bringing the upper hook to a lowermost position as seen in fig3 and 7 , with the lift arms extending vertically downward . the relative spacing between the axes of rotation 130 and 132 cause the rod and cylinder to telescope together reducing the distance between the hooks and raising the lower hook . as is apparent from the drawings ( e . g ., fig3 ), when the lifter is in the retracted position the actuator and lift arms are located in a low - profile , nesting arrangement in which the actuator and lift arms extend substantially vertically downward , with the first actuator arm 116 being located between the lift arm 106 and second actuator arm 118 . the lift arm is of sufficient length that when in the retracted position , the upper hook 110 is located just above , or proximal to the lower hook 114 . although the dimensions may vary , the lifter in accordance with the present invention may have a total length ( in the retracted position ) of about 23⅛ inches , a width of about 21⅞ inches and a depth or thickness of about 6 inches . such a lifter may be mounted at a height of from about 35½ inches up to about 53½ inches , and still work well in lifting and dumping typical collection carts in containers having an upper lift bar at about 34 - 35 inches above ground level . with the illustrated features of the present invention , the upper and lower hooks are in proximity when retracted but spaced apart ( e . g ., 14 - 15 inches apart ) in the dumping position to capture the lift surfaces of the container . because the upper hook rotates upwardly from an extreme lower position , it is able to engage under the upper lift surface in its normal path of travel , and it is unnecessary for the operator to lift or tilt the container in order to engage it properly with the upper hook . although described in terms of the illustrated and preferred embodiments , the present invention is not limited to the exact form or variety shown , and may take such other forms as may be immediately apparent from the above description or which may become apparent only after some study of the above lifter .
1
referring to the drawings in detail wherein like elements are indicated by like numerals , there is shown an embodiment of the totelock 1 of the present invention . in the example shown , the computer 5 is a laptop computer and the disk drive 3 is a 31 / 2 inch floppy drive . the computer secured could be a smaller notebook computer or a larger personal computer . the floppy drive 3 has a pivotal entry door ( not shown ) through which a 31 / 2 inch diskette ( not shown ) is inserted . when inserted the diskette engages a pair of rails 7 or equivalent guides for positioning the diskette when inserted into the drive 3 . the rails or guides 7 are usually made with small tab holes or protruding guide tabs 8 near to the drive 3 entry door . the totelock 1 consists of two plates 10 , 30 manufactured from rigid material . in this embodiment of the invention they are made from stainless steel . the plates 10 , 30 are of a size such that they will fit into a disk drive 3 of a computer 5 much like a diskette . the plates may be designated as a first plate 10 and a second plate 30 . the first plate 10 has a generally rectangular shape , with a front edge 11 , a back edge 12 , a right side edge 13 , a left side edge 14 , top 15 and bottom 16 surface planes , a predetermined length measured from the front edge 11 to the back edge 12 , and a predetermined width measured from the right edge 13 to the left edge 14 . the back edge 12 is defined as that edge first moved through the disk drive entry door . the bottom surface plane 16 is defined as that surface immediately engaging the guide rails 7 . the front edge 11 is formed into a plate shoulder 17 having a width larger than the width of the back edge 12 . the plate contains a body portion 19 defined as the area between the plate shoulder 17 , back edge 12 and bordered by the right and left side edges 13 , 14 . the back edge 12 width is nearly the width of the disk drive entry door . the first plate 10 also has a lock hole 18 formed in and substantially centered on the width of the plate shoulder 17 . the first plate 10 has a pair of tabs extending down from the bottom plane 16 . a right tab 20a and a left tab 20b of a predetermined length and predetermined distance from the front edge 11 and right 13 and left 14 edges , extend from the bottom surface plane 16 of the plate 10 at an angle of approximately seventy degrees measured from the plane defined by the area between the tabs 20 and the front edge 11 . the first plate 10 is inserted into the disk drive 3 and the tabs 20a and 20b position themselves into the guide rail tab holes or over the guide rail protruding guide tabs 8 . the first plate shoulder portion 17 and lock hole 18 remain outside the disk drive 3 when the first plate 10 is properly inserted into the disk drive 3 . the second plate 30 is approximately the same size and shape as the first plate 10 . the second plate 30 has a front edge 31 , a back edge 32 , a right edge 33 , a left edge 34 , top 35 and bottom 36 surface planes , a predetermined length measured from the front edge 31 to the back edge 32 , and a predetermined width measured from the right edge 33 to the left edge 14 . the second plate 30 also has a shoulder 37 formed along the front edge 31 and having a width larger than the width of the back edge 32 . the plate 30 also contains a body portion 39 defined as the area between the plate shoulder 37 , back edge 32 and bordered by the right and left side edges 33 , 34 . the second plate 30 has a lock hole 38 formed in and substantially centered on the width of the plate shoulder 37 . the second plate 30 is inserted into the disk drive 3 , through the entry door , onto the top surface plane 15 of the first plate 10 such that the second plate bottom surface plane 36 lies flat against the first plate top surface plane 15 . the second plate 30 has a pair of ridges 40 formed on its top surface plane 35 along the body portion 39 . the ridges 40 run from the shoulder portion 37 parallel to the right and left side edges 33 , 34 to the proximate area of the back edge 32 . the ridges 40 have a rounded profile . when inserted into the disk drive 3 , the ridges 40 are entirely inside the disk drive housing 4 . the right ridge 40a and left ridge 40b have a predetermined length and height , and are positioned a predetermined distance from the front edge 31 . the ridges 40a and 40b extend parallel to one another and the right and left edges 33 , 34 of the plate 30 , from the plate shoulder 37 toward the back edge 32 . the right ridge 40a and the left ridge 40b extend up away from the plate top surface plane 35 . the second plate 30 lock hole 38 formed in the shoulder portion 37 remains outside the disk drive housing 4 when the plate 30 is properly inserted into the drive slot . the lock hole 38 on the second plate 30 aligns with the lock hole 18 on the first plate 10 . the two plates 10 , 30 can then be locked together with a padlock 2 or other locking means . when the two plates 10 , 30 are locked together , they cannot as a pair be removed from the disk drive 3 without breaking the disk drive 3 itself . when both plates 10 , 30 are inserted and locked together , the disk drive 3 is unusable . in another embodiment , the padlock or locking means can be combined and tethered with an anti - theft means , such as a steel cable 6 having loops at both ends , and the computer 5 can be secured to a fixed object , such as a table 9 . the plates 10 , 30 as a pair are not removable from the disk drive 3 because of the tabs 20 on the first plate 10 , and the ridges 40 on the second plate 30 . the overall height of the tabs 20 combined with the ridges 40 , makes the combined height of the plates 10 , 30 too large to be removed as a pair from the computer disk drive 3 . the two plates 10 , 30 are designed such that they cannot be removed together and must be removed one at a time . to remove the plates 10 , 30 , the padlock 2 or other locking means must be removed , and the second plate 30 pulled from the disk drive 3 . the first plate 10 is then urged slightly further into the disk drive 3 and lifted upwardly thereby disengaging the tabs 20 from the guide rail tabs or holes 8 . the first plate 10 is then removed from the disk drive 3 . the disk drive 3 can then be utilized and the computer 5 can be moved to another location . it is understood that the above - described embodiment is merely illustrative of the application . other embodiments may be readily devised by those skilled in the art which will embody the principles of the invention and fall within the spirit and scope thereof .
8
the present invention relates to a vibration damper mechanism that connects a vacuum pump , particularly a turbo pump , to a vacuum chamber . the vibration damper mechanism consists of a flexible elastomer diaphragm that connects the pump to the chamber and enables the pump to move in all directions . the elastomer diaphragm provides a vacuum - tight seal . according to a preferred embodiment , the vibration damper mechanism consists of three or more dampers that carry the vacuum load and pump mass and isolate the pump vibration from the chamber . the dampers can utilize three or more different concepts of damping : the first , an elastomer damper with intermediate mass ; the second , an integrated air or pneumatic damper , the third a tuned damper wherein the pump &# 39 ; s main speed is tuned to the damper &# 39 ; s resonance via a closed loop . these concepts will be described in more detail with reference to the figures . referring to fig2 a , there is shown a sectional illustration of a pump ( 1 a ) with a damper mechanism constructed and operative in accordance with one embodiment of the present invention . in this embodiment , vacuum pump ( 1 a ) is connected to a base ( 2 ) via a standard vacuum - tight flange , iso style or other . a sandwich of two elastomer diaphragms ( 3 ) is built with one side on the base ( 2 ). the other side of these diaphragms ( 3 ) is connected to a static flange ( 4 ), which is coupled to the vacuum chamber . these double diaphragms are vacuum - tight and sealed to base ( 2 ) and static flange ( 4 ). the static flange ( 4 ) is connected to a vacuum chamber ( 5 ) via a standard vacuum flange , iso style or other . since gas permeation through the elastomer diaphragms ( 3 ) may be large , the space between the two diaphragms is connected via a tube ( 9 ) to the outlet of the vacuum pump ( 10 ), which is connected to a roughing pump . this serves to reduce the pressure between the diaphragms ( 3 ), thereby providing a double seal with an intermediate pump . according to an alternative embodiment of the invention , illustrated in fig2 d , the vacuum sealing may consist of a very thin metal diaphragm ( 31 ) whose ends are sealed by an elastomer , shaped , in this example , as two o - rings ( 32 ) on each side of the metal diaphragm . one side of the diaphragm 31 is mounted on the base ( 2 ) of the pump and the other side is mounted on a static flange ( 4 ) coupled to the vacuum chamber . in this way , the metal does not contact the vacuum chamber , and the elastomer serves to absorb the vibrations . in this option , only one diaphragm is required . since the atmospheric pressure tends to pull the vacuum pump into the vacuum chamber , it is essential to connect additional dampers between the vacuum pump and the vacuum chamber . in the embodiment of fig2 a , three additional dampers are provided . these dampers consist of two conventional elastomer dampers ( 6 ) with a damping mass ( 7 ) connected between the two elastomer dampers ( 6 ). a post ( 8 ), connected to the pump , supports the dampers . another way to achieve damping is shown in fig2 b , a sectional illustration of a pump ( 1 a ) with a damper mechanism constructed and operative in accordance with another embodiment of the present invention . pump ( 1 a ) is connected to the vacuum chamber ( 5 ) via a double elastomer seal ( 3 ), substantially as shown and described in fig2 a , and via a pneumatic vibration isolator ( 20 ) mounted between a static flange ( 4 ) coupled to the vacuum chamber and a post . the pneumatic damper ( 20 ) is connected to a pressurized air supply ( 21 ). another way to achieve a pneumatic vibration damper is shown in fig2 e . in this embodiment , the base ( 2 ) is connected to the static flange ( 4 ) by a flexible diaphragm ( 43 ), thus creating an annular volume ( 44 ). pressurizing this volume ( 44 ) from a source of pressurized air ( 41 ) serves to create the force needed to overcome the vacuum forces , thus achieving a pneumatic vibration isolator . still another way to achieve additional vibration isolation is shown in fig2 c , a sectional illustration of a pump ( 1 a ) with a damper mechanism constructed and operative in accordance with a further embodiment of the present invention . in this embodiment , a tuned damper is connected to the base of existing dampers . this embodiment can apply to the embodiment with elastomer dampers as well as to the embodiment having a pneumatic damper . the tuned damper consists of a spring ( 12 ) and a mass ( 13 ). the resonance frequency of the mass - spring system is roughly tuned to the pump main speed frequency . it is a particular feature of the present invention that this exact tuning is accomplished , not by adjusting the frequency of the tuned damper , as in conventional systems , but by adjusting the rotational speed of the pump to the frequency of the tuned damper . thus , an accelerometer ( 15 ) is coupled to the mass of the tuned damper and the acceleration of the mass measured . changing the rotational speed of the pump maximizes the acceleration measured by this accelerometer . when maximum acceleration of the mass is achieved , the rotational speed of the pump is exactly at the tuned mass frequency , which is optimal . it will be appreciated that the tuned damper frequency is designed to be at the desired rotational speed of the pump . it is a particular feature of the present invention that the damper mechanism is a horizontal system , not vertical as in conventional systems . thus , the pump is closer to the chamber and the damper can be very short . in this way , the pumping speed that is achieved in the chamber is very similar to the basic pumping speed of the pump . while the invention has been described with respect to a limited number of embodiments , it will be appreciated that many variations , modifications and other applications of the invention may be made . it will further be appreciated that the invention is not limited to what has been described hereinabove merely by way of example . rather , the invention is limited solely by the claims , which follow .
5
it has been fortuitously and unexpectedly discovered that novel ink compositions according to embodiments of the present disclosure advantageously exhibit desirable rheological properties . in addition , modified pigments , formulations , and methods of making modified pigments and formulations , are described . exemplary embodiments of the disclosed modified pigments , when used in ink formulations , produce images of high gloss , uniform area fill , and / or good black / color mixing . embodiments of the disclosed modified pigments have high stability , low viscosity , and compatibility with multiple solvent and paper types , as compared to other pigments . as shown in fig1 , embodiments of the ink composition 10 include both polymeric binders b attached to a pigment p and unattached / free polymeric binders f dispersed throughout a vehicle 16 . it is contemplated that the viscosity of the ink composition 10 may be lowered when the attached polymeric binders b and free polymeric binders f are chemically similar . without being bound to any theory , it is believed that this reduction in viscosity may be due in part to the addition of the chemically similar free polymeric binders f , which may substantially reduce electrostatic and / or electrosteric interactions between the attached binders b and the vehicle 16 . it is to be understood that the vehicle 16 is an aqueous vehicle in embodiments of the present disclosure . as used herein , “ aqueous vehicle ” refers to the vehicle 16 in which pigment / colorant p is placed to form an ink composition 10 . ink vehicles are known in the art , and a wide variety of ink vehicles may be used with embodiments of the compositions , systems and methods of the present disclosure . such aqueous vehicles 16 may include solvents , including but not limited to glycols , amides , pyrrolidones , and / or the like , and / or mixtures thereof in amounts ranging between about 0 . 01 and 20 wt %; alternately , between about 0 . 01 and 7 wt %; or between about 0 . 01 and 4 wt %. aqueous vehicles 16 may also optionally include one or more water - soluble surfactants / amphiphiles in amounts ranging between about 0 and 5 wt %; alternately , between about 0 . 1 and 2 wt %. the balance of the aqueous vehicle 16 is generally water in embodiments of the present disclosure . in embodiments of the ink composition 10 , one or more co - solvents may be added to the aqueous vehicle 16 in the formulation of the ink composition 10 . examples of suitable classes of co - solvents include , but are not limited to , aliphatic alcohols , aromatic alcohols , diols , caprolactams , lactones , formamides , acetamides , long chain alcohols , and mixtures thereof . examples of suitable co - solvent compounds include , but are not limited to , primary aliphatic alcohols of 30 carbons or fewer , primary aromatic alcohols of 30 carbons or fewer , secondary aliphatic alcohols of 30 carbons or fewer , secondary aromatic alcohols of 30 carbons or fewer , 1 , 2 - alcohols of 30 carbons or fewer , 1 , 3 - alcohols of 30 carbons or fewer , 1 , 5 - alcohols of 30 carbons or fewer , n - alkyl caprolactams , unsubstituted caprolactams , substituted formamides , unsubstituted formamides , substituted acetamides , unsubstituted acetamides , and mixtures thereof . some specific suitable examples of co - solvents include , but are not limited to 1 , 5 - pentanediol , 2 - pyrrolidone , 1 , 2 - hexanediol , 2 - ethyl - 2 - hydroxymethyl - 1 , 3 - propanediol , diethylene glycol , 3 - methoxybutanol , 1 , 3 - dimethyl - 2 - imidazolidinone , and mixtures thereof . the co - solvent concentration may range between about 0 . 01 wt . % and 50 wt . %. in an embodiment , the co - solvent concentration ranges between about 0 . 1 wt . % and 20 wt . %. in embodiments of the ink composition 10 of the present disclosure wherein water - soluble surfactants are added to the aqueous vehicle , it is to be understood that these surfactants may be added as free components to the ink composition 10 and are not otherwise associated or intended to become part of the polymeric binders b / unattached binders f described herein . non - limitative examples of suitable surfactants include fluorosurfactants , non - ionic surfactants , amphoteric surfactants , ionic surfactants , and / or mixtures thereof . examples of suitable surfactants include , but are not limited to the following commercially available tradenames : zonyls ( fluorosurfactants ), available from e . i . du pont de nemours and co . located in wilmington , del . and tergitols ( alkyl polyethylene oxides ), available from union carbide in piscataway , n . j . examples of amphiphiles / surfactants that may be used in embodiments of the present disclosure include , but are not limited to iso - hexadecyl ethylene oxide 20 and amine oxides , such as n , n - dimethyl - n - dodecyl amine oxide , n , n - dimethyl - n - tetradecyl amine oxide , n , n - dimethyl - n - hexadecyl amine oxide , n , n - dimethyl - n - octadecyl amine oxide , n , n - dimethyl - n -( z - 9 - octadec - enyl )— n - amine oxide , and mixtures thereof . the concentration of the amphiphiles / surfactants may range between about 0 wt . % and 5 wt . %. in an embodiment , the concentration of amphiphiles / surfactants ranges between about 0 . 1 wt . % and 2 wt . %. it is to be understood that various types of additives may be employed in the ink composition 10 according to embodiments of the present disclosure to optimize the properties of the ink composition 10 for specific applications . for example , biocides may be used in an embodiment of the ink composition 10 to inhibit growth of microorganisms . one suitable non - limitative example of a biocide is commercially available under the tradename proxel gxl ( a solution of 1 , 2 - benzisothiazolin - 3 - one ( bit ), sodium hydroxide , and dipropylene glycol ) from avecia inc . located in wilmington , del . sequestering agents such as edta may be included to substantially eliminate potential deleterious effects of heavy metal impurities ( if any ). buffer solutions may be used to control the ph of the ink composition 10 , as desired and / or necessitated by a particular end use . the ink composition 10 according to embodiments of the present disclosure includes pigment p dispersed throughout the aqueous vehicle 16 . it is to be understood that any suitable pigment p that is capable of having polymeric binders b attached thereto may be used . some non - limitative examples of suitable pigments include those supplied by cabot corp . in billerica , mass . non - limitative examples of some suitable polymer b attached pigments p are described in u . s . pat . no . 6 , 432 , 194 assigned to cabot corporation and issued to johnson et al . entitled “ method of attaching a group to a pigment ,” which patent is incorporated herein in its entirety . the pigment p may have any suitable polymeric binders b attached thereto . the attached polymeric binders b may be selected using a variety of parameters including , but not limited to molecular weight , acid number and / or the type of monomers within the polymeric binders b . in one embodiment , the molecular weight of the attached polymeric binders b ranges between about 4 , 000 and about 20 , 000 . in another embodiment , the acid number of the attached polymeric binders b may range between about 50 and about 300 . examples of suitable monomers within the polymeric binders b include , but are not limited to styrene , acrylic acid , substituted acrylic acids , maleic anhydride , and / or substituted maleic anhydrides . in addition , the pigment p can include pigments such as those described in more detail in part b . some non - limitative examples of polymeric binders b capable of attaching to the pigment p are polyurethane resins , styrene - acrylic resins / polymers / copolymers , styrene - maleic anhydride resins / polymers / copolymers , styrene - acrylic resins / polymers / copolymers having ethylene and / or propylene glycol graphed thereto , styrene - maleic anhydride resins / polymers / copolymers having ethylene and / or propylene glycol graphed thereto , and combinations thereof . styrene - acrylic resins / polymers / copolymers having ethylene and / or propylene glycol graphed thereto and styrene - maleic anhydride resins / polymers / copolymers having ethylene and / or propylene glycol graphed thereto , are discussed in more detail in part b ( e . g ., fig1 and 2 ). some suitable polyurethane resins are commercially available from avecia in manchester , england . some suitable styrene - acrylic resins / polymers are commercially available under the tradenames joncryl 586 ( j586 ), joncryl 671 ( j671 ) and joncryl 696 ( j696 ) from johnson polymer , inc . located in sturtevant , wis ., and sma ( styrene maleic anhydride ) polymers available from sartomer located in exton , pa . in an embodiment , the pigment p having polymeric binders b attached thereto is present in an amount ranging between about 1 wt . % and 10 wt . % of the ink composition and about 0 . 5 to 2 wt . % of the ink composition . in an alternate embodiment , the pigment p having polymeric binders b attached thereto is present in an amount ranging between about 3 wt . % and 5 wt . % of the ink composition 10 . an embodiment of the ink composition 10 further includes at least one unattached / free polymeric binder f dispersed throughout the aqueous vehicle 16 . it is to be understood that the unattached polymeric binders f may be substantially homogeneously and / or non - homogeneously mixed throughout the aqueous vehicle 16 . in an embodiment , the unattached polymeric binders f are present in an amount ranging between about 0 . 1 wt . % and 6 wt . % of the ink composition . in an alternate embodiment , the unattached polymeric binders f are present in an amount ranging between about 1 wt . % and 3 wt . % of the ink composition 10 . in an embodiment of the ink composition 10 of the present disclosure , selected unattached polymeric binders f are formed from a polymeric material that is chemically similar to the selected attached polymeric binders b . “ chemically similar ” as defined herein denotes compounds that have the same or similar molecular weight , acid number and / or monomer composition . it is to be understood that “ similar ” in regard to molecular weights as defined herein is contemplated to encompass compounds having molecular weights ranging between about 4000 and 18000 . similar to the attached polymeric binders b , in an embodiment of the ink composition 10 , the molecular weight of the unattached polymeric binders f ranges between about 4 , 000 and 20 , 000 , and the acid number ranges between about 50 and 300 . non - limitative examples of suitable unattached polymeric binders f include the polyurethane resins and styrene - acrylic resins / polymers as previously described in reference to the attached polymeric binders b . it is believed , without being bound to any theory , that when the unattached polymeric binders f and the attached polymeric binders b are chemically similar , the electrostatic and / or electrosteric interactions between the attached polymeric binders b and the aqueous vehicle 16 may be substantially reduced . this reduction may advantageously help to lower the viscosity of the ink composition 10 . the viscosity of the ink composition 10 of the present disclosure ranges between about 2 cps and 10 cps . in an alternate embodiment , the viscosity of the ink composition 10 of the present disclosure ranges between about 2 cps and 6 cps . the reduced viscosity of the ink composition 10 may advantageously help to improve ink reliability , ink durability , and print quality . fig2 illustrates an embodiment of the ink composition 10 deposited on a substrate 14 to form a pigmented ink system 12 . it is to be understood that the ink composition 10 may be deposited on the substrate 14 using any suitable printing technique , such as an ink jet printer . examples of suitable substrate 14 materials include , but are not limited to cellulosic materials ( e . g ., paper materials ), wood , textile materials , polymeric materials , metals and / or mixtures thereof . in a method of making an embodiment of the ink composition 10 , an amount of the pigment p having polymeric binders b attached thereto is admixed in a selected aqueous vehicle 16 to form an ink fluid . further , at least one unattached polymeric binder f may be admixed with the ink fluid to form the ink composition 10 . it is to be understood that the materials described above may be selected and that the attached polymeric binders b are substantially chemically similar to the unattached polymeric binders f . to further illustrate the present disclosure , the following examples are given . it is to be understood that these examples are provided for illustrative purposes and are not to be construed as limiting the scope of the present disclosure . table 1 of part a illustrates various examples of the ink composition 10 according to embodiments of the present disclosure . the examples labeled a - j , list the ingredients used , the viscosity of the embodiment of the ink composition 10 . comparing ink compositions c and d illustrates how the addition of unattached binders b may reduce the viscosity of the final ink composition 10 . example c contains cabot pigment with joncryl 671 attached thereto and no unattached binders in the aqueous vehicle 16 . the viscosity of ink composition c was 10 . 45 cps . example d contains the same composition as example c with the addition of 2 wt . % unattached joncryl 671 . the viscosity of example d was lowered to 6 . 3 cps , making the ink composition 10 more desirable for printing . without being bound to any theory , it is believed that the slight rise in viscosity between ink composition a and ink composition b may be due to the following . in this case , both the attached polymeric binder b and free polymeric binder f have low molecular weights , and the pigment p - binder b interactions are less than the vehicle 16 - binder b interactions . therefore , the ink viscosity increases slightly because of the vehicle 16 - binder b interaction . in other examples , the molecular weights of the polymers are higher ; thus there is more pigment p - vehicle 16 interaction . the ink compositions 10 according to embodiments of the present disclosure may offer many advantages , examples of which include , but are not limited to the following . the combination of the chemically similar attached polymeric binders b and unattached polymeric binders f may advantageously lower the viscosity of the ink composition 10 . the lower viscosity may result in improved pen reliability , ink durability , and / or high print quality . still further , the addition of unattached polymeric binders f that are chemically similar to the attached polymeric binders b may advantageously reduce the electrostatic and / or electrosteric interactions between the attached polymeric binders b and the aqueous vehicle 16 . in general , the modified pigment in fig3 includes , but is not limited to , a styrene - maleic anhydride co - polymer having a polyethylene glycol ( peg ) and / or polypropylene glycol ( ppg ) compound grafted thereon . the styrene - maleic anhydride co - polymer is attached covalently to a sulfatoethylsulfone - pigment via an amine - thio linkage ( hereinafter “ modified pigment a ”). typically , the peg / ppg and the sulfatoethylsulfone - pigment are disposed on different monomers of maleic anhydride . the modified pigment a is substantially resistant to chemical attacks from acids , bases , and salts . in addition , the modified pigment a is miscible with various co - solvents due , at least in part , to the ethylene glycol and / or propylene glycol . fig3 illustrates an embodiment of a representative reaction mechanism to produce the modified pigment a . a styrene - maleic anhydride co - polymer is provided and then reacted with aet - hcl ( aet = nh 2 ch 2 ch 2 sh ), and an amine terminated peg and / or ppg with a base ( e . g ., triethylamine ), where the components are in a solvent such as , but not limited to , dimethyl sulfide ( dms ). under typical reaction conditions , the ph is basic ( e . g ., above 10 . 5 ). the product of the reaction is the styrene - maleic anhydride co - polymer having an amine - thio linkage on a maleic anhydride monomer and an amine terminated peg and / or ppg on a different maleic anhydride monomer . the monomers can be randomly arranged or block arranged . the percentage of amine terminated peg and ppg grafted onto the styrene - maleic anhydride co - polymer backbone can range from about 0 . 01 to 90 %, about 0 . 01 to 50 %, or from about 5 to 20 % based on the anhydride groups . next , the product is reacted with naoh , a sulfatoethylsulfone - pigment , and sodium acrylate to produce modified pigment a . under typical reaction conditions , the ph is basic ( e . g ., above a ph of 10 . 5 ). the amount of the styrene - maleic anhydride co - polymer covalently bonded to the surface area of the sulfatoethylsulfone - pigment can range from about 0 . 01 to 50 %, about 0 . 01 to 20 %, or from about 5 to 15 %. the ratio of n to m can be about 1 . 1 , about 2 : 1 , about 3 : 1 , and about 4 : 1 . the value of o and p can each be from about 5 to 100 %, about 5 to 50 %, or about 5 to 10 % of the value of m . the molecular weight of the styrene - maleic anhydride co - polymer having peg and / or ppg ( e . g ., peg , ppg , and combinations thereof ( e . g ., co - polymers thereof )) grafted thereon can range from about 1000 to 100 , 000 , about 1000 to 30 , 000 , or about 1000 to 10 , 000 . the molecular weight of peg can range from about 300 to 10 , 000 mw , about 300 to 5 , 000 mw , about 500 to 2 , 000 mw . the molecular weight of ppg can range from about 300 to 5 , 000 mw , about 300 to 2 , 000 mw , or about 300 to 1 , 000 mw . the molecular weight of the co - polymer of polyethylene glycol and polypropylene glycol can range from between about 300 to 10 , 000 mw , 300 to 5 , 000 mw , or from 300 to 2 , 000 mw . in general , the modified pigment in fig4 includes , but is not limited to , a styrene - acrylate co - polymer having a peg and / or ppg grafted thereon , attached covalently to a sulfatoethylsulfone - pigment via an amine - thio linkage ( hereinafter “ modified pigment b ”). typically , the peg / ppg and the sulfatoethylsulfone - pigment are associated with different monomers of the acrylic monomer . the modified pigment b is substantially resistant to chemical attacks from acids , bases , and salts . in addition , the modified pigment b is miscible with various co - solvents due , at least in part , to the ethylene glycol and / or propylene glycol . fig4 illustrates an embodiment of a representative reaction mechanism to produce the modified pigment b . a styrene - acrylic co - polymer is provided and then reacted with nh 2 ch 2 ch 2 sh , hcl , and an amine terminated peg and / or ppg . under typical reaction conditions , ph is basic ( e . g ., above a ph of 10 . 5 ). r1 can be h or methyl . r2 can include an alkyl group . in particular , r2 can be h , methyl , ethyl , propyl , and butyl . the monomers can be randomly arranged or block arranged . the product of the reaction is the styrene - acrylic co - polymer having an amine - thio linkage on an acrylic monomer and an amine terminated peg and / or ppg on a different acrylic monomer . the percentage of amine terminated peg and ppg grafted onto the styrene - acrylic co - polymer backbone can range from about 1 to 90 %, about 1 to 50 %, and from about 5 to 20 % based on the reactive carboxylic acid groups . next , the product is reacted with naoh , a sulfatoethylsulfone - pigment , and sodium acrylate to produce modified pigment b . under typical reaction conditions , ph is basic ( e . g ., above ph of 10 . 5 ). the amount of the styrene - acrylic co - polymer covalently bonded to the surface area of the sulfatoethylsulfone - pigment can range from about 0 . 01 to 50 %, about 0 . 01 to 20 %, and from about 5 to 15 %. the value of x , y1 , and y2 in modified pigment b correspond to an acid number that is from about 3 to 500 , about 3 to 400 , about 3 to 300 , about 3 to 250 , about 3 to 200 , about 10 to 500 , about 10 to 400 , about 10 to 300 , about 10 to 250 , about 10 to 200 , about 25 to 500 , about 25 to 400 , about 25 to 300 , about 25 to 250 , about 25 to 200 , about 50 to 500 , about 50 to 400 , about 50 to 300 , about 50 to 250 , and about 50 to 200 . in addition , the value of x , y1 , and y2 in modified pigment b correspond to a glass transition temperature of about − 30 to 120 ° c ., about − 30 to 110 ° c ., about − 30 to 80 ° c ., about − 20 to 120 ° c ., about − 20 to 110 ° c ., about − 20 to 80 ° c ., about − 10 to 120 ° c ., about − 10 to 110 ° c ., about − 10 to 80 ° c ., about 0 to 120 ° c ., about 0 to 110 ° c ., about 0 to 80 ° c ., about 10 to 120 ° c ., about 10 to 110 ° c ., about 10 to 80 ° c ., about 20 to 120 ° c ., about 20 to 110 ° c ., and about 20 to 80 ° c . the value of k in modified pigment b can be from about 0 to 100 %, about 5 to 75 %, about 5 to 50 %, about 5 to 25 %, or about 5 to 10 % of the value of y1 . the value of z in modified pigment b can be from about 5 to 80 %, about 5 to 65 %, about 5 to 50 %, about 10 to 50 %, and about 10 to 30 % of the value of y1 . the molecular weight of the styrene - acrylic co - polymer having peg and / or ppg grafted thereon can range from about 1000 to 1000 , 000 , about 1 , 000 to 20 , 000 , about 2 , 000 to 15 , 000 . the molecular weight of peg can range from about 300 to 10 , 000 mw , about 300 to 5 , 000 mw , about 500 to 2 , 000 mw . the molecular weight of ppg can range from about 300 to 5 , 000 mw , about 300 to 2 , 000 mw , about 300 to 1 , 000 mw . the molecular weight of the co - polymer of polyethylene glycol and polypropylene glycol can range from between about 300 to 10 , 000 mw , 300 to 5 , 000 mw , and from 300 to 2 , 000 mw . in general , the modified pigment in fig5 includes , but is not limited to , a styrene - acrylic co - polymer having a peg and / or ppg grafted thereon , attached covalently to a sulfatoethylsulfone - pigment via an amine linkage ( hereinafter “ modified pigment c ”). typically , the peg / ppg and the sulfatoethylsulfone - pigment are disposed on different monomers of acrylic monomer . the modified pigment c is substantially resistant to chemical attacks from acids , bases , and salts . in addition , the modified pigment c is miscible with various co - solvents due , at least in part , to the ethylene glycol and / or propylene glycol . fig5 illustrates an embodiment of a representative reaction mechanism to produce the modified pigment c . the sulfatoethylamine - pigment is provided and reacted with a polyamine ( e . g ., primary amine , secondary amine , and polyethyleneimine ( pei )) to produce an amine terminated sulfatoethylsulfone - pigment . the amine terminated sulfatoethylamine - pigment is reacted with a styrene - acrylic co - polymer having the peg and / or the ppg grafted thereto to produce modified pigment c . the peg / ppg and the sulfatoethylamine - pigment are disposed on different monomers of the acrylic monomer . the monomers can be randomly arranged or block arranged . the styrene - acrylic co - polymer having the peg and / or the ppg grafted thereto can be fabricated in a similar manner as described above in reference to fig3 and 4 and the accompanying text . the percentage of amine terminated peg and ppg grafted onto the styrene - acrylic co - polymer backbone can range from about 0 . 01 to 90 %, about 0 . 01 to 50 %, and from about 5 to 20 % based on the anhydride groups . the amount of the styrene - acrylic co - polymer covalently bonded to the surface area of the amine terminated sulfatoethylamine - pigment can range from about 0 . 01 to 50 %, about 0 . 01 to 20 %, and from about 5 to 15 %. the value of a , b , and c in modified pigment c correspond to an acid number that is from about 3 to 500 , about 3 to 400 , about 3 to 300 , about 3 to 250 , about 3 to 200 , about 10 to 500 , about 10 to 400 , about 10 to 300 , about 10 to 250 , about 10 to 200 , about 25 to 500 , about 25 to 400 , about 25 to 300 , about 25 to 250 , about 25 to 200 , about 50 to 500 , about 50 to 400 , about 50 to 300 , about 50 to 250 , and about 50 to 200 . in addition , the value of a , b , and c in modified pigment c correspond to a glass transition temperature of about − 30 to 120 ° c ., about − 30 to 110 ° c ., about − 30 to 80 ° c ., about − 20 to 120 ° c ., about − 20 to 110 ° c ., about − 20 to 80 ° c ., about − 10 to 120 ° c ., about − 10 to 110 ° c ., about − 10 to 80 ° c ., about 0 to 120 ° c ., about 0 to 110 ° c ., about 0 to 80 ° c ., about 10 to 120 ° c ., about 10 to 110 ° c ., about 10 to 80 ° c ., about 20 to 120 ° c ., about 20 to 110 ° c ., and about 20 to 80 ° c . the molecular weight of the styrene - acrylic co - polymer having peg and / or ppg grafted thereon can range from about 1000 to 100 , 000 , about 1 , 000 to 20 , 000 , about 2 , 000 to 15 , 000 . the molecular weight of peg can range from about 300 to 10 , 000 mw , about 300 to 5 , 000 mw , about 500 to 2 , 000 mw . the molecular weight of ppg can range from about 300 to 5 , 000 mw , about 300 to 2 , 000 mw , about 300 to 1 , 000 mw . the molecular weight of the co - polymer of polyethylene glycol and polypropylene glycol can range from between about 300 to 10 , 000 mw , 300 to 5 , 000 mw , and from 300 to 2 , 000 mw . in general , the modified pigment in fig6 includes , but is not limited to , a styrene - maleic anhydride co - polymer having a peg and / or ppg grafted thereon , attached covalently to a sulfatoethylamine - pigment via an amine linkage ( hereinafter “ modified pigment d ”). typically , the peg / ppg and the sulfatoethylamine - pigment are disposed on different monomers of maleic anhydride monomer . the modified pigment d is substantially resistant to chemical attacks from acids , bases , and salts . in addition , the modified pigment d is miscible with various co - solvents due , at least in part , to the ethylene glycol and / or propylene glycol . fig6 illustrates an embodiment of a representative reaction mechanism to produce the modified pigment d . the sulfatoethylamine - pigment is provided and reacted with polyamine ( e . g ., primary amine , secondary amine , and polyethyleneimine ( pei )) to produce an amine terminated sulfatoethylsulfone - pigment . the amine terminated sulfatoethylamine - pigment is reacted with a styrene - maleic anhydride co - polymer having the peg and / or the ppg grafted thereto to produce modified pigment d . the peg / ppg and the sulfatoethylamine - pigment are disposed on different monomers of the maleic anhydride monomer . the monomers can be randomly arranged or block arranged . the styrene - maleic anhydride co - polymer having the peg and / or the ppg grafted thereto can be fabricated by reacting structure p with an amine terminated peg and / or ppg . the percentage of amine terminated peg and ppg grafted onto the styrene - maleic anhydride co - polymer backbone can range from about 0 . 01 to 90 %, about 0 . 01 to 50 %, and from about 5 to 20 % based on the anhydride groups . the amount of the styrene - maleic anhydride co - polymer covalently bonded to the surface area of the amine terminated sulfatoethylamine - pigment can range from about 0 . 01 to 50 %, about 0 . 01 to 20 %, and from about 5 to 15 %. the ratio of e to f can be about 1 : 1 , about 2 : 1 , about 3 : 1 , and about 4 : 1 . the value of g is about 5 to 100 %, about 5 to 75 %, about 5 to 50 %, or about 5 to 20 % of the value of f . the value of h is about 1 to 10 . the molecular weight of the styrene - maleic anhydride co - polymer having peg and / or ppg grafted thereon can range from about 1000 to 100 , 000 , about 1000 to 30 , 000 , about 1000 to 10 , 000 . the molecular weight of peg can range from about 300 to 10 , 000 mw , about 300 to 5 , 000 mw , about 500 to 2 , 000 mw . the molecular weight of ppg can range from about 300 to 5 , 000 mw , about 300 to 2 , 000 mw , about 300 to 1 , 000 mw . the molecular weight of the co - polymer of polyethylene glycol and polypropylene glycol can range from between about 300 to 10 , 000 mw , 300 to 5 , 000 mw , and from 300 to 2 , 000 mw . in embodiments including both the peg and ppg molecule , the ratio of peg to ppg can be about 100 : 1 , about 75 : 1 , about 50 : 1 , about 25 : 1 , about 10 : 1 , and about 1 : 1 . in general , the modified pigment in fig7 includes , but is not limited to , a styrene co - polymer having the styrene monomer attached covalently to a pigment ( hereinafter “ modified pigment e ”). in addition , the co - polymer includes , but is not limited to , monomer b , monomer c , and monomer d . monomer b is a hydrophobic monomer , while monomer c is a hydrophilic monomer . the monomers can be randomly arranged or block arranged . it should be noted that prior to reaction , the styrene monomer is an amine styrene monomer , but the amine group is not present in the modified pigment e per the diazonium reaction described below . in general , an amine - styrene co - polymer ( including monomer b , monomer c , and monomer d ) shown in fig7 is reacted with hx ( x can be cl , nitrate , and methane - sulfonic ), nano 2 , and water . the product of the reaction is a styrene co - polymer having a diazonium cation attached to the styrene benzene ring . subsequently , the styrene co - polymer having a diazonium cation is reacted with a pigment through a reaction involving the diazonium cation , and the pigment is covalently bonded to the pigment through the styrene benzene ring . diazonium chemistry and reaction parameters are discussed in u . s . pat . nos . 6 , 723 , 783 ; 5 , 554 , 739 ; 5 , 922 , 118 ; 5 , 900 , 029 ; 5 , 895 , 522 ; 5 , 885 , 335 ; 5 , 851 , 280 ; 5 , 837 , 045 ; and 5 , 922 , 118 , and u . s . patent applications 20030217672 and 20040007152 , each of which are incorporated herein by reference . the amount of the amine - styrene co - polymer covalently bonded to the surface area of the pigment can range from about 5 to 50 %, about 5 to 25 %, and from about 5 to 15 %. monomer b can include hydrophobic monomers such as , but not limited to , 2 - ethylhexyl methacrylate , 2 - hydroxyethyl methacrylate , acrylonitrile , vinylidene chloride , methyl methacrylate , methyl acrylate , ethyl acrylate , butyl acrylate , glycidyl , methacrylate , glycidyl acrylate , lauryl methacrylate , dodecyl methacrylate , styrene , chloromethyl styrene , benzyl methacrylate , butadiene , acrylamide , alkyl vinyl ether , silylated butadienes , divinylbenzene , trimethylsilyl methacrylate , alkoxysilane containing vinyl , p - vinylphenol , 2 - vinyl quinoline , m - nitrostyrene , 4 - hydroxystyrene , p - halomethyl styrene , 4 - acetoxy styrene , 4 - tert - butoxycarbonyloxy styrene and combination thereof . monomer c can include hydrophilic monomers such as , but not limited to , 2 - aminoethyl methacrylate hydrochloride , acrylic acid , methacrylic acid , p - styrene sulfonate , p - methyl amino styrene , vinyl alcohol , p - dimethylamino styrene , vinyl pyridine , 2 - methyl - 5 - vinyl pyridine , maleic anhydride , phenyl maleic anhydride , vinyl amine , vinyl acetate , ethylene - glycol methacrylate , propylene - glycol methacrylate , ethylene - glycol dimethacrylate , propylene - glycol dimethacrylate , trimethylolpropane trimethacrylate , 2 - sulfo - 1 - dimethylethyl acrylamide , 4 - styrene sulfonate , 2 - sulfoethyl methacrylate , 4 - styrene carboxylic acid , n - vinyl pyrrolidone , 1 - vinyl imidazole , vinyl benzoic acid , and combinations thereof . monomer d can include monomers such as , but not limited to , acrylate , acrylic acid , maleic anhydride , macro - mers , and combinations thereof . the value of q can be from about 1 to 100 , about 1 to 75 , about 1 to 50 , about 1 to 25 , and about 1 to 10 monomer units per chain . the value of r can be from about 1 to 100 , about 1 to 75 , about 1 to 50 , about 1 to 25 , and about 1 to 10 monomer units per chain . the value of s can be from about 1 to 100 , about 1 to 75 , about 1 to 50 , about 1 to 25 , and about 1 to 10 monomer units per chain . the value of t can be from about 1 to 100 , about 1 to 75 , about 1 to 50 , about 1 to 25 , and about 1 to 10 monomer units per chain . for each of the modified pigments ( or the precursor thereof ), the monomer including styrene can , in the alternative , include a substituted styrene . examples of a substituted styrene include , but are not limited to , p - methyl styrene , p - t - butyl styrene , p - chlorostyrene , p - bromostyrene , o - chlorostyrene , o - bromostyrene , 1 , 3 , 5 - trichlorostyrene , 1 , 3 , 5 - tribromostyrene , o - fluorostyrene , p - fluorostyrene , pentafluorostyrene , p - hydroxystyrene , p - pentylstyrene , and the like . for each of the modified pigments ( or the precursor thereof ), maleic anhydride can be substituted for another anhydride monomer , such as , but not limited to , succinic anhydride , and itaconic anhydride , in other embodiments . the pigment can include , but is not limited to , black pigment - based inks and colored pigment - based inks . colored pigment - based inks can include , but are not limited to , blue , brown , cyan , green , white , violet , magenta , red , orange , yellow , as well as mixtures thereof . the following black pigments can be used in the practice of this disclosure ; however , this listing is merely illustrative and not intended to limit the disclosure . the following black pigments are available from cabot : monarch ™ 1400 , monarch ™ 1300 , monarch ™ 1100 , monarch ™ 1000 , monarch ™ 900 , monarch ™ 880 , monarch ™ 800 , and monarch ™ 700 , cab - o - jet ™ 200 , cab - o - jet ™ 300 , black pearls ™ 2000 , black pearls ™ 1400 , black pearls ™ 1300 , black pearls ™ 1100 , black pearls ™ 1000 , black pearls ™ 900 , black pearls ™ 880 , black pearls ™ 800 , black pearls ™ 700 ; the following are available from columbian : raven 7000 , raven 5750 , raven 5250 , raven 5000 , and raven 3500 ; the following are available from degussa : color black fw 200 , color black fw 2 , color black fw 2v , color black fw 1 , color black fw 18 , color black s 160 , color black fw s 170 , special black 6 , special black 5 , special black 4a , special black 4 , printex u , printex 140u , printex v , and printex 140v tipure ™; and r - 101 is available from dupont . the pigment may also be chosen from a wide range of conventional colored pigments . for the purposes of clarification only , and not for limitation , some exemplary colorants suitable for this purpose are set forth below . the color of the second ink formulation can include , but is not limited to , blue , black , brown , cyan , green , white , violet , magenta , red , orange , yellow , as well as mixtures thereof . suitable classes of colored pigments include , for example , anthraquinones , phthalocyanine blues , phthalocyanine greens , diazos , monoazos , pyranthrones , perylenes , heterocyclic yellows , quinacridones , and ( thio ) indigoids . representative examples of phthalocyanine blues include copper phthalocyanine blue and derivatives thereof ( pigment blue 15 ). representative examples of quinacridones include pigment orange 48 , pigment orange 49 , pigment red 122 , pigment red 192 , pigment red 202 , pigment red 206 , pigment red 207 , pigment red 209 , pigment violet 19 and pigment violet 42 . representative examples of anthraquinones include pigment red 43 , pigment red 194 ( perinone red ), pigment red 216 ( brominated pyanthrone red ) and pigment red 226 ( pyranthrone red ). representative examples of perylenes include pigment red 123 ( vermillion ), pigment red 149 ( scarlet ), pigment red 179 ( maroon ), pigment red 190 ( red ), pigment violet 19 , pigment red 189 ( yellow shade red ) and pigment red 224 . representative examples of thioindigoids include pigment red 86 , pigment red 87 , pigment red 88 , pigment red 181 , pigment red 198 , pigment violet 36 , and pigment violet 38 . representative examples of heterocyclic yellows include pigment yellow 1 , pigment yellow 3 , pigment yellow 12 , pigment yellow 13 , pigment yellow 14 , pigment yellow 17 , pigment yellow 65 , pigment yellow 73 , pigment yellow 74 , pigment yellow 151 , pigment yellow 117 , pigment yellow 128 , pigment yellow 138 , and yellow pigment 155 . such pigments are commercially available in either powder or press cake form from a number of sources including , basf corporation , engelhard corporation and sun chemical corporation . examples of other suitable colored pigments are described in the colour index , 3rd edition ( the society of dyers and colourists , 1982 ). other examples of pigments include hostafinet series such as hostafine ™ yellow gr ( pigment 13 ), hostafine ™ yellow ( pigment 83 ), hostafine ™ red frll ( pigment red 9 ), hostafine ™ rubine f6b ( pigment 184 ), hostafine ™ blue 2g ( pigment blue 15 : 3 ), hostafine ™ black t ( pigment black 7 ), and hostafine ™ black ts ( pigment black 7 ), available from hoechst celanese corporation , normandy magenta rd - 2400 ( paul uhlich ), paliogen violet 5100 ( basf ), paliogen ™ violet 5890 ( basf ), permanent violet vt2645 ( paul uhlich ), heliogen green l8730 ( basf ), argyle green xp - 111 - s ( paul uhlich ), brilliant green toner gr 0991 ( paul uhlich ), heliogen ™ blue l6900 , l7020 ( basf ), heliogen ™ blue d6840 , d7080 ( basf ), sudan blue os ( basf ), pv fast blue b2go1 ( american hoechst ), irgalite blue bca ( ciba - geigy ), paliogen ™ blue 6470 ( basf ), sudan iii ( matheson , coleman , bell ), sudan ii ( matheson , coleman , bell ), sudan iv ( matheson , coleman , bell ), sudan orange g ( aldrich ), sudan orange 220 ( basf ), paliogen ™ orange 3040 ( basf ), ortho orange or 2673 ( paul uhlich ), paliogen ™ yellow 152 , 1560 ( basf ), lithol fast yellow 0991k ( basf ), paliotol yellow 1840 ( basf ), novoperm ™ yellow fg 1 ( hoechst ), permanent yellow ye 0305 ( paul uhlich ), lumogen yellow d0790 ( basf ), suco - gelb l1250 ( basf ), suco - yellow d1355 ( basf ), hostaperm ™ pink e ( american hoechst ), fanal pink d4830 ( basf ), cinquasia magenta ( dupont ), lithol scarlet d3700 ( basf ), toluidine red ( aldrich ), scarlet for thermoplast nsd ps pa ( ugine kuhlmann of canada ), e . d . toluidine red ( aldrich ), lithol rubine toner ( paul uhlich ), lithol scarlet 4440 ( basf ), bon red c ( dominion color company ), royal brilliant red rd - 8192 ( paul uhlich ), oracet pink rf ( ciba - geigy ), paliogen ™ red 3871k ( basf ), paliogen ™ red 3340 ( basf ), and lithol fast scarlet l4300 ( basf ). it should be noted that ratios , concentrations , amounts , and other numerical data may be expressed herein in a range format . it is to be understood that such a range format is used for convenience and brevity , and thus , should be interpreted in a flexible manner to include not only the numerical values explicitly recited as the limits of the range , but also to include all the individual numerical values or sub - ranges encompassed within that range as if each numerical value and sub - range is explicitly recited . to illustrate , a concentration range of “ about 0 . 1 % to about 5 %” should be interpreted to include not only the explicitly recited concentration of about 0 . 1 wt % to about 5 wt %, but also include individual concentrations ( e . g ., 1 %, 2 %, 3 %, and 4 %) and the sub - ranges ( e . g ., 0 . 5 %, 1 . 1 %, 2 . 2 %, 3 . 3 %, and 4 . 4 %) within the indicated range . table 1 of part b lists ink formulations incorporating embodiments of various modified pigments . tables 2 and 3 of part b compare performances of iq attributes on various glossy media . as shown , the ink formulation including the peg modified pigment delivers higher gloss and better media independence . fig8 illustrates a graph comparing a yellow pigment chemically modified with traditional styrene - acrylic polymer ( top curve , py74 yellow pigment , and a yellow pigment chemically modified with sma - peg polymer ( bottom curve ) such as that illustrated in fig3 . when the pigment was de - stabilized under various triggering conditions , such as ionic strength and ph , particles started to coagulate . the rate of coagulation was measured by monitoring the time evolution of the flocculation size as determined by dynamic light scattering ( dls ). a characteristic coagulation time was derived from fifting the dls data . the impact of trigger condition and surface modification type on the coagulation time was determined and provides critical insight as to how the pigment coagulation can be controlled to yield optimal print performance . the bottom curve ( sma - peg treated pigment ) was more stable than the yellow pigment chemically modified with traditional styrene - acrylic polymer . the stability directly translates into better photo image quality . photo paper typically triggers the flocculation of pigment dispersion by releasing salt or causing ph changes . both py74 pigment dispersions were made into 100 ppm stock solutions . from the stock solution 30 ul was injected into 3 ml of 0 . 01 mol hcl solution in a 1 cm disposable plastic cuvet to yield a particle concentrations of 1 ppm . after thorough mixing , the cuvet was placed into the dsl instrument and measurement started within 5 seconds . dls measurements were performed on a bic zetaplus from brookhaven instrument corp . which is equipped with a 30 mw , 670 nm solid state laser . scattered light at 90 ° was collected by a single mode fiber optic . autocorrelation was performed with bi - 9000at digital autocorrelator with a user selectable channels up to 512 . during this study 200 channels were used with bi - psdw software . synthesis example for a representative of modified pigment a in fig3 : a solution was prepared by dissolving poly - styrene - co - maleic anhydride ( sma ) ( available from sartomer company ) in dry dmf . to this stirred solution , at room temperature , under a steady stream of nitrogen gas , was added amine terminated poly - ethylene oxide - co - propylene oxide ( e . g ., jeffamine from huntsman corporation ) and 2 - aminoethanethiol hydrochloride as a solid in one portion and then triethylamine was added dropwise . the resultant mixture was heated at about 45 ° c . for about 30 minutes and then at room temperature for about 4 . 5 hours . the product was isolated by slowly dropping into vigorously stirred in hcl . after the addition , the mixture was stirred for another 60 minutes and then suction filtered , washed in hcl and then deionized water . the resulting product was briefly air dried to afford a free flowing white solid , which contained moisture . the moisture content could be measured by weight loss after heating at 110 ° c . for 1 hour . the aminoethanethiolated - poly ethylene oxide - co - propylene oxide sma polymer ( sma - peg - thio ) was dried at 110 ° c . results from elemental combustion analysis could be used to characterize the modified polymers . thiol was measured by titration with dtnb following a modification of ellman &# 39 ; s procedure ( ellman , g . l . ( 1958 ) arch . biochem . biophys . 74 , 443 ; bioconjugate techniques , greg t . hermanson , academic press , inc ., 1996 , p 88 ). the aqueous dispersion of black pearls ® 1100 carbon black ( available from cabot corporation ) having attached a 2 -( sulfatoethylsulfone ) group was prepared according to the procedure described in pct publication no . wo 01 / 51566 to yield a pigment dispersion . this dispersion was added dropwise to the solution of the sma - peg - thiol polymer made above ( dissolved with naoh ). an additional naoh was added to raise ph to about 12 - 13 . the resultant mixture was then stirred at about 40 - 50 ° c . for about 3 . 5 hours to give a dispersion of an embodiment of the modified pigment a . a sodium acrylate solution was prepared by dissolving acrylic acid into ddi water containing about 11 . 7 of na 2 co 3 . this solution was added to the modified pigment dispersion to “ cap ” any unreacted thiol groups . heating and stirring were continued for another 3 hours and the mixture was then allowed to cool to room temperature . the resultant dispersion was then purified by diafiltration to reach a final permeate polymer concentration of less than about 50 ppm . many variations and modifications may be made to the above - described embodiments . all such modifications and variations are intended to be included herein within the scope of this disclosure and protected by the following claims .
2
referring to fig1 in which the first embodiment of the electron gun according to the present invention is illustrated , this drawing shows a beam producing cathode k , a control grid g1 , a screen grid g2 , and electrodes g3 , g4 , g5 , g6 , g7 , and g8 . the electrodes are accelerating and focusing the electron beam from the said cathode , control grid g1 , and screen grid g2 . all of the electrodes are arranged at proper intervals . here , the general dimensions of the said electrodes are determined by the relationship between the diameters of the beam passing holes of the respective electrodes and the lengths of their bodies as shown in table 1 below . the inventor obtained the values of table 1 through repeated numeric analysis experiments . table 1______________________________________length of electrodes / diameters of holes l4 / d4 l5 / d5 l6 / d6 l7 / d7______________________________________ranges 0 . 18 - 0 . 55 0 . 36 - 1 . 45 0 . 07 - 0 . 18 1 . 09 - 1 . 73______________________________________ in the above table , l4 , l5 , l6 and l7 indicate the lengths of the electrodes g4 , g5 , g6 and g7 , while d4 , d5 , d6 and d7 indicate the diameters of the beam passing holes of the respective electrodes . of the said electrodes , the lengths of the electrodes placed in the main lens means may be variable within the allowable ranges as shown in table 2 below , depending on the application and other conditions of the electron gun , but assuming that all the beam passing holes have a uniform diameter of 5 . 5 mm . table 2______________________________________ g4 g5 g6 g7______________________________________lengths 1 . 0 - 3 . 0 2 . 0 - 8 . 0 0 . 4 - 1 . 0 6 . 0 - 9 . 5______________________________________ in the said main lens means , the electrodes g4 , g5 , g6 and g7 forming an auxiliary lens should preferably have narrow intervals between the adjacent ones , preferably 0 . 6 mm , while the interval between the electrodes g7 , and g8 may be desirably about 1 . 0 mm . the electrodes g1 , g2 form electron beams in cooperation with the cathode which is positioned upstream of the said electrodes g1 , g2 , forming a three - electrode tube portion , and these electrodes g1 , g2 should be designed in the normal type or properly depending on the application of the electron gun . the electrode g3 should also be based on the normal type , but the diameter of the outgoing side of the beam passing hole of this electrode may be formed in a size smaller than that of the electrode g4 properly in different embodiments . that is , as shown in the second embodiment of the present invention illustrated in fig8 the outgoing side beam passing hole 3hr of the electrode g3 can be formed in a size smaller than the beam passing holes of the electrodes g4 , g5 , g6 , g7 , and g8 , all of which have holes having the same diameter . further , referring to fig9 which illustrates the third embodiment of the present invention , the incident side beam passing hole 5hf of the electrode g5 has a larger diameter , unlike the beam passing hole 4h of the electrode g4 and the outgoing side beam passing hole 5hr of the electrode g5 , both of which have a same diameter . therefore , the diameters of the beam passing holes of the respective electrodes should satisfy the following formulas : where d3r indicates the diameter of the outgoing beam passing hole of the electrode g3 , d4 the diameter of the beam passing hole of the electrode g4 , and d5f the diameter of the incident side beam passing hole of the electrode g5 . of course , the above electrodes should come within the ranges specified in table 1 . in the embodiments of the present invention described above , the proportion of the applied focus voltage vf to the anode voltage eb should fall approximately within the range of 23 %- 34 %, and the most desirable focus voltage vf and anode voltage eb are , respectively , 7 kv and 25 kv in the case of a 20 - inch cathode ray tube . the above specified dimensions of the multistep focusing electron gun according to the present invention are the values obtained as a result of repeated experiments , and should apparently produce a satisfactory result . first , the variations of the performances of the multistep focusing electron gun in correspondence with the variations of the sizes of the electrodes as abtained through the experiments will be described . fig2 shows the variations of the size of the beam spot as against the variations of the lengths l4 , l5 of the electrodes g4 , g5 , and the variations of the ratio of the focus voltage vf to the anode voltage eb as against the variations of the lengths of the electrodes g4 , g5 for the first embodiment of the present invention . that is , in the case where the electrode g4 has a length of 1 . 4 mm , and the length of the electrode g5 is varied within the range of 2 . 0 - 6 . 5 mm , vf / eb falls within the range of 23 %- 34 %, and the variation of the beam size falls within the range of 1 . 8 - 2 . 1 mm approximately . further , as shown in fig3 if the length of the electrode g6 is 0 . 6 mm , and the length of the electrode g7 facing with the said electrode g6 opposingly is varied within the range of 6 . 0 - 9 . 5 mm , then the value of vf / eb is varied within the range of 30 - 32 %, and the size of the beam spots will stay in the range of 1 . 65 - 1 . 70 mm . the electron gun according to the present invention having such a characteristic and the conventional electron gun are compared in fig4 which shows that the electron gun according to the present invention forms a smaller beam spot compared with the conventional electron gun hi - bi , on the assumption that the cathode current ib is the same in both of them . especially , to see into the variations of the beam spot as against the variations of the focus voltage vf as shown in fig5 the electron gun according to the present invention forms a far smaller beam spot , and its variation range is also smaller under the same focus voltage applied . further , as shown in fig6 the electron gun according to the present invention forms a smaller beam spot , and shows a smaller variation range compared with the conventional electron gun . further , as shown in fig7 the focus characteristics on the peripheral areas of the screen is also improved in the electron gun of the present invention compared with the conventional electron gun . the conventional electron gun shows not only a larger beam spot , but also forms a larger halo around the beam spot , whereas the electron gun according to the present invention produces a smaller halo and a smaller beam spot . meanwhile , according to the second and third embodiments of the present invention which are illustrated in fig8 and 9 , respectively , the characteristics of the electron gun are further improved . that is , not only the spherical aberration is further improved , but also , an excellent focus characteristics is produced . in other words , in the second embodiment illustrated in fig8 an electrostatic unipotential lens is formed by means of the electrodes g3 , g4 , g5 and a weak diverging section i is formed by the combination of the electrode g3 having an outgoing side beam passing hole 3hr of a smaller diameter , and the electrode g4 having a beam passing hole 4h of a larger diameter . accordingly , when the electron beam is passing the section i , the electron beam experiences a weak diverging force , with the result that the electron beam enters with a smaller incident angle into the focusing section ii which is formed by the cooperation between the electrodes g4 , g5 . as a result , the spherical aberration on the screen surface of the cathode ray tube is improved , resulting in that clear and high quality images are produced on the screen . meanwhile , the third embodiment of the present invention as illustrated in fig9 has a more advanced constitution compared with the second embodiment . here , the beam passing hole of the electrode g5 forming a part of a beam focusing section ii &# 39 ; is formed in a smaller size compared with the beam passing holes of the electrodes g4 , and g6 , which are disposed at the opposite sides thereof , thereby producing a strong focusing force . electrode g5 comprises front and rear beam passing sections having beam passing holes 5hf and 5hr and corresponding beam passing diameters d5f , d5r and lengths l5f and l5r . therefore , in this embodiment , the beam diverging force is weakened through the diverging section i &# 39 ;, while the beam focusing force is reinforced through the focusing section ii &# 39 ;. consequently , the spherical aberration is greatly reduced , and the beam focus characteristics is markedly improved compared with the above embodiments . in short , the electron gun according to the present invention has the following advantages . the variations of the size of the image as against the variations of the magnification of the main lens and against the variations of the distance to the screen are reduced , while the spherical aberration most greatly affecting the pattern of the beam is remarkably improved , because the beam divergence angle can be easily adjusted by means of the auxiliary lenses . thus , the electron gun according to the present invention reduces the size of the beam spot by about 30 % compared with the conventional electron guns , thereby making it suitable for use in a cathode ray tube of a high fineness and high resolution . moreover the astigmatism in the peripheral areas is remarkably improved , thereby making it possible to improve the image quality . further , the first and second auxiliary lenses are provided in an adjustable form in their magnifications , thereby providing flexibilities in designing them for different purposes . moreover the voltage differences between the electrodes can be minimized compared with the conventional electron guns , thereby improving the voltage resistance characteristics .
7
it is contemplated that the teaching of the description set forth below is applicable to electric contact blocks and auxiliary contact blocks , including but not limited to normally open , normally closed , relay , timer or a motor starter contact . the present invention is therefore not intended to be limited to any particular type of electrical contact , such as in contact 100 . like reference numbers denote the same or similar features among the various views and figures . fig1 illustrates a contactor 100 as is known in the industry . the operation of a contactor is known in the industry and will not be described in detail . contactor 100 may be any shape but generally has front 106 , back ( not visible ), which is opposite the front 106 , and right and left sides 104 , and 112 respectively . above contactor 100 is a frontal block 200 . front 106 and back ( not visible ) comprise at least one port 102 for interconnecting wires for communication with an electric circuit . feet 108 provide means 110 for securing contactor 100 to an enclosure by screws or bolts . a port ( not shown ) interfaces with a frontal block 200 . fig2 is a perspective view of a frontal block 200 according to an aspect of the invention . frontal block 200 has a cover 202 over a housing 204 . frontal block 200 is fixed to contactor 100 by means of fixation lever 300 . wires are connected at terminal 404 for control of external electrical circuits . the fixation lever 300 of fig3 secures frontal block 200 to contactor 100 . the fixation lever 300 has protrusions 304 on either side of main body 305 . protrusions 304 fit into channels ( not shown ) in the base of housing 204 . spring body 306 is made of a flexible material and connects main body 305 with cover interface 302 . cover interface 302 rests within a channel in housing 204 . when frontal block is assembled with contactor , the cover interface 302 rests against the wall of pocket in contactor cover ( as shown in fig3 ). by applying pressure to the top of cover interface 302 the spring body 306 flexes causing cover interface 302 to move out of the channel in housing 204 and wall in contactor cover . housing 204 accommodates a carrier assembly 400 and two terminal assemblies 405 on either side of carrier assembly 400 . terminal assembly 405 may contain normally open terminals , normally closed terminals or a combination of either . the configuration of each is known in the art and will not be described in detail . carrier assembly 400 interfaces with contactor 100 through the base of housing 204 via lever 424 . motion in contactor 100 is transmitted through lever 424 causing carrier assembly 400 to move up or down in housing 204 . when at a rested state the carrier assembly 400 is generally extended into housing 204 . as shown in fig5 , the frontal block may contain a pair of normally open contacts 450 and a pair of normally closed contacts 451 . for normally open contact 450 a stationary contact 401 attached to terminal assembly 405 and rests below movable contact 402 . as carrier assembly is moved from the rested position to an energized position the stationary 401 and movable 402 contacts are brought together . when the carrier assembly 400 is in the rested position the stationary 401 and movable 402 contact is offset by spacer 700 . for normally closed contacts 451 a stationary contact 431 is attached to terminally assembly 405 and rests above a moveable contact 430 . as carrier assembly 400 is moved from a rested position to an energized position the moveable contact 430 is removed from contact with the stationary contact 431 . to prevent continued contact as the carrier assembly 400 is energized a spacer 800 constrains movable contact 430 . moveable contacts 402 and 430 are set in channels 460 , 461 and are backed by springs 422 , as shown in fig6 . the spring 422 in channel 460 is held at on end by peg 420 in carrier assembly 400 and at the other by moveable contact 402 . the spring 422 in channel 461 is held at one end by spring support 406 which sits in a groove in the housing 204 and at the other end by moveable contact 430 . each channel 460 , 461 may comprise a wall ( not numbered ) that may be inclined or angled to allow for the auto - cleaning of the contacts 402 , 430 as they move up and down within the channels . fig7 is a perspective view of spacer 700 . spacer 700 has upper protrusion 714 and lower protrusion 712 . upper protrusion 714 is inserted into groove 414 in carrier assembly 400 . lower protrusion 712 is inserted into grove 412 in carrier assembly 400 . the protrusions 712 and 714 located the spacer in channel 460 . fig8 is a perspective view of a spacer 800 . spacer 800 has groove 816 which mates with protrusion 416 in channel 461 . each channel contains protrusions 712 and 714 as well as groove 416 . therefore any channel 460 and 461 can accommodate either spacer . by interchanging , making removable , making reversible and / or making invertible certain parts , such as the contacts 402 and 430 and the spacers 700 and 800 , a normally open contact may become normally closed or a normally closed may become normally open absent use of any tools . for example , to switch from normally open to normally closed , spacer 800 is removed and spacer 700 is inserted . the spring 422 is moved from the upper position proximate to peg 420 to a lower position supported by spring support 406 . moveable contact 402 is flipped to be in position of moveable contact 430 . stationary contact 401 is replaced with stationary contact 431 . by reversing the process a normally closed contact will become normally open . while the invention has been described in terms of various specific embodiments , those skilled in the art will recognize that the invention can be practiced with modification within the spirit and scope of the claims .
7
present embodiments of the invention are shown in the above - identified figures and described in detail below . in describing the embodiments , like or identical reference numerals are used to identify common or similar elements . the figures are not necessarily to scale and certain features in certain views of the figures may be shown exaggerated in scale or in schematic in the interest of clarity and conciseness . please add / modify explanations of figures based on my addition and changes to the figures . referring now to the drawings , and in particular to fig1 a - 1e , shown therein and designated by reference numeral 10 is a stimulator device ( hereinafter referred to as “ stimulator device ”), constructed in accordance with the present invention , for providing stimulation to a gastrointestinal tract 12 of a user 14 . the gastrointestinal tract 12 of the user 14 includes the alimentary canal and organs associated with the alimentary canal such as the stomach , small intestine , large intestine , and the like . users 14 may include humans , mammals , or other multicellular organism having a gastrointestinal tract 12 . in general , the stimulator device 10 is placed in the appendix or within an appendicular region 16 and / or rectal region 18 of a lower digestive tract 17 of the user 14 . the vermiform appendix is located at the junction of the small intestine and the large intestine . the appendix is generally credited with no significant function and is most commonly explained as a vestigial structure within the body . it is routinely removed without any ill effects or side effects . however , the linkage of the appendix within the ens to the gastrointestinal tract 12 provides an avenue for electrical stimulation in the treatment of gastrointestinal disorders giving a desirable use and purpose for this vestigial structure . the rectum is also linked within the ens to the gastrointestinal tract 12 and offers another option for convenient placement of the stimulator device 10 . specifically , the relative proximity of the anal orifice to the rectum allows placement of the stimulator device 10 in the rectum without the need for extensive surgical procedures currently practiced in gastrointestinal stimulator placement . preferably , at least a portion of the stimulator device 10 is placed in contact with the appendicular wall 20 and / or rectal wall 22 of the user 14 . the stimulator device 10 may contact the external appendicular wall 20 and / or rectal wall 22 , the interior appendicular wall 20 and / or rectal wall 22 , and / or be within the appendicular wall 20 and / or rectal wall 22 . for example , the stimulator device may be placed in contact with the mucosal surface , underlying vascular submucosa , serosa , and / or layered muscularis externa of the appendicular wall 20 and / or rectal wall 22 . preferably , the stimulator device 10 is inserted into the submucosa of the appendicular wall 20 and / or rectal wall 22 . optionally , the stimulator device 10 may be attached to the appendicular wall 20 and / or rectal wall 22 to prevent migration of the stimulator device 10 through the gastrointestinal tract 12 . the stimulator device 10 may be attached to the appendicular wall 20 and / or rectal wall 22 through the use of projections , barbs , umbrella connectors , sutures , adhesives , and / or the like . additionally , multiple stimulator devices 10 may be placed within the user 14 . for example , the user 14 may have a first stimulator device 10 within the appendicular region 16 and a second stimulator device 10 within the rectal region 18 of the user 14 . once positioned in contact with the appendicular wall 20 and / or rectal wall 22 , the stimulator device 10 delivers pulses of a medium and provides stimulation to the gastrointestinal tract 12 through the enteric nervous system . placement of the stimulator device 10 within one area of the enteric nervous system provides stimulation not only at the area of contact , but also provides stimulation within other areas of the ens system . for example , placement of the stimulator device 10 within the appendicular region 16 can provide stimulation initiating peristaltic activity within the gastrointestinal tract 12 . stimulation of the gastrointestinal tract 12 through the enteric system will alter , inhibit , or excite gastrointestinal motor functions , activate intrinsic and extrinsic neuronal pathways and / or solicit hormonal / peptide releases . the effects of stimulation on these functions / pathways are related to the selection of stimulation parameters which are discussed in greater detail below and have therapeutic potentials for various diseases / disorders . the stimulator device 10 can thus be used for treating a variety of digestive and eating disorders as well as in use in treating chemotherapy - induced emesis . exemplary eating disorders include obesity , binging , bulimia , and the like . gastrointestinal disorders include dysphagia , gastroesophageal reflux diseases , functional dyspepsia , gastroparesis , postoperative ileus , irritable bowel syndrome , constipation , diarrhea , fecal incontinence , pain / discomfort , nausea and vomiting , and the like . the stimulator device 10 can be programmed with stimulation parameters prior to placement of the stimulator device 10 within the appendicular region 16 and / or rectal region 18 of the user 14 so that a particular disease or disorder will be treated . a health care provider or user may be presented with a variety of stimulator devices 10 with each stimulator device 10 pre - programmed to treat a different disorder . alternatively , the stimulator device 10 can be programmed to treat a particular disorder immediately prior to administration . alternatively , the stimulator device 10 can be programmed with a variety of different types of treatment regimens for different diseases and / or disorders so that the stimuli can be changed during treatment of the gastrointestinal disorder without need for the removal of the stimulator device 10 . as illustrated in fig1 b and 1e , the stimulator device 10 includes at least two electrodes 26 and 28 in communication with a pulse generator 30 . the electrodes 26 and 28 can be provided as one or multiple pairs and in varying shapes . for example , the electrodes 26 and / or 28 can be provided as a point electrode , a ring electrode , or a patch electrode . the electrodes 26 and 28 may be surgically implanted or insertably placed within the appendicular region 16 and / or rectal region 18 . for example , for the placement of stimulator into the appendix or rectum , colonoscopy or endoscopy can be utilized . for the placement of stimulator in other areas , various surgical techniques may be used depending on the location of placement . for example , both traditional surgical techniques and / or laparoscopic techniques may be used in placing the stimulator device 10 in the appendicular region 16 and / or rectal region 18 . preferably , laproscopic techniques , using small incisions in comparison to large incisions of traditional surgery , are used to place the stimulator device 10 . additionally , other forms of surgical placement , known now or developed within the future , may be used as long as the stimulation device is placed in contact with the appendicular wall 20 and / or rectal wall 22 of the user 14 . the electrodes 26 and 28 are in communication with the pulse generator 30 such that pulses can be provided from the pulse generator 30 to the electrodes 26 and 28 . the pulse generator delivers a frequency of pulses to the electrodes 26 and 28 providing emission of the medium to the appendicular wall 20 and / or rectal wall 22 . for example , the pulse generator 30 delivers pulses to the electrodes 26 and 28 in contact with the appendicular wall 20 such that the electrodes 26 and 28 provide stimulation to the gastrointestinal tract 12 of the user 14 through the enteric nervous system . the pulses provided by the pulse generator 30 to the electrodes 26 and 28 can be provided in a variety of different manners , such as intermittent pulses , continuous pulses , and / or a train of intermittent and / or continuous pulses . selection of the pulses is determined based on the particular gastrointestinal disease ( s ) and / or disorder ( s ) being treated as described in more detail below . such pulses can be delivered via the pulse generator 30 to the electrodes 26 and 28 via any suitable medium , such as electricity , acoustic waves , radiation , photons , or the like . preferably , the medium is in the form of electrical stimulation to the appendicular wall 20 and / or rectal wall 22 . the pulse generator 30 adjacent to the electrodes 26 and 28 or separate from the electrodes 26 and 28 . in one embodiment , the pulse generator 30 is separate from the electrodes 26 and 28 and inserted subcutaneously within the abdominal region . preferably , the pulse generator 30 is inserted subcutaneously within the abdominal region above the belt line of the user 14 . in another embodiment , as illustrated in fig1 c and 1d , the pulse generator 30 is adjacent to the electrodes 26 and 28 . additionally , pulse generator 10 may utilize an internal power source or an external power source . it is contemplated that the power source may be located external to the user 14 , provided the power source is in communication with the pulse generator 30 . for example , the power source may be provided external to the user 14 through a wireless mechanism , such as inductive loop coupling , electromagnetic control , or the like . the stimulator device may optionally include a controller 32 . the controller 32 communicates with the pulse generator 30 for controlling the pulses generated by the pulse generator 30 . the controller 32 can be analog , digital , or a combination of both . the controller 32 may be a computer , a microcontroller , a microprocessor , or the like . the controller 32 uses stimulation parameters to regulate the pulse generator 30 and provide a variety of different types of treatment regimens for different diseases and / or disorders . stimulation parameters , as discussed in more detail below , may include frequency , pulse width , amplitude , and the like . programming of the controller 32 can regulate pulses generated by the pulse generator 30 so that can the pulses change based upon the treatment regime for the user 14 . the controller 32 may be programmed with stimulation parameters prior to insertion and / or placement of the stimulator device 10 and / or after insertion and / or placement of the stimulator device 10 . shown in fig2 is a diagrammatic view of one example of the stimulator device illustrated in fig1 c and fig1 d constructed in accordance with the present invention . the stimulator device 10 is provided with two electrodes 26 and 28 , the pulse generator 30 , and the controller 32 . additionally , the stimulator device includes a housing 34 and a power source 36 . the housing 34 is constructed of a biocompatible , non - digestible material for use within the appendicular region 16 and / or the rectal region 18 of the user 14 . examples of biocompatible , non - digestible materials suitable for use in forming the housing 34 are , but not limited to , biocompatible metals , such as unalloyed titanium , wrought titanium alloy , nitrogen austenitic steel , stainless steel , and biocompatible plastic such as polyvinylchloride , polytetrafluoroethelyne , polyethersulfone , polyurethane , polycarbonate , polyetheretherketone and polypropylene . the housing 34 is sized and shaped for placement within the appendicular region 16 and / or rectal region 18 . preferably , the housing is sized and shaped for transport through the anal orifice . for example , the housing 34 can be shaped in the form of a capsule . however , it should be understood that the housing 34 can be provided in other shapes and / or sizes , so long as the housing 34 can be inserted through the anal orifice and / or placed in at least a portion of the appendicular region 16 and / or rectal region 18 preferably without causing any negative side effects , such as irritation . it is also desirable for the housing 34 to be sized and shaped so as not to block the appendicular region 16 and / or rectal region 18 leading to interference with the operation of the gastrointestinal tract 12 . further , it should be understood that rather than simply being constructed of a biocompatible , non - digestible material , the housing 34 can be formed of a non - biocompatible , or even digestible material that is coated with a biocompatible non - digestible material . the housing 34 is formed with the electrodes 26 and 28 separated by an insulating material 38 . the electrodes 26 and 28 are connected to the insulating material 38 so as to form a sealed container . the housing 34 defines an interior space containing the pulse generator 30 , the controller 32 , and the power source 36 . however , it should be understood that at least the power source 36 , and the controller 32 can be external to the housing 34 so long as the power source 36 and / or controller 32 can communicate and / or provide power , and / or control to the pulse generator 30 . as discussed above , the controller 32 communicates with the pulse generator 30 for controlling the pulses generated by the pulse generator 30 . the electrodes 26 and 28 supply a medium containing the pulses generated by the pulse generator 30 to the appendicular wall 20 and / or rectal wall 22 . as discussed above , the medium can be provided in a variety of forms such as electricity , acoustic waves , radiation , photons , or the like . the electrodes 26 and 28 can be provided as one or multiple pairs and can be provided on the housing 34 in various locations and different shapes . for example , the electrodes 26 and / or 28 can be provided as a point electrode , a ring electrode , or a patch electrode . the distance between the electrodes 26 and 28 in a pair can also vary . as shown in fig2 , the controller 32 is supported by the housing 34 and is contained within the interior space of the housing 34 . the controller 32 can be external to the housing 34 or at least portions of the controller 32 can be external to the housing 34 so long as the controller 32 can communicate with and / or control the pulse generator 30 . the power source 36 is also supported by the housing 34 . preferably , the power source 36 is within the internal space of the housing 34 . however , it is contemplated that the power source 36 may be located external to the housing 34 , provided the power source 36 is in communication with the pulse generator 30 and / or the controller 32 . for example , the power source 36 may be provided external to the user 14 through a wireless mechanism , such as inductive loop coupling , electromagnetic control , or the like . the housing 34 may optionally include means for attaching the stimulator device 10 to the appendicular wall 20 and / or rectal wall 22 . as previously discussed , attachment means include , but are not limited to , projections , barbs , umbrella connectors , sutures , adhesives , and / or the like . referring to fig3 , regulation of the pulse generator 30 by the controller 32 may include an open - loop system 40 , a closed loop system 42 , or a combination of the like . in the open loop system 40 , pulses are delivered to the electrodes 26 and 28 without the use of sensing inputs such as a sensor system 44 . in the closed loop system 42 , pulses are delivered to the electrodes 26 and 28 based on inputs to the controller 32 via the sensor system 44 . for example , the sensor system 44 can deliver electrical signals to the controller 32 that vary or are indicative of the following conditions : mechanical contractions , pressure , tension , electrical signals , temperature , ph or the like . although fig3 shows the controller 32 , it should be noted the stimulator device 10 may include the pulse generator 30 supplying pulses to the electrodes 26 and 28 without the use of the controller 32 . one embodiment of the open loop system 40 includes the controller 32 , the pulse generator 30 , and the electrodes 26 and 28 . the controller 32 is in communication with the pulse generator 30 and regulates pulses generated by the pulse generator 30 . the pulse generator 30 provides the pulses to the electrodes 26 and 28 . the controller 32 may optionally contain a timing mechanism , such as an internal clock , for further controlling the pulses . in another embodiment ( not illustrated ), the controller 32 is in direct communication with the electrodes 26 and 28 directly and alters the pulses supplied to the electrodes 26 and 28 directly . the closed - loop system 42 , as illustrated in fig3 , includes the controller 32 , the pulse generator 30 , the electrodes 26 and 28 , and the sensor system 44 . the sensor system 44 communicates with the controller 32 and detects environmental conditions external to the stimulator device 10 . the environmental conditions can be used to determine the location of the stimulator device 10 within the gastrointestinal tract 12 of the user 14 if the stimulator device 10 migrates . additionally the environmental conditions can be used to vary the frequency and / or intensity of the pulses generated by the pulse generator 30 as needed . the sensor system 44 can include one or more sensors for sensing a variety of different types of environmental factors which may be surrounding the stimulator device 10 . for example , mechanical contractions , pressure , tension , electrical signals , temperature , ph or the like . the information received from the sensor system 44 is fed back to the controller 32 so that the controller 32 can vary stimulation parameters and regulate pulses generated by the pulse generator 30 . for example , the sensor system 44 can detect the effect of stimulation to the appendicular region 16 and / or rectal region 18 . the location or effect of the stimulator device 12 within the user 14 is fed back to the controller 32 . the controller 32 then regulates the frequency , duration , and / or amplitude of the pulses generated by the pulse generator 30 based on the effect of the stimulator device 10 within the appendicular region 16 and / or rectal region 18 of the user 14 . the sensor system 44 can also provide a method for synchronized stimulation such that pulses can be provided to the appendicular region 16 and / or rectal region 18 of the user 14 upon detection by the sensor system 44 of a mechanical contraction within the user 14 . synchronizing each pulse with the intrinsic physiological activity of the user 14 may enhance gastrointestinal contractions and accelerate transport of nutrients along the gastrointestinal tract . as illustrated in fig3 , the stimulator device 10 may optionally include a telemetry system 46 that assists in providing external control , external programming , and / or permitting measurement and reporting of information regarding the stimulator device 10 and / or the environmental conditions surrounding the stimulator device 10 . the telemetry system provides communication between an internal controller , located within the user 14 such as the sensor system 44 and / or controller 32 , while an external controller 48 is external to user . the external controller 48 can be either proximally located to the user 14 or located at a distance to the user 14 so long as the telemetry system can provide communication between the internal controller , such as the sensor system 44 and / or controller 32 , and the external controller 48 . the communication can be through radio frequency , infrared light , laser light , visible light , acoustic energy , or the like . both the internal controller , such as the sensor system 44 and / or controller 32 , and external controller 48 are preprogrammed to provide monitoring , alerting , transmitting , and / or record - keeping of information generated and / or needed for the stimulator device 10 . in one embodiment , communication between the sensor system 44 , as the internal controller , and a microprocessor , as the external controller 48 , provides monitoring of environmental information surrounding the stimulator device 10 and provides an alerting function if the microprocessor and / or sensor system 44 detect abnormal conditions within the appendicular region 16 and / or rectal region 18 of the user 14 . in another embodiment , communication between the sensor system 44 , as the internal controller , and the microprocessor , as the external controller 48 , allows for the analysis of the environmental information using a decision - making algorithm to provide stimulation parameters . the environmental information is provided by the sensor system 44 and communicated by the telemetry system 46 to the microprocessor . the microprocessor uses the algorithm to determine the stimulation parameters . such stimulation parameters are communicated again through the telemetry system 46 to either the controller 32 and / or sensor system 44 to regulate the pulses generated by the pulse generator 30 . as previously discussed , stimulation parameters are utilized by the controller 32 to control the pulse generator 30 . stimulation parameters can include frequency , pulse width , amplitude , and the like . the pulses may be intermittent pulses , continuous pulses , and / or trains of intermittent and / or continuous pulses . the controller 32 can vary the stimulation parameters to provide variations in the pulses such that the pulse generator 32 provides long - pulse , short - pulse , dual phase pulses , trains of short - pulses , biphasic trains of pulses , or other variation of pulses . fig4 a - e graphically illustrates the relative duration and amplitude of a variety of the exemplary pulses which can be generated by a pulse generator 30 based on the various stimulation parameters provided by the controller 32 . it should be understood that the stimulation parameters utilized by the controller 32 can be modified according to the desires of the designer and / or the patient . fig4 a graphically illustrates repetitive long - pulses having a pulse width in the order of milliseconds . the long pulse method is able to ‘ pace ’ or entrain natural slow waves of the digestive tract . in this method , the electrical stimulus is composed of repetitive single pulses with a pulse width in the order of milliseconds and a stimulation frequency in the vicinity of the physiological frequency of the gastric slow wave as detailed in the article “ systematic review : applications and future of gastric electrical stimulation ” by j . zhang and j . d . z . chen in alimentary pharmacology & amp ; therapeutics , volume 24 , pages 991 - 1002 ( 2006 ) that is hereby incorporated by reference in its entirety . fig4 b graphically illustrates repetitive short pulses having a pulse width that is substantially shorter than the long pulse of fig4 a and is in the order of a few hundred microseconds as opposed to milliseconds . the stimulation frequency is usually a few times higher or substantially higher than the physiological frequency of the gastric slow wave . fig4 c graphically illustrates the combining of short pulses and long pulses into a dual phase pulsing . this repetitive pulsing method is composed of one short pulse , or a multitude of short pulses , in the order of a few hundred microseconds , followed by a long pulse , in the order of a few hundred millisecond . dual phase pulsing has been shown to provide normalizing of gastric dysrhythmia and improvement in the symptoms such as nausea and vomiting . alternatively , dual phase pulsing may include a long pulse followed by a short pulse , or other combinations of long and short pulses . fig4 d graphically illustrates repetitive trains of pulses derived from the combination of two signals . the first signal is a continuous short pulse with a high frequency . the second signal is a control signal to turn the pulses on and off . for example , the second signal can contain a stimulation parameter providing that the duration of the pulse is ‘ on ’ for x seconds and ‘ off ’ for y seconds . the addition of x and y can then determine the frequency of the pulse train . this kind of stimulation is frequently used in nerve stimulation and other related areas . it should be understood that trains of pulses can include trains of short - pulses , trains of long - pulses , and / or a combination of the both long and short pulses . fig4 e graphically illustrates biphasic trains of pulses in which pulse pairs are repeatedly symmetrically generated . the first pulse of each pair has a positive amplitude and the second pulse of each pair has a negative amplitude . similar to fig4 d , pulses are repeatedly generated from the combination of two signals . the first signal includes continuous pulse pairs that are repeatedly symmetrically generated . the second signal is a control signal to turn the pulses on and off . for example , the second signal can contain a stimulation parameter providing that the duration of the pulse is ‘ on ’ for x seconds and ‘ off ’ for y seconds . the addition of x and y can then determine the frequency of the pulse train . it is contemplated , that in certain applications , it may be beneficial to vary the pulses during treatment of the gastrointestinal disorder or in the treatment of multiple disorders . for example , short pulses may be used if the device is used for treating disorders associated with the nervous systems such as pain , nausea and vomiting , long pulses or train of pulses may be used if the device is used for treating disorders associated with the movement of nutrient through the gastrointestinal tract , such as obesity or impaired gastrointestinal motility ; a combination of short and long pulses will be used if the device is used to treat disorders affected by both the nervous systems and gastrointestinal motility . additionally , although a particular pulse may be used by stimulator device 10 , it may be beneficial to vary the amplitude , frequency , and / or duration of the pulse depending on location of the stimulator device 10 . as discussed above , the stimulator device 10 is used to emit a medium for treatment of eating disorders such as obesity or a gastrointestinal disorder or disease , such as dysphagia , gastroesophageal reflux diseases , functional dyspepsia , gastroparesis , postoperative ileus , irritable bowel syndrome , constipation , diarrhea , fecal incontinence , pain / discomfort , nausea and vomiting , obesity , eating disorders as well as in the treatment of chemotherapy - induced emesis . in general , use of the stimulator device 10 includes providing the stimulator device 10 to the user 14 . the stimulator device 10 is placed in the gastrointestinal tract 12 of the user 14 . methods of administering the stimulator device 10 include placement of the stimulator device within the appendicular region 16 and / or rectal region 18 of the user 14 such as through traditional surgical procedures , laparoscopic procedures , and the like . additionally , methods of administering the stimulator device 10 may include non - surgical methods such as insertion of the stimulator device 10 into the anal orifice of the user through the use of a delivery catheter . the delivery catheter includes an elongated tubular member having at least one end adapted for insertion into the anal orifice . the stimulator device 10 is supported by the elongated tubular member for deployment within the appendicular region 16 and / or rectal region 18 . once the stimulator device 10 is in contact with the appendicular wall 20 and / or rectal wall 22 , the stimulator device 10 delivers pulses of the medium for treatment of gastrointestinal diseases and / or disorders . such pulses can be intermittent pulses , continuous pulses , and / or trains of intermittent and / or continuous pulses as discussed previously . it is contemplated that the stimulator device 10 may be distributed in a variety of methods . one method of distribution may include providing the stimulator device 10 to the user 14 by a medical professional . for example , a pharmaceutical distributor can distribute the stimulator device 10 to a medical professional for use in treating gastrointestinal disorders , diseases , and / or for use in chemotherapy - induced emesis . alternatively , the stimulator device 10 can be distributed to a pharmacy and / or provided to a retailer for over - the - counter distribution to a user 14 for use in treating gastrointestinal disorders , diseases and / or for use in chemotherapy - induced emesis as well as obesity . the pharmacy and / or retailer may then sell the stimulator device 10 directly to the user 14 . additionally , the stimulator device 10 may be provided in a kit containing the delivery catheter . the foregoing disclosure includes the best mode for practicing the invention . it is apparent , however , that those skilled in the relevant art will recognize variations of the invention that are not described herein . while the invention is defined by the appended claims , the invention is not limited to the literal meaning of the claims , but also includes these variations .
0
the present invention is explained in detail below . it is noted that “%” indicates herein “ mass %” unless otherwise defined . with regard to alloy design of the present invention , first of all , p has been selected as having a particularly low eutectic temperature with ni among b , si and p that are incorporated in the aforementioned jis compositions , in order to lower the liquidus - line temperature . the eutectic composition of ni — p binary system is ni - 11 % p . nonetheless , it has been considered to use easily available fe — p as a raw material for adding p , instead of relatively less available ni — p . in the meantime , the p content in the commercially available fe — p raw material is about 25 %, the balance of 75 % being fe and impurities . thus , fe in an amount about three times as large as p is to be added at the same time . it has also been considered that addition of cr is essential for improving corrosion resistance . in view of the above , it has been considered that a p amount of about 11 %, an fe amount about three times as large as p , and a cr amount for ensuring sufficient corrosion resistance provide an approximate system of essential elements . furthermore , through a study as shown in examples , ranges of the additive amounts of these essential elements and minor additive elements as well as other conditions have been determined to reach the present invention . fe is an essential element which is accompanied by using an fe — p raw material , and is contained in the alloy in an amount of 21 to 40 %, preferably 22 to 35 %, more preferably 22 to 29 %. fe can reduce raw material cost by reducing the content of ni which is the base metal , but an increasing amount of fe leads to an increase in the liquidus - line temperature . however , fe can be added positively in an amount up to 21 % because fe in this amount can reduce the ni content almost without raising the liquidus - line temperature . on the other hand , addition of fe in an amount of more than 40 % results in a significant increase in the liquidus - line temperature . cr is an essential element for improving corrosion resistance , and is contained in the alloy in an amount of 10 to 30 %, preferably 14 to 28 %, more preferably 17 to 24 %. while an increasing amount of cr leads to an increase in the liquidus - line temperature , an additive amount of less than 10 % results in insufficient improvement in corrosion resistance , an additive amount of more than 30 % resulting in an excessive increase in the liquidus - line temperature . p is an essential element for lowering the liquidus - temperature , and is contained in the alloy in an amount of 7 to 11 %, preferably 7 . 5 to 10 . 5 %, more preferably 8 . 5 to 10 %. while excessive addition of p in an amount beyond an eutectic composition leads to an increase in the liquidus - line temperature , an additive amount of less than 7 % or more than 11 % results in a high liquidus - line temperature . the alloy according to the present invention uses an easily available fe — p raw material that comprises about 25 % of p as a raw material , with the mass ratio fe / p in the alloy being 2 . 6 to 5 , preferably 2 . 6 to 4 . 0 , more preferably 2 . 6 to 3 . 2 . p content of 25 % leads to fe / p = 75 / 25 = 3 . 0 . since p content in this raw material varies to some extent , the lower limit of fe / p is made 2 . 6 . however , a mass ratio fe / p of less than 2 . 6 results in a too small amount of fe compared to that of p , necessitating addition of p by using relatively less available ni — p other than the fe — p raw material . in addition , a mass ratio fe / p of more than 5 results in unbalance between the fe amount contributing to an increase in the liquidus - line temperature and the p amount contributing to a decrease in the liquidus - line temperature , leading to an excessive increase in the liquidus - line temperature of the alloy . b and si may be added as needed as an optional element since these elements have an effect of decreasing the liquidus - line temperature although such effect is not as well as that of p . in this case , 5 % or less of b and 4 . 5 % or less of si may be contained in the alloy so that the total amount of p + b + si may be 7 to 13 %. addition of more than 5 % of b or more than 4 . 5 % of si results in an increase in liquidus - line temperature . a total amount of p + b + si of more than 13 % also results in an increase in liquidus - line temperature . since b and si are not essential elements , the lower limit of the total amount of p + b + si is 7 % similarly to that of the p amount , while less than 7 % results in an increase in liquidus - line temperature . preferable b amount is 3 . 5 % or less , more preferably 2 . 5 % or less . preferable si amount is 3 . 5 % or less , more preferably 2 . 5 % or less . preferable total amount of p + b + si is 7 . 5 to 11 . 5 %, more preferably 8 . 5 to 10 %. v , co and mo are optional elements that have an effect of improving strength , respectively . 5 % or less of v , 5 % or less of co and 5 % or less of mo may be contained in the alloy so that the total amount of v + co + mo may be 10 % or less . in the alloy according to the present invention , addition of at least one element of v , co and mo in an amount of more than 5 % or the total amount of v + co + mo of more than 10 % results in an increase in liquidus - line temperature . preferable amount of each of v , co and mo is 1 % or less , while no addition of these elements is more preferred . in addition , preferable total amount of v + co + mo is 5 % or less , more preferably 0 %. the alloy according to the present invention does not contain active elements , such as ti , that can be easily oxidized , and thus can also be used as a paste in mixture with a normal binder as conventionally used . the alloy according to the present invention can also be used as a normal quenched ribbon or rolled ribbon as conventionally used . the present invention is explained in detail below with reference to examples . a quenched ribbon was prepared having a composition shown in table 1 and then subjected to a liquidus - line temperature measurement and a brazing test . the quenched ribbon was obtained by previously weighing out raw materials to constitute each composition shown in table 1 followed by ark melting to prepare about 50 g of a matrix material ; placing this matrix material into a quartz tube with a nozzle width of 25 mm to remelt this matrix material ; and tapping this molten material onto a copper roll with a diameter of 300 mm being rotated at 1500 rpm . the melting and tapping were conducted in ar atmosphere under a reduced pressure . this quenched ribbon was subjected to thermal analysis to measure the liquidus - line temperature . the quenched ribbon thus obtained was placed on a disk made of sus304 with a thickness of 1 mm and a diameter of 20 mm and subjected to brazing in vacuum at 1100 ° c ., followed by cross - section observation with an optical microscope for evaluation in accordance with the following criteria : a : quenched ribbon was fully melted and brazed . b : there remains a portion that was unmelted . evaluation on melting was performed by assessing whether the entire portion of the brazing material became a dendrite - like solidified structure . this brazed test piece prepared in the same way was used and subjected to a salt spray test in which the test piece was exposed to a 5 % nacl solution at 35 ° c . for 96 hours . the exposed surface was observed and evaluated in accordance with the following criteria : aa : no rust generated a : rust generated on part of the surface b : rust generated over the entire surface an ingot having a composition shown in table 1 was prepared by centrifugal casting . the size of the prepared ingot was such that the diameter was about 35 mm and the length was about 30 mm . a test piece was cut out of the ingot to the size of 1 . 8 mm square and a length of 20 mm , followed by a three - point bending test with a supporting - point distance of 10 mm . measured bending strength was evaluated in the following criteria . b : bending strength was less than 500 mpa a : bending strength was 500 mpa or more and less than 1000 mpa aa : bending strength was 1000 mpa or more comparative example no . 11 had to use relatively less available ni — p as a raw material for p and was inferior in brazability , due to the low fe content and the high mo content . comparative example no . 12 was inferior in brazability and corrosion resistance due to the high fe content and the high v + co + mo content . comparative example no . 13 was inferior in corrosion resistance due to the low cr content . comparative example no . 14 was inferior in brazability due to the high cr content . comparative example no . 15 was inferior in brazability and corrosion resistance due to the low p content and the low fe / p mass ratio . comparative example no . 16 was inferior in brazability and had a bending strength of less than 500 mpa , due to the high p content . comparative example no . 17 was inferior in brazability and corrosion resistance due to the high b content and the high fe / p mass ratio . comparative example no . 18 was inferior in brazability and poor in corrosion resistance and had a bending strength of less than 500 mpa , due to the high si content . comparative example no . 19 was satisfactory in brazability , corrosion resistance and bending strength , but had to use relatively less available ni — p as a raw material , due to the low fe content and the low fe / p mass ratio . in contrast , it can be understood that example nos . 1 to 10 satisfy the conditions of the present invention and thus are superior in the above characteristics . as described above , by selecting p , which has a particularly low eutectic temperature with ni among b , si and p , in order to lower the liquidus - line temperature and also by using relatively easily available fe — p as the raw material for adding p , it is possible to provide a ni — fe - based alloy brazing filler material which is inexpensive in raw material cost due to the reduction in the base metal ni content , retaining corrosion resistance and having brazability and bending strength .
1
the antistatic pressure - sensitive adhesive of the present invention can be applied to a variety of products including wall coverings , shelf liners and others , having decorative and protective uses . such products generally comprise poly - vinyl chloride films although other materials such as polyolefins , paper , fabric , polyester , saran or other plastic films can be employed . the vinyl film is prepared in a known manner and is printed or otherwise processed to produce a decorative surface for display when the film is applied to the substrate . to illustrate our invention , we have prepared an aqueous latex pressure - sensitive adhesive polymer composition comprising a copolymer of a vinyl ester and an alkyl acrylate . emulsifying systems are preferably nonionic although anionic systems and mixtures of the two can be employed . it is to be understood that while a pressure - sensitive adhesive formulation is provided herein , selection thereof is not particularly critical to the practice of the invention . an additional adhesive which we have discovered to be compatible with the antistatic additive of the present invention is a water - based latex pressure - sensitive adhesive such as psa - 42m , manufactured by stein - hall , a division of celanese coatings and specialties co . suitable acrylates have the formula : ## str1 ## wherein r is an alkyl radical having at least 4 carbon atoms , and suitable vinyl esters have the formula : ## str2 ## wherein r 1 is an alkyl radical having from 1 to 5 carbon atoms . these compounds are generally disclosed in u . s . pat . no . 3 , 268 , 357 , to which reference may be made . preferred compounds we have employed successfully are vinyl acetate comprising from about 0 to 60 % by weight of the composition and 2 - ethylhexyl acrylate or butyl acrylate comprising from about 40 to 100 % by weight of the composition . in example i , the formulation for a pressure - sensitive adhesive , prepared with a nonionic emulsifier , is given . examples ii and iii are similar copolymer formulations utilizing anionic and a mixed anionic - nonionic emulsifying system , respectively . the procedure followed in each of the examples involved charging the initial components to a three neck 1000 ml . flask equipped with an agitator and dispersing all the components in the water at a temperature of 70 ° c . polymerization of the monomers was conducted under a continuous atmosphere of nitrogen . the components which were continuously added were premixed and added over a period of 3 - 41 / 2 hours utilizing a dropping funnel with adjustable stopcock . temperature was maintained at 70 ° c . for the final addition the temperature was raised to 90 ° c . for one hour . physical properties of the adhesives are given in table i . the following examples are representative and illustrate the results achieved in the practice of our invention . ______________________________________example i : continuous addition total initial over 41 / 2 - hr . additioncomponent recipe charge period at 5 hrs . ______________________________________vinyl acetate ( vac ) 50 7 . 5 42 . 5 -- 2 ethylhexyl acrylate ( 2 - eha ) 50 7 . 5 42 . 5 -- potassium persulfate 0 . 5 0 . 1 0 . 3 0 . 1sodium bicarbonate 0 . 25 0 . 25 -- -- igepal co - 630 * 2 1 1 -- igepal co - 880 ** 4 2 2 -- cellosize wp - 09 *** 1 . 5 1 . 5 -- -- water 150 80 65 5______________________________________ * nonyl phenoxy poly ( ethylene oxy ) ethanol - 65 % ethylene oxide ( gaf corp .) ** nonyl phenoxy poly ( ethylene oxy ) ethanol - 86 % ethylene oxide ( gaf corp .) *** low viscosity grade hydroxy ethyl cellulose - union carbide example ii : continuous addition total initial over 41 / 2 - hr . additioncomponent recipe charge period at 5 hrs . ______________________________________vac 40 6 34 -- 2 - eha 60 9 51 -- potassium persulfate 0 . 45 0 . 15 0 . 25 0 . 05sodium bicarbonate 0 . 25 0 . 25 -- -- aerosol ot * 1 . 5 1 . 0 0 . 5 -- aerosol ma ** 1 . 5 -- 1 . 5 -- cellosize wp - 09 1 . 5 1 . 5 -- -- water 150 80 50 15 * dioctyl sulfosuccinate - american cyanamid ** hexyl sulfosuccinate diester - american cyanamid example iii : continuous addition total initial over 3 - hr . additioncomponent recipe charge period at 4 hrs . ______________________________________vac 40 6 34 -- 2 - eha 60 9 51 -- potassium persulfate 0 . 45 0 . 15 0 . 3 -- sodium bicarbonate 0 . 25 0 . 25 -- -- aerosol ot ( 75 %) 2 1 1 -- triton x405 * 4 -- 3 1cellosize wp - 09 1 . 5 1 . 5 -- -- water 145 80 50 15______________________________________ * ethoxylated octyl phenol ( 40 moles ethylene oxide ) rohm & amp ; haas table i example i example ii example iii______________________________________ % solids 41 % 37 % 40 %% conversion 97 % 88 % 95 % ph 4 . 7 4 . 7 4 . 4viscosity ( cps ) 65 140 95brookfield - 60 rpmsurface tension 36 . 4 28 . 2 34 . 3 ( dynes ) ______________________________________ to 100 parts of each of the examles was added 2 . 5 parts by weight of our preferred antistatic additive , stearamidopropyldimethyl - β - hydroxyethylammonium nitrate under very slow agitation with an air mixer for approximately one hour . although this compound has been found by us to be satisfactory as an antistat in terms of compatibility with the pressure - sensitive adhesives disclosed and reduction of static charges , other quaternary ammonium compounds such as those disclosed in u . s . pat . no . 3 , 347 , 362 can also be employed by those skilled in the art to achieve substantially the same results . similarly , the amount of the antistat employed can be varied from about 0 . 5 to 5 . 0 parts per 100 parts of the adhesive with satisfactory results . following the addition of the antistatic agent , each of the three examples was stored for two weeks after which the viscosity was again measured to determine if thickening had occurred . for example i , no increase in viscosity was observed . for example ii , immediate coagulation of the latex was observed upon addition of the antistat . another sample was tested by treatment with 2 . 8 parts by weight of a nonionic post stabilizer , triton x405 ( per 100 parts of solids ) prior to the addition of the antistat and found to be stable with minimal viscosity increase after two weeks . for example iii , a viscosity increase from 95 cps to 195 cps was observed . thus , it can be concluded that the antistat is most stable in a totally nonionically emulsified latex . application of the antistatic pressure - sensitive adhesive to the vinyl film can be performed , for example , with a ruling mill engraved cylinder of either 95 or 59 line engraving . the adhesive is transferred from the rotating cylinder to a silicone treated kraft paper passing under pressure between the cylinder and a rubber backup roller . the adhesive coated release paper was thereafter traversed at 100 yards per minute through a hot air oven at a temperature of 194 ° c . the dried , adhesive - coated paper was subsequently laminated to a pvc film and slit into appropriate widths . the preceding examples can be varied within the context of our total specification disclosure as it would be understood and practiced by one skilled in the art to achieve substantially the same results with a minimum of routine experimentation . the improved antistatic qualities of the adhesive - backed vinyl film described herein were readily observable by stripping the backing ( silicone coated kraft paper ) away from the adhesive coated film and bringing it toward the substrate to which it will be adhered . for a normal pressure - sensitive adhesive coated product , i . e ., one in which the adhesive - compatible ammonium salt disclosed herein has not been dispersed within the adhesive formulation , a static charge , caused by the stripping of the release paper will be retained by the vinyl film and cause an undesirable attraction to the substrate . however , the antistatic adhesive composition described herein dissipates the static charge and produces a film which is readily and conveniently applicable to the desired substrate . a test was run in which normal , or untreated , pressure - sensitive adhesive coated film products were compared with film products coated with the antistatic adhesive formulation of the present invention to determine the distance each could be brought to a painted wall without attraction . the release paper was stripped from the film of each sample and the film was slowly moved toward the wall . attraction between the untreated adhesive coated product and the wall occurred at six inches , whereas the product treated with the antistatic adhesive composition of the present invention was first attracted to the wall at a distance of only one inch . thus , it can be seen that the disclosed invention carries out the objects of the invention set forth above . as will be apparent to those skilled in the art , the composition of the antistatic pressure - sensitive adhesive can be varied by the selection of the various ingredients as well as the amounts thereof in order to optimize the desired antistatic properties while maintaining the desired compatibility between the pressure - sensitive adhesive formulation and the ammonium salt , and it is believed that the preparation and use of this composition can be determined without departing from the spirit of the invention herein disclosed and described , the scope of the invention being limited solely by the scope of the attached claims .
2
in the exemplary adapter 100 shown in fig1 , an led or led - based lamp 102 can be received into a led receptacle 104 . the adapter 100 can be received in a conventional receptacle 112 for light bulbs ( e . g ., an edison base socket ). fig1 shows a threaded portion 114 of the inner surface 116 of the conventional receptacle 112 . the outer surface 126 of adapter 100 also includes a threaded portion 128 so that adapter 100 can be screwed into the conventional receptacle 112 . it should be understood however , that an adapter having a threaded outer surface is illustrative only , and that adapters having an unthreaded surface or mating features such as pins or bumps ( e . g ., gu10 , mr16 sockets ) are within the scope of the present invention . the outer surface 126 of adapter 100 is conductive , i . e ., it may comprise or consist essentially of a conductive metal or metal alloy ( e . g ., copper , silver , aluminum , etc .). once received in the conventional receptacle 112 , the outer surface 126 of adapter 100 is in contact with the inner surface 116 of receptacle 112 . the adapter 100 has an electrical contact 132 that is electrically coupled to a base contact 134 of the conventional receptacle 112 when the adapter 100 is installed therein . the electrical contact 132 is electrically isolated from the outer conductive surface 126 of adapter 100 . such isolation can be achieved by surrounding the electrical contact 132 with an insulation material ( e . g ., plastic , ceramic , etc .) ( not shown ) so that the electrical contact 132 is not in direct physical contact with the outer conductive surface 126 . alternatively or in addition , the electrical contact 132 can include an inner conductive portion and an outer non - conductive portion for insulation . fig1 also shows solder 140 that is activated , i . e ., melted so that a substantially permanent bond is formed between the outer surface 126 of adapter 100 and the inner surface 116 of the receptacle 112 when the solder 140 resolidifies . as a result , receptacle 112 can no longer receive an incandescent light bulb . the led 102 , however , can be removed from the led receptacle 104 and replaced . the activation of solder 140 is described below with reference to fig2 a - 2c . a power converter / limiter 150 may be included in the adapter 100 and , if included , is connected to the electrical contact 132 and the outer conductive surface 126 of the adapter 100 . after the adapter 100 is installed within the conventional receptacle 112 , the power converter / limiter 150 receives the electric power supplied to the conventional receptacle 112 ( e . g ., ac line voltage ) and converts it into a type of power suitable for the operation of the led 102 ( e . g ., 12 v dc ), and may also limit the total power consumption to eliminate the user &# 39 ; s ability to modify a higher - power device for installation into the adapter . the power converter / limiter 150 provides the converted and / or conditioned power to the led 102 . the power converter / limiter 150 may , for example , be a solid - state transformer and / or a ac - dc rectifier , and may also contain a power - or current - limiting element . in some situations , a user may replace the led 102 with a relatively inexpensive light source receivable in the adapter 100 that consumes substantially more power than the led 102 . this would eliminate or mitigate the low - power - consumption benefits of using an led . in order to deter such a replacement , in some embodiments the total power output by the power converter / limiter 150 is limited to a predetermined threshold ( e . g ., the power required by the led 102 ). thus , another light source requiring substantially more power may not be received in the adapter 100 . bonding of an adapter embodiment 200 within a conventional receptacle 212 is illustrated in fig2 a - 2c . fig2 a shows a portion of the outer surface 206 of the adapter 200 and the inner surface 216 of a receptacle 212 . in this embodiment , surfaces 206 , 216 are smooth , and surface 206 is surrounded by a foil 222 . the foil may comprise or consist essentially of intermixed metal layers ( e . g ., layers of aluminum and nickel ). the foil may be chemically deposited to the surface or mechanically applied . solder 240 sandwiches the foil 222 , i . e ., is in contact with the inner and outer surfaces , 224 , 226 of foil 222 . solder 240 can be applied to both sides of foil 222 using known methods such as , for example , coating or electrochemical deposition . solder 240 can also take the form of a wire or band or a pattern of beads in contact with the surfaces 224 , 226 . adapter 200 can be supplied with foil 222 wrapped around its outer surface 206 . fig2 b shows adapter 200 received within receptacle 212 . as a result , foil 222 and solder 240 intervene between the outer surface 206 of adapter 200 and the inner surface 216 of receptacle 212 . fig2 b shows that solder 240 is not activated ( i . e ., not melted and , hence , not bonded to either surface 206 or surface 216 ). therefore , adapter 200 can be removed from the conventional receptacle 212 . as shown in fig2 c , the foil 222 and solder 240 may be activated by a current flow that occurs when electricity is supplied to the conventional receptacle 212 for the first time following introduction of adapter 200 therein . specifically , when a line voltage is applied between the inner surface 216 and the base contact 234 , the conversion circuitry converts the line voltage to power the led , and current flows through foil 222 and solder 240 . this current flow can activate foil 222 and solder 240 . in particular , the current flow causes foil 222 to release sufficient heat to melt the solder . releasing heat in response to current flow is an inherent property of a foil having intermixed metal layers . the solder 240 surrounding foil 222 melts and bonds with surfaces 206 , 216 as it cools and solidifies ; the foil 222 may disintegrate or dissolve into solder 240 . as a result , adapter 200 is substantially permanently affixed to the conventional receptacle 212 , and receptacle 212 can no longer receive an incandescent light bulb . the foil 222 and solder 240 can be activated alternatively or additionally by radiation of energy 242 . radiation 242 can be provided by a source 244 of radiation positioned proximate to the surface 206 of adapter 200 . for example , source 244 can be a microwave emitter , radiating electromagnetic energy that induces eddy currents in foil 222 , causing it to release heat and thereby activate solder 240 . the source of radiation 244 can alternatively be a laser emitter , or a separate electrical power supply . permanent bonding agents other than solder can be employed . for example , as shown in fig3 , a uv - or visible light - curable epoxy can be used as a bonding agent . the adapter 300 has an led receptacle 304 and a conducting outer surface 306 through which one or more windows 308 provide a line of sight . although surface 306 is shown two rectangular windows 308 , fewer ( i . e ., only one ) or more windows circumferentially distributed around receptacle 304 , and windows of different shapes and sizes ( e . g ., circle , oval , square , etc .) are within the scope of the present invention . windows 308 can be formed by cutting out portions of surface 306 or by punching or drilling holes in surface 306 . windows 308 may be fitted with flexible transparent panes 310 . such panes can be formed using a material sufficiently transparent to allows passage of uv or visible light . examples of such materials include clear plastic ( e . g ., polycarbonate ). transparent panes 310 are affixed within the windows 308 substantially permanently using methods such as gluing , clamping , riveting , etc . the conducting outer surface 306 , fitted with window panes 310 , can be threaded so that it may be screwed into a conventional incandescent receptacle . a layer 312 of a uv - or visible - light - curable epoxy is positioned in direct contact with the outer surface of window panes 310 . for example , window panes 310 can be coated with the curable epoxy . for a threaded adapter 300 , the epoxy may be applied as a bead in the spiral trough of the threads . the adapter 300 can be received in a conventional receptacle . initially , the epoxy layer 312 is not bonded to , but is in contact with , the adjacent inner surface of the conventional adapter . the conductive outer surface 306 of adapter 300 is in electrical contact with the inner surface of the conventional receptacle . for example , if the epoxy is only within the trough of the adapter threads , or is applied in a spiral or striped pattern around the outer adapter surface 306 , areas of direct mechanical contact between the outer surface 306 and the inner surface of the receptacle remain ( where the epoxy is not present and does not intervene ). when the optical radiation emitted from an optical source 314 positioned above the led receptacle 304 is directed inside the adapter 300 , the light propagates through the transparent windows 308 and activates — i . e ., causes cross - linking of — the uv or visible light - curable epoxy layer 312 . as a result , the adapter 300 is substantially permanently bonded to the conventional receptacle , while allowing the epoxy - free portions of conductive outer surface 306 to maintain electrical contact with the inner surface of the conventional receptacle . as a result , an led can be received in and removed from the led receptacle 304 of adapter 300 , but the adapter itself cannot be removed . in the embodiment illustrated in fig3 , the adapter 300 is typically exposed to a source 314 before receiving an led in the led receptacle 304 so that the light from the source 314 can be directed , without obstruction , inside the adapter 300 . alternatively , in the adapter embodiment 400 shown in fig4 , a uv led 402 is received in the led receptacle 404 . when the led is turned on for the first time , uv radiation 420 therefrom exposes the epoxy layers 412 . areas of the threaded portion may be fitted with flexible transparent regions 410 to permit transmission of uv radiation . although a uv - curable epoxy may be used as a bonding agent in adapters 300 , 400 , and a uv source used to activate the epoxy , it should be understood that any adhesive cross - linked by actinic radiation is suitable . other examples include uv - curable acrylic or methacrylic polymers combined with a tackifying resin and a photoinitiator , having described certain embodiments of the invention , it will be apparent to those of ordinary skill in the art that other embodiments incorporating the concepts disclosed herein may be used without departing from the spirit and scope of the invention . accordingly , the described embodiments are to be considered in all respects as only illustrative and not restrictive .
1
hereinafter , embodiments of the invention will be described in detail in reference to the appended drawings . [ 0018 ] fig1 is a structural view for showing an example of a multimedia conference terminal applied to the invention . as shown in fig1 the multimedia conference terminal of the invention operates in the environment of any operating system 107 such as widows 95 , 98 or nt , etc . which supports the internet , and has a video i / o ( input / output ) device 100 , an audio i / o device 101 , a video codec 102 , an audio codec 103 , a video and audio synchronization module 104 , a video / audio / control signal integration and extraction module 105 and a network interface module or card 106 as hardwares , and a system control and control interface module 108 and a data application module 109 as softwares . first , the video i / o device 100 receives image signals to produce video signals or replays received video signals , the audio i / o device 101 receives voice signals of a user to produce audio signals or replays received audio signals . the video codec 102 and the audio codec 103 compress the signals from the video and audio i / o devices 100 and 101 or restore the received signals . the video / audio synchronization module 104 compensates the difference between the restoring times of the video and audio signals . the video / audio / control signal integration and extraction module 105 has functions of converting video / audio / control signals into signals for transmission and extracting video / audio / control signals from transmitted signals . the network interface card 106 transmits the signals to a network or receives signals from the network . meanwhile , it is required that the multimedia conference terminal can interpret information about lower dynamic multicast trees for joining the dynamic multicast network and conform if a directly connected lower terminal is connected to the dynamic multicast network . when it is desired to release the connection with the dynamic multicast network , the multimedia conference terminal reports termination thereof to a directly connected higher terminal . also , it is required for the multimedia conference terminal to propagate the transmitted packet to a lower directory . [ 0024 ] fig2 is a structural view for showing an example of an autonomous system which is a basic unit of the dynamic multicast network applied to the invention . as shown in fig2 the autonomous system 210 ( hereinafter will be referred to as as ) has a rtp element 211 and rtp receiver terminals 212 . the rtp element 211 manages the as 210 and communicates with other elements . the rtp element 211 is connected to a media stream source as the root of the as 210 so that the rtp element 211 can receive a media stream 200 . it is also required that the rtp element 211 can construct the dynamic multicast network , and has ability to propagate to a lower tree , which has the rtp element 211 as the root about tree information or tree - info . the tree information has a new parent ip address about each of the rtp receiver terminals 212 . the rtp receiver terminals 212 transmit the multicast packet to other lower trees in order to effectively transmit information to rtp receiver terminals which are not connected to the multicast network . a rtp receiver terminal b is called “ lower terminal ” of rtp receiver terminal a , and the rtp receiver terminal a is called “ higher terminal ” of rtp receiver terminal b . the rtp receiver terminal b and another rtp receiver terminal c are called “ neighbor .” a higher terminal transmits rtp / rtcp audio and video sessions to a lower terminal . here , the rtp or real time protocol is a kind of application protocol for transmitting multimedia data which have real time property in a multimedia application . also , the rtp can use other network transmission protocols as lower protocol . in other words , when the lower protocol provides multicast distribution , data can be transmitted to a number of destinations . also , the rtcp or real time control protocol is a protocol for controlling the rtp . [ 0033 ] fig3 shows signal flows in an example of a procedure for dynamic multicast tree joining of the new multimedia terminal according to the invention , in which messages are transmitted to construct the dynamic multimedia tree in the multimedia conference service while distributing the load of the root node . as shown in fig3 the messages are transmitted to construct the dynamic multimedia tree in the multimedia conference service while distributing the load of the root node as follows : first , a new participant b or 300 sends a find rtp message 301 to find a rtp element for joining the nearest dynamic multicast tree . the find rtp message 301 includes ip address of the new participant and ip address information of the rtp element which is the root node of the dynamic multicast tree to which the ip address is notified . upon receiving the find rtp message 301 , first rtp element 310 transmits a reply rtp message 302 to the new participant b or 300 . upon receiving the reply rtp message 302 , the new participant b or 300 waits for a predetermined time period , and then selects a suitable rtp element and transmits a select rtp message 303 to the rtp element . here , it is confirmed if the first rtp element 310 is subscribed in the dynamic multicast tree that the participant b or 300 wants to join . if the first rtp element 310 is subscribed in the dynamic multicast tree that the participant b or 300 wants to join as a result of the confirmation , a message asking to join or ask - join message 304 is transmitted to the new participant b or 300 . if the first rtp element 310 is not subscribed in the dynamic multicast tree that the participant b or 300 wants to join as a result of the confirmation , a join message 311 is transmitted to second rtp element 320 that is the root node of 11 o the dynamic multicast tree . here , the join message 311 includes information that indicates ability of the first rtp element 310 . upon receiving the join message 311 from the first rtp element 310 , the second rtp element 320 constructs a dynamic multicast tree and transmits a tree - info message 312 to the first rtp element 310 . the tree - info message 312 includes ip address about a higher node of the first rtp element 310 . upon receiving the tree - info message 312 , the first rtp element 310 uses information included in the message to set ip addresses of the higher node and the rtp element . the first rtp element 310 transmits an ask message 331 to the ip address of the newly set higher node c or 330 . the ask message 331 includes the ip address and ability of the first rtp element . upon receiving the ask message 331 from the first rtp element 310 , the higher node c or 330 adds the ip address of the first rtp element 310 to a lower terminal list . the first rtp element 310 receives a reply message 332 and a connect message 333 and then receives a rtp / rtcp session 334 , and periodically transmits an alive message 335 to the higher node c or 330 to report the connection of the first rtp element 310 to the higher node c or 330 . the higher node c or 330 cancels the first rtp element 310 from the lower terminal list if the alive message 335 is not received for a predetermined time period . also , the higher node stops packet transmission and closes the rtp / rtcp session 334 if the alive message 335 is not received from the lower node . upon receiving the connect message 333 , the first rtp element 310 transmits the ask - join message 304 to the participant b or 300 . when the message is received from one of the cases including that the first rtp element 310 is subscribed in the dynamic multicast tree that the participant b or 300 wants to join and that the first rtp element 310 is subscribed in the dynamic multicast tree that the participant b or 300 wants to join , the participant b or 300 transmits the join message 305 to the first element 310 . the join message 305 includes information indicating ability of b or 300 . when the first rtp element 310 receives the join message 305 , the first rtp element 310 constructs the dynamic multicast tree and transmits the tree - info message 306 to the rtp receiver terminal b or 300 . the tree - info message 306 includes the ip address about the higher node of the terminal b or 300 and ip address of the rtp element that is the root of the as to which the terminal b or 300 will belong when the rtp element is not changed , and address of new rtp element when the rtp element is changed . if the ip address of the rtp element , which is the root of the as to which the terminal b or 300 will belong , is same as the ip address of the terminal b , the terminal b or 300 itself the root of the new as and also the higher terminal is the rtp element that is the root of another as . if the tree - info message 305 includes new rtp address , the join message is transmitted to the new rtp element , and the rtp receiver terminal b or 300 which received the tree - info message 305 uses the information included in the message to set the ip addresses of the higher terminal and the rtp element . the rtp receiver terminal b or 300 transmits an ask message 341 to an ip address of a higher node a or 340 which is newly set . the ask message 341 includes the ip address and ability of the terminal b or 300 . upon receiving the ask message 341 , the higher node a or 340 adds the ip address of the rtp receiver terminal b or 300 to a lower terminal list and transmits a reply message 342 to the receiver terminal b or 300 . upon receiving the reply message 343 and a connect message 343 , the receiver terminal b or 300 receives a rtp / rtcp session 344 , and periodically transmits an alive message 345 to the higher node a or 340 to report the connection of the receiver terminal b or 300 to the higher node a or 340 . the higher node a or 340 cancels the receiver terminal b or 300 from the lower terminal list if it does not receive the alive message 345 for a predetermined time period . also , the rtp receiver terminal stops the packet transmission and closes the rtp / rtcp session 344 if the alive 345 message is not received from the lower terminal . when the new rtp receiver terminal joins the conference , the receiver terminal transmits the join message to the rtp element that the address thereof is previously known , so as to report that the rtp receiver terminal will join the conference . when leaving the conference , the conference participant transmits a leave message to the rtp element of the as to which the conference participant belongs . also , the rtp element reconstructs the dynamic multicast network about the lower multicast network having the leaving rtp receiver terminal as the root and connects to the nearest node , and then transmits a new dynamic multicast tree - info to the previously notified rtp element . number of the lower terminals connected to the rtp receiver terminal differs according to the network environment and node ability . the ability of the node for constructing the tree is used when the rtp element constructs the dynamic multicast network . the dynamic multicast tree is modified if the rtp receiver terminal joins or leaves the conference . [ 0056 ] fig4 is a structural view for showing an example of the overall dynamic multicast tree for a multimedia conference applied to the invention . [ 0057 ] fig4 is an example in which the ass 210 are connected in a step configuration to construct the dynamic multicast network . the dynamic multicast tree is comprised of two kinds of trees , i . e ., inter as tree and intra as tree . the root of the inter as tree is the rtp element 211 that directly receives multimedia conference contents from the media stream source 200 , and connects the rtp elements in the shortest path . the previous multicast tree construction algorithm is used to construct the inter as tree , and dynamically determined when a new participant is added to the dynamic multicast tree . here , the rtp element to be connected to the media stream source is determined based upon number of hops among the media steam source 200 and the rtp element 211 , band width , number of connected lower terminals , etc . here , number of the hops means number of the rtp elements which are passed by from the media stream source 200 to the destination rtp element . the root of the intra as tree is the rtp element 211 . in the inter as tree , the rtp element 211 functions as a middle node between the rtp element 211 that is the root of the inter as tree which directly receives the conference contents from the media stream source 200 and the root node of another as . the intra as tree is connected to the rtp receiver terminal in the shortest path . it is required that the intra as tree construction information is managed by the rtp element and transmitted to the rtp receiver terminal in the course of the conference setting . [ 0061 ] fig5 a and fig5 b are a flow chart for showing a procedure in which a new participant joins a dynamic multicast tree according to an embodiment of the invention . in the procedure of joining the dynamic multicast tree , the new participant transmits a find rtp message to find a rtp element which can join a dynamic multicast tree nearest to the new participant in step 401 . in step 402 , upon receiving the find rtp message , the rtp element transmits a reply rtp message , and the new participant confirms if the reply rtp message is received . if the reply rtp message is not received , the new participant waits to receive the message again . upon receiving the reply rtp message , the new participant waits for a predetermined time period , and then selects a suitable rtp element and transmits a select rtp message to the rtp element in step 403 , and then waits to receive an ask - join message from the rtp element . if the ask - join message is received as a result of judgment in step 404 , the new participant transmits a join message to the rtp element in step 405 . if the ask - join message is not received , the new participant waits for the ask - join message again . after the reply rtp message and ask - join message are received and the join message is transmitted to the rtp element , if the new participant receives a tree - info message in step 406 , the new participant confirms if the address of the rtp element is changed from the previously known address to another one in step 407 . if the address of the rtp element is changed as a result of the confirmation of the address change , the new participant inspects if the changed address of the rtp element is that of the new participant in step 408 . if the changed address is not the address thereof as a result of the inspection , the new participant repeats to transmit the join message of joining with the address of the changed rtp element in the step 405 . if the changed address is the address thereof as a result of the inspection , the new participant transmits an ask message to a higher terminal to register the new participant in step 409 . here , the new participant itself is the rtp element so that the higher terminal becomes another rtp element . if the address of the rtp element is not changed as a result of the confirmation , the new participant transmits the ask message to the higher terminal to register the new participant in the step 409 . in step 410 , the multimedia terminal as a new participant receives a reply message and a connect message from the higher terminal . then , the multimedia terminal or new participant belongs to the dynamic multicast tree for the multimedia conference . in step 411 , the multimedia terminal receives a media stream transmitted from the media stream source 200 via the multimedia conference , and in step 412 , periodically transmits an alive message to the higher terminal to report aliveness thereof . in step 413 , it is determined to end or not . if selected not to end , the media stream is continuously received , and if selected to end , the foregoing procedure is terminated . [ 0073 ] fig6 is a flow chart for showing a procedure in which a new participant joins a dynamic multicast tree according to another embodiment of the invention . in the procedure of joining the dynamic multicast tree , it is determined if a find rtp message is received from the new participant in step 601 , and then in step 601 , a reply rtp message is transmitted to the new participant in the case of receiving the find rtp message . after the rtp message is transmitted in the step 602 , if a select rtp message is received from the new participant in step 603 , it is determined if the rtp element itself is subscribed in the dynamic multicast that the new participant wants to join in step 604 . if the rtp element is subscribed in the dynamic multicast that the new participant wants to join as a result of the determination in the step 604 , an ask - join message is transmitted to the new participant in step 611 , and then a join message is received from the new participant in step 612 . also , after a tree - info message is transmitted , it is proceeded to the step 601 of receiving the find rtp message . if the rtp element is not subscribed in the dynamic multicast that the new participant wants to join as a result of the determination in the step 604 , a join message including information which indicates ability of the rtp element to the root node of the dynamic multicast tree in step 605 , and it is determined if a tree - info message including ip address about a higher node of the rtp element is received from the root node in step 606 . here , upon receiving the tree - info message , the rtp element uses information included in the tree - info message to set the ip addresses of the higher node and the rtp element , and then transmits an ask message including the ip address and ability of the rtp element to the ip of the newly set higher node in step 607 . after receiving the ask message , the root node adds the ip address of the rtp element to a lower terminal list and transmits a reply message and a connect message . the rtp element determines if the reply message and connect message from the root node are received in step 608 . if the reply message and connect message are received , the rtp element receives a media stream in step 609 , and periodically transmits an alive message to the higher node to report the connection thereof in step 610 . then , the ask - join message is transmitted to the new participant . when the join message is received from the participant in step 612 , after the tree - info message is transmitted , it is proceeded to the step 601 of receiving the find rtp message . [ 0079 ] fig7 is a flow chart for showing a procedure in which a rtp receiver node joins as a node of a dynamic multicast tree to transmit a packet for a multimedia conference according to a further embodiment of the invention . upon receiving the packet from a higher terminal , a rtp receiver terminal 212 and a rtp element 211 connected to the dynamic multicast tree transmits the packet to a higher terminal . this is described according to the flow in fig7 as follows : first in step 701 , the rtp terminals and rtp elements which are connected to the dynamic multicast tree initialize demonstration . in step 702 , it is confirmed if the initialized demonstration will be terminated . if selected not to terminate the demonstration , in step 703 , it is confirmed if the packed is received . when the packet is received , the rtp terminals and rtp elements confirm if the packet donor is received from the higher node thereof in step 704 . if the multimedia terminal joining the dynamic multicast tree as a node received the packet from the higher terminal , the multimedia terminal which received the packet copies a lower terminal list maintained thereby to a temporary list in step 705 , and confirms if the temporary list is blank in step 706 . if the temporary list is not blank as a result of the confirmation in the step 706 , address of the lower terminal is extracted from the temporary list and information about the lower terminal is canceled in step 707 . about the packet received from the higher terminal , source of the packet is set as the address of the multimedia terminal , the destination of the packet is updated as the address of the extracted lower terminal in step 708 , and the packet is transmitted to the lower terminal in step 709 . upon receiving the packet , the terminal repeats the step 706 of confirming if the temporary list is blank or not . if the temporary list is not blank as a result of the confirmation in the step 706 , it means that all of the packets received from the higher terminal is transmitted to the lower terminal or there is no lower terminal so that it is proceeded to the step 702 of confirming termination . as described hereinbefore , the method of the invention can be stored in a record medium including cd - rom , ram , rom , floppy disk , hard disk , optical magnetic disk , etc . as a form of a realizable program that can be read by a computer . according to the invention , the method of constructing the multicast tree allows the terminals that are not connected to the multicast network to join the multimedia conference so that the expected overload to the root node can be distributed thereby efficiently constructing the grand conference . although the preferred embodiments of the invention have been disclosed for illustrative purpose , those skilled in the art will be appreciate that various modifications , additions and substitutions are possible , without departing from the scope and spirit of the invention as disclosed in the accompanying claims .
7
in accordance with the present invention , a method for treatment of inflammation is provided , which comprises administration of a therapeutically effective amount of the n - desulfated heparin . in the method of the present invention , the term “ therapeutically effective amount ” means the total amount of the n - desulfated heparin that is sufficient to show a meaningful patient benefit , that is , healing of pathological conditions characterized by leukocyte infiltration and deposition or increase in rate of healing of such conditions , whether administered in combination , serially or simultaneously . in practicing the method of treatment of this invention , a therapeutically effective amount of the n - desulfated heparin is administered to a mammal having a disease state . such disease states include inflammatory disorders such as various kinds of arthritis , asthma , dermatitis and psoriasis , acute respiratory distress syndrome , ulcerative colitis , various types of hepatitis , ischemia / reperfusion injury ( including myocardial , renal , skeletal muscular , intestinal , cerebral and pulmonary ischemia / reperfusion injury ), shock , severe trauma and transplant rejection . in practicing the method of the present invention , the n - desulfated heparin may be administrated alone or in combination with other therapies . for example , the non - anticoagulant heparin may optionally be used in combination with certain cytokines , lymphokines , or other hematopoietic factors such as m - csf , gm - csf , nksf , il - 1 , il - 2 , il - 3 , il - 4 , il - 5 , il - 6 , il - 7 , il - 8 , il - 9 , il - 10 , il - 11 , il - 12 , g - csf , meg - csf , and erythropoitin to treat inflammatory states . it is contemplated that the method of treatment will allow the non - anticoagulant heparin to synergize with the cytokine , lymphokine , or other hematopoietic factor , thereby augmenting the anti - inflammatory response . alternatively , the method of treatment will allow the n - desulfated heparin to minimize the potential side effects caused by the cytokine , lymphokine , or other hematopoietic factor . pharmaceutical compositions used to practice the method of the present invention may contain , in addition to the n - desulfated heparin , pharmaceutically acceptable carries , diluents , fillers , salts , buffers , stabilizers , and / or other materials well known in the art . the term “ pharmaceutically acceptable ” means a non - toxic material that does not interfere with the effectiveness of the biological activity of the active ingredient ( s ). the characteristics of the carrier or other material will depend on the route of administration . administration of the n - desulfated heparin used to practice the method of the present invention can be carried out in a variety of conventional ways , such as oral ingestion , or cutaneous , subcutaneous , or intravenous injection . intravenous administration to the patient is preferred . when a therapeutically effective amount of the n - desulfated heparin is administered orally , the non - anticoagulant heparin will be in the form of a tablet , capsule , powder , solution or elixir . when administrated in tablet form , the pharmaceutical composition of the invention may additionally contain a solid carrier such as a gelatin or an adjuvant . the tablet , capsule , and powder contain from about 5 to 95 % the n - desulfated heparin , and preferably from about 25 to 90 % the n - desulfated heparin . when administered in liquid form , a liquid carrier such as water , petroleum , oils and animal or plant origin such as peanut oil , mineral oil , soybean oil , or sesame oil , or synthetic oils may be added . the liquid form of the pharmaceutical composition may further contain physiological saline solution , dextrose or other saccharide solution , or glycols such as ethylene glycol , propylene glycol or polyethylene glycol . when administered in liquid form , the pharmaceutical composition contains from about 0 . 5 to 90 % by weight of the n - desulfated heparin , and preferably from about 1 to 50 % the n - desulfated heparin . when a therapeutically effective amount of the n - desulfated heparin is administered by intravenous , cutaneous or subcutaneous injection , the n - desulfated heparin will be in the form of a pyrogen - free , parentally acceptable protein solutions , having due regard to ph , isotonicity , stability , and the like , is within the skill in the art . a preferred pharmaceutical composition for intravenous , cutaneous , or subcutaneous injection should contain , in addition to the n - desulfated heparin , an isotonic vehicle such as sodium chloride injection , ringer injection , dextrose injection , dextrose and sodium chloride injection , lactated ringer injection , other vehicle as known in the art . the pharmaceutical composition used to practice the method of the present invention may also contain stabilizers , preservatives , buffers , antioxidants , or other additive known to those of skill in the art . the amount of the n - desulfated heparin in the pharmaceutical composition used to practice the method of the present invention will depend upon the nature and severity of the condition being treated , and on the nature of prior treatments which the patient has undergone . ultimately , the attending physician will decide the amount of the n - desulfated heparin with which to treat each individual patient . it is contemplated that the various pharmaceutical composition should contain about 0 . 1 μg to about 100 mg of the n - desulfated heparin per kg body weight . the duration of intravenous therapy using the pharmaceutical composition used to practice the method of the present invention will vary , depending on the severity of the disease being treated and the condition and potential idiosyncratic response of each individual patient . it is contemplated that the duration of each application of the n - desulfated heparin will be in the range of 12 to 24 hours of continuous intravenous administration . ultimately the attending physician will decide on the appropriate duration of intravenous therapy using the pharmaceutical composition of the present invention . the pharmacokinetics and the toxicity experiments of the n - desulfated heparin are being carried now . the sodium salt of heparin ( sigma ) was passed through a column of dowex ( strongly acidic cation exchanger 50 × 4 - 100 ; sigma ) and the effluent was neutralized with pyridine . it was then lyophilized to give a white powder [ inoue and nagasawa , carbohydr . res . 46 , 87 - 95 ( 1976 )]. the pyridine salt of heparin ( 100 mg dissolved in 0 . 25 ml of double destined and deionized h 2 o ) was mixed with 4 . 75 ml of dimethylsulfoxide ( dmso ; sigma ) at 50 ° c . for 2 hour ( sample no . 4 ), 1 hour ( sample no . 1 ), or 20 ° c . for 3 hours ( sample no . 3 ). the sample was diluted with an equal volume of h 2 o and the reaction was terminated by adjusting ph to 7 . 0 with 0 . 1 nnaoh [ nagasawa and inoue , carbohydr . res . 36 , 265 - 271 ( 1976 ); inoue and nagasawa , carbohydr . res . 46 , 87 - 95 ( 1976 ); tiozzo et al ., thromb . res . 70 , 99 - 106 ( 1993 )]. the sample no . 1 heparin was further dissolved in 1 nnaoh ( 4 % heparin concentration ) at 60 ° c . for 4 hours followed by neutralization to ph 7 . 0 with 1 n hcl ( sample no . 2 ). the pyridine salt of heparin was dissolved in 1 nnaoh ( 4 % heparin concentration ) followed by treatment at 40 ° c . ( sample no . 5 ) or at 60 ° c . ( sample no . 6 ) for 4 hours . further , the sodium salt of heparin was dissolved in 1 n naoh ( 4 % heparin concentration ) followed by treatment at 40 ° c . ( sample no . 7 ) or at 60 ° c . ( sample no . 8 ) for 4 hours . sample was then neutralized to ph 7 . 0 with 1 n hcl [ tiozzo et al ., thromb . res . 70 , 99 - 106 ( 1993 ); lloyd et al ., biochem . pharmacol . 20 , 637 - 648 ( 1971 )]. after chemical modification , these heparin derivatives were individually passed through a column of amberlite ira - 400 ( strongly basic anion exchanger ; sigma ) to remove the free sulfate ions . the effluent was neutralized to ph 7 . 0 with 1 n naoh . it was then desalted by passing through a column of bio - gel p - 2 ( bio - rad ). heparins were monitored at the optical densities of 214 nm and 230 nm . activated partial thromboplastin time ( aptt ) was measured using fresh human blood from healthy volunteers . the known amounts of heparin , low molecular weight heparin and the chemically modified heparin derivatives were added prior to the determination of aptt using silimat ™ ( biomeieux sa ) as activator . six assays were performed for each compound and the anticoagulant activity was expressed as the concentration ( ug / ml ) that doubles the aptt time ( 2 - aptt ). the higher concentration is parallel to the lower anticoagulant activity ( table 1 ). the same assay was carried to determine the aptt time of the mice in vivo ( fig4 .). solution and reagents : 5 % sodium nitrite , 33 % acetic acid , 3 . 8 % trichloroacetic acid , barium chloride - gelatin reagent ( prepared by dissolving 1 g of gelatin in 100 ml of water , incubated at 60 ° c . to make a complete dissolution , then put it at 4 ° c . overnight . the mixture was filtered after adding 0 . 5 g of barium chloride and was ready to use after standing for 4 hours at room temperature . this reagent was stored at 4 ° c . and could be used for about one week .) n - sulfates in heparin and various chemically modified heparin derivatives were determined by nitrous acid treatment as described [ inoue and nagasawa , anal . biochem . 71 , 46 - 52 ( 1976 )]. briefly , 0 . 5 ml of a sample solution was mixed with 0 . 5 ml of 5 % sodium nitrite and 0 . 5 ml of 33 % acetic acid . after shaking , the mixture was incubated at room temperature for 30 min and 4 . 5 ml of 3 . 8 % trichloroacetic acid was then added . after shaking again , 1 . 5 ml of the barium chloride - gelatin reagent was added . following shaking again immediately , the sample was left standing for 20 min and the turbidity of the sample was measured at 500 nm . the absolute n - sulfate mounts of all n - desulfated heparin sample were calculated with k 2 so 4 as control , while the relative n - sulfate mounts of all n - desulfated heparin were calculated using the starting heparin as 100 %. the contents of uronic acid of the no . 4 sample and heparin were determined according to the method of bitter and muir ( anal . biochem . 4 : 330 - 334 , 1962 ). the hexosamine contents were determined according to the method of elson and morgan ( biochem . j . 27 : 1824 - 1828 , 1993 ). the contents of free amino group , at a 2 mg / ml concentration , were determined as before ( yoshizawa et al ., biochim . biophys . acta ., 141 : 358 - 365 , 1967 ). reducing power , at a 2 mg / ml concentration , was measured using the 3 , 6 - dinitrophthalic acid method ( momose et al ., talanta , 4 : 33 - 37 , 1960 ). the average molecular weights were determined using the end group analysis ( hopwood and robinson , biochem . j . 135 : 631 - 637 , 1973 ). balb / c mice ( males , 5 weeks old , 20 ± 1 g body weight ) were purchased from shanghai animal center of chinese academy of sciences . negative control group contained 8 mice , they were intraperitoneally injected with 1 ml of sterile pyrogen - free saline . fifteen minutes later , mice were intravenously injected with 0 . 2 ml sterile pyrogen - free saline alone . the positive control group ( 12 mice ) was intraperitoneally injected with 1 ml of 3 % thioglycollate broth . fifteen minutes later , mice were intravenously injected with 0 . 2 ml saline . the mice of the anti - inflammation group ( 7 - 11 ) were intraperitoneally injected with 1 ml of 3 % thioglycollate broth . fifteen minutes later , mice were intravenously injected with saline containing 1 . 5 mg of low molecular weight heparin or any of the chemically modified heparin derivatives . mice were sacrificed at 2 hours . the peritoneal cavities were lavaged with 8 ml of ice - cold pbs containing 10 u / ml of heparin to prevent clotting . centrifuged at 1500 rpm for 5 mins . the total peritoneal leukocytes and their differentiation ( lymphocyte , monocyte and granulocyte ) were measured using cell - dyn1700 ( abbot laboratories , usa ). the mice of heparin therapeutic groups appear more active than the positive control group during the experiments time . shortly after the injection of the samples , few mounts of blood was bleeding from the pinpricks of the mice administrating the no . 4 sample , concomitantly the coagulant time was shorter than those groups administrating other heparin samples . furthermore , when collecting the total peritoneal infiltrated leukocytes , the group administrating no . 4 sample showed no inner bleeding phenomena , but other groups has little or more bleeding . the experiments watching above reflected the no . 4 sample has significant reduced anticoagulant activity while remaining the anti - inflammation effect . [ 0118 ] fig1 shows the result of the anti - inflammation screening assay in vivo , at the same time table 2 represents the inhibition percent of the peritoneal infiltrated inflammation leukocytes . 1 - ( cell   number   of   all   heparin   derivatives - cell   number   of   negative   control ) ( cell   number   of   positive   control - cell   number   of   negative   control ) all n - desulfated heparin has different anti - inflammation activity , the result showed that the total white blood cell inhibition percent is about 52 . 1 - 70 . 9 %, total lymphocyte inhibition percent is about 49 . 5 - 72 . 1 %, monocyte inhibition percent is about 47 . 6 - 82 %, granucyte inhibition is about 10 . 6 - 40 . 9 %, all n - desulfated heparin has better anti - inflammation activity than lmh which is commonly used in the art , besides , n0 . 4 sample is the best . swiss mice ( five weeks old , weigh 16 g ) were purchased from shanghai animal center of chinese academy of sciences . each group contained 9 - 11 mice . all the experiments were carried on under 25 ± 1 ° c ., because the bleeding time was varied according to environment temperature . bleeding times of mice were measured exactly as described previously ( dejana et al ., 1982 ). low molecular weight heparin and the chemically modified heparin derivatives ( all at 0 . 12 mg / mouse ; 7 . 5 μg / gram of body weight ) were injected into each swiss mouse 15 min prior to the tail cutting ( 2 mm from the tail tip ) with a razor blade . for determination of bleeding time , the amputated tail was sunk longitudinally in phosphate buffered saline , ph 7 . 4 , at 25 ° c . complete clotting was recorded after stopping the bleeding for 30 sec . and if the bleeding time was longer than 15 min , it was counted as 15 min . fig2 shows the result : at the condition of injection of 120 ug sample per mouse , no . 1 , no . 2 , no . 4 samples have significant shorter bleeding time than lmh , little longer that the saline group . the assay and the experiment condition were according to that of example 5 . the no . 4 sample and lmh were injected into the swiss mice with the mounts of 0 . 75 mg / kg , 2 . 5 mg / kg , 7 . 5 mg / kg and 22 . 5 mg / kg respectively to test the bleeding time . fig3 shows the result , with the administration mounts of lmh increasing , the bleeding time prolongs sharply , while the no . 4 group has no apparent prolonging . therefore , we can say : no . 4 sample has non - anticoagulant activity . effect of the no . 4 sample in the rabbit ischemia and reperfusion injury model ischemia and reperfusion injury assay . new zealand albino rabbits were purchased from shanghai animal center of chinese academy of sciences . each group contains 6 rabbits . general anesthesia was induced and maintained by peritoneal injection of pentobarbital sodium ( 45 mg / kg ). after subcutaneous injections of lidocaine at the bases of rabbit ears to block the supplemental local nerves , both ears were carefully amputated at their bases in sterile conditions under a surgical microscope . only the central artery , the central vein , and a small non - vascular cartilage bridge were left intact . the ear &# 39 ; s sensory nerves were transacted to render the ears in a permanently anesthetic condition and the ears were approximated to their bases with suture . a non - traumatic microvascular clip was then placed on the central artery of each ear to stop the blood flow for complete ischemia . after 6 h , the clip was removed and the ear was allowed to spontaneous reperfusion ( mihelcic et al ., 1994 ; lee et al ., 1995 ; han et al ., 1995 ). for the therapeutic intervention , one bolus of intravenous administration of saline alone , saline with heparin or the no . 4 sample was given at the beginning time of reperfusion ( removal of the microvascular clip ). measurements of tissue edema and necrosis . ear volume ( as a reflection of tissue edema ) was measured daily for seven continuous days following removal of the microvascular clip . ear volume was quantified by determination of the volume displacement after inserting the amputated portion of the ear ( to the level of the suture line ) into a fluid - filled vessel . tissue necrosis was assessed , in a double - blind manner , by the presence or absence of tissue necrosis ( defined as & gt ; 5 % skin sloughing of the total ear surface ) on day 7 ( han et al ., 1995 ). mycloperoxidase ( mpo ) assay . mpo activities were measured as previously described ( geng et al ., 1990 ; schierwagen et al ., 1990 ; mihelcic et al ., 1994 ). the ear tissues ( no skins ) were surgically taken 24 h after reperfusion . they were weighed and placed ( 0 . 5 g / ml ) in 50 mm potassium phosphate buffer , ph 6 . 0 , supplemented with 0 . 5 % hexadecyltrimethyl - ammonium bromide ( sigma ). they were subsequently homogenized by freeze - thaw three times and sonication twice . the mixtures were then centrifuged at 10 , 000 g for 10 min . the supernatants were heated at 60 ° c . for 2 h to inactivate potential inhibitors of mpo . for generation of standard curves , fresh blood was taken from healthy rabbits and rabbit neutrophils were isolated using ficoll - paque plus ( amersham pharmacia biotech ) according to the manufacturer &# 39 ; s instructions . these isolated neutrophils were more than 95 % pure based on differential staining of leukocytes . tissue histology . tissues were taken by the 3 - mm punch biopsy from the anesthetic ears 24 h after the operation . samples were fixed by immersion in bouin &# 39 ; s fixation solution ( 75 % picric acid , 24 % formaldehyde , 1 % acetic acid ) for 24 h at 24 ° c . followed by paraffin embedding . tissue sections ( 5 - μm thick ) were subsequently dewaxed and stained with hematoxylin and eosin . they were photographed at × 280 . 17 male piglets ( 6 . 0 - 7 . 4 kg body weight , average 6 . 7 kg ) were purchased from shanghai pasturage institute , shanghai academy of agricultural sciences ( saas ). the piglets were abrosiaed for 12 hours . before the operation the piglets were intramuscularly injected with prazosin ( 0 . 02 mg / kg ) and sedated with ketamine hydrochloride ( 7 mg / kg , made by shanghai middle west pharmaceutical co . ltd ). fifteen minutes later the piglets and the scarf skin for operation and intubation were cleaned . after the vein bypass established the piglets were given intravenous injection of with 2 . 5 mg / kg propofol ( fresenius , germany ) to induce anesthesia . the piglets were put on the infrared constant temperature table ( yqt - 2 , made by shanghai ) on their back . then 0 . 15 mg / kg vecuronium bromide ( made by china xianju pharmaceutical company , ltd .) was given ( i . v .) to relax the muscle . a ballonet catheter was inserted through the mouth and it was linked to a respiration machine ( siemens , 900c ). after conventional sterilization and laying sheets the right arteriae femoralis was separated . and 24g cannulas were left for artery blood sample collection . the femoral were linked to hemodynamics equipments , which could monitor the artery blood pressure and rhythm of heart . thirty minutes later all items indicating the basic condition were detected . the piglets were divided into three groups and were operated according to the method . after the operation anesthesia were stopped and the piglets came round naturally . the trachea cannulas were withdrawn when they could breath independently , pao 2 ( partial pressure of oxygen ) was lower than 40 mmhg , sao 2 ( oxygen saturation ) was higher than 95 percent and could react to pain stimulation . then the piglets were put in incubator where the temperature was maintained 21 centigrade . the piglets were intramuscularly injected with bucinnazine hydrochloride to ease pain and were given ( i . v .) glucose - lactate cycle solution ( 10 %, 5 ml / kg / h ). twenty - four hours later the piglets were induced anesthesia by intravenous injection and intubated into trachea again . the speed of injection was adjusted to 10 - 15 ml / kg / h according to heart rate , cvp ( central venous pressure ) and sap ( systemic arterial pressure ). after sterilization an incision was made in left femoral and a 24g cannula was inoculated for blood sample collection and hemodynamics monitoring . an incision was made in left venae jugulalis extema and an 18g catheter was left for cvp monitoring and venous blood sample collection . when the condition of the piglets was stable the right - down part on the abdomen was sterilized and laid sheet again . after different operations depending on different group the piglet belong the incision was closed . the piglets were given intravenous injection of gentamicin ( 20 , 000 units ) to prevent inflammation . when ali appeared the piglets were treated according to requirements of each group . sputum was suctioned every 2 hours during the experiment . 1 mg / kg propofol and 0 . 05 mg / kg vecuronium bromide were once injected discontinuously to maintain the breath frequency at 40 - 50 times per minute and v e at 0 . 3l / min / kg . the piglets were treated with 5 % nahco 3 solution in case acidosis emerged . when sap was lower than 60 mmhg , the piglets were given ( i . v .) dopamine to maintain the blood pressure . at the end of the experiment the piglets were sacrificed with 10 ml 10 % kcl solution ( i . v .). the piglets were divided into three groups at random before the experiment . group a ( control group , n = 5 ): the piglets were made an incision at the right - lower abdomen ( 3 cm ) and the intestine were agitated before the incision was closed . twenty - four hours later the incision was opened again and the intestine was agitated again . the incision was closed after the peritoneal cavity was washed with 200 ml saline ( 37c ). the animals were observed for 12 hours . group b ( model group , n = 6 ): an incision at the right - lower abdomen ( 3 cm ) was made followed by a 2 - cm perforation in the distal cecum ( 5 cm from the end ). it was sewed and 0 . 5 cm mucosa was evaginated in order to form an ostium with a diameter of 2 cm . the incision was then closured surgically . twenty - four hours later , the incision was opened again and the ostium was sewn up . the incision was eventually closured after washing the peritoneal cavity with 200 ml saline . ( 37 ° c .). the piglets were treated with machinery gassing after ali emergence . group c ( therapy group , n = 6 ): all procedures were exactly identical to group b except that 12 mg / kg no . 4 sample was intravenously administered in early phase of acute lung injury . a . pao 2 / fio 2 & lt ; 300 mmhg ( pao 2 : partial pressure of oxygen ; fio 2 : fraction inspired oxygen concentration ) b . pulmonary dynamics compliance ( cdyn ) is lower than that in basic condition by 30 %. perfusion fixation of lung : piglets were heparinized , the thorax was opened and the left and right main bronchia were separated . the left lung was inflated with air pressure of 30 cmh 2 o . one minute later some air was let out to keep the pressure at about 10 cmh 2 o . meanwhile the right ventricle and the left atria were opened and perfused with 4 % formalin at pressure of 65 cmh 2 o for 30 minutes . the left lung was kept in 4 % formalin . three days later lung tissue was taken at 0 , 2 , 6 and 9 point respectively in order to minimize the effect of gravity on the pathological change . tissue samples were subsequently dehydrated , embedded with paraffin , sliced up and stained with hematoxylin and eosin ( he ). tissue sections were observed with optical microscope and were classified into 5 grades according to edema , bleeding , infiltration of inflammation cell , pathological change coursed by epithelium injury of small air passage : 0 grade means normal ; 1 grade means that the pathological change is light and area limited ; 2 grade means that the pathological change is middling and limited ; 3 grade that the pathological change is middling but extensive or remarkable at some part ; 4 grade means that the pathological change is remarkable and extensive . the effects of no . 4 sample on the mouse model of acute liver injury hypersensitivity on swiss mice ( 18 - 22 g body weight ) were induced by smearing 1 % ( w / v ) pcl in absolute ethanol solution on abdomen after the ventral hair razed for 5 consecutive days . after another five days , 0 . 5 % pcl olive oil solution ( sigma chemical co . st . louis , mo .) was intrahepatically injected . blood samples were collected 18 hours for the measurements of alanine aminotransferase ( alt ). mice were intraperitoneal administered twice either saline , no . 4 sample ( 10 or 20 mg / kg ) or cyclophospamide ( 10 mg / kg ) at 0 and 5 hours after pcl intrahepatically injection . table 3 shows the results : the alt level of the positive control group is markedly increased compared with that of normal group . treatment with no . 4 ( both dosages ) or cyclophosphamide markedly deduced the alt level compared with positive control . human umbilical vein endothelial cells ( huvecs ; less than three passages ) were cultured on one - well chamber slide ( nalge nunc , naperville , ill .) pre - coated with 1 % gelatin as previously described ( geng et al ., 1990 ; asa et al ., 1995 ). for cytokine stimulation , monolayers of huvecs were incubated with 300 units / ml of tumor necrosis factor - α ( tnf - α ; promega , madison , wis .) for 12 h . slides were mounted in a flow chamber as before ( ma and geng , 2000 ). human promyeloid hl - 60 cells ( ccl 240 ) were purchased from american tissue culture collection ( rockville , md .). they were cultured in rpmi 1640 medium supplemented with 10 % heat inactivated newborn bovine calf serum ( bcs ), 4 mmol / l l - glutamine , 100 units / ml penicillin and 100 μg / ml streptomycin at 37 ° c . in the presence of 5 % co 2 . after washing once with pbs , hl - 60 cells were resuspended at 0 . 5 × 10 6 / ml in pbs supplemented with 10 mmol / l hepes , ph 7 . 4 , and 2 mmol / l cacl 2 in the presence of heparin , lmwh and the sample no . 4 at 22 ° c . for 15 min . they were then precisely injected through the flow chamber at 22 ° c . using a syringe pump . the wall shear stress used was 2 . 0 dyne / cm 2 . the numbers of bound cells were quantified from videotape recordings of 10 - 20 fields of view obtained ( 3 - 4 min after flowing cells through the chamber ). effect of the no . 4 sample on preventing the transmigration of human neutrophils through the monolayers of the stimulated huvecs huvecs ( 5 × 10 4 cells / well ) were seeded in the upper chambers of 24 - well transwell ® plates ( costar , cambridge , mass .) pre - coated with 1 % gelatin . for cytokine stimulation , monolayers of huvecs were incubated with 300 units / ml of tnf - α for 12 h ( geng et al ., 1997 ). fresh human blood was obtained from healthy volunteers according to the regulations of chinese academy of sciences . human neutrophils were isolated using ficoll - paque plus ( amersham pharmacia biotech , shanghai , china ) according to the manufacturer &# 39 ; s instructions . the isolated neutrophils were more than 95 % pure based on differential staining of leukocytes . after washing the upper chambers twice , human neutrophils ( 2 . 5 × 10 6 cells / ml ; more than 95 % purity ) were resuspended in serum - free m199 medium , in the presence of heparin , lmwh and the sample no . 4 , and added to the upper chambers of the transwell plates for 1 h . the upper wells were then removed and the cells sticking on the lower surface of the filters were released by repeated pipetting . cells in the lower chambers were counted using a hemocytometer .
0
a basic idea of the invention is to sum several piece - wise linear functions to obtain the desired transfer characteristics . any function , for example , logarithmic , quadratic , etc , can be approximated in the following form : where t 0 & lt ; t 1 & lt ; t 2 & lt ; t n - 1 for n & gt ; 4 and t 0 & gt ; 0 and where u ( t − t 0 ) is a unit step function of magnitude 1 when t & gt ; t 0 and zero otherwise . for example , the transfer characteristic shown in fig3 can be expressed in following form : f ( t )= 1 ( t − 1 ) u ( t − 1 )−( t − 2 ) u ( t − 2 )+ 2 ( t − 3 ) u ( t − 3 )− 2 ( t − 4 ) u ( t − 4 ) by forming such piece - wise linear ( pwl ) functions , any kind of transfer characteristic can be approximated . it is desirable to control two parameters of each of these pwl functions : the time of the conduction corners , ( i . e ., t 0 , t 1 , t 2 , etc .) as shown in fig3 , and also the slope at each corner . in fig4 , the branch outputs indicate the components of the pwl function and bold lines indicate the total output by summing the individual branches . from the plots shown in fig4 , it can be seen that by controlling the conduction corner and slope of each branch , any kind of transfer characteristic can be implemented . more branches are needed for a system with a more complicated transfer characteristic . for a more complex transfer characteristic , for example , f ( input )= input 2 , increasing the number of branches for a specific input range and output magnitude will make the output curve more accurate . the circuit configuration of a current mirror , which forms the basic cell of the invention , is shown in fig5 . the input stage consists of an npn transistor , q 1 , and an emitter resistor ( r in ). the output stage consists of an npn transistor , q 2 , an emitter resistor ( r out ), and a current source ( i offset ) that is applied to the emitter of q 2 . the ratio of both the transistors and resistors set the amplification factor or slope , and the i offset current is used to set the conduction corner . the output of the basic cell can be connected easily to other cells because of the open configuration of the circuit . npn transistor cells as well as pnp transistor cells can be used to build a larger circuit having the desired transfer characteristic . with npn and pnp basic cells , transfer characteristics as shown in fig4 c and 4 d can be implemented with the pnp cell realizing the negative branch of the pwl function . the input of the basic cell is considered to be a current signal . the input current drives a current output of a positive or negative slope according to the cell characteristics and is generated by an input system such as a voltage - to - current converter or a transconductance system . in the basic cell , instead of npn and pnp bjts , n - type and p - type mos transistors can be used with equal effect . i in r in −( i out + i offset ) r out = v t ln [( i out / i in )( a e1 / a e2 )] ( 1 ) where : v t is the thermal voltage of the transistors ; i in , i out are the current mirror input and output currents , respectively ; a e1 , a e2 are the emitter areas of q 1 and q 2 , respectively . if mos type devices are used instead of bjts , the above equation will follow the model of the relevant mos device used . as can be seen from fig6 , the transfer characteristic is governed by a linear part and a non - linear part , given respectively by : by observing equation ( 1 ), and making certain assumptions , the formula for the conduction corner ( equation ( 3 ) above ) can be derived . equation ( 3 ) models the conduction corner as the output transistor starts to conduct , at which point the output current is small relative to the input current . assumption 1 : taking the emitter area of both the input and output transistors to be the same . hence a e1 will be equal to a e2 . assumption 2 : at the point where the output transistor starts to conduct , i out is small compared to i offset . assumption 3 : if r out i offset & gt ; r in i in , the output transistor cannot conduct , hence i in & lt ; r out i offset / r in . it is important for the circuit designer to choose appropriate characteristics of the conduction corner in order to achieve the desired accuracy of the output curve . this is a matter of choosing the values of r in and r out , taking into account the temperature effect on the output current of the v t term from equation ( 1 ). when an input current is present , the potential at the base and emitter of q 1 will increase . a voltage comparison at the base and emitter of q 2 determines whether q 2 conducts . the potential at the emitter is set by i offset r out , and this setpoint can be changed easily through the offset current . q 2 will start to conduct when i in r in is greater than i offset r out . the output current of this basic cell will be summed together with other cells to form the output current of the system . the number of branches in the pwl function , and hence the number of basic cells required , will depend on the complexity of the desired transfer characteristic . the transfer characteristic of a basic current mirror cell is shown in fig6 . bold lines indicate the theoretical pwl branch while dotted lines show the actual transfer characteristic of the basic cell . by modulating the offset current i offset , it is possible to change the transfer characteristic , thereby providing a controllable adjustment . by increasing i offset , the output branch will shift to the right . similarly by decreasing i offset , the output branch can be shifted to the left . in fig6 , the dotted line gives the actual transfer characteristic of the basic cell . the transfer characteristic of the basic cell is the same as the theoretical pwl branch except at the conduction corner . the non - linearity of the transistor effectively allows the curve to be smoothed at the conduction corner . this does not represent a problem for the system , but instead it advantageously smoothes the output . in this way , so - called w -, s -, and c - corrections can be implemented in the horizontal or vertical directions ( as appropriate ) for controlling the display on a crt screen . a block diagram of a system of an embodiment of the invention is shown in fig7 . in this system , we define the input as a voltage source , v in , and hence a transconductance circuit is needed to convert the voltage input to a current input , i in . i in then acts as the input to a circuit comprising basic pnp or npn cells , or both , depending on the transfer desired characteristic . the output is then fed into an amplitude control circuit to obtain the same magnitude at the maximum input signal for each different transfer characteristic . the necessity of the amplitude control circuit can be seen from fig6 . by adjusting i offset , the output current amplitude is altered . in the exemplary system shown in fig7 , three adjustment signals are used , namely i offset1 , i offset2 and i offset3 . by modulating i offset1 the power ( v in r , r is the power ) of the proposed invention can be changed from r 1 to r 2 where r 1 and r 2 can be any arbitrary positive real numbers . next , with i offset1 a particularly interesting aspect is that i offset2 , i offset3 can be a combination of the first i offset1 . in this way , it is possible to generate a complete transfer characteristic that is easily adjustable by way of a single or multiple current controls . as shown in fig8 , it is possible to convert a curve of the form output = a 1 input 2 to a curve of the form output = a 2 input 4 , where a 1 and a 2 are constants , by adjusting the offset currents in order to move the conduction corners , p 1 , p 2 and p 3 . this dynamic adjustability advantageously allows dynamic adjustment of the transfer characteristic . all of the above u . s . patents , u . s . patent application publications , u . s . patent applications , foreign patents , foreign patent applications and non - patent publications referred to in this specification and / or listed in the application data sheet , are incorporated herein by reference , in their entirety . from the foregoing it will be appreciated that , although specific embodiments of the invention have been described herein for purposes of illustration , various modifications may be made without deviating from the spirit and scope of the invention . accordingly , the invention is not limited except as by the appended claims .
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