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reference will now be made in detail to one or more embodiments , examples of which are illustrated in the drawings . it should be understood that features illustrated or described as part of one embodiment may be used with another embodiment to yield still a further embodiment . the improved inflatable elastomeric pump for an infusion assembly may have the general configuration as described in u . s . pat . no . 5 , 284 , 481 for “ collapsible compact infusion apparatus ” issued feb . 8 , 1994 to soika et al ., the entire contents of which are incorporated herein by reference . deficiencies of the elastomeric pump portion of infusion pumps discussed at column 1 of that reference are addressed by the improved inflatable elastomeric pump as described herein . pressure conditions measured “ upstream ” or “ downstream ” of the invention will proportionally reflect conditions within the invention and specifically will reflect expansion and contraction states of the silicone tube . upstream pressures characterize those pressures that act on the liquid as it is injected into the tube to expand the tube from an initial unexpanded state to the maximum expanded state . the maximum expanded state accommodates a fill volume . because the liquid is injected from a syringe - type device through a one - way valve connector before it enters the tube , the pressure upstream of the one - way valve is dynamically measured while injection is occurring ; hence these upstream pressures are greater than the pressures within the tube . ( the syringe device and especially the valve connector can act as upstream flow restrictors and there typically is no allowance for equilibration of pressure conditions before and after the valve connector .) these upstream pressures move the liquid through the valve connector , then through one end of the mandrel and out the first port , and then against the inside surface of tube . the measured upstream pressures ahead of the valve connector are termed crack pressures and fill pressures . the crack pressures indicate the forces that must be transmitted by the liquid to overcome the initial resistance to expansion of the inflatable tube . fill pressures indicate gradual expansion of the tube between the fixed ends attached to the mandrel ; the expansion is in a general radial direction with respect to the center axis of the tube . the fill pressures initially decrease from the maximum crack pressure and then increase to a maximum when the fill volume is achieved . typical measured upstream pressure data is shown in fig1 a and 1b for multiple injection cycles into silicone tubes ( one injection of 100 milliliters fill volume per tube ). that is , fig1 a and 1b are graphs of the measure pressure of liquid in the inflatable tube versus ( y - axis ) for an individual injection cycle in 5 individual tubes ( x - axis ) ( each cycle , ˜ 15 second in duration ). the tubes of fig1 a & amp ; b all have 0 . 355 ″ id and 3 . 05 ″ length but have different wall thickness and / or durometer hardness on mandrels of the same dimensions . as indicated on fig1 a : groups a - c represent the injection of 100 milliliters ( mls or ml ) into 5 individual tubes made from an elastomeric silicone material having a measured durometer hardness of 25 a before processing into the tubes ( i . e ., a 25 a durometer hardness material ) and with 0 . 055 , 0 . 065 , and 0 . 075 inch wall thickness respectively and group d represents similar individual injections into tubes made from an elastomeric silicone material having a measured durometer hardness of 30 a before processing into the tubes ( i . e ., a 30 a durometer hardness material ) with wall thickness of 0 . 045 inches . as indicated in fig1 b : group 1 represents the injection of 100 ml into 5 individual tubes with 0 . 065 wall thickness and a 30 a durometer hardness material ; groups 2 , 3 , and 4 represent similar individual injections into tubes of 35 a durometer hardness material and respective wall thickness of 0 . 045 , 0 . 055 and 0 . 065 inches . for each individual injection ( cycle , ˜ 15 second in duration ) a maximum crack pressure is the left - most peak and a maximum fill pressure is the right - most peak . the groups of fig1 a and fig1 b illustrate the variations observed for crack and fill pressures for silicone tubes in general ( of the invention and not of the invention ). groups a - c ( fig1 a ) and group 1 ( fig1 b ) exhibit maximum crack pressures that are less than the maximum fill pressures ; group 4 ( fig1 b ) exhibits the reverse ; groups d ( fig1 a ), groups 2 and 3 ( fig1 b ) exhibit instances for such maximum pressures being greater than , less than , or equal to one another . the information depicted in fig1 a and 1b suggests that for tubes of the same inner diameter ( id ): silicone tubes of 30 a and less durometer hardness material exhibit maximum crack pressures that are less than the maximum fill pressures for silicone tubes of a given durometer hardness , the thicker the wall the greater the maximum crack pressure with respect to the maximum fill pressure more conclusive for tubes of a given id are the following relationships among fill pressures , wall thickness , and durometer hardness : at a given wall thickness , the greater the durometer hardness the greater the fill pressures at a given durometer hardness , the thicker the walls the greater the fill pressures thus there are numerous combinations for durometer hardness and wall thickness that one can choose to achieve a specific maximum fill pressure . one method for recording fill pressures is to average the minimum and maximum fill pressures into a single average fill pressure value for a given fill cycle . fig2 illustrates such minimum and maximum data points for calculating an average fill pressure ( ave fill pressure ) for a mandrel supported silicone tube of the invention with the tube having a 0 . 10 ″ wall thickness , an id of 0 . 355 inches , and a length of 3 . 05 inches . in fig2 , the y - axis represents the pressure of liquid in the inflatable tube and the x - axis is time in seconds . the cycle is approximately 15 seconds in duration , starting at about 35 seconds and ending at about 50 seconds . table 1 gives such average values for the data represented in fig1 and for additional groups t and e (, not shown in the fig1 but with 5 individual fill cycles each ) as ; these average fill pressure values correspond to the “ unsterilized as - made ” sample type values in table 1 . also presented in table 1 is data for other samples that are the same as the unsterilized as - made but after exposure to one of two types of sterilization : “ post - gamma ” values are for samples after their sterilization by exposure to gamma radiation ; “ post - eto ” values are for samples after their sterilization by exposure to ethylene oxide . as the values of table 1 indicate , ethylene oxide sterilization has negligible effect while gamma radiation increases the crack and fill pressures by ˜ 6 to ˜ 16 %. such impact due to sterilization conditions is also observed for other silicone tubes of 30 a durometer hardness material with walls up to 0 . 180 inch thickness , and presumedly greater . fig2 shows that both the maximum crack and fill pressures are less than 35 psig ; this criteria , regardless of time duration for the fill cycle , is a desirable characteristic of the invention . while crack and fill pressures reflect the pressure conditions that act on the silicone tubes , operating pressures directly provide information about the actual pressure conditions on the tubes . the operating pressures are measured downstream of the mandrel and silicone tube invention and have no intervening blockage in the liquid flow path from the silicone tube to the pressure sensor . thus the pressure acting on the silicone tube is transmitted hydrostatically and continuously downstream of the invention . because the downstream conduits are generally designed to delivery approximate flow rates of 1 - 4 ml / hour , pressure conditions against the silicone tube equilibrate relatively quickly with pressure conditions downstream of the mandrel and silicone tube assembly . when the pressure sensor is inserted into direct communication with the liquid in the conduit ( e . g . tubing ) within 2 feet of the first port the measured pressures via the sensor are essentially those acting on the silicone tube ; thus such operating pressures are portrayals of the actual pressures on the silicone tube . silicone tubes of interest for the invention share a common characteristic “ depressurization ” profile as liquid , initially at a fill volume , is squeezed out of the silicone tube and delivered downstream over time . fig3 provides an illustrative example of the characteristic depressurization curve ; the example is representative of the dimensions of tube 1 per table 2 and of a silicone with a durometer hardness of 30 a . in fig3 , the y - axis is average operating pressure of liquid in the inflatable tube and the x - axis is volume of liquid in the tube . additional exemplary dimensions for silicone tubes of the invention are given in table 2 . each of the tubes have mandrels that support the tube in the absence of contained liquid ; the respective mandrel ( for tubes 1 , 2 , 3 , 4 ) has an od sized to match the id of the tube and a length greater than the tube . silicones with a durometer hardness ( shore hardness ) of 35 a or less are suitable for forming the tube . such silicones in the dimensions represented by tubes 1 - 4 allow for allow expansion of the tube to contain liquids up to the indicated fill volumes . appropriate selection of silicones are ones that : form inflatable tubes ; result in any maximum pressures that are greater than 12 psig but less than 35 psig when inflated with a predetermined fill volume of liquid as measured a short distance downstream of the first port ; and provide sufficent constricting forces to expel almost all the fill volume liquid . exemplary silicones are : nusil 4020 ( also called med - 4020 ) with a shore hardness of 25 a ( as reported by the manufacturer ); nusil 4025 ( also called med - 4025 ) with a shore hardness of 30 a ( as reported by the manufacturer ); nusil 4030 ( also called med - 4035 ) with a shore hardness of 35 a ( as reported by the manufacturer ). nusil 4025 is a preferred silicone . the durometer hardness of the silicone that is used to make the tubes is a material parameter of the invention . values for the durometer hardness are measured and given per the shore a scale . the exemplary silicone polymers sold under the designation nusil med - 4020 , med - 4025 and med - 4035 , as well as other polymers ( e . g ., med - 4050 , med - 4065 ) are available from nusil technology , llc of carpinteria , calif ., usa . the shore hardness testing of plastics is most commonly measured by the shore ( durometer ) test using either the shore a or shore d scale . the shore a scale is used for “ softer ” rubbers while the shore d scale is used for “ harder ” ones . the shore a hardness is the relative hardness of materials such as rubber or soft plastics and can be determined with an apparatus known as a durometer and is sometimes also referred to as durometer hardness ( or durometer hardness ). the hardness value is determined by the penetration of the durometer indenter foot into the sample . if the indenter completely penetrates the sample , a reading of 0 is obtained , and if no penetration occurs , a reading of 100 results . the reading is dimensionless . because of the resilience of rubbers and plastics , the hardness reading may change over time so the indentation time is sometimes reported along with the hardness number . the durometer hardiness values measured for the tubes presented in connection with this invention are determined per astm d2240 procedures and use a time interval of approximately 1 second between initial indentor travel cessation and the recording of the indicated reading ( as considered standard ). the analogous iso test method to this astm test number is iso 868 . the given values for the material durometer hardness values are vendor provided . it is noted that processing of the silicone into an inflatable tube and curing the tube may have an impact on the shore hardness . sterilization of the tube and inflation / deflation or mechanical working of the material for at least one cycle may also have an impact on the shore hardness . table 3 reports the shore a hardness measured for a series of inflatable tubes corresponding to inflatable tube # 3 from table 2 ( inside diameter = 0 . 6 inch , outside diameter 0 . 88 inch , wall thickness 0 . 14 inch , design volume 400 milliliters ). these tubes were made by extruding nusil 4025 ( shore hardness of 30 a as reported by the manufacturer — also referred to as shore a hardness of 30 ). three ( 3 ) separate tubes were tested . the average results and corresponding standard deviations in table 3 are for the extruded & amp ; cured tube ; tube sterilized utilizing a conventional ethylene oxide ( eo ) sterilization cycle ; and sterilized tube loaded with sterile water and allowed to deflate over a period of approximately 279 hours ( i . e ., cycled ). the results are based on six ( 6 ) measurements per tube . as can be seen from table 3 , extruding the nusil 4025 into inflatable tubes and curing the tubes with heat increases the shore a hardness from a nominal value of 30 ( as reported by the manufacturer ) for the unprocessed material to a value of about 37 for the tube . sterilization with ethylene oxide and recoverable stretching do not appear to produce a meaningful change to the shore a hardness . a structural parameter of the invention is the wall thickness , t , of the inflatable tube . an exemplary range of wall thicknesses for silicone tubes made from nusil 4025 are greater than 0 . 075 inches up to 0 . 180 inches . another structural parameter is the inner diameter , id , of the tube and exemplary ranges are 0 . 355 inches to 0 . 600 inches . another parameter is the length , l , of the tube . the tube volume ( equivalently tube vol and v tube ) is derived from these parameters according to conventionally accepted mathematical relationships . also from the t , id , l , and tube vol values are certain ratios that can characterize the invention . appropriate combinations of the structural and material parameters yield tubes of the invention that accommodate fill volumes from 50 - 600 ml of liquid . fig4 shows averaged operating pressure profiles for expanded tubes that track their depressurization of liquid expelled from the expanded tube beginning from their fill volumes with respect to time ( infusion time ) reported in hours . the tubes used in making fig4 are examples of the invention , have the structural parameters of table 2 , and are made from nusil 4025 silicone which has a material parameter of 30 a durometer hardness . table 4 identifies these examples as examples 1 - 4 and their respective connection to table 2 . table 4 also specifies the operating pressure at ˜ 0 infusion time , which is essentially the equilibrated pressure that acts against the tube wall while containing all the fill volume . additional information in table 4 provides the design flow rates that indicate the degree of downstream restrictions that are intentionally made to modulate the flow rate and specifies the number of individual samples for the examples that were used to obtain the averaged operating pressure profiles . each profile of fig4 displays the depressurization characteristics of fig3 : a maximum operating pressure at 0 infusion time , a second peak towards the completion of depressurization , and a generalized plateau between the maximum operating and second peak pressures . the pressure values for ex . 1 are similar to those for the tube of fig3 ( tube 1 ) as expected since they have structural and material parameters in common . fig4 shows pressures with respect to time while fig3 shows them with respect to expelled volume ( volume in the tube and infusion time are interrelated ). it is noteworthy that the second peaks and plateaus of each profile have similar pressure values . as shown subsequently , the differences in the maximum operating pressures can be explained via ratios that are based on certain structural parameters . fig4 also indicates that almost all of the fill volume liquid is expelled at the completion of depressurization . this is an important feature of the invention . desirably , none of the tubes of the invention retain more than just a few milliliters of liquid upon complete depressurization . for example , the tubes of the present invention retain less than about 10 mls of liquid upon complete depressurization . as another example , the tubes of the present invention retain less than about 5 mls of liquid upon complete depressurization . as yet another example , the tubes of the present invention retain less than about 4 mls of liquid upon complete depressurization . as still another example , the tubes of the present invention retain less than about 2 . 5 mls of liquid upon complete depressurization . for purposes of characterizing tubes that are not representative of the invention , it has been found that tubes made from nusil 4025 ( material durometer hardness = 30 a ) with wall thickness of 0 . 075 or less lack sufficent constricting forces in the expanded tube to expel almost all of the fill volume at the desired operating pressures . the importance of having sufficent constricting force to expel the fill volume liquid is shown in fig5 . more particularly , fig5 is a graph of operating pressure of liquid expelled from the tube ( that is measured downstream from the silicone tube and support mandrel and before flow restrictors ) for four different sample sets of silicone tubes versus infusion time ( reported in hours ). all the tubes were made from nusil 4025 ( shore hardness 30 a ) with a length of 3 . 05 inches and an id of 0 . 355 inches and were filled with a fill volume liquid of 100 ml . the top curve of fig5 represents ex . 1 , a tube with 0 . 100 ″ thick wall and indicates acceptable pressure behavior with respect to the invention ; the next highest curve represents ex . c , a tube with 0 . 075 ″ thick wall ; the following curve represents ex . b , a tube with 0 . 065 ″ thick wall ; and the lowest curve represents ex . a , a tube with 0 . 055 ″ thick wall . after 50 hours , only the tube with 0 . 100 ″ thick wall expelled all of the fill volume liquid ; the other tubes had insufficient constricting forces to overcome the downstream restrictions that dramatically slowed expulsion of the 100 ml fill volume from those tubes . fig5 also provides a comparison of the maximum operating pressures that expand the tube walls away from the mandrel when the tubes contain all 100 ml of the fill volume liquid ; these pressures are the “ y ” intercepts of the curves at 0 infusion time . ( at 0 infusion time , when none of the fill volume has been expelled , the operating pressure essentially equals the expanding pressure that provides the force to counter the constricting forces that are inherent in the tube .) these expanding pressures for 100 ml fill volume liquid are given in table 5 . to further establish the direct connection between operating pressures and pressures acting against the tubes the following ‘ static ’ experiment was conducted . the pressures at a very short distance downstream of the first port were recorded as selected mandrel - supported silicone tubes , suitable for the invention , were inflated to and deflated from fill volumes in 25 ml increments . the selected tubes are identified as ex . 11 , 21 , 31 , and 41 and are described with respect to structural parameters in table 6 . these tubes were made from nusil 4025 , thus their material parameter was a durometer hardness of 30 a . that is , the tubes were made from a material having a durometer hardness of 30 a prior to processing into the tubes . table 6 also reproduces the recorded pressures ( pressure data points ) for each ex . 11 , 21 , 31 , and 41 with respective fill volumes of 100 , 250 , 400 , and 600 milliliters as obtained via the following ‘ inflation / deflation curves ’ procedure . these pressures were graphed in fig6 with respect to volume to give an inflation curve towards each respective fill volume and a deflation curve away from the fill volume . ( the pressure data points for injecting are shown as solid markers ; those of dispensing are unfilled markers .) inflation / deflation curves procedure for ex . 11 , 21 , 31 , and 41 ( the static experiment ): 1 . obtain a new mandrel and silicone tube assembly with attached downstream conduit 2 . cut the downstream conduit approximately 5 ″ from its connection end to the mandrel and attach male luer with two connection ports , one with a valve mechanism that is closed . 3 . connect the pressure transducer to the connection port without the valve mechanism and prime the line with saline before connection . 4 . using a syringe , inject 25 ml of saline for each pressure data point through the valve mechanism when opened . 7 . measure pressure as the silicone tube is depressurized ( emptied ) dispense 25 ml at a time by opening the valve mechanism . measure pressure one minute after 25 ml is dispensed until all of the fill volume is removed . the inflation curves of fig6 share characteristics of the crack and fill pressures previously described and the deflation curves closely mirror the operating pressures for tubes of similar structural and material parameters and relatively similar fill volumes . table 7 compares maximum , second peak and general plateau pressures as shown in fig6 per table 6 with maximum , second peak , and general plateau operating pressures as given in previous tables and figures . the magnitudes of the pressures at the fill volumes of fig6 also indicate a relationship between pressure and actual wall thickness . ex . 11 with the thinnest initial wall and shortest for length , thus it has the smallest tube volume ( per table 8 , equivalent to dimensions of tube 1 per table 2 ), has a pressure at its fill volume ( 100 ml ) that is comparable to that for ex . 41 ( at 600 ml fill volume ), which has the thickest initial wall and longest length , hence the greatest tube volume ( per table 8 , equivalent to dimensions of tube 4 per table 2 ). ex . 21 and ex . 31 have lower pressures at their fill volumes . one explanation for the magnitude differences in pressures at respective fill volumes is that : ex . 11 and ex . 41 should have comparably thinner actual walls at their fill volumes compared to ex . 21 and ex . 31 and therefore exert the greater constricting forces per unit surface area at these fill volume ; ex . 21 should have the next thinner actual wall at its fill volume and thus the next greater constricting force per unit area ; ex . 31 should have an actual wall thickness at its fill volume that is greater than that of ex . 21 and therefore has less constricting force per unit surface area . in other words ex . 11 and ex . 41 are expanded ( stretched ) more towards their limit of plastic deformation ( yield point , past which the tube will not quickly return to its original dimensions before filling ). ex . 21 and 31 should be respectively thicker and thus should allow for more expansion before reaching the actual thinness of ex . 11 at its fill volume . the operating pressures of ex . 1 - 4 per table 7 show similar magnitude differences that are consistent with the offered explanation : the maximum pressure of ex . 1 ( like ex . 11 ) is comparable to ex . 4 ( like ex . 41 ) while the maximum pressures for ex . 2 ( like ex . 21 ) and ex . 3 ( like ex . 31 ) are less . the offered explanation is further supported when the shape of each tube at its fill volume is assumed to be a sphere and tube is assumed to form a shell around the sphere . given the accepted volume - to - radius relationship for a sphere , the above assumptions , and the appropriate values of table 8 , the shell thicknesses at each fill volume calculate as : 0 . 0264 ″ for ex . 11 , 0 . 0306 ″ for ex . 41 ; 0 . 0399 ″ for ex . 21 ; 0 . 0372 ″ for ex . 31 . table 7 also gives maximum pressure values ( all operating pressures ) for examples ex . a , b , and c , which are lower than ex . 1 , and thus in contradiction to the preceding explanation . this contradiction can be explained if the initial crack and fill pressures for ex . a , b , and c tubes produced stretching forces that closely approached or exceeded the limit of plastic deformation so that these tubes will not recover their initial dimensions . the lack of respective second peaks in pressure per fig5 indicates this is the case . table 7 allows comparisons of the maximum pressures at fill volumes ( fill ) for tubes that are essentially the same : values for ex . 11 to those of ex . 1 ; those of ex . 21 to those of ex . 2 ; etc . the difference in the maximum pressures at fill can be explained as stress relaxation phenomena common to elastomeric materials . the measured pressures at fill for ex . 11 - ex . 41 were all made 1 minute after the fill volume was attained . the maximum pressures for ex . 1 - 4 are the operating pressures at 0 infusion time , which implies these examples have been containing the same respective fill volumes as for ex . 11 - ex . 41 for sufficiently long enough periods of time to allow some of the molecular entanglements that are initially present when the tubes are inflated to rearrange and dissipate some of the constricting energy . indeed , should the maximum pressure for ex . 11 have been held for a time longer than that given per the procedure , it is conceivable that the maximum pressure value for ex . 11 will decay to the lower maximum pressure value for ex . 1 . in other words , the maximum pressures at fill per the inflation / deflation curves procedure should decay to the equilibrium pressures as represented by the operating pressures at ) infusion time . when ratios based on structural parameters for the tubes of table 6 are compared in light of their pressure values , these ratios point to ranges that characterize the suitability for use in the invention . table 8 lists structural parameters and various ratios based on them . of primary relevance for defining dimensions for tubes that may be suitable candidates for use in the invention are the ratios of wall thickness t to tube inner radius r or the outer radius as shown in items j ) and k ) respectively . since these ratios are expressions of the same structural parameters , item j ), the ratio of t to the inner tube radius r , will be used to identify limitations . of secondary relevance is the ratio for the fill volume to the tube volume , as shown in item l ). given that tubes of ex . 1 - 4 and ex . 11 - 41 ( all from 30 a durometer hardness material ) exhibit preferred pressure behavior up to their respective fill volumes , their ratio values per item j ) and item l ) are within the range of acceptability for the invention . since ex . c exhibits unacceptable pressure behavior at its indicated fill volume , the value of the j ) ratio lies outside the lower limit of acceptability . the value of the item j ) ratio for ex . 4 & amp ; ex . 41 is determined to be within the acceptable range per its pressure behavior up to its fill volume and sets an upper limit in light of the value for the ratio of item l ) versus those for ex . a and ex . b , which have unacceptable pressure behaviors for their fill volumes . in other words , acceptable structural parameters for tubes suitable for the invention are defined by item j ) ratios from greater than 0 . 42254 to 0 . 6 . a graphic depiction of such an acceptable range is illustrated by fig8 which is derived from fill values of fig7 that are based on table 7 data points for maximum at fill values that correspond to operating pressures at 0 infusion time . fig7 shows the same information as fig6 but includes the maximum pressures per table 7 for ex . a - c ( unacceptable for the invention ) and ex . 1 - 4 ( acceptable for the invention ). fig8 plots the maximum pressures per table 7 for ex . a - c and ex . 1 - 4 with respect to their corresponding wall thickness ; clearly a lower bound of acceptability for tubes with id values of 0 . 355 inches exists for wall thickness between 0 . 075 and 0 . 100 inches and an upper bound seemingly exists for tubes of id values of 0 . 600 inches and a wall thickness of or near 0 . 180 inches . the relationship of the pressures at the fill volumes per the inflation / deflation curves procedure to the operating pressures was demonstrated by duplicating the filling part of the procedure to the fill volume with a new ( previously unexpanded ) set of ex . 11 , 21 , 31 , and 41 tubes , which are identified as ex . 11a , 21a , 31a , and 41a , and then modifying the procedure to allow 24 hours to lapse . once the pressures were recorded approximately 1 minute after reaching their fill volume , the tubes retained these fill volumes for approximately 24 hours , then the pressures at the fill volume were recorded again and the emptying part of the procedure was subsequently followed . as the results given in table 9 show , all the after 24 hours fill volume pressures were lower than the after 1 minute fill volume pressures by 30 - 34 %. comparing table 9 to table 6 values indicates that the 24 hour delay also results in lower pressures as liquid is removed . comparison of the operating pressures of table 4 to the after 24 hour fill volume pressures of table 9 for tubes of like structural parameters leads to the conclusion that these pressures are essentially the same . a factor that may account for the slightly higher operating pressure values of the examples of table 4 compared to the after 24 hour fill volume pressures of table 9 , in addition to possible inherent variations of the individual samples themselves , was the presence of a confining non - stretchable housing as described in u . s . pat . no . 5 , 284 , 481 around the tubes for table 4 examples , while the tubes of table 9 lacked such a housing . such a confining housing was also present for all the examples and samples used for table 1 , 3 , and 5 , while the examples of table 6 , 9 , and 10 lacked a confining housing around the tubes . the inflation / deflation curves procedure was also used to see if overfilling of the reservoirs would cause insufficient constricting forces in the expanded tube to expel the final amounts of liquid . an unexpanded tube ex . 11b with structural parameters like those of ex . 1 , 11 and 11a was filled to a fill volume of 200 ml according to the inflation / deflation curves procedure used to generate the values of table 9 ( with a 24 hour delay after reaching the fill volume ). the results are given in table 10 and show that , for this tube , the structural parameters are adequate to provide sufficient constricting forces to expel all the filled liquid . comparing the “ to fill vol ” values up to 100 mls for this ex . 11b to those of ex . 11a ( table 9 ) and ex . 11 ( table 6 ) shows there is a range in measured pressures that is most likely due to sample variability ( all these tubes have the same structural parameters ): 12 . 09 psig for ex . 11b , 17 . 14 psig for ex . 11a , and 18 . 11 psig for ex . 11 . the ratio of fill volume of 200 ml / tube vol is approximately 28 . comparative examples that further support the unique criteria of the invention are found from u . s . pat . no . 7 , 704 , 230 ; such comparative examples use reservoirs made of silicone that match the material parameters of the invention , yet their structural parameters are different from those found to be acceptable for the invention . within u . s . pat . no . 7 , 704 , 230 are descriptions of certain silicone reservoirs made of nusil 4025 that are understood to have cylindrical tube shapes that “ hold about 300 milliliters ”. these reservoirs are stated to have the following dimensions : comp . ex . 1 has “ a preferred axial length of about 3 . 5 inches , a preferred outer diameter of about 0 . 130 inches and a preferred inner diameter of about 0 . 080 inches ”; comp . ex . 2 and comp . ex . 3 each “ preferably has a wall with a thickness of about 0 . 063 inches ” and is presumed to have the same axial length and either the inner or the outer diameter of comp . ex . 1 . calculations for structural parameters and ratios like those of table 8 are made for these comparative examples based on these stated dimensions ; these are listed in table 11 . an additional comparative example , comp . ex . 4 , is given with an axial length of 3 . 5 inches and an inner diameter of 0 . 080 inches but with a wall thickness of 0 . 0315 inches ( half of 0 . 063 inches ). referring again to fig6 and 7 , it appears the tubes generally follow hooke &# 39 ; s law between zero pressure and a yield point above the designed operating pressure for the infusion pump ( i . e ., 6 psi ). this hooke &# 39 ; s law behavior is observed for both the inflation profile and the deflation cycle profile . for the present invention , the more important yield point is a “ deflation yield point ” that appears at about 7 to 8 psi in the deflation portion of the inflation / deflation cycle for all sizes of the infusion pumps ( i . e ., 100 ml to 400 ml ). with reference to fig6 and 7 as well as table 6 , the plot of pressure versus volume during inflation of “ ex . 11 to fill ” illustrates that pressure of fluid in the inflatable elastomeric tube increases in a substantially linear manner from zero to an inflation yield point ( at about 13 . 4 psig ) that is above the target operating pressure ( about 6 psig ) as the volume increases from 0 milliliters to a volume of about 25 milliliters . as another example , the plot of pressure versus volume during inflation of “ ex . 41 to fill ” illustrates that pressure of fluid in the elastomeric tube increases in a substantially linear manner from zero to an inflation yield point ( at about 18 . 5 psig ) that is above the target pressure ( about 6 psig ) as the volume increases from 0 milliliters to a volume of about 25 milliliters . once the pressure exceeds the inflation yield point , the pressure - volume relationship is generally non - linear . that is , as the volume of the fluid in the inflatable elastomeric tube increases , the pressure of the fluid in the inflatable elastomeric tube has a less predictable response and will increase or decrease with changes in volume changes . this response is non - hookean ( i . e ., does not follow hooke &# 39 ; s law ) and is attributed to stretching and deformation of the inflatable tube . as can be seen from fig6 and 7 , the plot of pressure versus volume during inflation of “ ex . 11 to fill ” illustrates that pressure of fluid in the inflatable elastomeric tube increases in a generally non - linear manner from the inflation yield point ( at about 13 . 4 psig ) to the end of the inflation cycle as the volume increases from about 24 milliliters to a volume of about 100 milliliters . as another example , the plot of pressure versus volume during inflation of “ ex . 41 to fill ” illustrates that pressure of fluid in the elastomeric tube responds in a generally non - linear manner from the inflation yield point ( at about 18 . 5 psig ) to the end of the inflation cycle as the volume increases from about 15 milliliters to a volume of about 600 milliliters . during deflation of the inflatable elastomeric tube , the pressure - volume relationship is generally non - linear until the pressure decreases below a deflation yield point . for example , the plot of pressure versus volume during deflation of “ ex . 11 from fill ” illustrates that pressure of fluid in the inflatable elastomeric tube decreases in a generally non - linear manner from the end of the inflation cycle / beginning of the deflation cycle to the deflation yield point ( at about 8 psig ) as the volume decreases from about 100 milliliters to a volume of about 25 milliliters . as another example , the plot of pressure versus volume during deflation of “ ex . 41 from fill ” illustrates that pressure of fluid in the elastomeric tube responds in a generally non - linear manner from the end of the inflation cycle / beginning of the deflation cycle to the deflation yield point ( at about 7 . 8 psig ) as the volume decreases from about 600 milliliters to a volume of about 25 milliliters . referring to “ ex . 11 from fill ” and to “ ex . 41 from fill ”, as the pressure decreases below the deflation yield point , the pressure and volume decrease in a substantially linear relationship until the volume decreases to 0 ml . it is believed that providing a deflation yield point that is above the target operating pressure of the infusion pump allows for the reliable and generally complete evacuation or depletion of the contents of the infusion pump . accordingly , the improved elastomeric pump can be described as an infusion pump providing a modified hysteresis profile with a deflation yield point that is above the target operating pressure of the pump . the additional thickness (& gt ; 0 . 100 ″) and choice of material ( nusil 4025a ) in the inflatable tube provides an extended range of hooke &# 39 ; s law response which is important in providing a uniform flow rate — particularly at low volumes associated with depletion of the pump contents . normally , the silicone elastomer ( even nusil 4025a ) is non - hookean as elasticity is stress dependent which can readily be seen in the other portions of the inflation - deflation profile . while various patents have been incorporated herein by reference , to the extent there is any inconsistency between incorporated material and that of the written specification , the written specification shall control . in addition , while the disclosure has been described in detail with respect to specific embodiments thereof , it will be apparent to those skilled in the art that various alterations , modifications and other changes may be made to the disclosure without departing from the spirit and scope of the present disclosure . it is therefore intended that the claims cover all such modifications , alterations and other changes encompassed by the appended claims . | 0 |
although the subject invention is functional with a wide variety of document transferring equipment that would benefit from operating at optimized speeds based on time intervals between incoming documents , preferably , utilization of the subject invention revolves around a typical inserter apparatus that places mailable items within a mailing envelope and associated equipment such as folders , collators , and the like . referring now to fig1 for illustrative purposes there is shown a typical insertion system 5 that is utilized for controlling , generating , moving , and transferring by including selected inserts in mailed statements . generally , comprising the illustrative insertion system is a document preparation apparatus or printer 10 , document moving means or folder 15 , controlling computer 20 , and transferring means or specifically a mail inserter apparatus 25 employed the subject invention . usually , the subject invention includes means for not only accepting already existing mail items , but for generating mail items such as a simplex or duplex printer 10 . by way of example for bulk mailing situations , billing statements having one to a plurality of document pages are produced , according to prepared data , by the printer 10 , folded into a proper size 30 by the folder 15 , and inserted , via a conveyor belt system 28 , into a mailing envelope ( not shown ) by the inserter 25 , along with other envelope inserts held within various hoppers 35 . the inserter 25 not only fills the envelope with selected documents , it transfers each mail item between the folder 15 and the next processing stage ( not shown ) such as packing shipping trays and the like . although the preferred manner for operating the subject invention is to have the printer 10 coupled immediately , via the moving means or folder 15 , to the inserter 25 , the printing of the documents could be done off - line and a stack of the documents with different page counts could then be sent through the moving means or folder 15 to the inserter 25 . thus , when the term &# 34 ; generating &# 34 ; a document is employed in this disclosure , it refers to situations in which the relevant documents are either printed immediately before being handled by the folder 15 or printed separately and then handled at a later time by the folder 15 , under direction by the controller 20 which has information concerning the exact page count for each bill . in either case , a greater time is required to move a complete multiple page bill from the printer or stack to the inserter 25 than for a one page bill . one example of a commercially available printer 10 which can be interfaced ( via a moving means ) with the inserter apparatus 25 and controlling computer 20 for use with the subject invention is the delphax systems 300ie printer and post - processing system interface . as indicated above , the invention also includes a transferring means or inserter apparatus 25 which has means for mechanically interfacing to the printer 10 . the mechanical interface means that moves the items from the printer 10 to the inserter 25 preferably includes mail item moving means in the form of a transfer tray , collator , or folder 15 . the overall subject system 5 is driven by suitable data processing means , often in the form of a microprocessor , personal computer 20 , or other equivalent means , connected to the system 5 ( including printer 10 , inserter 25 , and other associated components ) by suitable and standard interfacing means for communication . computer 20 generally includes standard data input means , such as keyboard , floppy disk drives and equivalent means , and interface cables , as well as existing or future data storage means and data display means . preferably , the computer 20 is proximate to mail handling components of the subject invention or , optionally , located in a separate computer room to isolate the operator from noise associated with mail item preparation . the moving means or folder 15 and the transferring means or inserter 25 are driven by integrated system controlling means , preferably in the form of integrated system controller computer 20 . interfacing communication means , preferably in the form of network linking means such as ethernet interface and parallel interface provide data communication from the printer 10 to system controller computer 20 . interfacing communication means allows control instructions from system controller computer 20 to be directed to inserter apparatus 25 . the system control computer 20 generally includes means for monitoring the position and movement of mail items along the inserter apparatus 25 ( similar means are usually included in the printer 10 and moving means or folder 15 for monitoring the position and movement pages within the printer 10 and folder 15 ). the monitoring means is typically in the form of one or more photocell detectors or other equivalent position detecting means , which note the presence or absence of mail items at particular locations on the inserter 25 . information shared between the printer 10 and the controller 20 includes how many document pages will be present in any given billing statement packet . since the controller 20 also operates the inserter 25 , the controller 20 is in a position to maximize the efficiency of the operational speed of the inserter 25 , in relation to the size of an incoming packet . a typical transferring means or inserter 25 is a phillipsburg inserter , but other equivalent machines are acceptable for use with the subject process . the speed of the inserter is determined by noting with appropriated means the position of the inserter shaft angle . by looking &# 34 ; up - stream &# 34 ; into the oncoming flow of document packets being created by the printer 10 , the subject invention permits a synchronicity of the operational speed of the inserter 25 to match the variable speed of the incoming stream of document packets from the printer 10 which is generally the time required to receive the packets . generally , the controller 20 &# 34 ; looks &# 34 ; or processes page count and timing factors for : 1 ) the packet arriving at the inserter 25 from the printer 10 ; 2 ) the packet being generated by the printer 10 which will immediately follow item 1 ; and 3 ) the packet that is produced by the printer 10 which will immediately follow item 2 . should a preprinted stack of document pages be utilized instead of freshly printed pages , the controller 20 would adjust to process suitable page count and timing factors for the moving of the pages from the stack to the inserter 25 or generally the time required to receive the pages from the stack . the controller 20 analyzes the information , in view of a subject algorithm , described by example below , and adjusts the speed of the inserter 25 . if a &# 34 ; finer tuning &# 34 ; for the operational speed of the inserter 25 is required or desired , the subject controller 20 may look even further up - stream than only the next packet to be produced and incorporate this data into the process . specifically , fig2 shows a state diagram or machine illustrating the typical operational steps comprising a preferred embodiment of the subject invention and initiated by the controller 20 . the system controller or computer 20 is programmed with an algorithm that starts the operation of and controls the speed of the transferring means or inserter 25 in a manner that produces an inserter that runs as slowly as is reasonable for any given document packet size ( packet size reflecting the number of pages within the packet and the time required to print the packet ). the speed of the moving means or folder 15 is not normally altered by the subject system . for illustrative purposes only and not by limitation , each document packet will be a billing statement or bill . since , in actual practice , most bills are large enough ( require a significant amount of time to print ) that the inserter would run too slowly if the slowest possible inserter speed was used , most inserter motions are of a start / stop nature . that is , the inserter finishes a cycle and comes to a complete stop before the next bill arrives . for smaller bills , the subject system inserter speed control algorithm will cycle the inserter at a speed that will catch the bill while the machine is still in motion from the last bill ( controlled operation speed variations combined with adjustments as to when each insert cycle is initiated ). this requires very precise control of the machine &# 39 ; s speed and knowledge of the time between bills . because of this , the actual details of the implementation varies among different printers and / or printer speeds for any one printer . the following example incorporates the fig2 state diagram with individual steps and illustrates how the subject speed control system functions for a printer that operates at approximately 340 ms between bill pages or a maximum of approximately 3 pages per second . other time intervals are within the realm of the subject invention , including times necessary merely to move pages within a preprinted stack of documents to the inserter 25 via a moving means or folder 15 . the subject invention programming within the controller permits the operational decisions necessary for the system to operate . for this example , it will be assumed that the following sequence of bills is produced by the printer : 1 . the system is at rest , so the state diagram is at circle 100 of fig2 ( all of the &# 34 ; circle &# 34 ; references denote location in the fig2 state diagram ). in circle 100 , the system is waiting for information for the next bill concerning the number of pages it contains . 2 . as the sequence of bills example above indicates , a two page bill is coming first , followed by another two page bill , and then a five page bill . this allows time to do a start / stop motion for the first bill on the inserter 25 , so the state diagram advances to circle 200 . the inserter 25 waits for the bill to arrive . it is noted that should the second or third bill be only one page in length ( not shown in the above sequence example ), then there would not be enough time to do a start / stop motion on the inserter and the state diagram would advance to circle 500 instead of circle 200 . the procedure noted in circle 500 is a &# 34 ; catch on the fly &# 34 ; profile that accommodates that there is no time to waste with a one page bill immediately following the one that is coming . after the &# 34 ; catch on the fly &# 34 ; procedure , the state diagram advances to circle 800 discussed in detail below . 3 . the current two page bill arrives at the inserter 25 . the state diagram advances to circle 300 . 4 . select a speed for the inserter that results in an approximately 700 ms cycle time . given the approximately 340 ms timing of the proposed printer , the 700 ms results in continuous motion for a stream of two page bills . the state diagram advances to circle 700 . 5 . noting the above sequence of bills , another two page bill is coming to the inserter 25 . the state diagram advances to circle 200 . 6 . the current two page bill arrives at the inserter 25 . the state diagram advances to circle 300 . 7 . the same inserter speed as in step 4 is used again for this two page bill . the inserter 25 has not come to a complete stop , therefore , the resulting cycle time is less than approximately 700 ms . this results in making up some of the error introduced by not completing the cycle before the arrival of this bill . if there was a long stream of two page bills , the error would eventually be eliminated and the inserter 25 would stop before the next bill arrived . this technique is utilized for two and three page bills and results in a much smoother motion of the inserter 25 . for example , see the second timing graph or diagram discussed below and seen in fig3 b . the state diagram advances to circle 700 . 8 . the controller detects that a five page bill is coming . this five page bill is followed by a one page bill thus , there is no time to use a start / stop motion by the inserter 25 on the five page bill before the one page bill arrives . the state diagram advances to circle 1000 . 9 . the controller 20 records or stores the time at which the five page bill leaves the folder 15 . this time is used for adaptive speed control in step 12 below . the controller selects a speed that results in the inserter 25 running at full speed when the five page bill arrives at the inserter 25 . the full speed start times and velocities are carefully calculated to make sure that the inserter 25 will never exceed the top speed of approximately one cycle / 340 ms , for the exemplary printer 10 . because it takes the inserter 25 more than approximately 340 ms to accelerate to full speed from a complete stop , an empty slot ( in the conveyor 28 sequence ) will be created before the five page bill arrives at the inserter 25 . the state diagram advances to circle 800 . 10 . the five page bill arrives as the inserter 25 reaches full speed and is at rotational position denoted as &# 34 ; 0 &# 34 ; which is needed to catch the bill . the state diagram advances to circle 600 . 11 . the first one page bill is coming to the inserter 25 . the controller 20 detects and stores the time at which the one page bill exits the folder 15 . since the bill is only one page , no time exists to slow the inserter 25 down . the state diagram advance to circle 900 . 12 . the controller 20 fine tunes the speed of the inserter 25 to generate a suitable speed profile . this fine tuning accommodate the fact that the one page bill is not exactly 340 ms behind the five page bill ( transport , folding , and like variations introduce this difference in timing ). the times recorded for the actual exiting of bills from the folder 15 are employed in this process . the state diagram advances to circle 800 . 13 . the first one page bill arrives at the inserter 25 . the inserter 25 is at rotational position denoted as &# 34 ; 0 .&# 34 ; the state diagram advances to circle 600 . 14 . the second one page bill ( see sequence noted above ) is detected as coming . the controller 20 stores the time at which the bill exits the folder 15 . the state diagram advances to circle 900 . 15 . once again the controller 20 adjusts the speed of the inserter 25 to allow for the fact that the bills are not exactly 340 ms apart . the state diagram advances to circle 800 . 16 . the second one page bill arrives at the inserter 25 . the inserter 25 is at rotational position denoted as &# 34 ; 0 &# 34 ;. the state diagram advances to circle 600 . 17 . the controller 20 notes that a two page bill is coming next from the printer 10 . if the bill after this two page bill was greater than one page ( in fact it is one page ), the inserter 25 would be directed to slow down . but , if the inserter 25 slows down for the two page bill , it would not be able to speed back up in time for the actual one page bill that follows it in the exemplary sequence . the controller 20 records or stores the exit time from the folder 15 for the two page bill . the state diagram advances to circle 900 . 18 . the controller 20 makes the fine tuning adjustments to the speed of the inserter 25 to allow for the fact that the bills are not exactly 680 ms ( 2 × 340 ms ) apart . in this example , since the next bill is a two page bill , an empty slot will occur in the conveyor 28 of the inserter 25 . the state diagram advances to circle 800 . 19 . the two page bill arrives at the inserter 25 . the state diagram advances to circle 600 . 20 . the controller 20 notes that another one page bill is coming , but since there is no bill behind it . this still requires a full speed cycle , since this bill will arrive at the inserter 25 340 ms after the previous one . the controller 20 records or stores the time at which the bill exits the folder 15 . the state diagram advances to circle 900 . ( had there been time to do a start / stop because of the next bill being of sufficient size , the controller 20 would have recorded the time at which the bill exited the folder and the state diagram would have advanced to circle 400 . following circle 400 , the state diagram would have then proceeded to circle 300 and then circle 700 before ending at circle 100 .) 21 . once again the controller 20 adjusts the speed of the inserter 25 to allow for the fact that the bills are not exactly 340 ms apart . the state diagram advances to circle 800 . 22 . the last one page bill arrives at the inserter 25 . the inserter 25 is at rotational position denoted a &# 34 ; 0 &# 34 ;. the state diagram advances to circle 600 . 23 . no more bill messages arrive , therefore , the inserter 25 comes to a stop or rest . the state diagram advances to circle 100 . to further clarify the subject inventions , three timing diagrams are presented in fig3 a , 3b , and 3c . each diagram has inserter velocity on the vertical axis and time on the horizontal axis . fig3 a illustrates a typical timing profile utilized by the subject system for processing two sequential three page bills . the inserter has sufficient time to operate under the stop / start mode and the velocity of the inserter is selected to be as slow as practicable . fig3 b depicts a typical timing profile used by the subject system for handling two sequential two page bills ( see step 7 above ). since less time is available between bills , the inserter velocity is higher in fig3 b case than in the fig3 a situation . the second bill is caught as the inserter is in the process of accelerating . fig3 c portrays the situation in which the initial bill in a two bill sequence is of any page size and second bill is a one page bill . since the one page bill arrives only about 340 ms after the first bill , no time exists for a start / stop motion . the overall velocity for this option is the highest of the three depicted cases . the invention has now been explained with reference to specific embodiments . other embodiments will be suggested to those of ordinary skill in the appropriate art upon review of the present specification . although the foregoing invention has been described in some detail by way of illustration and example for purposes of clarity of understanding , it will be obvious that certain changes and modifications may be practiced within the scope of the appended claims . | 1 |
an embodiment of the present invention is described with reference to the figures using reference designations as shown in the figures . referring to fig1 the adaptive receiving antenna pattern is depicted in both its contour form in two angular directions φ and θ as a pattern taken through a plane containing the desired signal s and the interference source i . the main beam pattern has a peak gain level at its center . beyond this main beam region are sidelobes , not shown , whose maxima are substantially weaker than the main beam . the location of the peak gain level is commonly defined by an axis in two angular coordinates describing the pattern , or gain variation of the antenna with angular change . this axis is referred to as the boresight axis because it contains the maximum pattern gain level at a maximum receiving sensitivity . the main beam pattern is defined by a gain profile as a function of angular displacements , φ and θ . the main beam gain profile is approximated by gaussian curve for a typical circular reflector antenna , as shown , having a typical conical beam pattern with the gain of the antenna pattern in the boresight direction at a maxima normalized to unity gain . as the direction towards the desired signal source is angularly displaced from the boresight line of sight , the effective antenna gain decreases from unity gain . when interference is not present , the boresight axis bs is aligned with the desired signal s . in this way , the peak gain of the antenna is coincident with a line of sight towards the desired signal source so that maximum signal power of the desired signal is received . the alignment of the boresight axis bs with line of sight towards the desired signal source may be accomplished by several well understood methods . in some cases , knowledge of the location of desired signal source may be adequate to align the boresight axis bs with the desired signal source s . this technique is commonly referred to as open loop pointing . in other cases , where the location of the desired signal source s is not known with sufficient accuracy , antenna positioning techniques referred to as tracking are employed to align the boresight axis bs with the desired single source s . tracking techniques are closed loop pointing methods are also well understood . without interference , maximum receiving performance is achieved when the antenna boresight bs is aligned with the line of sight towards the desired signal source s and the maximum signal to noise ratio is achieved . when interference is present , the performance of the receiving system is degraded . the amount of degradation depends on the level of the interference and the spectra of both the interference and desired signal . the effects of interference are quantified by determining a desired signal to interference ratio which indicates the relative amount of power between the desired signal and interference signal . an increased desired signal to interference ratio improves the reception of the desired signal . acceptable system performance depends jointly on the desired signal to interference ratio and the desired signal to noise ratio . when repositioning the boresight to br away from the line of sight bs towards the desired single source in direction d to maximize the desired signal to interference ratio , the desired signal to noise ratio must be maintained at an acceptable level to adequately receive the desired signal . the system maintains normal antenna pointing with the boresight axis bs aligned towards the desired signal source until the presence of interference signal is detected from an interference source i . the line of sight towards the interference source i is presumed to be different than the line of sight towards the desired signal source s . when the presence of interference is detected , the antenna boresight is repositioned from its original alignment bs towards desired signal source to a new position br in a direction r away from the interference source i . at the original boresight alignment towards the desired signal source , the interference signal is received at a lower gain level than the desired signal source signal because the interference and desired signal level are not spatially collocated along the same line of sight . the desired signal to interference ratio depends on both the power densities of the incident desired signal and interference signal and the difference in the antenna gain levels for the desired signal and interference signal directions . this difference in the antenna gain levels will be referred to as the antenna rejection ar . the antenna pattern is repositioned to boresight br towards r and away from the interference i . when the antenna alignment s is changed to r at the repositioned boresight alignment br away from the interference source i , the antenna rejection ar increases to ar &# 39 ;. the amount of antenna rejection ar at the original boresight bs aligned towards the desired signal source s is less than the antenna rejection ar &# 39 ; when the repositioned boresight br is aligned r away from the interference source i . the desired signal to interference ratio is increased by repositioning the beam from s to r because the antenna rejection increases from ar to ar &# 39 ;. however , the repositioning from s to r results in a reduction in the desired signal power because the desired signal now arrives at an angle removed from the antenna boresight maxima at the highest gain value . this desired signal level reduction sl causes a reduction in the desired signal to noise ratio . a minimum desired signal to noise ratio threshold exists corresponding to acceptable system performance . in operation , the minimum desired signal to noise threshold level is typically exceeded to maintain acceptable performance during variations in link performance resulting from component variations , propagation loss variations , and other factors . the amount that the system exceeds the minimum threshold level is referred to as a signal margin . the antenna beam may be repositioned away from the desired signal source by an amount corresponding to the available signal margin . the desired signal is received when the system operates at or above the desired signal to noise ratio threshold level . the desired signal to interference signal ratio after beam repositioning from s to r has been increased over the desired signal to interference signal ratio when the antenna boresight bs was aligned towards the desired signal source s . thus , the beam repositioning from s to r increases the desired signal to interference ratio while maintaining the signal to noise ratio at or above the required desired signal to noise ratio threshold level . the beam may be repositioned so that the interference is aligned with the null that exists between the main antenna beam and the sidelobes . such a situation may be practical when the interference is located near the edge of the beam . but when the line of sight towards the interference signal is near the line of sight towards the desired signal source , the signal loss sl may be excessive . as is the case in all techniques for interference protection , limits exist on the amount of interference rejection reduction ar that can be achieved while maintaining the desired signal to noise ratio above the threshold level . the beam repositioning can be implemented in a variety of ways , and two exemplar embodiments will be described . the first embodiment is for an open loop pointing design shown in fig2 and the second is for a closed loop tracking design shown in fig3 . independent of the implementation , a means must exist to distinguish interference from the desired signal , a feature common to all adaptive designs . adaptive repositioning of the main beam for interference suppression requires an ability to detect the desired source signal s in the presence of the interfering signal i . in the exemplar embodiments , signal coding techniques are preferably used to identify the desired signals . a code is embedded in the desired signal and this code is also known to the receiving system where beam repositioning is applied . a variety of such codes exist , for example , hopping the carrier frequency in a random sequence or a pseudo - random bit stream . such techniques are commonly used in spread spectrum systems . spread spectrum systems use a modulation technique to reduce interference effects . spread spectrum modulation is used for both interference reduction and identifying the desired signal for antenna beam repositioning . the coded signal is assumed to be unknown by the interference source , and the code and its sequence is not present in the interference signal . such codes are commonly used in code division multiple access spread spectrum modulation systems . the embedded code is modulated into a user signal to create the desired signal . identification of the coded desired signal from the interfering signal enables adaptive control to reposition the main beam . open loop and closed loop control are preferred methods of repositioning the main beam . referring to fig2 an open loop receive antenna system includes an antenna 10 , preamplification 12 , and a receiver 14 which demodulates the coded desired signal . the antenna 10 may be a typical circular reflector antenna for receiving modulated source signals from a transmitter , not shown . the receiver 14 may be a conventional receiver such as a microdyne digital receiver with digital bit synchronizer , carrier tracking loop and spread spectrum demodulation . the function of the receiver 14 is to demodulate the received signal . cdma spread spectrum modulation is preferably used , though other modulation methods may be used as well . the transmitter is used to broadcast the modulated coded source signal typically over a given coverage area covering a plurality of users assigned respective codes within the cdma modulation scheme . the source signal comprises one or more superimposed desired signals modulated by respectively assigned codes . the transmitter typically continuously broadcasts the source signal at a given constant down link total power level . an embedded wideband code spreads the bandwidth of the source signal as a modulation method , and the wide band code is known to both the transmitter and receiver 14 . an embedded code determines spectrum spread modulation and identifies a respective desired signal . the antenna 10 receives various signals including the source signal s comprising many coded desired signals , one of which is the desired signal with an embedded code referred to as the pointing signal p to be received . the antenna 10 also collects the interfering signal i . the preamplifier 12 amplifies the source signal s and interfering signal i as well as establishing a noise signal n which is present in any system . the source signal s is preamplified 12 and delivered to the receiver 14 for demodulation . the preamplifier 14 is preferably a low noise preamplifier . the adaptive technique is embodied in a power detector 16 , code generator 18 , a mixer 20 , an integrator 22 , position processor 24 and positioned 26 . the receiver 14 performs frequency conversion , desired signal acquisition , and demodulation of the desired signal . in spread spectrum modulation , the source signal is a composite signal having several superimposed desired signals modulated by respective codes . a component of the source signals is the pointing signal p comprising the embedded code signal and the desired signal . the open loop antenna system detects the total input power received by the antenna 10 by the total power detector 16 , reproduces the code by the code generator 18 , cross correlates the source signal s using the mixer 20 and pointing integrator 22 for detecting the presence of the desired signal of the coded pointing signal p . the cross correlation elements 20 and 22 and the total power detector 16 are used to detect the desired pointing power pp separated from the total power tp that also include interference i and noise n components . in many systems , the total power tp is detected 16 for monitoring link quality and diagnostic purposes . the positioned 26 positions the antenna 10 in response to commands from the position processor 24 . the processor 24 receive total power signal tp from the power detector 16 where s is the source power , gs is the antenna gain in the direction of the source signal , i is the power of the interfering signal , gi is the antenna gain in the direction of the interfering signal and n is the power of noise . the mixer 20 and integrator 22 provide a cross - correlated pointing signal pp . p is the power of the pointing signal . the processor 24 analyzes the tp and pp power levels and generates angular coordinates which are communicated to a positioner 26 which repositions the antenna 10 to those angular coordinates . the positioner 26 may be a two axis gimbal positioner . when interference is not present , the position processor 24 computes the angular location of the desired signal source relative to the current position of antenna and commands the positioner 26 to point the antenna boresight in alignment towards the desired signal source . the open loop control system enables open loop positioning to determine the direction of the source signal in the absence of interference . one such open loop positioning technique is the step positioning method . step positioning alternately measures the pointing signal p at two angular step positions equally and oppositely displaced from a nominal pointing position at the source signal . when an antenna is directed towards the source signal s , both alternate measurements of the power level of the receive signal will be the same . the alternative measurements may be continuously monitored requiring continuous dithering of the antenna position during open loop positioning . when the two power level are not the same , the open loop system can compute a new nominal position and adjust the antenna to the new nominal position . the step position process is the same for both angular coordinates of a conventional two gimbal positioner 26 . the received signal including the source signal s is correlated to the code , using the mixer 20 and integrator 22 . a coded signal 18 is generated identifying the coded pointing signal p within the composite source signal s . the open loop adaptive antenna system cross correlates the received source signal from the amplifier 12 with a replica of the pointing signal p provided by the code generator 18 . the relative proportions of the source signal s and pointing signal p are predetermined . a ratio of the total power tp and the coded power signal pp can be measured and compared with the predetermined value . if the measured value differs from the predetermined value , then the presence of an interfering signal is detected . when interference initiates , its presence is indicated in the total power detector 16 . the total power detector 16 measures the sum of the signal power , the interference power , and the unavoidable noise power . for communication applications , the noise power and signal power remains at a relatively fixed level , so that when interference is initiated , its presence is clearly indicated by a level change in the power detector tp . the tp / pp power ratio of the total signal power and the pointing signal power is continuously monitored when positioning the antenna towards the desired signal source to indicate the presence or initiation of the interfering signal . the pointing signal p does not correlate to the interfering signal i so that beam positioning adjustments are made in the presence of the interfering signal . a communication system typically has a minimum bit error rate requirement . the system can be calibrated in the absence of interference and in the presence of noise to determine the minimum pp value to sustain an acceptable error rate within a given signal to noise ratio p / n . the available pointing signal margin is the difference between the measured pointing signal power pp and the pp minimum value . the antenna can be repositioned so long as there remains a signal margin , that is when pp is greater than the pp minimum value . an indication of the received signal level is provided by integrator 22 . the coded desired signal is correlated with a replica of the code 18 . the code is not correlated with the system noise or the interference signal . thus , the output of the correlator 22 responds only to the desired signal containing the code and provides a response that is proportional to the received desired signal level . the correlation level at the output of the integrator 22 can be calibrated to establish a level corresponding to the threshold signal power for acceptable system performance . the difference between actual correlation level measured at a given time and the threshold level is the signal margin . in this way , the available signal margin can be determined . when interference is detected , then the antenna positioner 26 can be commanded to reposition from its current pointing alignment in the direction of the source signal away from the source of interference . when interference has been detected , the antenna can be repositioned with the desired signal to noise ratio within an available signal margin . several open loop repositioning methods may be used to reposition the antenna in the presence of interference . one repositioning method is the angular offset method . an angular offset corresponding to the available signal margins of the received pointing signal is used to step reposition the antenna away from the desired source signal . the antenna is offset from the original boresight alignment with the desired signal source by an amount corresponding to the available signal margin . the antenna is then controlled to be rotated around the original desired signal source while maintaining the angular offset at a constant value . by monitoring the tp / pp power ratio during angular offset rotation about the source signal direction and stopping the antenna rotation when the tp / pp power ratio is at a minimum value , the antenna will be positioned at a location away from the direction of the interfering signal . when the pointing signal p is not within acceptable margin , that is , pp is less than a pp minimum value , the angular offset can be reduced by angular steps followed by respective rotations to hunt for a position in which the pointing signal can be received , that is , pp is greater than the pp minimum value yet with reduced interference . after an angular offset , the antenna is rotated about the original boresight alignment with the desired signal . the correlator output 22 measuring the received desired signal level should not vary with rotation . the correlator output pp also indicates the threshold signal level . the total power detector 16 will vary with rotation indicating a maximum value when the position is closest to the interference and the desired minimum value when farthest from the interference . at this point , the interference is minimized subject to the constraint of maintaining the threshold level of the desired signal to noise ratio . alternative methods for repositioning the antenna could be used as well , for example , a spiral repositioning method using increasing steps and angular displacements can be used for repositioning the beam away from the source of interference . referring to fig3 a closed loop antenna system includes a conventional quadrature antenna 10a having two sets of dual feeds , each having respective positive gain profiles angularly offset from a center boresight position . each orthogonal plane has two opposing feed signals . the two feed signals are communicated through a conventional a hybrid 11 providing a sum signal and a difference signal . the sum signal is the sum of the two feed gain profiles and is characterized by a large gain profile at the center position . the difference signal is the difference between the two feed gain profiles and is characterized by a null at the center position with a positive gain profile and negative gain profile angular displaced on respective sides of the center null position , as is well known . the hybrid 11 provide a sum signal , to an amplifier 12a communicating the sum signal ss and a sum noise signal ns to a sum channel power detector 16a , a sum mixer 20a and a cross correlation mixer 20c , and provides a difference signal to an amplifier 12b communicating the difference signal sd and a difference noise signal nd to a sum channel power detector 16b , a sum mixer 20b and the cross correlation mixer 20c . the sum channel power detector 16a provides for a sum channel total power signal tps . the difference power detector 16b provides for a difference channel total power signal tpd . the sum mixer 20a and sum integrator 22a provide a sum channel pointing power signal pps . the difference mixer 20b and difference integrator 22b provide a difference channel pointing power signal ppd . the cross correlation mixer 20c and cross correlation integrator 23 provide a cross correlation power signal cc . the received signal level is monitored with power detectors 16a and 16b and correlated with the coded signal indicated by the mixers 20a and 20b and the integrators 22a and 22b . the operations are performed for both the sum and difference channels . in addition , the sum and difference channels are cross correlated by the mixer 20c and the cross correlation integrator 23 . this cross correlation provides additional information to be used in determining the initiation of interference and monitoring the reduction of interference power during antenna beam repositioning . the measured signal quantities depend on the antenna gain values . ss is the power of the sum channel source signal . gss is sum channel gain in the direction of the source transmitter . is is the power of sum channel interference signal . gis is the sum channel gain in the direction of the interference . ns is the power of sum channel noise signal . sd is the power of the difference channel source signal . gsd is difference channel gain in the direction of the source transmitter . id is the power of the difference channel interference signal . gid is the difference channel gain in the direction of the interference . nd is the power of difference channel noise signal . closed loop systems for antenna pointing are preferably used in applications where the knowledge of the desired signal location lacks the accuracy required for open loop pointing and occurs when the antenna beamwidth is an appreciable fraction of the uncertainty in pointing direction . in operation , the antenna 10a provides a sum and a difference beam to perform the pointing alignment . closed loop tracking is referred to as monopulse processing . in practice , the sum beam has a maximum value on the boresight axis . the sum beam is preamplified and routed to the receiver 14 for demodulation . the difference beam contains a minima on the boresight axis . by measuring and maximizing the ratio of the sum and difference channel powers tps and tpd , the alignment of the antenna boresight with the desired signal is accomplished in the absence of interference . the closed loop system maintains alignment pointing towards the desired signal by periodically sampling the sum and difference beams . a conventional means of producing the sum and difference beams is with a multiple horn feed system in the focal region , where the horns are combined in a hybrid network 11 . in this case , the sum beam consists of the sum of the horns and the difference beam consists of the subtraction of the horns to form a null on the boresight axis . a variety of different implementations , e . g ., multiple horn feeds , multimode feed designs , etc exist to generate the sum and difference beams . the source signal s is received by the antenna 10a and sum and difference source signals ss and sd are communicated through the hybrid 11 . the sum source signal ss is preamplified 12a and routed to the receiver 14 for demodulation . the source signal s is also routed to the sum total power detector 16a providing the tps output . the sum source signal is also correlated with a replica of the code 18 to provide the sum desired signal pointing power pps level unobscured by either system noise or interference . the correlated output pps for the sum channel 22a can be calibrated to establish a threshold level for acceptable system operation and the measured output at any given time can be used to determine the available signal margin . the difference source signal sd is amplified by preamplifier 12b and communicated to the difference power detector 16b providing the difference total power signal tpd . the difference source signal ssd is correlated with a replica of the code 18 to provide the difference desired pointing power signal ppd . when interference is absent , the position processor 24 monitors tps , pps , tpd and ppd to determine whether the antenna boresight is aligned with the desired signal source and the amount to reposition the antenna using the positioner 26 to align the antenna towards the desired signal source . the ratio of the sum and difference channel pointing integrators 22a and 22b determine the displacement of the antenna boresight from the desired signal and the sign of this ratio describes the direction of the displacement . specifically , the ratio of 22a to 22b relates to the angular displacement and directions of the main beam in both planes to track source signal transmitter . typically , this ratio pps / ppd is monitored and minimized to track the desired signal . when the total power ratio is above a predetermined tracking value , the antenna is considered to be tracking the source signal . during tracking , the main beam is positioned in the direction of the source and pps is at a maximum value when gss is at a maximum , and ppd is at a minimum value when gsd is at the null value . when the total power ratio is above the predetermined tracking value , the magnitude and sign of the total power ratio is used to reposition the antenna to track the signal source . the sign of the ratio varies between opposite sides of the main beam axis to determine which direction to reposition the antenna . the ratio ppd / pps indicates the direction of the reposition due to the positive and negative gain profiles on respective sides of the null center position of the difference channel . thus , tracking of the source can be accomplished without dithering of the main beam . when the ratio is above the tracking value , a threshold level , realignment to the source is necessary . the magnitudes of pps / ppd ratio can be initially calibrated to angular displacements in a look - up table as a tracking map , such that , the processor 24 may use the tracking map table to store calibration data to cross reference the total power ratio to the angular displacements , for realignment in both orthogonal planes . the processor 24 adds the angular displacements respectively to the current angular position to generate the new tracking coordinates for both planes . the correlation used to obtain pps 22a , and ppd 22b results in antenna tracking that is insensitive to interference interference is indicated by the total power detectors 16a and 16b and also by the cross correlation integrator 23 . each of these detectors 16a and 16b have different sensitivity characteristics , and one or both may be used to detect the presence of interference . the two total power detectors 16a and 16b contain an interference component is and id , respectively , and thereby provide an indication of the presence of interference . the cross correlation integrator output 23 also provides an indication of interference . the correlation process removes the noise components because the sum and difference channel noise components are uncorrelated . like the power detector 16a and 16b , the source power s has a relatively constant power when the beam is aligned to the source . when interference is initiated , the tps , tpd and cc output indicate the presence of interference . the selection of the interference indicators , tps , tpd or cc and use depends on the system applications and specifics . some system may have desired signal level variations that can be misinterpreted as interference , e . g ., ehf systems operating above 30 ghz experience propagation losses that vary with rainfall rates . in this case , the cc output of the cross correlation integrator 23 divided by the product of the sum 22a and difference 22b pointing integrators , pps × ppd , yields an output that is independent of the desired signal level so that interference initiation is clearly indicated by changes in the cc output . in still other applications where spread spectrum modulation techniques are used to provide additional interference protection , the desired signal component in the receive bandwidth may have a smaller value than the noise level , and in these applications , additional signal processing referred to as despreading is used to achieve a usable , processed signal to noise ratio . in this spread spectrum application , antenna repositioning may not be desirable for lower level interference that is adequately protected by spread spectrum modulation . in spread spectrum applications , interference that is sufficiently strong to require the additional protection afforded by antenna beam repositioning is indicated when the interference level exceeds the noise level in the rf bandwidth as indicated by the total power detector 16a . various interference detection methods provide various tradeoffs for specific applications . the cross correlation power signal cc is preferably used to determine the presence of interference . the cross correlation power signal between the sum and difference signal provide increased sensitivity to the presence of interference than the total power signal tps or tpd . in spread spectrum modulation applications , the source power is often lower than the noise power in the input bandwidth . the mixer 20c and integrator 23 provide cross correlation of coherent signals . the sum source signal ss and difference source sd are coherent and cross correlate , and the sum interference signal is and difference interference signal id are also coherent and also cross correlate , but the sum noise signal ns and the difference noise signal nd are not coherent and therefore do not cross correlate , so that , the cross correlation output is dependent on the ss , sd , is , id , but not ns and nd . the total power signals tips and tpd have noise components , whereas the cross correlation power signal cc has no noise signal component , so the cross correlation power signal is preferably used to determine the presence of interference in noisy systems . when tracking the source signal with the main beam directed towards the source , the gsd gain value is at the null value , such that , the source signal component of cc value is zero thereby providing a sensitive indication of the presence of interference . in the presence of interference , cross - correlation is dominated by interference because the antenna is pointed at the null of the difference pattern , so that , gsd is a zero , and the sssd term is zero . the cross - correlation value may be calibrated to an interference threshold value cci , such that , when the cross - correlation power signal cc is greater than the cross - correlation interference threshold , that is cc & gt ; cci , interference is considered significant , such that , modulation protection may not be sufficient thereby requiring adaptive antenna repositioning . typically , the source signal power transmission level does not vary over the life of the source transmitter . in the case where the receive source signal may vary , such as during rain conditions within an ehf link , where the link is dependent upon dynamic environmental changes , the cross - correlation power signal cc may vary , which may falsely indicate the present of interference , and render cc calibration ineffective . an environmentally insensitive cross correlation ratio can be used to indicate interference . the cross correlation ratio is equal to the square of cross - correlation power signal cc divided by the product of the pointing power signal pps and ppd . this quotient is insensitive to link performance and source signal variation , because the source signal and the coded component p wary equally . when interference is absent , the cross - correlation ratio is equal to a fixed value and is insensitive to link performance . this cross - correlation ratio value can be calibrated to a predetermined cross - correlation ratio threshold value and used to indicate the initiation of significant interference . when interference initiates , a variety of methods may be employed to reposition the beam away from the interference . an angular step method may be used with the added benefit of monitoring the interference reduction from the power detectors 16a and 16b and cross correlation output cc . a map estimation method estimates the interference location from the sum and difference power levels of the detectors 16a and 16b . the desired pointing signals pps and ppd are known in both channels , and the sum and difference total power ratio tps / tpd for the interference components is and id can be determined . knowing the sum and difference variations of the antenna pattern through calibration , the measured total power ratio can be compared with stored values in the processor 24 to estimate the interference direction . knowing the interference direction , the antenna can be repositioned away from the interference to the extent provided by the signal margin indicated by the sum channel correlation 22a compared to a calibrated signal threshold level that defines the signal margin . another antenna map method moves the antenna beam to minimize the interference component in the cross correlation output cc of integrator 23 . the variation in the signal power component pps or ppd in the output of the integrators 22a and 22b at a given time can be measured and compared to angular variation of the antenna pattern known from calibration . an antenna map can be constructed using known antenna sum and difference patterns so that the signal component variation of pps and ppd with beam repositioning can be determined and subtracted from the cross correlation integrator 23 to isolate the variation in the interference component . variations of the interference components is and id over beam repositioning determine the direction towards the interference . the interference term in the cross correlation integrator 23 depends on the difference pattern gain level which is minimized when the antenna boresight is aligned with the interference . knowing the interference location and the available signal margin from 22a , the position processor 24 can command the antenna to reposition itself away from the interference while maintaining an acceptable signal level which can be validated by comparing the sum channel integrator output 22a with a threshold level for acceptable signal reception . these examples illustrate alternative means for using the measured information in the processor 24 to achieve the goal of repositioning the antenna to maintain the minimum acceptable signal level while maximizing the desired signal to interference ratio . the preferred close loop embodiment detects interference initiation by three distinct indications , the power detectors 16a and 16b and the cross correlation cc of integrator 23 . the desired signal is measured by the sum and difference correlations 22a and 22b . the desired signal level relative to threshold value for acceptable operation can be determined by calibration . the present invention employs beam alignment rather than altering the beam pattern and can be applied to many antenna systems . multiplicity of antenna elements , adaptive weighing circuitry and combiners , and adaptive equalization is not required . this invention reduces main beam interference , and thus complements existing sidelobe cancelers that do not cancel main beam interference . a significant advantage of this system is that unlike conventional adaptive antenna designs , adaptive equalization is not required to reduce interference for wide bandwidth signal reception . the exemplar embodiments may be modified and enhanced . those modification or enhancement may fall within the spirit and scope of the following claims . | 7 |
before describing the present invention in detail , it is to be understood that this invention is not limited to particularly exemplified formulas or ingredients as such may , of course , vary . it is also to be understood that the terminology used herein is for the purpose of describing particular embodiments of the invention only , and is not intended to limit the scope of the invention in any manner . all publications , patents and patent applications cited herein , whether supra or infra , are hereby incorporated by reference in their entirety to the same extent as if each individual publication , patent or patent application was specifically and individually indicated to be incorporated by reference . it must be noted that , as used in this specification and the appended claims , the singular forms “ a ,” “ an ” and “ the ” include plural referents unless the content clearly dictates otherwise . thus , for example , reference to a “ indicating agent ” includes two or more such agents . 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 the invention pertains . although a number of methods and materials similar or equivalent to those described herein can be used in the practice of the present invention , the preferred materials and methods are described herein . sugar nectar compositions can include any mixture of liquid saccharides commonly ingested by wild , domestic , or agricultural birds . those practiced in the art recognize that this generally means solutions containing sucrose , but can also contain other sugars such as fructose , glucose , simple sugars , complex sugars , or other ingredients such as dextrin , starch , salts , minerals and mixtures thereof . many birders prepare their own sugar nectars by combining water and granulated sucrose . these are commonly prepared in a water : sucrose ratio of 4 : 1 by volume , but can range from ratios of 5 : 1 to 2 : 1 . sugar nectars are available commercially pre - made , and often contain dyes , and artificial preservatives . sugar nectars are also commercially sold as liquid concentrates ranging from 50 % sucrose to 70 % sucrose , and powdered concentrates that are nearly 100 % sucrose . pre - made commercial nectars comprised of a sugar and water mixture that can range from a sucrose content of 15 % to 25 % sugar by weight . generally the sugar is in the form of sucrose , commonly cane sugar sucrose , but can also contain other sugars such as fructose or glucose . a nectar feeder is a device designed to dispense or display liquid food for the purpose of giving access of the food to birds . examples of which are inverted feeders and saucer feeders . an inverted feeder has a central reservoir that is suspended over the feeding ports and releases nectar from above . the effects of vacuum keep the nectar from flowing freely out the ports , keeping the ports filled at optimum levels . inverted feeders can be top filling or bottom filling style . a saucer feeder is a simple dish filled with nectar that has ports above the reservoir , allowing birds to dip their bills into the nectar supply . a nectar feeder can be as simple as an inverted glass bottle with a tube at the bottom , or as complicated as a multiple feeding - port feeder with insect - resistant barriers . they all have in common a reservoir to hold the nectar , and feeding ports which restrict the free flow of the nectar out of the feeder while providing nectar access to the hummingbirds . the spoilage reducing compositions of the present invention comprise : ( a ) an effective amount of a transition metal salt ; ( b ) optionally , an acidifying agent ; © optionally , a functional additive ; and ( d ) optional adjuncts . the spoilage reducing compositions may also be in shaped form , such as a geometric shape , which may be placed into the feeder . the spoilage reducing composition can occur with the sugar nectar , or can occur in packets or containers , as a powder or liquid concentrate . it can also occur premixed with sugar nectar . an effective amount of the spoilage reducing composition is that amount of material , or greater , that is needed to have any noticeable effect on the reduction of microbial growth in a nectar feeder . testing shows that 2 ppm weight percent or less of the spoilage reducing composition can have significant effects on the reduction of spoilage , and it is anticipated that the minimum effective level is much less than that amount . the spoilage reducing composition can also be used as an antimicrobial solution for treating the exterior or interior of any type of wild bird feeder . in the spoilage reducing compositions of the present invention , the transition metal salt serves in the capacity to hinder the growth of microbes , thus prolonging sugar nectar freshness and reducing sugar nectar spoilage in wild bird nectar feeders . many of the transition metal salts react with water to create oxygen , thought to be effective in inhibiting the growth of microbes . the spoilage reducing composition should result in a level of transition metal salt in the feeder , that is below the level that would harm nectar feeding birds , and preferably be in the micronutrient range . transition metal salts are compounds comprised of a metal cation from the d - block elements of the periodic table and an anion . transition metal cations include copper , zinc , manganese , iron , and silver . transition metal cations can be in several different valance states . the transition metal salt could be selected from the group consisting of a copper salt , a zinc salt , an iron salt , a nickel salt , a cobalt salt , a molybdenum salt , a chromium salt , a manganese salt , a silver salt and mixtures thereof . the transition metal salt can contain copper cations such as in copper sulfate . the transition metal salt can be copper salt in any one of several valance states such as a copper ( ii ) salt , a copper ( i ) salt and mixtures thereof . the transition metal salt can contain any anion combined with copper , such as copper chloride , copper nitrate , copper citrate , copper acetate , copper carbonate , copper sulfate , copper hydroxide , copper sulfide , copper oxide , copper phosphate , copper borate , copper gluconate and mixtures thereof . the transition metal salt can be a mineral ore of copper , such as azurite , malachite , bornite , cuprite , chalcopyrite , chalcocite , chrysocolla , and mixtures thereof . the transition metal salt can contain zinc cations such as in zinc gluconate . the transition metal salt can contain any anion combined with zinc , such as zinc chloride , zinc nitrate , zinc citrate , zinc acetate , zinc carbonate , zinc sulfate , zinc hydroxide , zinc sulfide , zinc oxide , zinc phosphate , zinc borate , zinc gluconate , and mixtures thereof . the transition metal salt can be a mineral ore of zinc , such smithsonite , sphalerite , wurtzite , hydrozincite , and mixtures thereof . the transition metal salt can contain silver metal cations such as in silver nitrate . the transition metal of the transition metal salt can be in any one of several valance states . the transition metal of the transition metal salt can be a nanomaterial comprised of a transition metal salt , or combination of transition metal salts . the transition metal of the transition metal salt can be a transition metal or nanosized transition metal that creates a salt when added to the sugar nectar . the transition metal salt can contain any anion combined with the transition metal cation such as a metal chloride , metal nitrate , metal citrate , metal acetate , metal carbonate , metal sulfate , metal hydroxide , metal sulfide , metal oxide , metal phosphate , metal borate , metal gluconate and mixtures thereof . the transition metal salt can be a mineral ore of a transition metal , such as a mineral metal carbonate , mineral metal sulfate , mineral metal hydroxide , mineral metal sulfide , mineral metal oxide , mineral metal silicate , mineral metal borate , mineral metal phosphate , mineral metal chloride , and mixtures thereof . an acidifying agent is any compound that increases the ph of the sugar nectar . acidifying agents include citric acid , lactic acid , fumaric acid , ascorbic acid , carbonic acid , phosphoric acid , acetic acid , boric acid , hydrochloric acid , sulfuric acid , oxalic acid , and tartaric acid . acidifying agents can be included in solid or liquid in form . the acidifying agent serves to keep the transition metal cation in a more chemically free state , available for reaction . the acidifying agent may also play a role in enhancing the ability of the transition metal cation to produce free oxygen , an important component for antimicrobial action . functional materials that may further be combined with the present inventive compositions include coloring agents , anti - caking agents and binding agents . additional functional materials include , but are not limited to vitamins , anti - microbial agents , anti - molding agents , odor absorbers , spoilage indicators , flavorants , and fragrance . the functional materials may be present in any desirable weight percent with respect to the spoilage reducing composition . in general , the functional materials are generally employed at an effective level , such level being sufficient with respect to the spoilage reducing composition , to adequately perform their function . a coloring agent may also be added to enhance the aesthetic nature of the spoilage reducing composition . however , a coloring agent is not necessary , and many hummingbird experts advise against it . coloring agents include , but are not limited to dyes , pigments , and polymeric colorants . non - limited examples of dyes include acid blue 9 dye , methylene blue , and wool violet . examples of pigment are hematite , cu - phthalocyanine or ultramarine blue . examples of polymeric colorants are various products under the liquitint ™ name produced by milliken chemical . suitable impermeable packaging means include , for example , but are not limited to containers of glass , plastic , waxed paper , and other materials known in the art for storing and dispensing liquid products . other suitable impermeable packaging means include but are not limited to containers or film composed of glass , polyvinylchloride ( pvc ), cellulose , cellophane , thermoplastics , silicones , polyethylene , or polypropylene . for prototype testing , an inoculation medium , designated as shf - 1 was prepared by mixing the contents of several spoiled hummingbird feeders , to represent a variety of microorganisms including the black mold typical of spoiled hummingbird feeders . the term of “ spoilage ” as used herein means the visible appearance of microbial growth , determined by observing the nectar for turbidity , and black or white spots . the copper content of the base sugar nectar was & lt ; 0 . 05 ppm . a stock solution of sugar nectar was prepared by mixing sucrose and water in a 1 : 4 ratio , and stirred until completely dissolved . the water used was room temperature tap water to replicate a typical consumer preparation . 100 ml of sugar nectar was placed in transparent cups and inoculated with 5 drops of shf - 1 . varying amounts of copper sulfate 0 . 1 % solution were added to the tubes to achieve trace concentrations ranging from 0 ppm to 50 ppm . the compositions were left at 70 degrees for four weeks . a stock solution of sugar nectar was prepared by mixing sucrose and tap water in a 1 : 4 ratio , and stirred until completely dissolved . 100 ml of sugar nectar was placed in transparent plastic tubes , and inoculated with 5 drops of shf - 1 . varying amounts of copper sulfate 0 . 1 % solution were added to the tubes to achieve trace concentrations ranging from 0 ppm to 4 ppm , and the tubes were mixed and capped . the tubes were left outside for four weeks at ambient ( seasonal range was 50 - 90 deg f .). a stock solution of sugar nectar was prepared by mixing sucrose and tap water in a 1 : 4 ratio , and stirred until completely dissolved . sugar nectar was placed in small hummingbird feeders and inoculated with 5 drops of shf - 1 . varying amounts of copper sulfate 0 . 1 % solution were added to the tubes to achieve trace concentrations ranging from 6 ppm to 10 ppm . the feeders tubes were left outside , used by hummingbirds and exposed to seasonal temperatures ranging from 60 to 100 deg f . since the natural foods consumed by hummingbirds are at 20 ppm copper or more , it is clear from these examples that transition metals such as copper are effective at naturally inhibiting microbial growth even at trace micronutrient levels . | 0 |
fig1 shows an example of a lead - acid battery in which the plenum stabilization material in accordance with the present invention has been employed successfilly . the battery includes a case 1 having side walls 2a and 2b , a bottom wall 3 and a lid 4 . positive electrode plates 5 and negative electrode plates 6 , as well as separators 7 , are stacked in case 1 in a known manner to form two cells of the battery . some of the electrode plates are monopolar while others are bipolar , as indicated by the intercell weft wires 8 . such plates are described in u . s . pat . no . 4 , 964 , 878 , the entirety of which is incorporated herein by reference . each cell provides two volts so that the aggregate total output of the battery is four volts . additional plates could be stacked or more cells could be added to increase the aggregate output of the battery . terminal connections 9a and 9b are secured to alternate monopolar plates and exit case 1 for connection to a load . a pressure release valve 10 is formed through the upper portion of side wall 2b to allow excess gas to escape from case 1 . drain holes 11 ( which are sealed ) are formed in the opposed side wall 2a , and are used during manufacture of the battery , as explained below . the battery in fig1 is manufactured by stacking the monopolar electrode plates , bipolar electrode plates and separators , and securing the stacks using compression cages , such as those described in u . s . pat . no . 5 , 409 , 787 , the entirety of which is incorporated herein by reference . the stacked assemblies are then positioned within case 1 on support pins 12 . the terminal connections 9a and 9b are arranged and attached and then lid 4 is welded onto the top of case 1 . fig1 shows that lid 4 also includes support pins 12 , and the compression cages are designed to engage pins 12 ( top and bottom ) to maintain the spatial relationship between the edges of the plate stacks and the interior side walls of case 1 . the case is then turned on its side so that side wall 2a is arranged as the bottom of the case , and the entire case is placed in a vacuum chamber . with the entirety of the battery under vacuum , acid is introduced , through the hole that will receive valve 10 , into the interior of case 1 and absorbed by separators 7 . excess acid is allowed to drain under the influence of gravity through drain holes 11 . after the separators have absorbed the appropriate amount of acid , the battery is removed from the vacuum chamber and maintained upright temporarily to allow any remaining free acid within case 1 to drain through holes 11 . holes 11 are then sealed , vent 13 is attached to the fill hole , and the battery is charged to form the active battery plates . fig2 shows a battery that is substantially identical to the battery shown in fig1 except that a plenum stabilization material 20 fills the spaces in and around the internal battery components . the battery of fig2 is formed in the same manner as that of fig1 except that , after drain holes 11 have been sealed , plenum stabilization material 20 is heated to a liquid , flowable state , and then introduced into the battery case 1 through the same fill hole used to introduce the acid . an additional vent hole 21 is formed in side wall 2b of case 1 to allow air within the battery case to escape as the plenum stabilization material fills the space within case 1 . the plenum stabilization material is added to the case until full , and then valve 10 is attached as in fig1 and vent hole 21 is sealed in the same manner as drain holes 11 . the plenum stabilization material solidifies in situ upon cooling . the plenum stabilization material 20 can be any material capable of being introduced into the battery case 1 in liquid , flowable form , and then solidified , usually through cooling , in situ to provide a structural matrix that maintains the relative positions of the components and prevents short circuit conditions between the electrode plates due to mossing or other conditions ( e . g ., the pooling of free acid ). the ability of the plenum stabilization material to change state reversibly from solid to liquid is important from a manufacturing standpoint , in that it must be in flowable , liquid form to facilitate its introduction into the spaces and voids formed among the components within the battery case . the ability of the plenum stabilization material to change state reversibly from solid to liquid is more important , however , from a use standpoint . once in the battery case , the material solidifies to provide mechanical support for the internal components during battery use , and thus , enhance the vibration resistance of the battery . the material becomes liquid under conditions of severe overcharging of the battery during recharging cycles . this enhances the ability of the plenum stabilization material to act as a conductive heat transfer medium to conduct heat away from areas of short circuits among the battery plates and terminal connections . while the plenum stabilization material can be any substance capable of reversible changes in state between solid and liquid , it preferably is a compound containing long - chained hydrocarbon molecules , more preferably a wax , and most preferably a high melting point petroleum wax . one example of such a petroleum wax is a microcrystalline wax known as shellmax 400 , manufactured by shell oil company . the plenum stabilization material can also be a thermoplastic , so long as it can undergo reversible changes in state from solid to liquid . fig3 and 4 show side and top views of the battery of fig2 in an overcharging situation . the excess gas formed at electrode plates 5 and 6 escapes from the proximity of the plates due to crack formation in plenum stabilization material 20 , and causes case 1 to separate from plenum stabilization material 20 under a ballooning effect ( shown in an exaggerated fashion in fig3 and 4 ). the plenum stabilization material preferably should also be incapable of bonding permanently to the material of the battery case ( e . g ., polypropylene ), so as to allow this separation to occur during overcharging conditions . separation of case 1 from plenum stabilization material 20 forms a common plenum 30 in which the gas evolved from electrodes 5 and 6 collects and communicates with valve 10 . this common plenum design allows for the use of a single valve 10 to service all cells within the battery case , which in turn simplifies the overall battery design and reduces manufacturing cost . the use of plenum stabilization material in accordance with the present invention substantially increases the recharging cycle life and improves the short circuit withstandability of batteries . as tested in lead - acid batteries , for example , the use of plenum stabilization material in accordance with the present invention in a battery of the type depicted in fig1 increased the recharge cycle life of the battery from about 300 cycles to in excess of 700 cycles . additionally , when exposed to an intentional internal short circuiting situation , a battery of the type shown in fig1 failed catastrophically after only 15 minutes , whereas the same battery with the present plenum stabilization material employed therein did not fail even after 4 hours . while the present invention has been particularly shown and described with reference to the preferred mode as illustrated in the drawings , it will be understood by one skilled in the art that various changes in detail may be effected therein without departing from the spirit and scope of the invention as defined by the claims . for example , although the above description is in the context of lead - acid batteries , it is believed that the present invention could be employed in other types of batteries as well . additionally , while the plenum stabilization material is shown as contacting the electrode plates directly , it is possible to position each cell within a plastic bag to further isolate it electrically from other cells in the battery . | 7 |
unless otherwise stated , the following terms used in the specification and claims have the meanings described below . “ alkyl ” refers to a saturated aliphatic hydrocarbon group including c1 - c20 straight chain and branched chain groups . preferably an alkyl group is an alkyl having 1 to 12 carbon atoms . representative examples include , but are not limited to methyl , ethyl , n - propyl , isopropyl , n - butyl , isobutyl , tert - butyl , sec - butyl , n - pentyl , 1 , 1 - dimethyl propyl , 1 , 2 - dimethyl propyl , 2 , 2 - dimethyl propyl , 1 - ethyl propyl , 2 - methylbutyl , 3 - methylbutyl , n - hexyl , 1 - ethyl - 2 - methylpropyl , 1 , 1 , 2 - trimethylpropyl , 1 , 1 - dimethylbutyl , 1 , 2 - dimethylbutyl , 2 , 2 - dimethylbutyl , 1 , 3 - dimethylbutyl , 2 - ethylbutyl , 2 - methylpentyl , 3 - methylpentyl , 4 - methylpentyl , 2 , 3 - dimethylbutyl , n - heptyl , 2 - methylhexyl , 3 - methylhexyl , 4 - methylhexyl , 5 - methylhexyl , 2 , 3 - dimethylpentyl , 2 , 4 - dimethylpentyl , 2 , 2 - dimethylpentyl , 3 , 3 - dimethylpentyl , 2 - ethylpentyl , 3 - ethylpentyl , n - octyl , 2 , 3 - dimethylhexyl , 2 , 4 - dimethylhexyl , 2 , 5 - dimethylhexyl , 2 , 2 - dimethylhexyl , 3 , 3 - dimethylhexyl , 4 , 4 - dimethylhexyl , 2 - ethylhexyl , 3 - ethylhexyl , 4 - ethylhexyl , 2 - methyl - 2 - ethylpentyl , 2 - methyl - 3 - ethylpentyl , n - nonyl , 2 - methyl - 2 - ethylhexyl , 2 - methyl - 3 - ethylhexyl , 2 , 2 - diethylpentyl , n - decyl , 3 , 3 - diethylhexyl , 2 , 2 - diethylhexyl , and the isomers of branched chain thereof . more preferably an alkyl group is a lower alkyl having 1 to 6 carbon atoms . representative examples include , but are not limited to methyl , ethyl , n - propyl , isopropyl , n - butyl , isobutyl , tert - butyl , sec - butyl , n - pentyl , 1 , 1 - dimethylpropyl , 1 , 2 - dimethylpropyl , 2 , 2 - dimethylpropyl , 1 - ethylpropyl , 2 - methylbutyl , 3 - methylbutyl , n - hexyl , 1 - ethyl - 2 - methylpropyl , 1 , 1 , 2 - trimethylpropyl , 1 , 1 - dimethylbutyl , 1 , 2 - dimethylbutyl , 2 , 2 - dimethylbutyl , 1 , 3 - dimethylbutyl , 2 - ethylbutyl , 2 - methylpentyl , 3 - methylpentyl , 4 - methylpentyl , 2 , 3 - dimethylbutyl etc . the alkyl group may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkyxoyl , alkylsulfo , alkylamino , halogen , thiol , hydroxyl , nitro , cyanide , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ cycloalkyl ” refers to a saturated and / or partially unsaturated monocyclic or polycyclic hydrocarbon group and has 3 to 20 carbon atoms . preferably a cycloalkyl group is a cycloalkyl having 3 to 12 carbon atoms . more preferably a cycloalkyl group is a cycloalkyl having 3 to 10 carbon atoms . representative examples of monocyclic cycloalkyl groups include , but are not limited to cyclopropyl , cyclobutyl , cyclopentyl , cyclopentenyl , cyclohexyl , cyclohexenyl , cyclohexadienyl , cycloheptyl , cycloheptatrienyl , cyclooctyl etc . polycyclic cycloalkyl groups include the cycloalkyl having spiro ring , fused ring and bridged ring . “ spiro cycloalkyl ” refers to a 5 to 20 membered polycyclic hydrocarbon group with rings connected through one common carbon atom ( called a spiro atom ), wherein one or more rings may contain one or more double bonds , but none of the rings has a completely conjugated pi - electron system . preferably a spiro cycloalkyl is 6 to 14 membered , and more preferably is 7 to 10 membered . according to the number of the common spiro atoms between spiro rings , spiro cycloalkyl is divided into monocyclic spiro ring , bicyclic spiro ring or multicyclic spiro ring , and preferably refers to monocyclic spiro ring or bicyclic spiro ring . more preferably spiro cycloalkyl is 4 - membered / 4 - membered , 4 - membered / 5 - membered , 4 - membered / 6 - membered , 5 - membered / 5 - membered , or 5 - membered / 6 - membered monocyclic spiro ring . representative examples of spiro cycloalkyl include , but are not limited to the following groups : “ fused cycloalkyl ” refers to a 5 to 20 membered polycyclic hydrocarbon group , wherein each ring in the system shares an adjacent pair of carbon atoms with other ring , wherein one or more rings may contain one or more double bonds , but none of the rings has a completely conjugated pi - electron system . preferably a fused cycloalkyl group is 6 to 14 membered , and more preferably is 7 to 10 membered . according to the number of membered rings , fused cycloalkyl is divided into fused bicyclic ring , tricyclic ring , tetracyclic ring or multicyclic ring , preferably fused bicyclic ring or tricyclic ring . more preferably fused cycloalkyl is 5 - membered / 5 - membered , or 5 - membered / 6 - membered fused bicyclic ring . representative examples of fused cycloalkyl include , but are not limited to the following groups : “ bridged cycloalkyl ” refers to a 5 to 20 membered polycyclic hydrocarbon group , wherein every two rings in the system share with two disconnected carbon atoms . the said rings could have one or more double bonds but have no completely conjugated pi - electron system . preferably a bridged cycloalkyl is 6 to 14 membered , and more preferably is 7 to 10 membered . according to the number of membered rings , bridged cycloalkyl is divided into bridged bicyclic ring , tricyclic ring , tetracyclic ring or multicyclic ring , preferably bicyclic ring , tricyclic ring or tetracyclic ring bridged cycloalkyl , and more preferably bicyclic ring or tricyclic ring bridged cycloalkyl . representative examples of bridged cycloalkyl include , but are not limited to the following groups : the said cycloalkyl can be fused to aryl , heteroaryl or heterocyclic alkyl , wherein the ring connected with the parent structure is cycloalkyl . representative examples of bridged cycloalkyl include , but are not limited to indanylacetic , tetrahydronaphthalene , benzocycloheptyl and so on . said cycloalkyl may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ alkenyl ” refers to an alkyl defined as above that has at least two carbon atoms and at least one carbon - carbon double bond . for example , it refers to vinyl , 1 - propenyl , 2 - propenyl , 1 -, 2 - or 3 - butenyl etc . the alkenyl group may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ alkynyl ” refers to an alkyl defined as above that has at least two carbon atoms and at least one carbon - carbon triple bond . for example , it refers to ethynyl , 1 - propynyl , 2 - propynyl , 1 -, 2 - or 3 - butynyl etc . the alkynyl group may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ heterocyclic alkyl ” refers to a 3 to 20 membered saturated and / or partially unsaturated monocyclic or polycyclic hydrocarbon group having one or more heteroatoms selected from the group consisting of n , o and s ( o ) m ( wherein m is 0 , 1 or 2 ) as ring atoms , but excluding — o — o —, — o — s — or — s — s — in the ring , the remaining ring atoms being c . preferably , heterocyclic alkyl is 3 to 12 membered having 1 to 4 said heteroatoms ; more preferably , is 3 to 10 membered . representative examples of monocyclic heterocyclic alkyl include , but are not limited to pyrrolidyl , piperidyl , piperazinyl , morpholinyl , sulfo - morpholinyl , homopiperazinyl and so on . polycyclic heterocyclic alkyl includes heterocyclic alkyl having spiro ring , fused ring and bridged ring . “ spiro heterocyclo alkyl ” refers to a 5 to 20 membered polycyclic heterocyclic alkyl group with rings connected through one common carbon atom ( called a spiro atom ), wherein said rings have one or more heteroatoms selected from the group consisting of n , o and s ( o ) p ( wherein p is 0 , 1 or 2 ) as ring atoms , the remaining ring atoms being c , wherein one or more rings may contain one or more double bonds , but none of the rings has a completely conjugated pi - electron system . preferably a spiro heterocyclic alkyl is 6 to 14 membered , more preferably is 7 to 10 membered . according to the number of common atoms , spiro heterocyclic alkyl is divided into monocyclic spiro heterocyclic alkyl , bicyclic spiro heterocyclic alkyl or multicyclic spiro heterocyclo alkyl , preferably monocyclic spiro heterocyclic alkyl or bicyclic sipro heterocyclo alkyl . more preferably spiro heterocyclic alkyl is 4 - membered / 4 - membered , 4 - membered / 5 - membered , 4 - membered / 6 - membered , 5 - membered / 5 - membered , or 5 - membered / 6 - membered monocyclic spiro heterocyclo alkyl . representative examples of spiro heterocyclic alkyl include , but are not limited to the following groups : “ fused heterocyclic alkyl ” refers to a 5 to 20 membered polycyclic heterocyclic alkyl group , wherein each ring in the system shares an adjacent pair of carbon atoms with another ring , wherein one or more rings may contain one or more double bonds , but none of the rings has a completely conjugated pi - electron system , and wherein said rings have one or more heteroatoms selected from the group consisting of n , o and s ( o ) p ( wherein p is 0 , 1 or 2 ) as ring atoms , the remaining ring atoms being c . preferably a fused heterocyclic alkyl is 6 to 14 membered , more preferably is 7 to 10 membered . according to the number of membered rings , fused heterocyclic alkyl is divided into fused bicyclic ring , tricyclic ring , tetracyclic ring or multicyclic ring , preferably fused bicyclic ring or tricyclic ring . more preferably fused heterocyclic alkyl is 5 - membered / 5 - membered , or 5 - membered / 6 - membered fused bicyclic ring . representative examples of fused heterocyclic alkyl include , but are not limited to the following groups : “ bridged heterocyclic alkyl ” refers to a 5 to 14 membered polycyclic heterocyclic alkyl group , wherein every two rings in the system share with two disconnected carbon atoms , said rings could have one or more double bonds but have no completely conjugated pi - electron system , and said rings have one or more heteroatoms selected from the group consisting of n , o and s ( o ) m ( wherein m is 0 , 1 or 2 ) as ring atoms , the remaining ring atoms being c . preferably a bridged heterocyclic alkyl is 6 to 14 membered , more preferably 7 to 10 membered . according to the number of membered rings , bridged heterocyclic alkyl is divided into bridged bicyclic ring , tricyclic ring , tetracyclic ring or multicyclic ring , preferably bicyclic ring , tricyclic ring or tetracyclic ring bridged heterocyclic alkyl , more preferably bicyclic ring or tricyclic ring bridged heterocyclic alkyl . representative examples of bridged heterocyclic alkyl include , but are not limited to the following groups : the said heterocyclic alkyl can be fused to aryl , heterocyclic alkyl or cycloalkyl , wherein the ring connected with the parent structure is a heterocyclic alkyl . representative examples of heterocyclic alkyl include , but are not limited to the following groups : and so on . the heterocyclic alkyl may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ aryl ” refers to a 6 to 14 membered all - carbon monocyclic ring or multicyclic fused ring ( a “ fused ” ring system means that each ring in the system shares an adjacent pair of carbon atoms with another ring in the system ) group , and has a completely conjugated pi - electron system . preferably aryl is 6 to 10 membered , such as phenyl and naphthyl . said aryl can be fused to heteroaryl , heterocyclic alkyl or cycloalkyl , wherein the ring connected with the parent structure is aryl . representative examples of aryl include , but are not limited to the following groups : the aryl group may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ heteroaryl ” refers to an aryl having 1 to 4 heteroatoms selected from the group consisting of n , o and s as ring atoms and have 5 to 14 annular atoms , preferably 5 - to 10 - membered ring , more preferably 5 - or 6 - membered ring . the examples of heteroaryl groups include furyl , thienyl , pyridyl , pyrrolyl , n - alkyl pyrrolyl , pyrimidinyl , pyrazinyl , imidazolyl , and the like . said heteroaryl can be fused with the ring of aryl , heterocylic group or cycloalkyl , wherein the ring connected with the parent structure is heteroaryl . representative examples include , but are not limited to the following groups : the heteroaryl group may be substituted or unsubstituted . when substituted , the substituent group ( s ) is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 and — c ( o ) nr8r9 . “ alkoxyl ” refers to — o -( alkyl ) group , wherein the alkyl is defined as above . representative examples include , but are not limited to , methoxy , ethoxy , propoxy , butoxy , and the like . the alkoxyl may be substituted or unsubstituted . when substituted , the substituent is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxyl , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 or — c ( o ) nr8r9 . “ cycloalkoxy ” refers to an — o -( cycloalkyl ) group , wherein the cycloalkyl is defined as above . representative examples include , but are not limited to , cyclopropyloxy , cyclobutyloxy , cyclopentyloxy , cyclohexyloxy , and the like . the cycloalkoxy may be substituted or unsubstituted . when substituted , the substituent is preferably one or more groups independently selected from the group consisting of alkyl , alkenyl , alkynyl , alkoxyl , thioalkyl , alkylamino , halogen , thiol , hydroxyl , nitro , cyano , cycloalkyl , heterocyclic alkyl , aryl , heteroaryl , cycloalkoxy , heterocylic alkoxyl , cycloalkylthio , heterocylic alkylthio , oxo , — or7 , — s ( o ) mr7 , — c ( o ) r7 , — c ( o ) or7 , — nr8r9 or — c ( o ) nr8r9 . “ optional ” or “ optionally ” means that the subsequently described event or circumstance may or may not occur , and that the description includes instances where the event or circumstance may or may not occur . for example , “ heterocycle group optionally substituted by an alkyl group ” means that the alkyl may or may not be present , and the description includes situations where the heterocycle group is substituted by an alkyl group and situations where the heterocycle group is not substituted by the alkyl group . “ substituted ” refers to when one or more hydrogen atoms of the group , preferably 5 for maximum , more preferably 1 - 3 , are independently replaced by the corresponding number of substituents . absolutely , substituents are in their only possible chemical position . technicians in the field are able to determine ( experimentally or theoretically ) possible or impossible substituents without paying excessive efforts . for example , it is unstable when bonding an amino group or hydroxyl group having free hydrogen with carbon atoms having an unsaturated bond ( such as olefinic ). a “ pharmaceutical composition ” refers to a mixture of one or more of the compounds described herein , or physiologically / pharmaceutically acceptable salts or prodrugs thereof , with other chemical components , such as physiologically / pharmaceutically acceptable carriers and excipients . the purpose of the pharmaceutical composition is to facilitate administration of a compound to an organism , with the benefit of intaking the active ingredient more effectively . the conditions , diseases and maladies collectively referred to as “ syndrome x ” ( also known as metabolic syndrome ) are detailed in johannsson , j . clin . endocrinol . metab ., 1997 ; 82 , 727 - 734 incorporated herein by reference . in order to complete the purpose of the invention , the invention applies the following technical solution : a process for preparing a compound of formula ( i ) or a pharmaceutically acceptable salt or stereoisomer thereof according to the present invention comprises the following steps of : under basic conditions , compound ( a ) was reacted with cholorosilicane reagent to obtain a silyl protected compound ( b ) at room temperature , which is treated with nah and benzyl bromide to obtain compound ( c ). in methanol solution , silyl protecting group of compound ( c ) is deprotected by an acyl chloride to obtain hydroxy compound ( d ), which is oxidized to obtain aldehyde ( e ). then the compound ( e ) was reacted with sodium hydroxide in formaldehyde solution to obtain double - hydroxy compound ( f ) ( also called compound ( ia )). upon treated with trifluoroacetic acid ( tfa ), the compound ( ia ) was converted to compound ( ib ), and the benzyl protecting groups of compound ( ib ) was reduced by palladium / carbon catalytic hydrogenation to obtain a compound of formula ( i ), wherein r1 - r6 are as defined in the formula ( i ) above ; and x and y are hydroxyl protecting groups , preferably alkyl or benzyl group . the present invention is further described by the following examples which are not intended to limit the scope of the invention . the structures of all compounds were identified by nuclear magnetic resonance ( 1h nmr ) and / or mass spectrometry ( ms ). 1h nmr chemical shifts were recorded as ppm ( 10 - 6 ). 1h nmr was performed on a bruker avance - 400 spectrometer . the appropriate solvents included deuterated - methanol ( cd3od ), deuterated - chloroform ( cdcl3 ) and deuterated - dimethyl sulfoxide ( dmso - d6 ) with tetramethylsilane ( tms ) as the internal standard . ms was determined on finnigan lcq ad ( esi ) mass spectrometer ( thermo , model : finnigan lcq advantage max ). hplc was determined on agilent 1200dad high pressure liquid chromatography spectrometer ( sunfire c18 150 × 4 . 6 mm chromatographic column ) and waters 2695 - 2996 high pressure liquid chromatography spectrometer ( gimini c18 150 × 4 . 6 mm chromatographic column ). the thin - layer silica gel used was yantai huanghai hsgf254 or qingdao gf254 silica gel plate . the dimension of the plates used in tlc was 0 . 15 mm to 0 . 2 mm , and the dimension of the plates used in product purification was 0 . 4 mm to 0 . 5 mm . column chromatography generally used was yantai huangha 200 to 300 mesh silica gel as carrier . the starting materials of the present invention were known or purchased from abcr gmbh & amp ; co . kg , acros organics , aldrich chemical company , accela chembio inc , darui finechemical co ., ltd and so on , or they could be prepared by the conventional synthesis methods in the prior art . the term “ argon atmosphere ” or “ nitrogen atmosphere ” refers to such an atmosphere that a reaction flask was equipped with a balloon filled with about 1 l argon or nitrogen . the term “ hydrogen atmosphere ” refers to that a reaction flask was equipped with a balloon filled with about 1 l hydrogen . pressured hydrogenation reactions were performed with parr 3916ekx hydrogenation spectrometer and ql - 500 hydrogen generator or hc2 - ss hydrogenation spectrometer . in hydrogenation reactions , the reaction system was generally vacuumed and filled with hydrogen ; while repeated the above operation three times . unless otherwise stated , the reaction was carried out in a nitrogen or argon atmosphere . unless otherwise stated , the solution used in examples refers to an aqueous solution . room temperature was the most ambient reaction temperature , which was 20 ° c .- 30 ° c . the reaction process in the examples was monitored by thin layer chromatography ( tlc ). the developing solvent system comprises dichloromethane and methanol system , hexane and ethyl acetate system , petroleum ether and ethyl acetate system , and acetone . the ratio of the volume of the solvent was adjusted according to the polarity of the compounds . the elution system of column chromatography and the developing solvent system of thin layer chromatography comprises : a : dichloromethane and methanol system , b : n - hexane and ethyl acetate system , c : dichloromethane and acetone system . the ratio of the volume of the solvent was adjusted according to the polarity of the compounds , and sometimes it was also adjusted by adding a basic agent such as triethylamine or an acidic agent such as acetic acid . ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 1a ( prepared according to the method in wo2010022313 ) ( 3 . 0 g , 6 . 06 mmol ) was dissolved in 20 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 148 mg , 1 . 21 mmol ) and tbscl ( 1 . 1 g , 7 . 27 mmol ) in turn . the reaction mixture was stirred for 16 hours , then concentrated under reduced pressure . the residue was dissolved in 100 ml ethyl acetate and 100 ml water and partitioned . the aqueous phase was extracted with ethyl acetate ( 100 ml ), and the organic layer was washed with water ( 50 ml ), combined , dried over anhydrous magnesium sulfate , filtered and concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 1b ( 3 . 0 g , yellow solid ), yield : 81 . 1 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 50 ( dd , 1h ), 7 . 38 ( m , 2h ), 7 . 08 ( d , 2h ), 6 . 82 ( d , 2h ), 4 . 04 ( m , 5h ), 3 . 88 ( m , 1h ), 3 . 82 ( m , 2h ), 3 . 75 ( m , 1h ), 3 . 59 ( m , 1h ), 3 . 40 ( m , 2h ), 3 . 07 ( m , 1h ), 3 . 06 ( s , 3h ), 0 . 90 ( s , 9h ), 0 . 53 ( m , 4h ), 0 . 10 ( s , 3h ), 0 . 07 ( s , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 1b ( 3 . 0 g , 4 . 92 mmol ) was dissolved in 50 ml n , n - dimethyl formamide and cooled to 0 ° c . 60 % nah ( 984 mg , 24 . 6 mmol ) was added . then the reaction mixture was warmed to room temperature and stirred for 15 minutes before benzyl bromide ( 2 . 95 ml , 24 . 6 mmol ) was added . the mixture was stirred for 16 hours . the reaction mixture was concentrated under reduced pressure after 5 ml methanol were added . the residue was dissolved in 100 ml ethyl acetate and partitioned . the organic extracts were washed with water ( 50 ml × 2 ) and combined , dried over anhydrous magnesium sulfate , filtered and concentrated under reduced pressure obtain the crude title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ]- tert - butyl - dim - ethyl - silane 1c ( 4 . 26 g , yellow grease ), which was used directly without purification in the next step . crude [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 1c ( 4 . 26 g , 4 . 92 mmol ) was dissolved in 30 ml methanol , followed by addition of acetyl chloride ( 52 μl , 0 . 74 mmol ). the reaction mixture was stirred for 1 hour . the reaction mixture was concentrated under reduced pressure and purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 1d ( 2 . 3 g , yellow grease ), yield : 62 . 2 %. 1h nmr ( 400 mhz , cdcl 3 ): δ 7 . 35 ( m , 13h ), 7 . 20 ( m , 3h ), 7 . 03 ( m , 4h ), 6 . 80 ( d , 2h ), 4 . 92 ( m , 3h ), 4 . 70 ( m , 1h ), 4 . 50 ( m , 1h ), 4 . 17 ( m , 1h ), 4 . 05 ( m , 3h ), 3 . 85 ( m , 6h ), 3 . 70 ( m , 2h ), 3 . 40 ( m , 1h ), 3 . 30 ( m , 1h ), 3 . 07 ( s , 3h ), 0 . 63 ( m , 2h ), 0 . 48 ( m , 2h ). oxalyl chloride ( 0 . 19 ml , 2 . 2 mmol ) was dissolved in 10 ml methylene chloride , cooled to − 78 ° c ., followed by dropwise addition of 5 ml of a solution of dimethylsulfoxide in methylene chloride and 10 ml [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 1d ( 1 . 3 g , 1 . 7 mmol ) in methylene chloride . the mixture was stirred for 30 minutes at − 78 ° c . thereafter , the mixture was warmed to room temperature and stirred for 1 - 2 hours after triethylamine ( 1 . 18 ml , 8 . 5 mmol ) was added . the reaction mixture was partitioned after 10 ml , 1 m hydrochloric acid were added . the organic phase was washed with saturated sodium chloride solution ( 10 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the crude title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 1e ( 1 . 3 g , colorless oil ), which was used directly without purification in the next step . ms m / z ( esi ): 780 . 3 [ m + 18 ]. crude ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 1e ( 1 . 3 g , 1 . 7 mmol ) was dissolved in 15 ml 1 , 4 - dioxane , followed by addition of 37 % formaldehyde solution ( 2 . 6 ml , 34 mmol ) and a solution of sodium hydroxide ( 204 mg , 5 . 1 mmol ) in 5 . 1 ml water into the reaction mixture . the reaction mixture was stirred for 4 hours at 70 ° c ., then cooled to 50 ° c . and stirred for 16 hours . the reaction mixture was extracted with ethyl acetate ( 20 ml × 3 ) after 20 ml saturated sodium chloride solution were added . the organic extract was washed with saturated sodium bicarbonate solution ( 20 ml ), saturated sodium chloride solution ( 20 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure . then 20 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ) were added into the residue , before sodium borohydride ( 130 mg , 3 . 4 mmol ) was added . the reaction mixture was stirred for 30 minutes and concentrated under reduced pressure . the residue was dissolved in ethyl acetate ( 50 ml ) and partitioned . the organic extract was washed with saturated sodium chloride solution ( 10 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure , then the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 1f ( 320 mg , colorless oil ), yield : 23 . 7 %. [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol if ( 320 mg , 0 . 4 mmol ) was dissolved in 10 ml methylene chloride and cooled to − 10 ° c ., followed by addition of trifluoroacetic acid ( 62 ml , 0 . 8 mmol ). the mixture was stirred for 1 hour . thereafter , the reaction mixture was partitioned after 10 ml saturated sodium bicarbonate solution were added . the aqueous phase was extracted with dichlormethane ( 10 ml ) and the organic extract was washed with saturated sodium chloride solution ( 10 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 1g ( 230 mg , colorless oil ), yield : 75 . 3 %. ms m / z ( esi ): 780 . 3 [ m + 18 ]. 1 h nmr ( 400 mhz , cdcl 3 ): δ 7 . 33 ( m , 12h ), 7 . 15 ( m , 4h ), 7 . 05 ( m , 2h ), 6 . 86 ( d , 2h ), 6 . 76 ( d , 2h ), 4 . 77 ( m , 4h ), 4 . 27 ( m , 2h ), 4 . 00 ( m , 6h ), 3 . 83 ( m , 3h ), 3 . 70 ( m , 4h ), 3 . 38 ( m , 1h ), 0 . 63 ( m , 2h ), 0 . 48 ( m , 2h ). [( 1s , 2s , 3s , 4r , 55 )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 1g ( 220 . 3 mg , 0 . 29 mmol ) was dissolved in 10 ml mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of 1 , 2 - dichlorobenzene ( 0 . 34 ml , 3 mmol ) and palladium / carbon ( 90 mg , 10 %). the mixture was exchanged with h 2 three times and stirred for 3 hours , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[[ 4 -[ 2 -( cyclopropoxy ) ethoxy ] phenyl ] methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 1 ( 140 mg , white solid ), yield : 100 %. ms m / z ( esi ): 510 . 2 [ m + 18 ]. 1 h nmr ( 400 mhz , cd 3 od ): δ 7 . 45 ( d , 1h ), 7 . 36 ( m , 2h ), 7 . 10 ( d , 2h ), 6 . 82 ( m , 2h ), 4 . 14 ( d , 1h ), 4 . 05 ( m , 4h ), 3 . 83 ( m , 3h ), 3 . 78 ( m , 1h ), 3 . 66 ( m , 2h ), 3 . 57 ( m , 2h ), 3 . 40 ( m , 1h ), 0 . 56 ( m , 2h ), 0 . 48 ( m , 2h ). 5 - bromo - 2 - chloro - benzoyl chloride 2a ( 7 . 22 g , 28 . 45 mmol ) and 1 , 2 - difluoro - 3 - methoxybenzene 2b ( 4 . 1 g , 28 . 45 mmol , prepared according to the method in cn2003468a ) were dissolved in 50 ml methylene chloride and cooled to 0 ° c ., followed by addition of aluminum trichloride ( 3 . 4 g , 25 . 6 mmol ) in batch . the mixture was stirred for 16 hours . then , the mixture was partitioned after 20 ml 1 m hydrochloric acid were added and extracted with dichloromethane ( 50 ml × 2 ). the organic extract was washed with saturated sodium carbonate solution ( 50 ml ) and saturated sodium chloride solution ( 50 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - difluoro - 4 - methoxy - phenyl ) one 2c ( 5 . 1 g , yellow solid ), yield : 49 . 5 %. ms m / z ( esi ): 362 . 9 [ m + 18 ]. ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - difluoro - 4 - methoxy - phenyl ) one 2c ( 5 . 1 g , 14 . 1 mmol ) was dissolved in 40 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ) and cooled to 0 ° c ., followed by addition of sodium borohydride in batch ( 1 . 07 g , 28 . 2 mmol ). the reaction mixture was stirred for 30 minutes . thereafter , the reaction mixture was concentrated under reduced pressure after 10 ml acetone were added . the resulting residue was dissolved in ethyl acetate ( 100 ml ) and partitioned . the organic extract was washed with water ( 20 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methanol 2d ( 5 . 1 g , yellow grease ), yield : 99 . 6 %. ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methanol 2d ( 5 . 1 g , 14 . 1 mmol ) was dissolved in 40 ml methylene chloride , followed by addition of triethyl silane ( 6 . 75 ml , 42 . 3 mmol ) and dropwise addition of boron trifluoride diethyl ether ( 3 . 57 ml , 28 . 2 mmol ). the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was partitioned after 20 ml saturated sodium carbonate solution were added . the aqueous phase was extracted with dichlormethane ( 20 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound 1 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 , 3 - difluoro - 4 - methoxy - benzene 2e ( 3 . 55 g , white solid ), yield : 72 . 4 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 36 - 7 . 33 ( m , 1h ), 7 . 30 - 7 . 27 ( m , 2h ), 6 . 81 - 6 . 79 ( m , 1h ), 6 . 73 - 6 . 69 ( m , 1h ), 4 . 00 ( s , 2h ), 3 . 92 ( s , 3h ). 1 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 , 3 - difluoro - 4 - methoxy - benzene 2e ( 3 . 55 g , 10 . 2 mmol ) was dissolved in 30 ml mixed solution ( thf and toluene , v : v = 1 : 2 ) and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli in n - hexane ( 4 . 9 ml , 12 . 26 mmol ). after stirring for 1 hour at − 78 ° c ., a solution of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 5 . 24 g , 11 . 22 mmol , prepared according to the method in wo2010048358 ) in toluene ( 30 ml ) was added . the reaction mixture was stirred for 3 hours at − 78 ° c . thereafter , the reaction mixture was concentrated under reduced pressure after 30 ml saturated sodium carbonate solution were added . the residue was dissolved in 30 ml saturated sodium chloride solution and extracted with ethyl acetate ( 50 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 2g ( 1 . 31 g , white solid ), yield : 27 . 9 %. ms m / z ( esi ): 429 . 1 [ m − 31 ] ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 2g ( 1 . 31 g , 2 . 84 mmol ) was dissolved in 15 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 70 mg , 0 . 57 mmol ) and trimethyl - chloro - silane ( 514 mg , 3 . 4 mmol ). the reaction mixture was stirred for 16 hours and then concentrated under reduced pressure . the resulting residue was dissolved in 150 ml ethyl acetate and washed with pyridine ( 50 ml × 2 ), water ( 30 ml ) and saturated sodium chloride solution ( 30 ml ) in turn . the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 2 - methoxy - 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 3 , 4 , 5 - triol 2h ( 1 . 63 g , pale yellow solid ), yield : 100 %. ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 2 - methoxy - 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 3 , 4 , 5 - triol 2h ( 1 . 63 g , 2 . 84 mmol ) was dissolved in 30 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 570 mg , 14 . 2 mmol ). then the reaction mixture was warmed to room temperature and stirred for 45 minutes . thereafter , benzyl bromide ( 1 . 7 ml , 14 . 2 mmol ) was added before the reaction mixture was stirred overnight . the reaction mixture was concentrated under reduced pressure after 5 ml methanol were added . after 150 ml ethyl acetate and 50 ml water were added into the residue , the resulting residue was partitioned and the organic extract was washed with water ( 50 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] trimethyl - silane 21 ( 2 . 4 g , yellow grease ), with yield : 100 %. [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] trimethylsilane 21 ( 2 . 4 g , 2 . 84 mmol ) was dissolved in 20 ml methanol and stirred for 1 hour after addition of acetyl chloride ( 30 μl , 0 . 43 mmol ). the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 - meth oxy - tetrahydropyran - 2 - yl ] methanol 2j ( 1 . 25 g , yellow solid ), with yield : 60 . 4 %. oxalyl chloride was dissolved in 5 ml methylene chloride and cooled to − 78 ° c ., followed by dropwise addition of 3 ml solution of dimethyl sulfoxide (( 0 . 26 ml , 3 . 59 mmol ) in methylene chloride . the reaction mixture was stirred for 15 minutes , before 5 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 2j ( 1 . 25 g , 1 . 71 mmol ) in methylene chloride was dropwise added . the mixture was stirred for 40 minutes . the triethylamine ( 1 . 19 ml , 8 . 55 mmol ) was dropwise added , before the reaction mixture was warmed to room temperature and stirred for 1 . 5 hours . thereafter , the reaction mixture was washed with 5 ml 1 m hydrochloric acid and the organic extract was collected , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 2k ( 1 . 24 g , yellow solid ), which was used in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 2k ( 1 . 24 g , 1 . 71 mmol ) was dissolved in 15 ml 1 , 4 - dioxane , followed by 37 %- 40 % aqueous solution of formaldehyde ( 2 . 8 ml , 34 . 2 mmol ) and 1 . 5 ml of sodium hydroxide solution ( 205 mg , 5 . 13 mmol ). the reaction mixture was stirred overnight at 70 ° c . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 30 ml ethyl acetate and 15 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 15 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 2m ( 1 . 29 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 2m ( 1 . 29 g , 1 . 71 mmol ) was dissolved in 15 ml of mixed solution ( thf and meoh , v : v = 1 : 2 ), followed by addition of sodium borohydride ( 129 mg , 3 . 42 mmol ). the reaction mixture was stirred for 20 minutes . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 30 ml ethyl acetate and 15 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 15 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tri - benzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 2n ( 520 mg , white solid ), with yield : 40 %. [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 2n ( 500 mg , 0 . 66 mmol ) was dissolved in 10 ml dichloromethane , followed by dropwise addition of trifluoroacetic acid ( 0 . 2 ml , 2 . 62 mmol ). the reaction mixture was stirred for 1 . 5 hours . thereafter , the reaction mixture was washed with 10 ml saturated sodium bicarbonate solution and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 2p ( 360 mg , white solid ), with yield : 75 . 3 %. ms m / z ( esi ): 746 . 2 [ m + 18 ]. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 2p ( 350 mg , 0 . 48 mmol ) was dissolved in 10 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 0 . 55 ml , 4 . 8 mmol ) and palladium / carbon ( 300 mg , 10 %) in turn . the mixture was exchanged with h 2 three times and stirred for 3 hours , filtered with silica gel and the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[( 2 , 3 - difluoro - 4 - methoxy - phenyl ) methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 2 ( 210 mg , white solid ), yield : 95 . 5 %. ms m / z ( esi ): 459 . 1 [ m + 1 ]; 1 h nmr ( 400 mhz , cd 3 od ): δ 7 . 42 ( m , 3h ), 6 . 81 ( m , 2h ), 4 . 16 ( d , 1h ), 4 . 10 ( s , 2h ), 3 . 87 ( s , 3h ), 3 . 82 ( m , 2h ), 3 . 68 ( m , 2h ), 3 . 55 ( m , 1h ), 3 . 61 ( m , 1h ). 2 , 3 - difluorophenol 3a ( 4 g , 30 . 7 mmol ) was dissolved in 60 ml acetone , followed by addition of potassium carbonate ( 6 . 36 g , 46 . 1 mmol ) and ethyl iodide ( 3 . 19 ml , 39 . 9 mmol ). the reaction mixture was stirred for 5 hours at 70 ° c . thereafter , the reaction mixture was filtered . the filtrate was concentrated under reduced pressure . the resulting residue was dissolved in 100 ml ethyl acetate , and washed with water ( 100 ml ) and saturated sodium chloride solution ( 100 ml ), and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound 1 - ethoxy - 2 , 3 - difluoro - benzene 3b ( 4 . 82 g , yellow grease ), yield : 99 . 4 %. 1h nmr ( 400 mhz , cdcl3 ): δ 6 . 95 - 6 . 89 ( m , 1h ), 6 . 78 - 6 . 71 ( m , 1h ), 4 . 12 ( q , 2h ), 1 . 45 ( t , 3h ). 5 - bromo - 2 - chloro - benzoyl chloride 2a ( 7 . 74 g , 30 . 5 mmol ) was dissolved in 200 ml dichloromethane , followed by addition of 1 - ethoxy - 2 , 3 - difluoro - benzene 3b ( 4 . 82 g , 30 . 5 mmol ) and aluminum trichloride ( 4 . 07 g , 30 . 5 mmol ). the reaction mixture was stirred for 16 hours . thereafter , the mixture was partitioned after 100 ml 2 m hydrochloric acid were added . the organic extract was washed with saturated sodium chloride solution ( 100 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methanone 3c ( 8 . 0 g , yellow grease ), yield : 70 . 2 %. ms m / z ( esi ): 376 . 9 [ m + 1 ]. ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methanone 3c ( 8 . 0 g , 21 . 3 mmol ) was dissolved in 240 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of potassium borohydride ( 1 . 73 g , 32 . 0 mmol ) in an ice bath . the reaction mixture was stirred for 16 hours at room temperature . thereafter , 50 ml 1 m hydrochloric acid were added . the reaction mixture was concentrated under reduced pressure and extracted with dichloromethane ( 100 ml × 2 ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methanol 3d ( 8 . 0 g , yellow grease ), which was used directly in the next step without purification . ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methanol 3d ( 8 . 0 g , 21 . 2 mmol ) was dissolved in 150 ml of mixed solution ( acetonitrile and dichloromethane , v : v = 2 : 1 ), followed by addition of triethylsilane ( 10 . 1 ml , 63 . 6 mmol ) and boron trifluoride etherate ( 5 . 3 ml , 42 . 4 mmol ). the reaction mixture was stirred for 3 hours , before 100 ml 2 m potassium hydroxide were added . the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system c to obtain the title compound 1 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 4 - ethoxy - 2 , 3 - difluoro - benzene 3e ( 5 . 5 g , white solid ), yield : 72 . 4 %. ms m / z ( esi ): 360 . 5 [ m + 1 ]. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 36 - 7 . 27 ( m , 3h ), 6 . 81 - 6 . 76 ( dd , 1h ), 6 . 72 - 6 . 68 ( dd , 1h ), 4 . 17 - 4 . 13 ( q , 2h ), 4 . 10 ( s , 2h ), 1 . 50 - 1 . 47 ( t , 3h ). 1 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 4 - ethoxy - 2 , 3 - difluoro - benzene 3e ( 5 . 5 g , 15 . 3 mmol ) was dissolved in 20 ml thf and cooled to − 78 ° c ., followed by dropwise addition of a solution of n - buli in n - hexane ( 7 . 3 ml , 18 . 3 mmol ). the reaction mixture was stirred for 1 hour at − 78 ° c . 30 ml solution of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 7 . 5 g , 16 . 1 mmol ) in thf at − 78 ° c . were added before the reaction mixture was stirred for 2 hours at − 78 ° c . a solution ( 51 ml ) of 0 . 6 m methanesulfonic acid in methanol was added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure , dissolved in water ( 50 ml ) and extracted with ethyl acetate ( 100 ml × 4 ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 3f ( 3 . 05 g , white solid ), yield : 45 . 5 %. ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 3f ( 3 . 0 g , 6 . 8 mmol ) was dissolved in 30 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 166 mg , 1 . 36 mmol ) and tbscl ( 1 . 23 g , 8 . 2 mmol ) in turn . the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure before 150 ml ethyl acetate were added . the reaction mixture was washed with saturated copper sulfate solution ( 100 ml ) and saturated sodium chloride solution ( 100 ml ) in turn . the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 2 - methoxy - tetrahydro - pyran - 3 , 4 , 5 - triol 3g ( 3 . 75 g , white solid ), yield : 99 . 7 %. ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 3g ( 3 . 75 g , 6 . 8 mmol ) was dissolved in 30 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 1 . 36 g , 34 mmol ). the reaction mixture was warmed and stirred for 45 minutes at room temperature before tetrabutylammonium iodide ( 125 mg , 0 . 34 mmol ) and benzyl bromide ( 4 . 01 ml , 34 mmol ) were added in turn . after stirring for 16 hours at room temperature , the reaction mixture was concentrated under reduced pressure after 10 ml methanol were added . the resulting residue was dissolved in 100 ml ethyl acetate and partitioned . the organic extract was washed with water ( 50 ml × 2 ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] tert - butyl - dimethyl - methoxy ] silane 3h ( 4 . 2 g , colourless grease ), yield : 75 . 0 %. [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] tert - butyl - dimethyl - methoxy ] silane 3h ( 4 . 7 g , 5 . 46 mmol ) was dissolved in 50 ml methanol , followed by addition of acetyl chloride ( 80 mg , 0 . 82 mmol ). the reaction mixture was stirred for 1 hour at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydro - pyran - 2 - yl ] methanol 31 ( 2 . 5 g , yellow grease ), yield : 61 . 4 %. oxalyl chloride ( 0 . 37 ml , 4 . 37 mmol ) was dissolved in 20 ml dichloromethane and cooled to − 78 ° c ., followed by dropwise addition of a solution ( 10 ml ) of dimethyl sulfoxide ( 0 . 5 ml , 7 . 05 mmol ) in dichloromethane and a solution ( 20 ml ) of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 3i ( 2 . 5 g , 3 . 36 mmol ) in dichloromethane in turn . the reaction mixture was stirred for 30 minutes at − 78 ° c . triethylamine ( 2 . 33 ml , 16 . 8 mmol ) was added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was partitioned after 15 ml 1 m hydrochloric acid were added . the organic extract was washed with saturated sodium chloride solution ( 20 ml × 2 ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 3j ( 2 . 4 g , yellow grease ), yield : 96 . 0 %. ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 3j ( 2 . 4 g , 3 . 23 mmol ) was dissolved in 20 ml 1 , 4 - dioxane , followed by addition of 5 ml 37 % formaldehyde solution and 13 ml 1 m sodium hydroxide . the reaction mixture was stirred for 21 hours at 70 ° c . thereafter , the reaction mixture was extracted with ethyl acetate ( 50 ml × 3 ) after 20 ml of saturated sodium chloride solution were added . the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 3k ( 1 . 6 g , yellow grease ), yield : 64 . 0 %. ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 3k ( 1 . 6 g , 2 . 1 mmol ) was dissolved in 35 ml of mixed solution ( thf and meoh , v : v = 2 : 5 ), followed by addition of sodium borohydride ( 78 mg , 4 . 2 mmol ). the reaction mixture was stirred for 2 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 3m ( 1 . 0 g , yellow grease ), yield : 62 . 5 %. [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 3m ( 1 . 0 g , 1 . 29 mmol ) was dissolved in 10 ml dichloromethane , followed by addition of trifluoroacetic acid ( 0 . 19 ml , 2 . 58 mmol ). the reaction mixture was stirred for 4 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 3n ( 500 mg , yellow grease ), yield : 52 . 1 %. ms m / z ( esi ): 760 . 3 [ m + 18 ]. 1h nmr ( 400 mhz , cd3od ): δ 7 . 37 - 7 . 30 ( m , 13h ), 7 . 23 - 7 . 18 ( m , 3h ), 6 . 91 - 6 . 89 ( m , 2h ), 6 . 68 ( dd , 1h ), 6 . 55 ( dd , 1h ), 4 . 93 - 4 . 90 ( m , 2h ), 4 . 79 - 4 . 56 ( m , 4h ), 4 . 30 - 4 . 28 ( m , 2h ), 4 . 18 - 4 . 05 ( m , 4h ), 3 . 83 - 3 . 49 ( m , 5h ), 1 . 33 ( t , 3h ). [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 3n ( 550 mg , 0 . 74 mmol ) was dissolved in 20 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 0 . 84 ml , 7 . 4 mmol ) and palladium / carbon ( 300 mg , 10 %). the mixture was exchanged with h2 three times and stirred for 3 hours . thereafter , the reaction mixture was filtered after a small amount of ethyl acetate was added . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 3 ( 160 mg , white solid ), yield : 45 . 7 %. ms m / z ( esi ): 472 . 2 [ m + 1 ]. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 43 - 7 . 37 ( m , 3h ), 6 . 80 - 6 . 76 ( m , 2h ), 4 . 16 - 4 . 07 ( m , 5h ), 3 . 85 - 3 . 70 ( m , 2h ), 3 . 70 - 3 . 51 ( m , 4h ), 1 . 34 ( t , 3h ). 2 - fluorophenol 4a ( 6 . 7 g , 60 mmol ) was dissolved in 66 ml acetone , followed by addition of ethyl iodide ( 6 . 3 ml , 78 mmol ) and potassium carbonate ( 12 . 4 g , 90 mmol ). the reaction mixture was refluxed in an oil bath for 5 hours . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 100 ml ethyl acetate and 60 ml water were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound 1 - ethoxy - 2 - fluoro - benzene 4b ( 6 . 9 g , red grease ), yield : 82 . 1 %. ms m / z ( esi ): 280 . 2 [ 2m + 1 ]. 5 - bromo - 2 - chloro - benzoyl chloride 2a ( 12 . 4 g , 48 . 8 mmol ) and 1 - ethoxy - 2 - fluoro - benzene 4b ( 6 . 84 g , 48 . 8 mmol ) were dissolved in 100 ml dichloromethane and cooled to 0 ° c ., followed by addition of aluminum trichloride ( 5 . 86 g , 44 mmol ) in batch . the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was partitioned after 20 ml 2 m hydrochloric acid was dropwise added in an ice bath . the aqueous phase was extracted with 30 ml dichloromethane and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 3 - fluoro - phenyl ) methanone 4c ( 12 . 7 g , yellow solid ), yield : 72 . 6 %. ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 3 - fluoro - phenyl ) methanone 4c ( 12 . 7 g , 35 . 5 mmol ) was dissolved in 100 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of sodium borohydride ( 2 . 68 g , 70 mmol ) in batch in an ice bath . the reaction mixture was warmed and stirred for 30 minutes at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure after 15 ml acetone were added . the residue was dissolved in 150 ml ethyl acetate and washed with saturated sodium chloride solution ( 50 ml × 2 ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 3 - fluoro - phenyl ) methanol 4d ( 12 . 7 g , orange grease ), which was used directly in the next step without purification . ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 3 - fluoro - phenyl ) methanol 4d ( 12 . 7 g , 35 . 3 mmol ) was dissolved in 100 ml dichloromethane , followed by addition of triethyl silicane ( 16 . 9 ml , 106 mmol ) and dropwise addition of boron trifluoride etherate ( 8 . 95 ml , 70 . 6 mmol ). the reaction mixture was stirred for 3 hours . thereafter , the reaction mixture was partitioned after 50 ml saturated sodium bicarbonate solution were added . the aqueous phase was extracted with ethyl acetate ( 100 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 1 - ethoxy - 2 - fluoro - benzene 4e ( 10 g , pale yellow grease ), yield : 82 . 4 %. 1h nmr ( 400 mhz , cdcl 3 ): δ 7 . 33 - 7 . 27 ( m , 3h ), 6 . 95 - 6 . 90 ( m , 3h ), 4 . 14 ( q , 2h ), 4 . 01 ( s , 2h ), 1 . 49 ( t , 3h ). 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 1 - ethoxy - 2 - fluoro - benzene 4e ( 7 . 36 g , 21 . 4 mmol ) was dissolved in 30 ml thf and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli in n - hexane ( 10 . 27 ml , 25 . 7 mmol ). after stirring for 1 hour at − 78 ° c ., a solution ( 20 ml ) of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 11 g , 23 . 6 mmol ) in thf was added before the reaction mixture was stirred for 2 hours at − 78 ° c . then the reaction mixture was warmed and stirred for 16 hours at room temperature after 2 . 8 ml methylsulfonic acid and 71 ml methanol were added . thereafter , the reaction mixture was concentrated under reduced pressure after 100 ml saturated sodium carbonate solution were added . the residue was dissolved in 50 ml saturated sodium chloride , extracted with ethyl acetate ( 100 ml × 3 ). the organic extract was combined , dried over anhydrous magnesium sulfate , filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 4f ( 5 . 7 g , white solid ), yield : 58 . 3 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 56 ( s , 1h ), 7 . 48 ( dd , 1h ), 7 . 37 ( dd , 1h ), 6 . 95 - 6 . 87 ( m , 3h ), 4 . 08 - 4 . 07 ( m , 4h ), 3 . 91 ( m , 1h ), 3 . 93 - 3 . 73 ( m , 2h ), 3 . 56 - 3 . 53 ( m , 1h ), 3 . 45 - 3 . 43 ( m , 1h ), 3 . 30 ( s , 2h ), 3 . 08 ( s , 3h ), 1 . 35 ( t , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 4f ( 5 . 7 g , 12 . 5 mmol ) was dissolved in 50 ml pyridine , followed by addition of tbscl ( 2 . 26 g , 15 mmol ) and 4 - dimethyl - amino pyridine ( 305 mg , 2 . 5 mmol ) in turn . the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure . the residue was dissolved in 200 ml ethyl acetate and washed with saturated copper sulfate solution ( 50 ml × 3 ). the organic extract was combined , dried over anhydrous magnesium sulfate , filtered and concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 4g ( 7 . 14 g , colourless grease ), which was used directly without purification in the next step . ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 4g ( 7 . 14 g , 12 . 5 mmol ) was dissolved in 100 ml n , n - dimethyl formamide , followed by addition of 60 % nah ( 2 . 5 g , 62 . 5 mmol ) in an ice bath . the reaction mixture was warmed and stirred for 40 minutes at room temperature . the mixture was stirred for 16 hours after benzyl bromide ( 7 . 5 ml , 62 . 5 mmol ) was added . thereafter , the reaction mixture was concentrated under reduced pressure after 20 ml methanol were added . the residue was dissolved in 200 ml ethyl acetate and 50 ml water and partitioned . the aqueous phase was extracted with ethyl acetate ( 50 ml ). the organic extracts were washed with water ( 50 ml ), then saturated sodium chloride ( 50 ml ), combined , dried over anhydrous magnesium sulfate , filtered and concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethylsilane 4h ( 10 . 5 g , yellow grease ), yield : 99 . 8 %. [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethylsilane 4h ( 10 . 52 g , 12 . 5 mmol ) was dissolved in 50 ml methanol , followed by dropwise addition of acetyl chloride ( 0 . 13 ml , 1 . 9 mmol ). the reaction mixture was stirred for 1 hour . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 4i ( 7 . 6 g , yellow grease ), yield : 83 . 6 %. oxalyl chloride ( 1 . 17 ml , 13 . 6 mmol ) was dissolved in 20 ml dichloromethane and cooled to − 78 ° c ., followed by dropwise addition of a solution ( 20 ml ) of dimethyl sulfoxide ( 1 . 56 ml , 21 . 9 mmol ) in dichloromethane and a solution ( 50 ml ) of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 4i ( 7 . 6 g , 10 . 45 mmol ) in dichloromethane . the reaction mixture was stirred for 30 minutes at − 78 ° c . triethylamine ( 7 . 25 ml , 52 . 3 mmol ) was added before the reaction mixture was warmed and stirred for 2 hours at room temperature . thereafter , the reaction mixture was partitioned after 50 ml 1 m hydrochloric acid were added . the organic extract was washed with saturated sodium chloride solution ( 50 ml × 2 ). the aqueous phase was extracted with dichloromethane ( 50 ml ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 4j ( 7 . 58 g , colourless grease ), which was used directly without purification in the next step . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 4j ( 7 . 6 g , 10 . 45 mmol ) was dissolved in 80 ml 1 , 4 - dioxane , followed by addition of 15 . 8 ml 37 % formaldehyde solution and sodium hydroxide ( 31 . 35 ml , 31 . 35 mmol ) in turn . the reaction mixture was stirred for 16 hours at 70 ° c . thereafter , the reaction mixture was extracted with ethyl acetate ( 50 ml × 4 ) after 50 ml saturated sodium chloride solution were added . the organic extract was washed with saturated sodium bicarbonate solution ( 50 ml ) and saturated sodium chloride solution ( 50 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 4k ( 7 . 9 g , colourless grease ), which was used directly without purification in the next step . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 4k ( 7 . 9 g , 10 . 45 mmol ) was dissolved in 50 ml of mixed solution ( thf and meoh , v : v = 2 : 3 ), followed by addition of sodium borohydride ( 794 mg , 20 . 9 mmol ). the reaction mixture was stirred for 30 minutes . thereafter , the reaction mixture was concentrated under reduced pressure after a small amount of acetone was added and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 4m ( 1 . 11 g , colourless grease ), yield : 14 . 1 %. [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ]- phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 4m ( 1 . 11 g , 1 . 46 mmol ) was dissolved in 20 ml dichloromethane and cooled to − 10 ° c ., followed by addition of trifluoroacetic acid ( 0 . 23 ml , 3 mmol ). the reaction mixture was warmed and stirred for 2 hours and partitioned after 20 ml saturated sodium bicarbonate solution were added . the aqueous phase was extracted with dichloromethane ( 20 ml × 2 ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 4n ( 830 mg , colourless grease ), yield : 78 . 3 %. ms m / z ( esi ): 742 . 3 [ m + 18 ]. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 4n ( 830 mg , 1 . 14 mmol ) was dissolved in 20 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 1 . 3 ml , 11 . 4 mmol ) and palladium / carbon ( 500 mg , 10 %). the mixture was exchanged with h2 three times and stirred for 3 hours and filtered . thereafter , the reaction mixture was eluted with a small amount of ethyl acetate . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[( 4 - ethoxy - 2 , 3 - difluoro - phenyl ) methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 4 ( 420 mg , white solid ), yield : 81 . 0 %. ms m / z ( esi ): 472 . 2 [ m + 18 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 47 ( s , 1h ), 7 . 42 - 7 . 35 ( m , 2h ), 6 . 95 - 6 . 87 ( m , 3h ), 4 . 16 - 4 . 14 ( m , 1h ), 4 . 06 - 4 . 02 ( m , 4h ), 3 . 85 - 3 . 70 ( m , 2h ), 3 . 67 - 3 . 54 ( m , 4h ), 1 . 37 ( t , 3h ). 5 - bromo - 2 - chloro - benzoyl chloride 2a ( 10 . 8 g , 42 . 5 mmol ) was dissolved in 100 ml dichloromethane , followed by addition of 2 , 3 - dihydrobenzofuran 5a ( 5 . 11 g , 42 . 5 mmol ) and addition of aluminum trichloride ( 6 . 8 g , 51 . 0 mmol ) in batch . the reaction mixture was stirred for 2 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - dihydrobenzofuran - 5 - yl ) methanone 5b ( 10 . 47 g , white solid ), yield : 72 . 9 %. ms m / z ( esi ): 339 . 0 [ m + 1 ]; 1h nmr ( 400 mhz , cdcl 3 ): δ 7 . 73 ( d , 1h ), 7 . 58 ( dd , 1h ), 7 . 53 ( dd , 1h ), 7 . 47 ( d , 1h ), 7 . 32 ( d , 1h ), 6 . 81 ( d , 1h ), 4 . 68 ( t , 2h ), 3 . 26 ( t , 2h ). ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - dihydrobenzofuran - 5 - yl ) methanone 5b ( 10 . 47 g , 31 . 0 mmol ) was dissolved in 100 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ) and cooled to 0 ° c ., followed by addition of sodium borohydride ( 2 . 35 g , 62 . 0 mmol ) in batch . the reaction mixture was stirred for 30 minutes at 0 ° c . thereafter , the reaction mixture was concentrated under reduced pressure after 20 ml acetone were added . the resulting residue was dissolved in 250 ml ethyl acetate and partitioned . the organic extract was washed with water ( 100 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - dihydrobenzofuran - 5 - yl ) methanol 5c ( 10 . 5 g , pale yellow grease ), yield : 99 . 7 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 88 ( d , 1h ), 7 . 34 ( dd , 1h ), 7 . 18 ( d , 1h ), 7 . 16 ( s , 1h ), 7 . 11 ( dd , 1h ), 6 . 73 ( d , 1h ), 6 . 05 ( s , 1h ), 4 . 56 ( t , 2h ), 3 . 18 ( t , 2h ), 2 . 27 ( s , 1h ). ( 5 - bromo - 2 - chloro - phenyl )-( 2 , 3 - dihydrobenzofuran - 5 - yl ) methanol 5c ( 10 . 5 g , 30 . 9 mmol ) was dissolved in 100 ml dichloromethane , followed by addition of triethylsilane ( 14 . 8 ml , 92 . 7 mmol ) and dropwise addition of boron trifluoride etherate ( 7 . 8 ml , 61 . 8 mmol ). the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound 5 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 , 3 - dihydrobenzo - furan 5d ( 10 . 0 g , pale yellow grease ), yield : 100 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 29 - 7 . 21 ( m , 3h ), 7 . 00 ( s , 1h ), 6 . 93 ( d , 1h ), 6 . 73 ( d , 1h ), 4 . 56 ( t , 2h ), 3 . 98 ( s , 2h ), 3 . 18 ( t , 2h ). 5 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 , 3 - dihydrobenzofuran 5d ( 10 . 0 g , 30 . 9 mmol ) was dissolved in 90 ml of mixed solution ( thf and toluene , v : v = 1 : 2 ) and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli in n - hexane ( 14 . 83 ml , 37 . 1 mmol ). after stirring for 1 hour at − 78 ° c ., a solution of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 15 . 87 g , 33 . 9 mmol ) in toluene ( 90 ml ) was dropwise added before the reaction mixture was stirred for 3 hours at − 78 ° c . a solution of 0 . 6 m methanesulfonic acid in methanol ( 103 ml ) was added before the reaction mixture was stirred for 16 hours . thereafter , the reaction was concentrated under reduced pressure after 100 ml saturated sodium carbonate solution were added . the residue was extracted with ethyl acetate ( 100 ml × 3 ) after 50 ml saturated sodium chloride solution were added and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system e to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 5e ( 6 . 3 g , white solid ), yield : 46 . 7 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 53 ( d , 1h ), 7 . 45 ( dd , 1h ), 7 . 35 ( d , 1h ), 7 . 03 ( s , 1h ), 6 . 91 ( d , 1h ), 6 . 60 ( d , 1h ), 4 . 48 ( t , 2h ), 4 . 13 - 3 . 91 ( m , 3h ), 3 . 84 - 3 . 73 ( m , 2h ), 3 . 61 - 3 . 56 ( m , 1h ), 3 . 44 - 3 . 39 ( m , 1h ), 3 . 11 ( dd , 3h ), 3 . 07 ( s , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 5e ( 6 . 3 g , 14 . 44 mmol ) was dissolved in 60 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 353 mg , 2 . 89 mmol ) and tert - butyl - dimethyl - chloro - silane ( 2 . 61 g , 17 . 32 mmol ) in turn . the reaction mixture was stirred for 16 hours and concentrated under reduced pressure . the resulting residue was dissolved in 200 ml ethyl acetate and partitioned . the organic extract was washed with water ( 50 ml ) and saturated sodium chloride solution ( 50 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 5f ( 7 . 96 g , pale yellow solid ), which was used directly in the next step without purification . ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 5f ( 7 . 96 g , 14 . 4 mmol ) was dissolved in 80 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 2 . 89 g , 72 . 21 mmol ). then the reaction mixture was warmed to room temperature and stirred for 15 minutes . thereafter , benzyl bromide ( 8 . 58 ml , 72 . 21 mmol ) was added before the mixture was stirred for 16 hours . the reaction mixture was concentrated under reduced pressure after 10 ml methanol were added . followed by addition of 200 ml ethyl acetate , the reaction mixture was washed with water ( 50 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] tert - butyl - dimethyl - methoxy ] silane 5g ( 11 . 86 g , black grease ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] tert - butyl - dimethyl - methoxy ] silane 5g ( 11 . 86 g , 14 . 4 mmol ) was dissolved in 100 ml methanol , followed by addition of acetyl chloride ( 152 μl , 2 . 17 mmol ). the reaction mixture was stirred for 1 hour and concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 5h ( 9 . 0 g , yellow liquid ), yield : 88 . 1 %. oxalyl chloride ( 0 . 76 ml , 8 . 91 mmol ) was dissolved in 10 ml methylene chloride and cooled to − 78 ° c ., followed by dropwise addition of 10 ml of mixed solution ( methylene chloride and dimethyl sulfoxide , v : v = 10 : 0 . 85 ). the reaction mixture was stirred for 15 minutes . then 25 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 5h ( 4 . 2 g , 5 . 94 mmol ) in methylene chloride was dropwise added before the mixture was stirred for 40 minutes . the reaction mixture was warmed to room temperature and stirred for 2 hours after triethylamine ( 4 . 29 ml , 29 . 69 mmol ) was dropwise added . thereafter , the reaction mixture was partitioned after 35 ml 1 m hydrochloric acid were added , the organic extract was washed with saturated sodium chloride solution ( 35 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmeth - yl ) phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 51 ( 4 . 19 g , pale yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 51 ( 4 . 19 g , 5 . 9 mmol ) was dissolved in 45 ml 1 , 4 - dioxane , followed by addition of 9 . 6 ml 37 % formaldehyde solution and dropwise addition of 17 . 82 ml 1 m sodium hydroxide solution . the reaction mixture was stirred for 16 hours at 70 ° c . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 100 ml ethyl acetate and 50 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 100 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 5j ( 4 . 36 g , pale yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 5j ( 4 . 36 g , 5 . 93 mmol ) was dissolved in 50 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of sodium borohydride ( 0 . 45 g , 11 . 9 mmol ). the reaction mixture was stirred for 30 minutes . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 5k ( 1 . 26 g , white solid ), yield : 28 . 8 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 53 ( dd , 1h ), 7 . 44 ( d , 1h ), 7 . 35 ( d , 1h ), 7 . 31 - 7 . 26 ( m , 5h ), 7 . 25 - 7 . 18 ( m , 8h ), 7 . 04 - 7 . 02 ( m , 2h ), 6 . 90 ( s , 1h ), 6 . 80 ( d , 1h ), 6 . 54 ( d , 1h ), 4 . 90 - 4 . 79 ( m , 4h ), 4 . 73 ( d , 1h ), 4 . 54 ( d , 1h ), 4 . 46 - 4 . 41 ( m , 2h ), 4 . 20 ( t , 1h ), 4 . 10 - 4 . 00 ( m , 5h ), 3 . 88 ( dd , 2h ), 3 . 74 ( d , 1h ), 3 . 15 ( s , 3h ), 3 . 06 - 3 . 00 ( m , 2h ). [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 5k ( 1 . 2 g , 1 . 63 mmol ) was dissolved in 25 ml dichloromethane , followed by dropwise addition of trifluoroacetic acid ( 0 . 5 ml , 6 . 52 mmol ). the reaction mixture was stirred for 1 . 5 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 5m ( 580 mg , white solid ), yield : 50 . 4 %. ms m / z ( esi ): 722 . 3 [ m + 18 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 48 - 7 . 39 ( m , 3h ), 7 . 35 - 7 . 23 ( m , 10h ), 7 . 21 - 7 . 11 ( m , 3h ), 6 . 97 ( s , 1h ), 6 . 90 ( d , 1h ), 6 . 84 ( d , 2h ), 6 . 57 ( d , 1h ), 4 . 83 ( d , 4h ), 4 . 44 ( t , 2h ), 4 . 23 ( m , 2h ), 4 . 07 - 4 . 00 ( m , 3h ), 3 . 95 ( dd , 1h ), 3 . 87 ( d , 1h ), 3 . 79 ( d , 1h ), 3 . 73 - 3 . 69 ( m , 2h ), 3 . 56 ( d , 1h ), 3 . 01 ( t , 2h ). [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 5m ( 100 mg , 0 . 14 mmol ) was dissolved in 5 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 208 mg , 1 . 42 mmol ) and palladium / carbon ( 10 mg , 10 %). the mixture was exchanged with h2 three times and stirred for 1 . 5 hours , filtered and the filtrate was concentrated under reduced pressure . the resulting residue was purified by thin layer chromatography with developing solvent system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -( 2 , 3 - dihydrobenzofuran - 5 - ylmethyl ) phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 5 ( 58 mg , white solid ), yield : 93 . 5 %. ms m / z ( esi ): 435 . 1 [ m + 1 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 47 ( d , 1h ), 7 . 39 - 7 . 35 ( m , 2h ), 7 . 04 ( s , 1h ), 6 . 93 ( d , 1h ), 6 . 62 ( d , 1h ), 4 . 50 ( t , 2h ), 4 . 17 ( d , 1h ), 4 . 03 ( s , 2h ), 3 . 88 - 3 . 79 ( m , 2h ), 3 . 71 - 3 . 65 ( m , 2h ), 3 . 62 - 3 . 56 ( m , 2h ), 3 . 15 ( t , 2h ). n - methyl - n - methoxylamine hydrochloride ( 3 . 41 g , 35 mmol ) was dissolved in 140 ml methylene chloride . triethylamine ( 14 . 6 ml , 105 mmol ) was added and the reaction mixture was stirred for 10 minutes . then the reaction mixture was stirred for 16 hours after 5 - bromo - 2 - chloro - benzoic acid 6a ( 8 . 24 g , 35 mmol ) and bis ( 2 - oxo - 3 - oxazolidinyl ) phosphonic chloride ( 10 . 69 g , 42 mmol ) were added in turn . thereafter , the reaction mixture was extracted with ethyl acetate ( 80 ml × 3 ) after 120 ml water were added . the organic extract was washed with saturated sodium chloride solution ( 60 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound 5 - bromo - 2 - chloro - n - methoxy - n - methyl - benzamide 6b ( 7 . 50 g , pale yellow solid ), yield : 76 . 9 %. ms m / z ( esi ): 280 . 0 [ m + 1 ]; 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 46 - 7 . 44 ( m , 2h ), 7 . 29 - 7 . 26 ( m , 1h ), 3 . 49 ( s , 3h ), 3 . 37 ( s , 3h ). trifluoromethoxybenzene 6c ( 11 . 35 g , 70 mmol ) was dissolved in 3 . 57 ml liquid bromine , followed by addition of iron ( 0 . 24 g ). the reaction mixture was stirred for 16 hours at 100 ° c . 450 ml of dichloromethane were added and the organic extract was washed with 6 m hydrochloric acid ( 140 ml ), 10 % sodium hydrogen sulfite solution ( 140 ml ) and saturated sodium chloride solution ( 140 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound 1 - bromo - 4 -( trifluoromethoxy ) benzene 6d ( 14 . 1 g , yellow solid ), yield : 83 . 8 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 54 - 7 . 50 ( m , 2h ), 7 . 11 - 7 . 09 ( m , 2h ). magnesium ( 0 . 12 g , 5 mmol ) and iodine ( i2 , catalytic ) were added into the reaction flask , followed by dropwise addition of a solution ( 5 ml ) of 1 - bromo - 4 -( trifluoromethoxy ) benzene 6d ( 1 . 2 g , 5 mmol ) in thf . the reaction mixture was refluxed for 1 hour to obtain the title compound 1 - bromo - magnesium - 4 -( trifluoromethoxy ) benzene 6e ( 1 . 32 g ), which was used directly in the next step without purification . 5 - bromo - 2 - chloro - n - methoxy - n - methyl - benzamide 6b ( 5 . 16 g , 18 . 5 mmol ) was dissolved in 50 ml thf , followed by dropwise addition of 1 - bromo - magnesium - 4 -( trifluoromethoxy ) benzene 6e ( 13 . 21 g , 49 . 8 mmol ). the reaction mixture was stirred for 2 hours . thereafter , the reaction mixture was partitioned after 200 ml saturated sodium chloride solution , 200 ml water and 150 ml ethyl acetate were added . the aqueous phase was extracted with ethyl acetate ( 150 ml ) and the organic extract was washed with saturated sodium chloride solution ( 200 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-[ 4 -( trifluoromethoxy ) phenyl ] methanone 6f ( 4 . 08 g , pale yellow solid ), yield : 58 . 1 %. ms m / z ( esi ): 380 . 9 [ m + 1 ]; 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 88 - 7 . 84 ( m , 2h ), 7 . 58 ( dd , 1h ), 7 . 51 ( d , 1h ), 7 . 35 ( d , 1h ), 7 . 32 - 7 . 30 ( m , 2h ). ( 5 - bromo - 2 - chloro - phenyl )-[ 4 -( trifluoromethoxy ) phenyl ] methanone 6f ( 4 . 35 g , 11 . 5 mmol ) was dissolved in 40 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ) and cooled to 0 ° c ., followed by addition of sodium borohydride ( 0 . 87 g , 23 . 0 mmol ) in batch . the reaction mixture was stirred for 30 minutes at 0 ° c . thereafter , the reaction mixture was concentrated under reduced pressure after 10 ml acetone were added . the reaction mixture was partitioned after 100 ml ethyl acetate and 50 ml water were added and the organic extract was washed with saturated sodium chloride solution ( 50 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-[ 4 -( trifluoromethoxy ) phenyl ] methanol 6g ( 4 . 4 g , pale yellow grease ), which was used directly in the next step without purification . 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 80 ( d , 1h ), 7 . 43 - 7 . 40 ( m , 2h ), 7 . 36 ( dd , 1h ), 7 . 20 ( t , 3h ), 6 . 16 ( s , 1h ). ( 5 - bromo - 2 - chloro - phenyl )-[ 4 -( trifluoromethoxy ) phenyl ] methanol 6g ( 4 . 37 g , 11 . 5 mmol ) was dissolved in 35 ml dichloromethane , followed by addition of triethyl silane ( 5 . 49 ml , 34 . 4 mmol ) and dropwise addition of boron trifluoride etherate ( 2 . 9 ml , 22 . 9 mmol ). the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 20 ml saturated sodium bicarbonate solution were added . the aqueous phase was extracted with dichloromethane ( 25 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system c to obtain the title compound 4 - bromo - 1 - chloro - 2 -[[ 4 -( trifluoro - methoxy ) phenyl ] methyl ] benzene 6h ( 3 . 0 g , colourless grease ), yield : 71 . 6 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 33 - 7 . 29 ( m , 2h ), 7 . 26 - 7 . 24 ( m , 1h ), 7 . 21 - 7 . 18 ( m , 2h ), 7 . 15 ( d , 2h ), 4 . 06 ( s , 2h ). 4 - bromo - 1 - chloro - 2 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] benzene 6h ( 2 . 33 g , 6 . 38 mmol ) was dissolved in 40 ml of mixed solution ( thf and n - hexane , v : v = 1 : 3 ) and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli in n - hexane ( 3 . 83 ml , 9 . 57 mmol ). after stirring for 1 . 5 hours at − 78 ° c ., a solution ( 30 ml ) of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 4 . 47 g , 9 . 57 mmol ) in mixed solution ( thf and n - hexane , v : v = 1 : 3 ) was dropwise added before the reaction mixture was stirred for 2 hours at − 78 ° c . a solution ( 32 ml ) of 0 . 6 m methanesulfonic acid in methanol was added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was partitioned after 150 ml of saturated sodium carbonate solution were added . the aqueous phase was extracted with ethyl acetate ( 100 ml × 3 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 61 ( 1 . 38 g , white solid ), yield : 45 . 2 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 61 ( d , 1h ), 7 . 51 ( dd , 1h ), 7 . 40 ( d , 1h ), 7 . 31 - 7 . 29 ( m , 2h ), 7 . 17 ( d , 2h ), 4 . 23 - 4 . 12 ( m , 2h ), 3 . 94 ( d , 1h ), 3 . 86 - 3 . 75 ( m , 2h ), 3 . 95 - 3 . 59 ( m , 2h ), 3 . 47 - 3 . 42 ( m , 1h ), 3 . 10 ( s , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 61 ( 1 . 33 g , 2 . 78 mmol ) was dissolved in 12 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 67 . 93 mg , 0 . 55 mmol ) and tbscl ( 0 . 50 g , 3 . 34 mmol ) in turn . the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 75 ml ethyl acetate and 75 ml water were added . the aqueous phase was extracted with ethyl acetate ( 50 ml × 2 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 6j ( 1 . 60 g , white solid ), yield : 97 . 6 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 55 ( d , 1h ), 7 . 46 ( d , 1h ), 7 . 41 ( d , 1h ), 7 . 26 ( d , 2h ), 7 . 17 ( d , 2h ), 4 . 17 ( s , 2h ), 4 . 04 ( d , 1h ), 3 . 92 - 3 . 88 ( m , 1h ), 3 . 77 ( t , 1h ), 3 . 61 - 3 . 59 ( m , 1h ), 3 . 09 ( s , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 6j ( 1 . 60 g , 2 . 69 mmol ) was dissolved in 15 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 0 . 54 g , 13 . 5 mmol ). then the reaction mixture was warmed and stirred for 15 minutes at room temperature before benzyl bromide ( 1 . 6 ml , 13 . 5 mmol ) was added . after stirring for 16 hours , the reaction mixture was concentrated under reduced pressure after 5 ml methanol were added . then the resulting residue was dissolved in ethyl acetate ( 100 ml ) and washed with water ( 50 ml × 2 ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 6k ( 2 . 32 g , yellow grease ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 6k ( 2 . 32 g , 2 . 69 mmol ) was dissolved in 12 ml methanol , followed by addition of acetyl chloride ( 16 μl , 0 . 40 mmol ). the reaction mixture was stirred for 1 . 5 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 6m ( 1 . 22 g , pale yellow grease ), yield : 60 . 7 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 54 - 7 . 52 ( m , 2h ), 7 . 41 ( d , 1h ), 7 . 32 - 7 . 22 ( m , 13h ), 7 . 18 ( d , 2h ), 7 . 08 - 7 . 04 ( m , 4h ), 4 . 91 - 4 . 85 ( m , 3h ), 4 . 75 ( d , 1h ), 4 . 52 ( d , 1h ), 4 . 17 - 4 . 09 ( m , 3h ), 4 . 00 ( d , 1h ), 3 . 94 - 3 . 83 ( m , 3h ), 3 . 75 - 3 . 69 ( m , 2h ), 3 . 09 ( s , 3h ). oxalyl chloride ( 0 . 21 ml , 2 . 45 mmol ) was dissolved in 5 ml dichloromethane and cooled to − 78 ° c . the mixture was stirred for 15 minutes after 5 ml solution of dimethyl sulfoxide ( 0 . 24 ml , 3 . 26 mmol ) in dichloromethane were added . then 10 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 6m ( 1 . 22 g , 1 . 63 mmol ) in dichloromethane were added before the mixture was stirred for 40 minutes . then the reaction mixture was warmed and stirred for 1 . 5 hours at room temperature after triethylamine ( 1 . 18 ml , 8 . 15 mmol ) was added and partitioned after 10 ml 1 m hydrochloric acid were added . the organic extract was washed with saturated sodium chloride solution ( 10 ml × 2 ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 6n ( 1 . 21 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 6n ( 1 . 21 g , 1 . 63 mmol ) was dissolved in 12 ml 1 , 4 - dioxane , followed by addition of 2 . 65 ml 37 % formaldehyde solution and dropwise addition of 4 . 89 ml 1 m sodium hydroxide . the reaction mixture was stirred for 16 hours at 70 ° c . thereafter , the reaction mixture was concentrated under reduced pressure and was partitioned after 30 ml of saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydro - pyran - 2 - carbaldehyde 6p ( 1 . 27 g , pale yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 6p ( 1 . 27 g , 1 . 63 mmol ) was dissolved in 10 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ) and followed by addition of sodium borohydride ( 0 . 12 g , 3 . 26 mmol ) in batch . the reaction mixture was stirred for 1 . 5 hours . thereafter , the reaction mixture was concentrated under reduced pressure and was partitioned after 30 ml of ethyl acetate were added . the organic extract was washed with saturated sodium chloride solution ( 15 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system e to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 6q ( 400 mg , white solid ), yield : 31 . 5 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 58 ( dd , 1h ), 7 . 54 ( d , 1h ), 7 . 39 ( d , 1h ), 7 . 31 - 7 . 24 ( m , 13h ), 7 . 16 ( d , 2h ), 7 . 11 - 7 . 06 ( m , 4h ), 4 . 92 ( d , 1h ), 4 . 76 ( d , 1h ), 4 . 66 - 4 . 59 ( m , 1h ), 4 . 27 - 4 . 22 ( m , 2h ), 4 . 17 - 4 . 10 ( m , 2h ), 4 . 07 - 4 . 04 ( m , 3h ), 3 . 99 - 3 . 95 ( m , 2h ), 3 . 77 ( d , 1h ), 3 . 65 - 3 . 60 ( m , 2h ), 3 . 35 ( s , 2h ), 3 . 18 ( s , 3h ). [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl -] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 6q ( 400 mg , 0 . 51 mmol ) was dissolved in 10 ml dichloromethane , followed by addition of trifluoroacetic acid ( 0 . 15 ml , 2 . 05 mmol ). the reaction mixture was stirred for 1 . 5 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 6r ( 290 mg , white solid ), yield : 76 . 1 %. 1h nmr ( 400 mhz , dmso - d6 ): δ 7 . 59 ( dd , 1h ), 7 . 50 - 7 . 44 ( m , 2h ), 7 . 34 - 7 . 15 ( m , 17h ), 6 . 83 ( d , 2h ), 5 . 22 ( t , 1h ), 4 . 81 - 4 . 74 ( m , 4h ), 4 . 32 ( d , 1h ), 4 . 11 - 4 . 08 ( m , 3h ), 4 . 07 - 4 . 04 ( m , 1h ), 3 . 93 ( d , 1h ), 3 . 87 ( t , 1h ), 3 . 79 - 3 . 71 ( m , 3h ), 3 . 59 ( dd , 1h ), 3 . 52 ( d , 1h ). [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 6r ( 150 mg , 0 . 20 mmol ) was dissolved in 10 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 0 . 23 ml , 2 mmol ) and palladium / carbon ( 60 mg , 10 %). the mixture was exchanged with h2 three times and stirred for 1 hour . thereafter , the reaction mixture was filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system e to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[[ 4 -( trifluoromethoxy ) phenyl ] methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo -[ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 6 ( 82 mg , white solid ), yield : 86 . 0 %. ms m / z ( esi ): 477 . 1 [ m + 1 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 54 ( d , 1h ), 7 . 46 - 7 . 39 ( m , 2h ), 7 . 30 ( d , 2h ), 7 . 17 ( d , 2h ), 4 . 17 ( d , 3h ), 3 . 86 ( d , 1h ), 3 . 80 ( d , 1h ), 3 . 72 - 3 . 68 ( m , 2h ), 3 . 62 ( dd , 1h ), 3 . 58 ( d , 1h ). 2 , 2 , 2 - trifluoroethanol 7a ( 7 . 2 ml , 100 mmol ) was dissolved in 300 ml dichloromethane , followed by addition of triethylamine ( 28 ml , 200 mmol ). the reaction mixture was cooled to 0 ° c . the reaction mixture was warmed and stirred for 16 hours at room temperature after a solution ( 100 ml ) of p - toluene sulfonyl chloride ( tscl ) ( 30 g , 150 mmol ) in dichloromethane was dropwise added . thereafter , the reaction mixture was extracted with dichloromethane ( 100 ml × 3 ) after 100 ml water were added . the organic extract was washed with saturated sodium chloride solution ( 50 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound 2 , 2 , 2 - trifluoroethyl 4 - methylbenzenesulfonate 7b ( 25 g , colourless liquid ), yield : 98 . 4 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 88 - 7 . 76 ( m , 2h ), 7 . 44 - 7 . 33 ( m , 2h ), 4 . 35 ( d , 2h ), 2 . 47 ( s , 3h ). 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ] phenol 7c ( 14 . 5 g , 48 . 7 mmol , prepared according to the method in wo2009026537 ) was dissolved in 300 ml dmf , followed by addition of cesium carbonate ( 31 . 7 g , 97 . 5 mmol ). the reaction mixture was stirred for 10 minutes . the reaction mixture was stirred for 8 hours at 80 ° c . after 2 , 2 , 2 - trifluoroethyl - 4 - methylbenzenesulfonate 7b ( 12 . 4 g , 48 . 7 mmol ) was added . thereafter , the reaction mixture was filtered and washed with a small amount of ethyl acetate before the filtrate was concentrated under reduced pressure . the resulting residue was partitioned after 100 ml water and 50 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 100 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 100 ml ), combined and concentrated . the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound 4 - bromo - 1 - chloro - 2 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] benzene 7d ( 7 . 26 g , white solid ), yield : 39 . 2 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 32 ( s , 1h ), 7 . 30 - 7 . 24 ( m , 2h ), 7 . 21 - 7 . 14 ( m , 2h ), 6 . 98 - 6 . 87 ( m , 2h ), 4 . 38 ( d , 2h ), 4 . 06 ( s , 2h ). 4 - bromo - 1 - chloro - 2 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] benzene 7d ( 6 . 15 g , 16 . 2 mmol ) was dissolved in 150 ml of mixed solution ( thf and n - hexane , v : v = 2 : 3 ) and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli in n - hexane ( 10 ml , 24 . 3 mmol ). the reaction was stirred for 1 hour at − 78 ° c . before a solution ( 35 ml ) of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyl - oxymethyl ) tetrahydropyran - 2 - one 2f ( 8 . 32 g , 17 . 8 mmol ) in n - hexane was dropwise added . then , the reaction mixture was stirred for 2 hours at − 78 ° c . before 50 ml methanol and 3 . 2 ml methylsulfonic acid were added . the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure and was partitioned after 30 ml saturated sodium bicarbonate solution and 10 ml water were added . the aqueous phase was extracted with ethyl acetate ( 100 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 20 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 7e ( 3 . 93 g , white solid ), yield : 49 . 2 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 57 ( d , 1h ), 7 . 49 ( dd , 1h ), 7 . 38 ( d , 1h ), 7 . 18 ( d , 2h ), 6 . 99 - 6 . 88 ( m , 2h ), 4 . 49 ( q , 2h ), 4 . 19 - 4 . 01 ( m , 3h ), 3 . 99 - 3 . 91 ( m , 1h ), 3 . 89 - 3 . 71 ( m , 2h ), 3 . 66 - 3 . 55 ( m , 1h ), 3 . 49 - 3 . 39 ( m , 1h ), 3 . 14 - 3 . 04 ( s , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 7e ( 3 . 8 g , 7 . 71 mmol ) was dissolved in 100 ml dmf , followed by addition of dmap ( 188 mg , 1 . 54 mmol ), tbscl ( 1 . 39 g , 9 . 25 mmol ) and pyridine ( 50 ml ) in turn , and the reaction mixture was stirred for 36 hours . thereafter , the reaction mixture was concentrated under reduced pressure and partitioned after 150 ml water were added . the aqueous phase was extracted with ethyl acetate ( 100 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxy - methyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 7f ( 2 . 94 g , yellow grease ), yield : 62 . 8 %. 1h nmr ( 400 mhz , dmso - d6 ): δ 7 . 94 ( s , 2h ), 7 . 45 ( d , 1h ), 7 . 40 ( d , 1h ), 7 . 35 - 7 . 28 ( m , 1h ), 7 . 17 - 7 . 05 ( m , 2h ), 7 . 01 - 6 . 90 ( m , 2h ), 5 . 00 ( d , 1h ), 4 . 84 - 4 . 74 ( m , 2h ), 4 . 68 ( q , 2h ), 4 . 11 - 3 . 87 ( m , 3h ), 3 . 73 ( dd , 1h ), 3 . 60 - 3 . 46 ( m , 1h ), 3 . 42 ( ddd , 1h ), 3 . 14 ( td , 1h ), 2 . 92 ( s , 3h ), 0 . 05 - 0 . 02 ( m , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 7f ( 2 . 90 g , 4 . 78 mmol ) was dissolved in 70 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 955 mg , 23 . 9 mmol ). the reaction mixture was warmed and stirred for 1 hour at room temperature before benzyl bromide ( 3 . 0 ml , 23 . 9 mmol ) was added . after stirring for 3 hours , 5 ml methanol and 10 ml water were added . the reaction mixture was partitioned after 100 ml water and 30 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 50 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phen yl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 7g ( 4 . 60 g , pale yellow liquid ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 7g ( 4 . 19 g , 4 . 78 mmol ) was dissolved in 30 ml methanol , followed by addition of acetyl chloride ( 51 μl , 0 . 72 mmol ). the reaction mixture was stirred for 1 hour . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 7h ( 1 . 1 g , white grease ), yield : 30 . 1 %. 1h nmr ( 400 mhz , dmso - d6 ): δ 7 . 55 - 7 . 43 ( m , 2h ), 7 . 39 - 7 . 28 ( m , 6h ), 7 . 28 - 7 . 16 ( m , 9h ), 7 . 11 - 7 . 03 ( m , 1h ), 7 . 01 ( dd , 2h ), 6 . 90 ( d , 2h ), 4 . 91 - 4 . 73 ( m , 4h ), 4 . 73 - 4 . 58 ( m , 3h ), 4 . 42 ( d , 1h ), 4 . 17 - 3 . 87 ( m , 4h ), 3 . 83 - 3 . 62 ( m , 4h ), 3 . 53 ( dd , 1h ), 3 . 24 ( d , 1h ), 3 . 08 - 2 . 86 ( m , 3h ). oxalyl chloride ( 0 . 16 ml , 1 . 87 mmol ) was dissolved in 5 ml dichloromethane and cooled to − 78 ° c ., followed by dropwise addition of dimethyl sulfoxide ( 0 . 2 ml , 2 . 88 mmol ) in dichloromethane ( 3 ml ). the reaction mixture was stirred for 15 minutes , before 10 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 7h ( 1 . 10 g , 1 . 44 mmol ) in dichloromethane were added and stirred for 40 minutes . then the reaction mixture was warmed and stirred for 3 hours at room temperature after triethylamine ( 1 . 0 ml , 7 . 21 mmol ) was dropwise added . thereafter , the reaction mixture was partitioned after 5 ml 1 m hydrochloric acid were added , the aqueous phase was extracted with ethyl acetate ( 10 ml × 2 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 7i ( 1 . 06 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 71 ( 1 . 06 g , 1 . 39 mmol ) was dissolved in 20 ml 1 , 4 - dioxane , followed by addition of 2 . 3 ml 37 % formaldehyde solution and 4 ml 2 . 9 m sodium hydroxide . the reaction mixture was stirred for 25 hours at 70 ° c . thereafter , the reaction mixture was concentrated under reduced pressure before 20 ml water and 10 ml saturated sodium chloride solution were added . the reaction mixture was extracted with ethyl acetate ( 30 ml × 3 ). the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ]- methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 7j ( 1 . 1 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 7j ( 1 . 1 g , 1 . 39 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 1 : 2 ), followed by addition of sodium borohydride ( 106 mg , 2 . 78 mmol ) in batch . the reaction mixture was stirred for 30 minutes before 20 ml of water , then 30 ml of water were added . the reaction mixture was extracted with ethyl acetate ( 50 ml × 3 ). the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 7k ( 100 mg , yellow grease ), yield : 9 . 1 %. [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 7k ( 100 mg , 0 . 13 mmol ) was dissolved in 10 ml dichloromethane , followed by addition of 0 . 1 ml trifluoroacetic acid . the reaction mixture was stirred for 1 hour . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 7m ( 22 mg , white solid ), yield : 22 . 9 %. ms m / z ( esi ): 778 . 3 [ m + 18 ]. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 7m ( 20 mg , 0 . 03 mmol ) was dissolved in 10 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 31 μl , 0 . 27 mmol ) and palladium / carbon ( 20 mg , 10 %) in turn . the mixture was exchanged with h2 three times and was stirred for 2 hours . thereafter , the reaction mixture was filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by thin layer chromatography with developing solvent system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 , 2 - trifluoroethoxy ) phenyl ] methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 7 ( 9 mg , white solid ), yield : 69 . 2 %. ms m / z ( esi ): 491 . 1 [ m + 1 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 48 ( m , 1h ), 7 . 40 - 7 . 38 ( m , 2h ), 7 . 18 - 7 . 16 ( d , 2h ), 6 . 93 - 6 . 91 ( d , 2h ), 4 . 51 - 4 . 45 ( q , 2h ), 4 . 17 - 4 . 15 ( d , 1h ), 4 . 08 ( s , 2h ), 3 . 81 - 3 . 78 ( d , 1h ), 3 . 78 - 3 . 71 ( d , 1h ), 3 . 69 - 3 . 67 ( m , 2h ), 3 . 62 - 3 . 57 ( m , 2h ). 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 1 - ethoxy - 2 - fluoro - benzene 4e ( 31 . 7 g , 92 . 3 mmol ) was dissolved in 300 ml dichloromethane , followed by addition of boron tribromide ( 11 . 4 ml , 120 mmol ) in an ice bath , then the reaction mixture was warmed and stirred for 4 hours . thereafter , the reaction mixture was extracted with ethyl acetate ( 100 ml × 4 ) after 300 ml saturated sodium carbonate solution was dropwise added slowly . the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluorophenol 8a ( 28 . 1 g , white solid ), yield : 96 . 7 %. 1h nmr ( 400 mhz , cdcl 3 ): δ 7 . 36 - 7 . 18 ( m , 3h ), 7 . 01 - 6 . 80 ( m , 3h ), 5 . 08 ( br , 1h ), 3 . 99 ( s , 2h ). 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluoro - phenol 8a ( 10 . 0 g , 31 . 75 mmol ) was dissolved in 150 ml thf , followed by addition of triphenylphosphine ( 16 . 6 g , 63 . 5 mmol ) and azodicarboxylic acid diisopropyl ester ( 12 . 6 ml , 63 . 5 mmol ). the reaction mixture was stirred for 30 minutes . the reaction mixture was stirred for 18 hours after 3 ml cd3od were added . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was recrystallized with petroleum ether , filtered , and collected as a product . the product was re - dissolved in 50 ml methanol before 2 ml hydrogen peroxide were added . followed by stirring for 1 minute , the reaction mixture were partitioned after 5 g sodium thiosulfate , 40 ml water and 50 ml ethyl acetate were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 30 ml ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the residue was purified by silica gel chromatography with elution system d to obtain the title compound 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluoro - 1 -( trideuteriomethoxy ) benzene 8b ( 8 . 2 g , white solid ), yield : 77 . 4 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 37 - 7 . 32 ( m , 1 h ), 7 . 32 - 7 . 28 ( m , 2 h ), 6 . 99 - 6 . 89 ( m , 3 h ), 4 . 02 ( s , 2 h ). 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluoro - 1 -( trideuteriomethoxy ) benzene 8b ( 8 . 2 g , 24 . 6 mmol ) was dissolved in 150 ml of mixed solution ( thf and n - hexane , v : v = 2 : 3 ) and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli ( 14 . 8 ml , 36 . 9 mmol ) in n - hexane . after stirring for 2 hours at − 78 ° c ., a solution ( 40 ml ) of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetra - hydropyran - 2 - one 2f ( 12 . 6 g , 27 . 1 mmol ) in n - hexane was dropwise added . then , the reaction mixture was stirred for 3 hours at − 78 ° c . 40 ml methanol and 4 . 79 ml methanesulfonic acid were added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure and was partitioned after 40 ml saturated sodium bicarbonate solution , 100 ml ethyl acetate and 100 ml water were added . the aqueous phase was extracted with ethyl acetate ( 50 ml × 4 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxytetrahydropyran - 3 , 4 , 5 - triol 8c ( 8 . 2 g , white solid ), yield : 83 . 6 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 47 - 7 . 29 ( m , 3 h ), 6 . 93 - 6 . 78 ( m , 3 h ), 4 . 08 - 3 . 98 ( m , 2 h ), 3 . 98 - 3 . 78 ( m , 5 h ), 3 . 73 ( d , 1 h ), 3 . 47 ( s , 6 h ). ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 8c ( 9 . 2 g , 20 . 6 mmol ) was dissolved in 80 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 502 mg , 4 . 11 mmol ) and tert - butyl - dimethyl - chloro - silane ( 3 . 72 g , 24 . 7 mmol ). the reaction mixture was stirred for 24 hours and concentrated under reduced pressure , and was partitioned after 80 ml ethyl acetate and 80 ml water were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 8d ( 2 . 4 g , yellow grease ), yield : 20 . 9 %. ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 8d ( 2 . 4 g , 4 . 29 mmol ) was dissolved in 70 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 857 mg , 21 . 4 mmol ). then the reaction mixture was warmed to room temperature and stirred for 1 hour . thereafter , benzyl bromide ( 2 . 56 ml , 21 . 4 mmol ) was added before the mixture was stirred for 3 hours . 5 ml methanol and 100 ml water were added before the reaction mixture was extracted with ethyl acetate ( 50 ml × 3 ). the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - 1 - silane 8e ( 3 . 56 g , yellow solid ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 8e ( 3 . 56 , 4 . 29 mmol ) was dissolved in 30 ml methanol and stirred for 4 hours after addition of acetyl chloride ( 95 . 5 μl , 1 . 34 mmol ). thereafter , the reaction mixture was concentrated under reduced pressure . the reaction mixture was extracted with ethyl acetate ( 30 ml × 3 ) after 30 ml water were added . the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 8f ( 2 . 2 g , yellow solid ), yield : 73 . 3 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 42 - 7 . 27 ( m , 13 h ), 7 . 24 - 7 . 14 ( m , 3 h ), 6 . 98 ( d , 2 h ), 6 . 89 - 6 . 72 ( m , 3 h ), 4 . 96 - 4 . 87 ( m , 3 h ), 4 . 71 - 4 . 67 ( m , 1 h ), 4 . 51 ( d , 1 h ), 4 . 18 ( t , 1 h ), 4 . 07 ( d , 1 h ), 3 . 95 - 3 . 84 ( m , 3 h ), 3 . 83 - 3 . 77 ( m , 1 h ), 3 . 76 - 3 . 64 ( m , 2 h ), 3 . 30 ( d , 1 h ), 3 . 07 ( s , 3 h ). oxalyl chloride ( 0 . 34 ml , 3 . 93 mmol ) was dissolved in 5 ml dichloromethane and cooled to − 78 ° c . a solution ( 10 ml ) of dimethyl sulfoxide ( 0 . 43 ml , 6 . 04 mmol ) in dichloromethane was added before the mixture was stirred for 15 minutes . then 15 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 8f ( 2 . 2 g , 3 . 02 mmol ) in methylene chloride were added before the mixture was stirred for 45 minutes . thereafter , triethylamine ( 2 . 1 ml , 15 . 1 mmol ) was added before the mixture was warmed to room temperature and stirred for 2 . 5 hours . 5 ml 1 m hydrochloric acid solution were added before the mixture was extracted with dichloromethane ( 15 ml × 2 ). the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 8g ( 2 . 1 g , yellow liquid ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy )- phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 8g ( 2 . 1 g , 2 . 94 mmol ) was dissolved in 50 ml 1 , 4 - dioxane , followed by addition of formaldehyde solution ( 5 . 4 ml , 72 . 2 mmol ) and 3 . 94 ml 3 m sodium hydroxide . the reaction mixture was stirred for 6 hours at 50 ° c . thereafter , the reaction mixture was extracted with ethyl acetate ( 20 ml × 3 ) after 20 ml of water were added . the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 8h ( 2 . 5 g , yellow liquid ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 8h ( 2 . 5 g , 3 . 36 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 1 : 2 ), followed by addition of sodium borohydride ( 269 mg , 6 . 72 mmol ) in batch . the reaction mixture was stirred for 2 hours , then quenched with 40 ml water . the reaction mixture was extracted with ethyl acetate ( 40 ml × 3 ). the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 81 ( 350 mg , yellow liquid ), yield : 15 . 9 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 41 - 7 . 19 ( m , 16 h ), 7 . 04 ( dd , 2 h ), 6 . 86 - 6 . 76 ( m , 3 h ), 5 . 01 - 4 . 87 ( m , 3 h ), 4 . 71 - 4 . 59 ( m , 2 h ), 4 . 44 - 4 . 31 ( m , 2 h ), 4 . 06 - 3 . 92 ( m , 3 h ), 3 . 87 - 3 . 76 ( m , 3 h ), 3 . 68 ( d , 1 h ), 3 . 25 ( d , 1 h ), 3 . 07 ( s , 3 h ). [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 8i ( 350 mg , 0 . 47 mmol ) was dissolved in 20 ml dichloromethane , followed by 0 . 5 ml addition of trifluoroacetic acid . the reaction mixture was stirred for 2 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 8j ( 200 mg , colourless liquid ), yield : 59 . 7 %. ms m / z ( esi ): 731 . 3 [ m + 18 ]. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 8j ( 190 mg , 0 . 27 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 391 mg , 2 . 66 mmol ) and palladium / carbon ( 20 mg , 10 %) in turn . the mixture was exchanged with h2 three times and stirred for 3 hours . thereafter , the reaction mixture was filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system f to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( trideuteriomethoxy ) phenyl ] methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 8 ( 74 mg , white solid ), yield : 62 . 7 %. ms m / z ( esi ): 461 . 1 [ m + 18 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 59 - 7 . 45 ( m , 1 h ), 7 . 45 - 7 . 33 ( m , 2 h ), 7 . 06 - 6 . 84 ( m , 3 h ), 4 . 16 ( d , 1 h ), 4 . 05 ( d , 2 h ), 3 . 93 - 3 . 76 ( m , 2 h ), 3 . 75 - 3 . 52 ( m , 4 h ). 2 - iodothiophene ( 1 . 05 g , 5 mmol ) was dissolved in 6 ml of mixed solution ( dimethyl ether and water , v : v = 2 : 1 ), followed by addition of 4 - fluorophenylboronic acid 9a ( 700 mg , 5 mmol ), potassium carbonate ( 1 . 38 g , 10 mmol ) and tetrakis ( triphenyl phosphine ) palladium ( 173 mg , 0 . 15 mmol ). the mixture was microwaved for 30 minutes at 100 ° c . thereafter , the reaction mixture was extracted with ethyl acetate ( 20 ml × 3 ) after 10 ml water were added . the organic extract was washed with saturated sodium chloride solution ( 20 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system c to obtain the title compound 2 -( 4 - fluorophenyl ) thiophene 9b ( 767 mg , white solid ), yield : 86 . 1 %. alcl3 ( 1 . 5 g , 11 mmol ) was dissolved in 10 ml methylene chloride and cooled to − 10 ° c ., followed by addition of 5 - bromo - 2 - chloro - benzoyl chloride 2a ( 2 . 54 g , 10 mmol ) and 2 -( 4 - fluorophenyl ) thiophene 9b ( 1 . 78 g , 10 mmol ). the reaction mixture was stirred for 30 minutes and then warmed to room temperature and stirred for another 16 hours . thereafter , the reaction mixture was cooled to − 10 ° c . the reaction mixture was extracted with ethyl acetate ( 50 ml × 2 ) after a small amount of water and 20 ml 1 m hydrochloric acid were added . the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methanone 9c ( 1 . 5 g , yellow solid ), yield : 37 . 9 %. ( 5 - bromo - 2 - chloro - phenyl )-[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methanone 9c ( 3 . 7 g , 10 . 4 mmol ) was dissolved in 40 ml thf and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli in n - hexane ( 5 ml , 12 . 5 mmol ). the reaction mixture was stirred for 1 hour at − 78 ° c . 30 ml solution of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 4 . 85 g , 10 . 4 mmol ) in thf were added before the reaction mixture was stirred for 2 hours at − 78 ° c . a solution ( 60 ml ) of 0 . 6 m methanesulfonic acid in methanol was added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure and extracted with ethyl acetate ( 40 ml × 3 ) after 30 ml saturated sodium carbonate solution were added . the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 9d ( 1 . 8 g , orange solid ), yield : 36 . 7 %. ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 9d ( 1 . 8 g , 3 . 8 mmol ) was dissolved in 20 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 93 mg , 0 . 76 mmol ) and tbscl ( 686 mg , 4 . 55 mmol ) in turn . the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure , dissolved in 30 ml ethyl acetate and was partitioned after 30 ml water were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tertbutyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 9e ( 2 . 0 g , orange solid ), yield : 89 . 7 %. ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 9e ( 2 . 0 g , 3 . 4 mmol ) was dissolved in 20 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 680 mg , 17 mmol ). the reaction mixture was warmed to room temperature and stirred for 30 minutes . thereafter , benzyl bromide ( 2 . 0 ml , 17 mmol ) was added before the mixture was stirred for 16 hours . the reaction mixture was concentrated under reduced pressure after 10 ml methanol were added and was partitioned after 30 ml ethyl acetate and 30 ml water were added . the aqueous phase was extracted with ethyl acetate ( 20 ml × 3 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 9f ( 2 . 9 g , yellow grease ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 9f ( 2 . 9 g , 3 . 37 mmol ) was dissolved in 20 ml methanol , followed by addition of acetyl chloride ( 38 μl , 0 . 5 mmol ). the reaction mixture was stirred for 2 hours and was partitioned after 30 ml ethyl acetate and 30 ml water were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 2 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and then the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 9g ( 1 . 9 g , yellow solid ), yield : 76 . 0 %. oxalyl chloride ( 0 . 27 ml , 3 . 12 mmol ) was dissolved in 8 ml dichloromethane and cooled to − 78 ° c . the reaction mixture was stirred for 15 minutes before 4 ml solution of dimethyl sulfoxide ( 0 . 36 ml , 5 . 04 mmol ) in dichloromethane were added . then 8 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 9g ( 1 . 8 g , 2 . 4 mmol ) in dichloromethane were dropwise added . the reaction mixture was stirred for 30 minutes . then triethylamine ( 1 . 66 ml , 12 mmol ) was added before the reaction mixture was warmed to room temperature and stirred for 1 hour . thereafter , the reaction mixture was partitioned after 12 ml 1 m hydrochloric acid were added , the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 9h ( 1 . 8 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 9h ( 1 . 53 g , 2 . 1 mmol ) was dissolved in 15 ml 1 , 4 - dioxane , followed by addition of 3 . 4 ml 37 % formaldehyde solution and 6 . 3 ml 1 m sodium hydroxide . the reaction mixture was stirred for 16 hour at 70 ° c ., and was partitioned after 50 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 50 ml × 3 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 91 ( 2 . 0 g , pale yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 91 ( 2 . 0 g , 2 . 1 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 1 : 20 ), followed by addition of sodium borohydride ( 238 mg , 6 . 3 mmol ) in batch . the reaction mixture was stirred for 1 hour . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution systems b and e to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 9j ( 420 mg , pale yellow solid ), yield : 25 . 8 %. 1h nmr ( 400 mhz , cd3od ): δ 7 . 55 ( d , 2h ), 7 . 48 - 7 . 45 ( m , 3h ), 7 . 32 - 7 . 28 ( m , 5h ), 7 . 25 - 7 . 21 ( m , 9h ), 7 . 16 ( d , 2h ), 7 . 07 - 7 . 03 ( m , 3h ), 6 . 63 ( d , 1h ), 4 . 91 ( d , 1h ), 4 . 83 ( d , 1h ), 4 . 75 ( d , 1h ), 4 . 54 ( d , 1h ), 4 . 26 - 4 . 17 ( m , 2h ), 4 . 10 - 4 . 04 ( m , 5h ), 3 . 94 ( d , 1h ), 3 . 78 ( d , 1h ), 3 . 36 ( d , 1h ), 3 . 26 ( s , 3h ), 2 . 34 ( s , 3h ). [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 9j ( 130 mg , 0 . 17 mmol ) was dissolved in 10 ml methanol , followed by addition of a solution ( 4 ml ) of 2 m hydrochloric in ethyl acetate and palladium / carbon ( 260 mg , 20 %). the mixture was exchanged with h2 three times and stirred for 16 hours . thereafter , the reaction mixture was filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by hplc to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 3 -[[ 5 -( 4 - fluorophenyl )- 2 - thienyl ] methyl ]- 4 - methyl - phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 9 ( 11 mg , white solid ), yield : 13 . 8 %. ms m / z ( esi ): 473 . 2 [ m + 1 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 57 - 7 . 56 ( m , 2h ), 7 . 48 ( d , 1h ), 7 . 39 - 7 . 37 ( m , 1h ), 7 . 19 ( d , 1h ), 7 . 15 ( d , 1h ), 7 . 10 - 7 . 06 ( m , 2h ), 6 . 67 ( d , 1h ), 4 . 18 ( d , 3h ), 3 . 88 - 3 . 81 ( m , 2h ), 3 . 73 - 3 . 68 ( m , 2h ), 3 . 65 - 3 . 62 ( m , 2h ), 2 . 33 ( s , 3h ). 4 [( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluoro - phenol 8a ( 6 . 0 g , 19 . 05 mmol ) was dissolved in 100 ml thf , followed by addition of triphenylphosphine ( 9 . 98 g , 38 . 1 mmol ) and azodicarboxylic acid diisopropyl ester ( 7 . 7 ml , 38 . 1 mmol ). the reaction mixture was stirred for 30 minutes . 2 . 5 ml ethanol - d6 were added before the reaction mixture was stirred for 18 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was recrystallized with petroleum ether , filtered and collected as a filter cake . the filter cake was dissolved in 50 ml methanol before 2 ml of hydrogen peroxide were added . after stirring for 1 minute , the mixture was partitioned after 5 g sodium thiosulfate , 40 ml water and 50 ml ethyl acetate were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 30 ml ), combined , dried over anhydrous magnesium sulfate and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluoro - 1 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) benzene 10a ( 5 . 78 g , colourless liquid ), yield : 86 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 38 - 7 . 24 ( m , 3h ), 6 . 99 - 6 . 83 ( m , 3h ), 4 . 02 ( s , 2h ). 4 -[( 5 - bromo - 2 - chloro - phenyl ) methyl ]- 2 - fluoro - 1 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) benzene 10a ( 5 . 78 g , 16 . 6 mmol ) was dissolved in 125 ml of mixed solution ( thf and n - hexane , v : v = 2 : 3 ) and cooled to − 78 ° c ., followed by dropwise addition of a solution of nbuli ( 8 . 53 g , 18 . 26 mmol ) in n - hexane . after stirring for 2 hours at − 78 ° c ., a solution ( 40 ml ) of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxy - methyl ) tetrahydropyran - 2 - one 2f ( 12 . 6 g , 27 . 1 mmol ) in n - hexane was dropwise added . the reaction mixture was stirred for 3 hours at − 78 ° c . 40 ml methanol and 4 . 79 ml methanesulfonic acid were added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was concentrated under reduced pressure and was partitioned after 40 ml saturated sodium bicarbonate solution , 100 ml ethyl acetate and 100 ml water were added . the aqueous phase was extracted with ethyl acetate ( 50 ml × 4 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 10b ( 1 . 6 g , yellow solid ), yield : 20 . 9 %. ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 10b ( 1 . 6 g , 3 . 47 mmol ) was dissolved in 40 ml pyridine , followed by addition of 4 - dimethylamino pyridine ( 64 mg , 0 . 52 mmol ) and tbscl ( 0 . 57 g , 3 . 8 mmol ) in turn . the reaction mixture was stirred for 24 hours and concentrated under reduced pressure and was partitioned after 50 ml ethyl acetate and 50 ml water were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 10c ( 1 . 7 g , yellow liquid ), yield : 85 %. ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 10c ( 1 . 7 g , 2 . 90 mmol ) was dissolved in 50 ml dmf and cooled to 0 ° c ., followed by addition of 60 % nah ( 620 mg , 14 . 0 mmol ). then the reaction mixture was warmed to room temperature and stirred for 1 hour . thereafter , benzyl bromide ( 1 . 90 ml , 14 mmol ) was added before the mixture was stirred for 3 hours . the reaction mixture was extracted with ethyl acetate ( 50 ml × 3 ) after 5 ml methanol and 100 ml water were added . the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 10d ( 2 . 45 g , yellow liquid ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 10d ( 2 . 45 g , 2 . 90 mmol ) was dissolved in 30 ml methanol , followed by addition of acetyl chloride ( 50 μl , 0 . 4 mmol ). the reaction mixture was stirred for 4 hours . thereafter , the reaction mixture was concentrated under reduced pressure before 30 ml water were added . then the resulting residue was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and then the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 10e ( 1 . 2 g , yellow liquid ), yield : 56 . 8 %. oxalyl chloride ( 0 . 36 ml , 3 . 93 mmol ) was dissolved in 5 ml dichloromethane and cooled to − 78 ° c . 10 ml solution of dimethyl sulfoxide ( 0 . 35 ml , 4 . 92 mmol ) in dichloromethane were added and stirred for 15 minutes , then 15 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 10e ( 1 . 2 g , 1 . 64 mmol ) in dichloromethane were added and stirred for 45 minutes . then triethylamine ( 1 . 2 ml , 8 . 2 mmol ) was added before the reaction mixture was warmed and stirred for 2 . 5 hours at room temperature . thereafter , the reaction mixture was extracted with dichloromethane ( 15 ml × 2 ) after 5 ml 1 m hydrochloric acid were added . the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 10f ( 1 . 2 g , yellow liquid ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 10f ( 1 . 2 g , 1 . 64 mmol ) was dissolved in 40 ml 1 , 4 - dioxane , followed by addition of formaldehyde solution ( 2 . 2 ml , 7 . 54 mmol ), potassium hydroxide ( 0 . 27 g , 4 . 92 mmol ) and benzyl alcohol ( 177 mg , 1 . 64 mmol ). the reaction mixture was stirred for 6 hours at 50 ° c . thereafter , the reaction mixture was extracted with ethyl acetate ( 20 ml × 3 ) after 20 ml water were added . the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydro - oxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 10g ( 0 . 64 g , yellow liquid ), which was used directly in the next step without purification . [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 10g ( 640 mg , 0 . 83 mmol ) was dissolved in 20 ml methylene chloride , followed by dropwise addition of trifluoroacetic acid ( 0 . 5 ml ). the mixture was stirred for 2 hours . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system d to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 10h ( 300 mg , pale yellow solid ), yield : 41 . 0 %. ms m / z ( esi ): 747 . 3 [ m + 18 ]. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 10h ( 300 mg , 0 . 41 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of 1 , 2 - dichlorobenzene ( 600 mg , 4 . 10 mmol ) and palladium / carbon ( 30 mg , 10 %) in turn . the mixture was exchanged with h2 three times and stirred for 3 hours . thereafter , the reaction mixture was filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by reversed - phase column chromatography with elution system f to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[[ 3 - fluoro - 4 -( 1 , 1 , 2 , 2 , 2 - pentadeuterioethoxy ) phenyl ] methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 10 ( 134 mg , white solid ), yield : 70 . 0 %. ms m / z ( esi ): 477 . 1 [ m + 18 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 49 ( d , 1h ), 7 . 46 - 7 . 30 ( m , 2h ), 7 . 05 - 6 . 81 ( m , 3h ), 4 . 17 ( d , 1h ), 4 . 06 ( s , 2h ), 3 . 86 ( d , 1h ), 3 . 79 ( s , 1h ), 3 . 75 - 3 . 51 ( m , 4h ). ( 5 - bromo - 2 - chloro - phenyl )-( 4 - ethoxy - 3 - fluoro - phenyl ) methanone 4c ( 15 . 0 g , 41 . 96 mmol ) was dissolved in 120 ml thf , followed by addition of alcl3 ( 12 . 3 g , 92 mmol ) and addition of sodium borodeuteride ( 7 . 00 g , 167 . 2 mmol ) in batch and 150 ml trifluoroacetic acid in an ice bath . the reaction mixture was warmed to room temperature and stirred for 2 hours . thereafter , the reaction was quenched with 15 ml acetone and the reaction mixture was concentrated under reduced pressure . the residue was dissolved in 150 ml ethyl acetate and washed with saturated sodium chloride solution ( 50 ml × 2 ). the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )- deuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methanol 11a ( 15 . 6 g , orange grease ), which was used directly in the next step without purification . ( 5 - bromo - 2 - chloro - phenyl )- deuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methanol 11a ( 6 . 4 g , 18 . 3 mmol ) was dissolved in 40 ml trifluoroacetic acid , followed by addition of sodium borodeuteride ( 1 . 6 g , 38 mmol ). the reaction mixture was stirred for 3 hours . thereafter , the mixture was quenched with 50 ml saturated sodium bicarbonate solution and partitioned . the aqueous phase was extracted with ethyl acetate ( 100 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound 4 -[( 5 - bromo - 2 - chloro - phenyl )- dideuterio - methyl ]- 1 - ethoxy - 2 - fluoro - benzene 11b ( 4 . 3 g , colourless grease ), yield : 67 . 8 %. 1h nmr ( 400 mhz , cdcl 3 ): δ 7 . 43 - 7 . 23 ( m , 3h ), 7 . 03 - 6 . 85 ( m , 3h ), 4 . 21 - 4 . 08 ( m , 2h ), 1 . 54 - 1 . 44 ( m , 3h ). 4 -[( 5 - bromo - 2 - chloro - phenyl )- dideuterio - methyl ]- 1 - ethoxy - 2 - fluoro - benzene 11b ( 5 . 00 g , 16 . 4 mmol ) was dissolved in a mixed solution of 50 ml thf and 75 ml n - hexane and cooled to − 78 ° c ., followed by dropwise addition of nbuli ( 9 . 00 ml , 21 . 6 mmol ). after stirring for 2 hours at − 78 ° c ., a solution ( 30 ml ) of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 7 . 4 g , 15 . 8 mmol ) in n - hexane was added and the reaction mixture was stirred for 2 hours at − 78 ° c . 3 . 5 ml methanesulfonic acid and 40 ml methanol were added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the mixture was quenched with 100 ml saturated sodium carbonate solution and concentrated under reduced pressure . the residue was dissolved after 50 ml saturated sodium chloride solution were added and extracted with ethyl acetate ( 100 ml × 3 ). the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluorophenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 11c ( 2 . 4 g , colourless liquid ), yield : 36 . 4 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 57 - 7 . 34 ( m , 3h ), 7 . 04 - 6 . 81 ( m , 3h ), 4 . 20 - 3 . 80 ( m , 8h ), 3 . 52 ( s , 3h ), 2 . 54 ( br . s ., 4h ), 1 . 41 - 1 . 24 ( m , 3h ). ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 11c ( 2 . 4 g , 5 . 24 mmol ) was dissolved in 40 ml dichloromethane , followed by addition of dmap ( 97 mg , 0 . 79 mmol ), imidazole ( 1 . 07 mg , 15 . 7 mmol ) and tbscl ( 0 . 87 g , 5 . 76 mmol ) in turn . the reaction mixture was stirred for 16 hours . thereafter , the reaction mixture was concentrated under reduced pressure . the reaction mixture was washed with saturated copper sulfate solution ( 50 ml × 3 ) after 200 ml ethyl acetate were added . the organic extracts were combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 11d ( 2 . 87 g , pale yellow solid ), which was used directly in the next step without purification . ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 11d ( 2 . 87 g , 5 . 02 mmol ) was dissolved in 60 ml dmf , followed by addition of 60 % nah ( 1 . 00 g , 25 . 1 mmol ) in an ice bath . then the reaction mixture was warmed to room temperature and stirred for 40 minutes , before benzyl bromide ( 3 . 00 ml , 25 . 1 mmol ) was added and stirred for 3 hours . the reaction was quenched with 20 ml methanol and the reaction mixture was concentrated under reduced pressure . the resulting residue was dissolved in 200 ml ethyl acetate and 50 ml water and partitioned . the aqueous phase was extracted with 50 ml ethyl acetate . the organic extracts were washed with 50 ml water and 50 ml saturated sodium chloride solution in turn , and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluorophenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 11e ( 3 . 00 g , yellow grease ), yield : 99 . 8 %. [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluorophenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 11e ( 4 . 22 g , 5 . 02 mmol ) was dissolved in 30 ml methanol and stirred for 1 hour after addition of acetyl chloride ( 0 . 05 ml , 0 . 75 mmol ). thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluorophenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 11f ( 1 . 45 g , yellow grease ), yield : 55 . 0 %. oxalyl chloride ( 0 . 3 ml , 3 . 57 mmol ) was dissolved in 20 ml dichloromethane and cooled to − 78 ° c . 10 ml solution of dimethyl sulfoxide ( 0 . 39 ml , 5 . 48 mmol ) in dichloromethane were added before 15 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 11f ( 2 g , 2 . 74 mmol ) in methylene chloride were added in turn and stirred for 30 minutes at − 78 ° c . thereafter , the mixture was warmed to room temperature and stirred for 2 hours after triethylamine ( 1 . 9 ml , 13 . 7 mmol ) was added . the mixture was quenched with 5 ml 1 m hydrochloric acid and partitioned . the aqueous phase was extracted with dichloromethane ( 20 ml ) and the organic extract was washed with saturated sodium chloride solution ( 20 ml × 2 ), combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 11g ( 2 . 00 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluorophenyl ) methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 11g ( 2 . 00 g , 2 . 74 mmol ) was dissolved in 30 ml 1 , 4 - dioxane , followed by addition of 4 . 1 ml 37 % formaldehyde solution and sodium hydroxide solution ( 330 mg , 2 . 74 mmol ) in turn . the reaction mixture was stirred for 6 hours at 70 ° c . thereafter , the reaction mixture was extracted with ethyl acetate ( 20 ml × 4 ) after 20 ml saturated sodium chloride solution were added . the organic extract was washed with saturated sodium bicarbonate ( 20 ml ) and saturated sodium chloride solution ( 20 ml ) and combined , dried over anhydrous magnesium sulfate and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 11h ( 2 . 1 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 11h ( 2 . 07 g , 2 . 74 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 2 : 3 ), followed by addition of sodium borohydride ( 200 mg , 5 . 48 mmol ). the reaction mixture was stirred for 2 hours . thereafter , the reaction was quenched with a small amount of acetone and the reaction mixture was concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 11i ( 0 . 20 g , colourless grease ), yield : 10 %. 1h nmr ( 400 mhz , cdcl3 ): δ 7 . 39 - 7 . 19 ( m , 16h ), 7 . 04 ( dd , 2h ), 6 . 89 - 6 . 74 ( m , 3h ), 5 . 03 - 4 . 86 ( m , 3h ), 4 . 72 - 4 . 59 ( m , 2h ), 4 . 45 - 4 . 30 ( m , 2h ), 4 . 05 ( q , 2h ), 3 . 98 ( dd , 2h ), 3 . 90 - 3 . 80 ( m , 2h ), 3 . 75 - 3 . 62 ( m , 1h ), 3 . 25 ( d , 1h ), 3 . 06 ( s , 3h ), 1 . 42 ( t , 3h ). [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 11i ( 0 . 50 g , 6 . 60 mmol ) was dissolved in 2 ml dichloromethane and cooled to − 10 ° c ., before 1 ml trifluoroacetic acid was added . the reaction mixture was warmed and stirred for 2 hours at room temperature . thereafter , the reaction was quenched with 5 ml saturated sodium bicarbonate and partitioned . the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by silica gel chromatography with elution system b to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 11j ( 300 mg , white solid ), yield : 62 . 6 %. ms m / z ( esi ): 744 . 0 [ m + 18 ]. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluorophenyl ) methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 11j ( 300 mg , 0 . 41 mmol ) was dissolved in 10 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 600 mg , 0 . 41 mmol ) and palladium / carbon ( 30 mg , 10 %). the mixture was exchanged with h2 three times and stirred for 3 hours . thereafter , the reaction mixture was filtered and eluted with a small amount of ethyl acetate . the filtrate was concentrated under reduced pressure . the resulting residue was purified by silica gel chromatography with elution system a to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[ dideuterio -( 4 - ethoxy - 3 - fluoro - phenyl ) methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 11 ( 143 mg , white solid ), yield : 76 . 0 %. ms m / z ( esi ): 474 . 1 [ m + 18 ] 1h nmr ( 400 mhz , cd3od ): δ 7 . 49 ( d , 1h ), 7 . 45 - 7 . 36 ( m , 2h ), 7 . 00 - 6 . 88 ( m , 3h ), 4 . 17 ( d , 1h ), 4 . 08 ( q , 2h ), 3 . 89 - 3 . 77 ( m , 2h ), 3 . 73 - 3 . 54 ( m , 4h ), 1 . 40 ( t , 3h ). under n2 , 60 % nah ( 10 . 2 g , 254 . 27 mmol ) and 40 ml dmf were added into a 500 ml reaction flask and cooled to 0 ° c . 2 , 2 - difluoroethanol 12a ( 23 g , 280 . 3 mmol ) was dissolved in 40 ml dmf and then dropwise added into the mixture within 4 hours at 0 ° c . the reaction mixture was then warmed to room temperature . after 30 minutes , a solution of bromobenzene ( 39 . 92 g , 254 . 25 mmol ) in dmf ( 40 ml ) and cubr ( 0 . 35 g , 2 . 43 mmol ) were added in turn before the reaction mixture was warmed and stirred for 16 hours at 160 ° c . thereafter , the reaction mixture was cooled to room temperature and filtered . the filtrate was washed with n - hexane . 5 % hydrochloric acid ( 160 ml ) was added to the filtrate before the resulting residue was extracted with n - hexane ( 160 ml × 3 ). the organic extract was washed with saturated sodium chloride solution ( 50 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound 2 , 2 - difluoroethoxybenzene 12c ( 32 . 97 g , yellow liquid ), yield : 82 . 0 %. under ar protection , 5 - bromo - 2 - chloro - benzoic acid ( 35 g , 148 . 6 mmol ) was dissolved in toluene ( 230 ml ), followed by addition of dmf ( 0 . 5 ml ) at room temperature , then the reaction mixture was cooled to 0 ° c . the reaction mixture was heated to 100 ° c . after thionyl chloride ( 44 g , 372 mmol ) was dropwise added . after 5 hours , the reaction mixture was concentrated under reduced pressure to obtain the title compound 5 - bromo - 2 - chloro - benzoyl chloride 12n ( 35 . 5 g , pale yellow grease ), yield : 94 . 0 %. under ar protection , 5 - bromo - 2 - chloro - benzoyl chloride 12n ( 37 . 7 g , 148 . 6 mmol ) was dissolved in 350 ml dichloromethane and 2 , 2 - difluoroethoxybenzene 12c ( 25 g , 158 . 6 mmol ) was added and stirred until dissolved , and cooled to 0 ° c ., followed by addition of alcl3 ( 19 . 1 g , 142 . 4 mmol ) in batch . the reaction mixture was stirred for 2 hours at 0 ° c ., then poured into 300 ml ice water and stirred for 30 minutes and partitioned . the aqueous layer was extracted with dichloromethane ( 100 ml ). the organic layer was combined and partitioned after methanol ( 50 ml ), dichloromethane ( 100 ml ) and water ( 200 ml ) were added . the organic layer was washed with saturated nacl solution ( 200 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 5 - bromo - 2 - chloro - phenyl )-[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methanone 12o ( 56 g , yellow grease ), yield : 99 . 0 %. under ar protection , ( 5 - bromo - 2 - chloro - phenyl )-[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methanone 12o ( 55 . 7 g , 148 . 6 mmol ) was dissolved in 400 ml acetonitrile , triethyl silane ( 46 . 54 g , 401 . 22 mmol ) was added and cooled to 0 ° c ., followed by the slow dropwise addition of boron trifluoride etherate ( 57 g , 401 . 22 mmol ). then the reaction mixture was heated to 50 ° c . and stirred for 16 hours . thereafter , the reaction mixture was cooled to room temperature before mtbe ( 200 ml ) was added and 300 ml saturated sodium bicarbonate solution were dropwise added , and partitioned . the organic extracts were washed with 200 ml saturated nacl solution and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by column chromatography to obtain the title compound 4 - bromo - 1 - chloro - 2 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] benzene 12p ( 20 g , colourless grease ), yield : 20 . 0 %. ms m / z ( esi ): 362 . 0 [ m + 1 ]. under ar protection , 4 - bromo - 1 - chloro - 2 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] benzene 12p ( 26 . 5 g , 73 . 3 mmol ), mtbe ( 266 ml ) and n - hexane ( 133 ml ) were added into a 1 l reaction flask , stirred uniformly and cooled to − 78 ° c ., followed by dropwise addition of 2 . 4 m nbuli ( 52 ml , 124 . 6 mmol ) in 30 minutes . after stirring for 50 minutes at − 78 ° c ., a mixed solution of ( 3r , 4s , 5r , 6r )- 3 , 4 , 5 - tris ( trimethylsilyloxy )- 6 -( trimethylsilyloxymethyl ) tetrahydropyran - 2 - one 2f ( 55 g , 117 . 3 mmol ) in mtbe and n - hexane ( 60 ml : 30 ml ) was added within 20 minutes at − 78 ° c . before the reaction mixture was stirred for 4 hours at − 78 ° c . thereafter , 130 ml methanol were added before stirring for 20 minutes . then the reaction mixture was warmed to room temperature and stirred for 16 hours after methanesulfonic acid ( 25 g , 256 . 55 mmol ) was added . 500 ml saturated sodium bicarbonate were added to the reaction mixture , stirred for 1 hour and partitioned . the aqueous phase was extracted with mtbe ( 100 ml × 2 ) and the organic extract was combined , concentrated and purified by column chromatography ( eluant : dichloromethane : methanol = 100 : 1 ˜ 10 : 1 ) to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 12e ( 5 g , pale yellow solid ), yield : 10 %. ms m / z ( esi ): 492 . 46 [ m + 18 ]. ( 2s , 3r , 4s , 5s , 6r )- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 -( hydroxymethyl )- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 12e ( 4 g , 8 . 43 mmol ) was dissolved in 40 ml dichloromethane , followed by addition of dmap ( 103 mg , 0 . 84 mmol ), tbscl ( 1 . 4 g , 9 . 27 mmol ) and imidazole ( 1 . 72 g , 25 . 3 mmol ) in turn . the reaction mixture was stirred for 16 hours . 40 ml saturated sodium bicarbonate were added before the reaction mixture was stirred and partitioned . thereafter , the organic extract was washed with 0 . 1 n hydrochloric acid ( 20 ml ) and saturated sodium chloride solution ( 40 ml ), dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 12f ( 4 . 96 g , pale yellow solid ), yield : 100 %. 60 % nah ( 1 . 9 g , 47 . 21 mmol ) and 15 ml thf were added into a 100 ml reaction flask and cooled to 0 ° c ., followed by dropwise addition of ( 2s , 3r , 4s , 5s , 6r )- 6 -[( tert - butyl ( dimethyl ) silyl ) oxymethyl ]- 2 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 - methoxy - tetrahydropyran - 3 , 4 , 5 - triol 12f ( 4 . 96 g , 8 . 43 mmol ) in thf ( 18 ml ) within 10 minutes at 0 ° c . the reaction mixture was stirred for 30 minutes . then a solution of benzyl bromide ( 7 . 21 g , 42 . 15 mmol ) in n , n - dimethyl formamide ( 10 ml ) was dropwise added before the reaction mixture was warmed and stirred for 16 hours at room temperature . thereafter , the reaction mixture was partitioned after 200 ml ethyl acetate , saturated sodium bicarbonate ( 70 ml ) and water ( 50 ml ) were added . the organic extract was washed with 0 . 01 n hydrochloric acid ( 60 ml ) and saturated sodium chloride solution , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 12g ( 7 . 25 g , pale yellow liquid ), which was used directly in the next step without purification . [[( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methoxy ] tert - butyl - dimethyl - silane 12g ( 4 . 10 g , 4 . 78 mmol ) was dissolved in 30 ml methanol , followed by addition of acetyl chloride ( 51 μl , 0 . 72 mmol ). the reaction mixture was stirred for 1 hour . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by column chromatography to obtain the title compound [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoro - ethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 12h ( 1 . 23 g , white grease ), yield : 34 . 6 %. oxalyl chloride ( 0 . 18 ml , 2 . 16 mmol ) was dissolved in 5 ml methylene chloride and cooled to − 78 ° c ., followed by dropwise addition of a solution ( 3 ml ) of dimethyl sulfoxide ( 0 . 23 ml , 3 . 31 mmol ) in methylene chloride , and the reaction mixture was stirred for 15 minutes . 10 ml solution of [( 2r , 3r , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 12h ( 1 . 23 g , 1 . 66 mmol ) in methylene chloride were dropwise added before the mixture was stirred for 40 minutes . the reaction mixture was warmed to room temperature and stirred for 3 hours after triethylamine ( 1 . 2 ml , 8 . 31 mmol ) was dropwise added . thereafter , the reaction mixture was partitioned after 5 ml 1 m hydrochloric acid were added . the aqueous phase was extracted with ethyl acetate ( 20 ml × 2 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoro - ethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 12i ( 1 . 10 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 12i ( 1 . 10 g , 1 . 48 mmol ) was dissolved in 20 ml 1 , 4 - dioxane , followed by addition of 2 . 5 ml of 37 % formaldehyde solution and dropwise addition of 4 ml of 2 . 9 m sodium hydroxide solution . the reaction mixture was stirred for 25 hours at 70 ° c . thereafter , the reaction mixture was concentrated under reduced pressure before 20 ml water and 10 ml saturated sodium chloride solution were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure to obtain the title compound ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 12j ( 1 . 09 g , yellow grease ), which was used directly in the next step without purification . ( 2s , 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - carbaldehyde 12j ( 1 . 09 g , 1 . 42 mmol ) was dissolved in 30 ml of mixed solution ( thf and meoh , v : v = 1 : 2 ), followed by addition of sodium borohydride ( 108 mg , 2 . 83 mmol ) in batch . the reaction mixture was stirred for 30 minutes before 20 ml water and 30 ml water were added . the aqueous phase was extracted with ethyl acetate ( 30 ml × 3 ) and the organic extract was washed with saturated sodium chloride solution ( 30 ml ) and combined , dried over anhydrous magnesium sulfate , and filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by column chromatography to obtain the title compound [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyl - oxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 12k ( 293 mg , yellow grease ), yield : 27 . 0 %. [( 3s , 4s , 5r , 6s )- 3 , 4 , 5 - tribenzyloxy - 6 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 2 -( hydroxymethyl )- 6 - methoxy - tetrahydropyran - 2 - yl ] methanol 12k ( 293 mg , 0 . 38 mmol ) was dissolved in 10 ml dichloromethane , followed by dropwise addition of trifluoroacetic acid ( 0 . 1 ml ). the reaction mixture was stirred for 1 hour . thereafter , the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by column chromatography to obtain the title compound [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 12m ( 76 mg , white solid ), yield : 27 . 6 %. [( 1s , 2s , 3s , 4r , 5s )- 2 , 3 , 4 - tribenzyloxy - 5 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octan - 1 - yl ] methanol 12m ( 76 mg , 0 . 10 mmol ) was dissolved in 10 ml of mixed solution ( thf and meoh , v : v = 1 : 1 ), followed by addition of o - dichlorobenzene ( 103 μl , 0 . 9 mmol ) and palladium / carbon ( 180 mg , 10 %). the mixture was exchanged with h2 three times and stirred for 2 hours , then filtered . the filtrate was concentrated under reduced pressure and the resulting residue was purified by column chromatography to obtain the title compound ( 1s , 2s , 3s , 4r , 5s )- 5 -[ 4 - chloro - 3 -[[ 4 -( 2 , 2 - difluoroethoxy ) phenyl ] methyl ] phenyl ]- 1 -( hydroxymethyl )- 6 , 8 - dioxabicyclo [ 3 . 2 . 1 ] octane - 2 , 3 , 4 - triol 12 ( 17 mg , pale yellow solid ), yield : 34 . 0 %. ms m / z ( esi ): 490 . 24 [ m + 18 ]; 1h nmr ( 400 mhz , cd3od ): δ 7 . 48 - 7 . 49 ( m , 1h ), 7 . 37 - 7 . 39 ( m , 2h ), 7 . 15 - 7 . 17 ( d , 2h ), 6 . 88 - 6 . 91 ( d , 2h ), 6 . 02 - 6 . 29 ( ddt , 1h ), 4 . 23 - 4 . 24 ( d , 1h ), 4 . 20 - 4 . 21 ( d , 1h ), 4 . 16 - 4 . 17 ( d , 1h ), 4 . 08 ( s , 2h ), 3 . 78 - 3 . 88 ( m , 2h ), 3 . 67 - 3 . 72 ( m , 2h ), 3 . 55 - 3 . 57 ( m , 2h ). the following methods can be used to determine the inhibitory activity of the compounds according to the present invention for sglt1 and sglt2 . experimental methods are briefly described as follows . sglt1 or sglt2 instantaneous transfer strain ( cell density : 1 − 1 . 5 × 104 ) was seeded into each well of a 96 - well plate ( prepared according to existing literature “ diabetes , 57 , 1723 - 1729 , 2008 ”, wherein cdna of sglt1 and sglt2 was purchased from origene ) and incubated in a humidified environment containing 5 % co2 at 37 ° c . for 48 hours . then each well of the 96 - well plate was washed with 200 μl sodium - free buffer twice and 90 μl sodium - containing buffer solution containing test compounds having different concentrations was added , each of the test compounds having its corresponding concentration repeated in three wells . the compounds were incubated at 37 ° c . for 15 minutes and then each well of the 96 - well plate was incubated with [ 14c ] methyl α - d - glucopyranoside ( 10 μl , totally 0 . 1 μci ) for another 2 hours at 37 ° c . thereafter , supernatant was removed ; the cell pellet was washed twice with precooling no - sodium buffer and lysed in 200 mm naoh ( 100 μl ). 100 μl scintillation fluid was added and mixed and 14c was quantitatively detected using liquid scintillation . the ic50 values of the compounds can be calculated using the aggregation rate at different concentrations . conclusion : the compounds of the present invention have high selectivity and significantly inhibit sglt2 . the purpose was to observe the effect of the test compounds on blood glucose levels of glucose - load mice . determination and analysis of sugar content in the blood collected from the mouse tail was determined at different times within 2 hours of administration to provide preliminary evaluation of the hypoglycemic activity in vivo . the compounds tested were compounds of example 1 , example 2 and example 4 . the experimental animals used were 24 healthy icr mice ( weighing 20 - 24 g ), 12 female and 12 male , purchased from shanghai super — b & amp ; k laboratory animal corp . ltd ., animal production license number : scxk ( shanghai ) 2008 - 0016 . to prepare the drug , a certain amount of compounds were weighed and dissolved in water ( pure water own ) and formulated into an aqueous solution of 0 . 1 mg / ml ( 5 % dmso for solubilization ). the administered dose was 1 mg / kg , blank and water groups ( containing 5 % dmso ). 20 % glucose solution ( 4 g / kg , 0 . 8 ml each mouse ) was given after 15 minutes of administration . administering in dose and measuring the blood glucose value (− 15 minutes ). 20 % glucose solution ( 4 g / kg , 0 . 8 ml each mouse ) was given 15 minutes after administering , then the blood glucose value of each mouse was measured at minute 0 , 15 , 30 , 45 , 60 , 120 using roche accu - chek , and the decline rate of the medicine - time area under the curve ( auc ) was calculated . conclusion : concerning the compounds according to the present invention after 15 minutes of administering , the blood glucose was significantly decreased . it will be appreciated by those skilled in the art that changes could be made to the embodiments described above without departing from the broad inventive concept thereof . it is understood , therefore , that this invention is not limited to the particular embodiments disclosed , but it is intended to cover modifications within the spirit and scope of the present invention as defined by the appended claims . | 2 |
referring first to fig1 - 3 , an exemplary embodiment of a fluid content monitor 10 constructed in accordance with the present disclosure is shown . the monitor 10 can be used , for example , to measure residual free or total chlorine levels in water . the monitor 10 is equally well - suited for other chemical or industrial processes but is described herein with respect to chlorine monitoring using colorimetric dpd ( n , n - diethyl - p - phenylenediamine ) chemistry . the residual chlorine monitor 10 includes a strong , shatterproof case 12 with a removable front cover 14 . the case 12 is also small in size relative to prior art monitors and corrosion - resistant to provide simple installation in a wide array of locations . as shown in fig1 , the front cover 14 defines a window 16 to allow operator monitoring and control . the window 16 provides access to a control panel 18 having touch pad controls 20 and a display panel 22 . the viewing window 16 also allows inspection of a test sample holder or cuvette 30 that contains the fluid being tested . referring to fig2 , the residual chlorine monitor 10 is shown with the cover removed and removable first and second containers 40 a , 40 b for chemical reagents secured within the case 12 , while in fig3 the monitor 10 is shown with the containers removed . as shown in fig2 and 3 , the monitor 10 includes a colorimeter 100 that receives the sample cuvette 30 , and a pump assembly 200 for transferring the reagents from the reagent containers 402 , 40 b to the cuvette 30 . as described in greater detail below , the cuvette 30 is removably mounted within the colorimeter 100 to allow for periodic cleaning or replacement . the colorimeter 100 measures the concentration of a known constituent , e . g ., chlorine , of a solution by comparison with colors of standard solutions of that constituent . referring to fig2 and 3 , the chlorine monitor 10 includes an inlet line 60 for receiving a water sample to be tested , and a pressure regulator 62 and inlet valve 64 for controlling flow of the water sample to the cuvette 30 for testing . a drain valve 70 controls flow from the cuvette 30 to a drain line 72 after testing has been completed . according to one exemplary embodiment , both the inlet valve 64 and the drain valve 70 are solenoid - actuated valves . electrical power is provided to the chlorine monitor 10 and to the various electrical and electronic components thereof through a connector 80 that extends through the case 12 as shown in fig1 - 3 . in the exemplary embodiment shown , a second connector 82 allows the monitor 10 to be attached to one or more alarms ( not shown ), which are activated when the test results fall outside of predetermined parameters . a third connector 84 allows for on - line communication between the monitor 10 and a remote location . although not viewable in the drawings , the chlorine monitor 10 also includes an electronic controller ( i . e ., computer processor ) that is operatively connected to the various components of the monitor 10 . the controller is programmed to control : delivery of the water sample to the cuvette 30 using the water inlet valve 64 ; delivery of the reagents to the cuvette 30 using the pump assembly 200 , testing of the sample using the colorimeter 100 ; and draining of the sample from the cuvette 30 after testing using a water drain valve 70 . signals representing photometric measurements provided by the colorimeter 100 are processed by the electronic controller , which then displays the results on the display panel 22 . the control panel 18 allows the operator to program and run the residual chlorine monitor 10 according to parameters and operations programmed into the controller . preferably , the electronic controller is a microprocessor located within the case 12 and is easily configured to exchange signals with other devices via a local area network and the like . in another embodiment , the electronic controller is remotely located from the chlorine monitor 10 . referring to fig4 - 6 , various detailed views of the pump assembly 200 are shown . the pump assembly 200 includes a pump 210 , a pump actuator 230 , first and second reagent tubes 250 a , 250 b , and check valves 260 a - d . the pump assembly 200 delivers precisely measured and timed dosages of indicator reagent and buffer reagent to the water in the cuvette 30 . the pump 210 is mounted within the case 12 by a bracket 212 and includes a generally cup - shaped pump body 214 having a sidewall 216 extending from an end wall 218 to define an interior pump chamber 220 . the sidewall 216 includes two openings 222 adjacent the end wall 218 for the reagent tubes 250 a , 250 b as described below . a housing 232 of the pump actuator 230 is secured to an entrance of the pump chamber 220 ( with screw threads and a setscrew 213 for example ), as best shown in fig6 . referring to fig6 , the pump 210 also includes a pump hammer 224 within the chamber 220 of the body 214 for reciprocating linear movement between a retracted position moved away from the end wall 218 of the body , as shown in fig7 , and an extended position moved towards the end wall 218 , as shown in fig8 . referring in particular to fig6 , the pump actuator 230 is a solenoid . the solenoid includes electromagnet coils ( not viewable ) located in the housing 232 that are electrically activated through pump solenoid wires 233 connected to the electronic controller . a magnetic armature 234 is slidably mounted within a central opening 235 of the housing 232 , and the armature 234 is connected to the hammer 224 of the pump 210 ( with set screws 225 for example ) so that an electrical charge delivered to the solenoid 230 by the electronic controller causes linear movement of the armature 234 . the upper end of the armature 234 carries a circumferential retaining ring 236 , and a helical pump return spring 238 is disposed between the upper end of the housing 232 and the retaining ring 236 . the return spring 238 normally biases the retaining ring 236 and the attached armature 234 into the retracted position shown in fig7 . the solenoid 230 is adapted to extend the hammer 224 of the pump 210 when energized and retract the hammer 224 when not energized . with reference to fig3 - 6 , the first reagent tube 250 a connects the first reagent container 40 a with the cuvette 30 , and the second reagent tube 250 b connects the second reagent container 40 b with the cuvette 30 . both tubes 250 a , 250 b extend from the bottoms of the reagent containers 40 a , 40 b , through covers 42 a , 42 b of the reagent containers , pass through the openings 222 in the pump body 216 , and continue to a nozzle 102 . the nozzle 102 of the colorimeter 100 extends into the cuvette 30 . air vent tubes 44 a , 44 b also extend from the covers 42 a , 42 b . the openings 222 in the pump sidewall 216 are located so that the tubes 250 a , 250 b lay between the hammer 224 and the end wall 218 of the pump 210 . both tubes 250 a , 250 b include an inlet check valve 260 a , 260 b , respectively , between the reagent containers 40 a , 40 b and the pump 210 , and an outlet check valve 260 c , 260 d , respectively , between the pump 210 and the colorimeter 100 . the check valves 260 a - d operate to limit the flow of reagent in a single direction from the reagent containers 40 a , 40 b to the cuvette 30 during the pumping cycle . the check valves 260 a - d also prevent air from entering the tubes 250 a , 250 b during the pumping cycle . to perform testing , the chlorine monitor 10 is primed , i . e ., the reagents are added in equal proportion to a test sample in the cuvette 30 . to prime the monitor 10 , the pump 210 operates so that the reagents are delivered from their respective containers to the cuvette 30 . typically , the electronic controller is programmed to deliver signals to the pump actuator 230 so that the hammer 224 is repeatably driven between the retracted position shown in fig7 and the extended position shown in fig8 . in the extended position shown in fig8 , the hammer 224 squeezes the segments of the tubes 250 a , 250 b in the chamber 220 to a substantially closed position against the end wall 218 of the pump 210 to create pressure in the tubes 250 a , 250 b . because the check valves 260 a - d only allow flow towards the cuvette 30 , the fluid in the tubes 250 a , 250 b is urged and moves toward the cuvette 30 . when the hammer 224 returns to the retracted position shown in fig7 , the outlet check valves 260 c , 260 d prevent backflow and a vacuum is created in the tubes to draw the reagents in equal amounts from their respective containers 40 a , 40 b , through the inlet check valves 260 a , 260 b , and into the portions of the tubes 250 a , 250 b located between the inlet check valves 260 a , 260 b and the outlet check valves 260 c , 260 d . each tube 250 a , 250 b may comprise a single piece or may be formed by conically interconnected separate tube segments 1 - 3 , as shown for example in fig6 ( the tube segments positioned in the reagent containers 40 a , 40 b are not shown in fig6 ). preferably , the tube segments 250 a - 2 , 250 b - 2 located within the pump body 214 are resiliently flexible and are composed of silicone or similar material . the diameter may be selected to provide for a desired corresponding pumping pressure . the other tube segments 250 a - 1 , 250 a - 3 , 250 b - 1 , 250 b - 3 may comprise a plastic such as polypropylene or other relatively rigid material . the diameter of the tubes 250 a , 250 b is normally relatively small so that excess reagent does not remain within the tube while the pump 210 is not in use . a smaller diameter also helps to facilitate pumping of the reagents through the respective check valves 260 a - d . in the exemplary embodiment shown , the tubes 250 a , 250 b have equal diameters and equal lengths such that equal amounts of buffer and indicator reagent are drawn through the pumping operation . the reagent containers 40 a , 40 b are thereby depleted together , which facilitates reagent replacement and maintenance of the chlorine monitor 10 . in another embodiment , the separate tubes are combined by a t - shaped fitting to allow a single tube to pass through the pump 210 or a single tube to pass into the cuvette 30 . in another possible embodiment , the reagents are delivered in unequal amounts . one way to accomplish this is to provide duplicate metering pumps for each tube such that the electronic controller can direct compression of one or both tubes at a time . by independently compressing each tube the ratio of delivery can be modified as desired by the user . in other words , the reagents can be delivered in any ratio , which is determined by the ratio of respective hammer strikes . further , using different size tubing for the tubes can more permanently vary the reagent ratio . referring now to fig9 - 11 , the colorimeter 100 is shown in detail . photometric components of the colorimeter 100 , which are shown best in fig1 , include at least one light source 104 and a light detector or photodiode 106 , for performing colorimetric testing of the sample within the cuvette 30 . the primary light source 104 for measuring the level or concentration of chlorine may comprise , for example , a green light emitting diode ( led ) 104 providing a 515 nm light source . typically , the photodiode 106 is positioned 180 ° from the primary light source 104 . in operation , the primary light source 104 directs light through the sample water mixed with reagents in the cuvette 30 to the photodiode 106 , which takes measurements representing the level or concentration of chlorine in the water and provides electronic signals representing these measurements . a secondary light source 108 , which is also positioned 180 ° from the photodiode 106 , is provided for sample level and flow measurement , and may comprise a red led . the exemplary embodiment also provides a white led 110 positioned behind the cuvette 30 to illuminate the cuvette 30 for viewing by an operator . the colorimeter 100 includes a body 112 defining a cuvette portal 114 for removably receiving the cuvette 30 , and a passageway 116 extending through the cuvette portal 114 . the nozzle 102 is removably secured in the passageway 116 and is adapted to extend into the cuvette 30 when secured in the passageway 116 and lock the cuvette 30 in the passageway 116 . in the exemplary embodiment shown , the nozzle 102 is secured with screw threads and can be loosened and tightened by hand to release and secure the cuvette 30 during cleaning or replacement of the cuvette 30 . the cuvette 30 is substantially tubular and includes open ends 31 a , 31 b that align with the passageway 116 of the body 112 . the discharge ends of the tubes 250 a , 250 b enter the nozzle 102 at intersecting angles to provide improved mixing of the reagents . according to one exemplary embodiment a 10 ° angle is formed between the tubes 250 a , 250 b at the top of the nozzle 102 . as shown best in fig1 , the body 112 of the colorimeter 100 further includes a sample port 118 intersecting the passageway 116 . a tube 33 for the water sample is connected between the water inlet valve 64 ( shown best in fig3 ) and the sample port 118 of the colorimeter 100 . the sample port 118 is offset from a central axis of the passageway 116 of the colorimeter 100 to promote a swirling effect and a mixing of the water and reagents . the sample port 118 extends into the passageway 116 below the cuvette 30 . as shown best in fig1 , the body 112 of the colorimeter 100 also has an overflow port 120 intersecting the passageway 116 above the cuvette 30 . the nozzle 102 includes side openings 121 for overflow from the cuvette 30 to flow through the overflow port 120 to overflow tubes 74 , 76 connected to the drain 71 ( an air vent tube 78 is connected to the overflow tubes and drain ). as shown best in fig9 and 11 , the colorimeter 100 includes a spring 122 for ejecting the cuvette 30 out of the cuvette portal 114 upon removal of the nozzle 102 from the cuvette 30 . a resiliently flexible retainer 124 is provided in front of the portal 114 for supporting the ejected cuvette 30 so that the cuvette 30 is not allowed to fall and be damaged . the illustrated embodiments can be understood as providing exemplary features of certain embodiments , and therefore , components and / or aspects of the illustrations can be , without limitation , otherwise combined , interconnected , sequenced , separated , interchanged , positioned , and / or rearranged without materially departing from the disclosed systems or methods . for example , the nozzle and / or discharge tubes may or may not extend into the cuvette . in other embodiments , the discharge tubes may combine the reagent ( s ) with the fluid remotely from the cuvette and / or the nozzle would facilitate the mixing at another point . for another example , it is envisioned that the reagent ( s ) can be selected to interact with , and thus monitor , a plurality of compounds independently and collectively such as lead , fluoride and the like . from the foregoing it may be seen that the present disclosure provides for a fluid content monitor 10 with a solenoid - operated pump assembly 200 and a colorimeter 100 including a removable cuvette 30 . while this disclosure has provided a detailed description of exemplary embodiments , numerous modifications and variations of the fluid content monitor 10 , pump assembly 200 , and colorimeter 100 , all within the scope of the disclosure , will readily occur to those skilled in the art . accordingly , it is understood that this description is illustrative only of the principles of the disclosure and is not limitative thereof . | 8 |
an embodiment of the present invention will be described below in detail with reference to the drawings . fig1 is a front view showing a digital copier in accordance with an embodiment of the present invention . as shown in fig1 , the digital copier comprises an auto document feeder ( adf ) 10 , a scanner unit 20 , and a printer engine section 30 . the auto document feeder 10 loads and supplies each document d to a read position r ( described later ). the scanner unit 20 optically reads an image from the document d supplied by the auto document feeder 10 or manually to convert the image into image data . the printer engine section 30 comprises a charger , a laser unit , a photosensitive drum , a developing device , a transfer roller , and a fixing device ( none of them are shown ). the charger charges a surface of the photosensitive drum to a predetermined potential . the laser unit forms an electrostatic latent image on the surface of the photosensitive drum on the basis of image data from the scanner unit 20 . the developing device develops the electrostatic latent image on the photosensitive drum using toner . the transfer roller transfers the toner image formed on the photosensitive drum to a sheet . the fixing device fixes the toner image transferred to the sheet . in this configuration , the printer engine section 30 copies the document image read by the scanner unit 20 to the sheet . fig2 is a sectional view showing the internal structure of the auto document feeder 10 in accordance with the embodiment of the present invention . as shown in fig2 , the auto document feeder 10 is composed of a sheet feeding tray 11 on which a plurality of documents d are placed , a conveying device 12 that takes each of the documents d out of the sheet feeding tray 11 to convey the document d along a conveying path c ( described later ), and a sheet discharging tray 13 that accommodates a plurality of documents d discharged by the conveying device 12 . the conveying device 12 comprises a first and second guide members 121 and 122 . the first and second guide members 121 and 122 comprise smooth guide surfaces 121 a and 122 a , respectively , inside . the u - shaped conveying path c is provided in the gap between the guide surfaces 121 a and 122 a so that the document d can be conveyed along the conveying path c . the conveying path c connects the sheet feeding tray 11 and the sheet discharging tray 13 together . a read position r is provided in a portion of the conveying path c which is closest to the scanner unit 20 ; a document image is read at the read position r . the first guide member 121 is placed outside the second guide member 122 . the first guide member 121 has a rectangular opening 121 b formed in its area corresponding to the read position r . this allows the document d conveyed along the conveying path c to be located opposite the scanner unit 20 on passing through the read position r . the conveying path c has a pickup roller 123 , a separate roller 124 , a registration roller 125 , a first conveying roller 126 a , a second conveying roller 126 b , a stabilizing roller 127 , a third conveying roller 126 c , and a sheet discharging roller 128 which are arranged in this order from an upstream side in a direction in which the document d is conveyed . the pickup roller 123 picks up each of the documents d in the sheet feeding tray 11 and loads it into the conveying path c of the conveying device 12 . when a plurality of documents d are loaded by the pickup roller 123 , the separate roller 124 passes only the uppermost document d through , while blocking the passage of the remaining documents d . the registration roller 125 registers the document d the passage of which is not blocked by the separate roller 124 . the first to third conveying rollers 126 a to 126 c convey the document d registered by the registration roller 125 , along the conveying path c . the stabilizing roller 127 stabilizes the behavior of the document d conveyed by the first to third conveying rollers 126 a to 126 c . the sheet discharging roller 128 discharges the document d conveyed by the first to third conveying rollers 126 a to 126 c , from the conveying path c . each of the rollers 123 to 128 has a plurality of ( in the present embodiment , four ) roller pieces around a horizontally supported drive shaft at predetermined intervals . when each of the drive shafts is rotated , all roller pieces provided around the drive shaft rotate concurrently . pinch rollers 129 are arranged immediately below the respective sheet discharging roller pieces 128 . each of the pinch rollers 129 is rotatably disposed in a groove portion 121 b of the first guide member 121 ( lower guide member 121 c described later ). each of the pinch rollers 129 is contacted with an outer peripheral surface of the sheet discharging roller 128 under pressure by elastic means such as a leaf spring . the separate roller 124 , registration roller 125 , first to third conveying roller 126 a to 126 c , and sheet discharging roller 128 constitute respectively roller pairs together with driven rollers arranged opposite them across the conveying path c . for example , the separate roller 124 constitutes a separate roller pair together with a corresponding driven roller . that portion of the first guide member 121 which lies downstream of the read position r is located below that portion of the second guide member 122 which lies downstream of the read position r . thus , in the description below , the portion of the first guide member 121 located downstream of the read position r is called a lower guide portion 121 c . the portion of the second guide member 122 located downstream of the read position r is called an upper guide portion 122 c . fig3 is a schematic diagram showing the sheet discharging portion 120 according to the embodiment as viewed from a downstream side in the direction in which the document d is conveyed . fig4 is a schematic diagram showing the sheet discharging section 120 in accordance with the embodiment as viewed from the front of the auto document feeder . as shown in fig3 and 4 , the lower guide portion ( guide member ) 121 c has a guide surface 121 d located below the lowermost portion of the sheet discharging roller 128 . it is noted that the guide surface 121 d is a part of the guide surface 121 a . the lower guide portion 121 c comprises a plurality of ( in the present embodiment , four ) projecting portions 130 located substantially immediately below its drive shaft of the sheet discharging roller 128 . the number of projecting portions 130 is not particularly limited . the projecting portions 130 are disposed so that two of the four sheet discharging roller pieces 128 arranged at the opposite ends of the sheet discharging roller are each sandwiched between the projecting portions 130 . the upper end of the each projecting portion 130 projects upward from the lowermost portion of the sheet discharging roller 128 . each projecting portion 130 comprises a first inclined surface 130 a on its side surface located upstream in the conveying direction of the document d ; the first inclined surface 130 a becomes higher as it approaches its downstream end in the conveying direction . each projecting portion 130 also comprises a second inclined surface 130 b on its top surface which becomes higher as it approaches its downstream end in the conveying direction and which is gentler than the first inclined surface 130 a . thus , when the document d reaches the projecting portions 130 , parts of the document d which correspond to the projecting portions 130 are scooped up by the first inclined surface 130 a and run onto the second inclined surfaces 130 b . on the other hand , parts of the document d which are corresponding to the roller pieces of the sheet discharging roller 128 are guided by the upper and lower guide portions 121 c and 122 c as they are and then advance between the sheet discharging roller 128 and the pinch roller 129 . as described above , the document d from which a document image has been read is guided by the lower guide portion 121 c . the document d is then discharged onto the sheet discharge tray 13 by the sheet discharging roller 128 . the lower guide portion 121 c ( including the projecting portions 130 ), sheet discharging roller 128 , and sheet discharging tray 13 thus constitute a sheet discharging portion ( sheet discharging device ) 120 that discharges the document d from the conveying path c of the conveying device 12 . in the present embodiment , a common contact plane p for the sheet discharging roller 128 and pinch roller 129 corresponds to the contact plane between the sheet discharging roller and the sheet in accordance with the present invention . as shown in fig2 , the scanner unit 20 comprises a glass plate ( not shown ) at a position corresponding to the read position r . the glass plate 21 is colorless and transparent and has a reader ( not shown ) provided on its scanner unit 20 side . the reader comprises a first carriage , a second carriage , an image forming lens , and a ccd sensor ( none of them are shown ). the first carriage is provided with an exposure lamp ( not shown ) that irradiates the document d passing on a surface of the glass plate , and a first mirror that reflects reflected light from the document surface in a predetermined direction . a second and third mirrors ( not shown ) are attached to the second carriage to reflect the reflected light from the first mirror in a predetermined direction . the light emitted from the exposure lamp passes through the glass plate to the surface of the document d passing through the read position r . then , the light reflected off the document surface passes through the glass plate back to the scanner unit 20 . the light is reflected by the first to third mirrors and then guided to the image forming lens . the light converged by the image forming lens is detected by the ccd sensor . the detection signal is used to create image data . a document glass board ( not shown ) is provided on the top surface of the scanner unit 20 so that the document d is manually placed on the document glass board . the document glass board is used to read a document image without the use of the auto document feeder 10 . the document d from which the document image has been read is conveyed to the sheet discharging roller 128 while being guided by the upper and lower guides 121 c and 122 c . once the conveyed document d reaches the projecting portions 130 of the lower guide portion 121 c , parts of the document d which correspond to the projecting portions 130 are scooped up by the first inclined surface 130 a and run onto the second inclined surfaces 130 b . however , parts of the document d which are corresponding to the roller pieces of the sheet discharging roller 128 are guided by guide surfaces 121 d and 122 d of the upper and lower guide portions 121 c and 122 c as they are and then advance between the sheet discharging roller 128 and the pinch roller 129 . this causes the parts of the document d discharged onto the sheet discharging tray 130 to advance in different directions . the document d discharged to the sheet discharging tray 13 has a locally substantially s - shaped cross section , that is , the document is corrugated . corrugated documents d are sequentially stacked on the sheet discharging tray 13 . an alternate long and short dash line ( a ) in fig3 shows the advancing direction of the parts of the document d which are corresponding to the projecting portions 130 . an alternate long and two short dashes line ( b ) in fig3 shows the advancing direction of the parts of the document d which are corresponding to the roller pieces of the sheet discharging roller 128 . the document d having run onto the projecting portions 130 is in contact only with the second inclined surface 130 b until it is discharged to the sheet discharging tray 13 . thus , the first inclined surface 130 a is used to scoop up the leading end of the document d when it reaches the projecting portions 130 . [ table 1 ] indicates the misalignment of documents d discharged onto the sheet discharging tray 13 with respect to the conveying direction . [ table 2 ] indicates the misalignment of the documents d discharged onto the sheet discharging tray 13 with respect to a lateral direction of the documents d , that is , a direction orthogonal to the conveying direction . in [ table 1 ] and [ table 2 ], lt , lt - r , lg , ld , and st - r denote the sizes of the documents d . the numerical values in [ table 1 ] and [ table 1 ] represent the levels of misalignment of the documents d . a larger numerical value indicates a higher level of misalignment . a smaller numerical value indicates a lower level of misalignment . in the present comparison , the speed at which the document d is conveyed is about 210 mm / sec . as shown in [ table 1 ], the auto document feeder 10 according to the present embodiment is far more excellent in the alignment of the discharged documents d than a conventional auto document feeder that uses a flange portion provided on the sheet discharging roller to corrugate the documents . as shown in [ table 2 ], the auto document feeder 10 according to the present embodiment is far more excellent , for most document types , in the alignment of the discharged documents d than the conventional auto document feeder that uses the flange portion provided on the sheet discharging roller to corrugate the documents . [ table 3 ] indicates the misalignment of the documents d discharged onto the sheet discharging tray 13 with respect to the conveying direction . [ table 4 ] indicates the misalignment of the documents d discharged onto the sheet discharging tray 13 with respect to the lateral direction of the documents d , that is , the direction orthogonal to the conveying direction . in [ table 3 ] and [ table 4 ], a3 , a4 , and a4 - r denote the sizes of the documents d . the numerical values in [ table 3 ] and [ table 4 ] represent the levels of misalignment of the documents d . a larger numerical value indicates a higher level of misalignment . a smaller numerical value indicates a lower level of misalignment . as shown in [ table 3 ] and [ table 4 ], the misalignment generally falls within a narrow range even with a small variation in misalignment depending on the weight of the document d . the above results indicate that the auto document feeder 10 according to the present embodiment significantly improves the alignment of the discharged documents d than the conventional auto document feeder that uses the flange portion provided on the sheet discharging roller to corrugate the documents . the lower guide portion 121 c according to the present embodiment comprises the plurality of projecting portions 130 , which project upward from the lowermost portion of the sheet discharging roller 128 . the document discharged to the sheet discharging tray 13 thus has an s - shaped cross section , that is , the document is corrugated . this allows the discharged documents d to advance straight more properly . the present embodiment thus reduces the time for which a document d discharged later rubs against documents d already stacked on the sheet discharging tray 13 . the present embodiment also reduces the area over which the document d discharged later comes into frictional contact with the documents d already stacked on the sheet discharging tray 13 . this makes the documents d on the sheet discharging tray 13 difficult to move , thus improving the alignment of the documents d on the sheet discharging tray 13 . furthermore , the projecting portions 130 according to the present embodiment are provided on the lower guide portion 121 c . this drastically reduces the manufacture costs compared to the conventional technique of providing a flange portion at one or both ends of the sheet discharging roller 128 . moreover , each projecting portion 130 comprises the first inclined surface 130 a on its side surface located upstream in the conveying direction of the document d ; the first inclined surface 130 a becomes higher as it approaches its downstream end in the conveying direction . this reduces a possible load on the document d running onto the projecting portions 130 . the document d is thus prevented from being damaged . the lower guide portion 121 c has the guide surface 121 d disposed below the lowermost portion of the sheet discharging roller 128 . this allows the parts of the document d corresponding to the projecting portions 130 to rise high on running onto the projecting portions 130 . the document d is thus significantly corrugated . moreover , the auto document feeder 10 according to the present embodiment significantly improves the alignment of the discharged documents d than the conventional auto document feeder that uses the flange portion provided on the sheet discharging roller to corrugate the documents . the sheet discharging portion 120 is applicable not only to the auto document feeder but also to , for example , a fixer . the present invention is not limited to the above embodiments proper . in implementation , the components of the embodiments can be varied without departing from the spirit of the present invention . further , various inventions can be formed by properly combining a plurality of components disclosed in the above embodiments . for example , some of the components shown in the embodiments can be deleted . moreover , components of the different embodiments may be properly combined . additional advantages and modifications will readily occur to those skilled in the art . therefore , the invention in its broader aspects is not limited to the specific details and representative embodiments shown and described herein . accordingly , various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents . | 1 |
as usual in the representation of microcomponents , the various drawings are not drawn to scale . fig1 is a simplified cross - section view of a tunable microresonator formed according to an embodiment of the present invention . the microresonator is formed of a stacking of thin layers and comprises a piezoelectric layer 1 sandwiched between an upper electrode 2 and a lower electrode 3 . electrode 3 may be a thin conductive layer that forms a strip extending above a cavity 4 in an electrically - insulating substrate 5 , the ends of the strip resting on the upper surface of substrate 5 . the bottom of cavity 4 is covered with a metal layer forming a setting electrode 6 . as illustrated in fig2 , in top view , the lateral edges of the strip forming lower electrode 3 are spaced apart from the edges of cavity 4 . the width of upper electrode 2 is in this example equal to the width of lower electrode 3 . electrodes 2 and 3 of the microresonator are connected to components of an electric circuit . when the microresonator is excited by means of an a . c . voltage 7 at a frequency equal to a resonance frequency of the microresonator , an electromechanical transduction phenomenon of the power between electrode 2 and piezoelectric film 1 and , conversely , a restitution of the mechanical power of piezoelectric film 1 in electric form on electrode 3 , can be observed . when a d . c . voltage 8 is applied between setting electrode 6 and lower electrode 3 of the microresonator , a constraint is exerted on lower electrode 3 . as a result , the resonance frequency of the microresonator varies . this variation is a function of the value of d . c . voltage 8 . according to an alternative embodiment of a microresonator according to the present invention , a support membrane is placed between the lower electrode and the cavity . like the lower electrode , the support membrane is a strip extending above the cavity . the support membrane may for example be made of nitride . the present invention aims at a process for manufacturing a microresonator such as described hereabove in relation with fig1 . the process comprises 4 successive steps which will be detailed hereafter . in a first phase illustrated in fig3 to 5 , a conductive portion and a resin portion laid on the conductive portion are formed on an insulating layer . in a first step , illustrated in fig3 , a portion 11 of a conductive material , conventionally copper or aluminum , is formed on an insulating portion 10 . conductive portion 11 will form the microresonator setting electrode . at the next step , illustrated in fig4 , the entire structure comprising conductive portion 11 and insulating layer 10 is covered with a resin layer 12 . a polymer resin of a type currently used in an integrated circuit forming process may for example be used in steps comprising the forming of a mask by photolithography . the deposition is performed so that the upper surface of the resin is flat , preferably after annealing . in a next step , illustrated in fig5 , resin layer 12 is etched to obtain a resin portion 13 laid on conductive portion 11 . in the case where resin layer 12 is photosensitive , for example , “ positive ”, it may be provided to insolate the portions which are desired to be kept and to then conventionally remove the non - insolated portions . resin portion 13 may be smaller or larger than conductive portion 11 . generally , a portion of any material likely to be selectively etched or removed with respect to the other materials constitutive of the various elements formed during the process of the present invention may be formed on conductive portion 11 . the embodiment of the first phase illustrated in fig3 to 5 is particularly well adapted to the case where a microresonator is desired to be included in an integrated circuit . insulating layer 10 will correspond in this case to the insulating layer placed between the penultimate and the last metal interconnect level of the integrated circuit . conductive portion 11 may be a portion of the last interconnect level . an alternative implementation of the first phase of the method according to the present invention starts from a substrate covered at its front surface with an insulating layer . a conductive layer is deposited on the insulating layer of the substrate , after which a resin layer is deposited on the conductive layer . the resin layer and the conductive layer are then successively etched to obtain a resin portion laid on a conductive portion . the same mask may be used to etch the two layers . two superposed portions having the same shape in top view is then obtained . this alternative implementation of the first phase particularly applies to the forming of a microresonator as a discrete component , where conductive portion 11 is not a portion of a layer , other portions of which are used for other purposes . in a second phase of the process of the present invention , as illustrated in fig6 , an insulating layer 20 is deposited over the entire structure formed of portions 11 , 13 , and of insulating layer 10 . the thickness of deposited insulating layer 20 is at least equal to the cumulated thickness of portions 11 and 13 . insulating layer 20 is for example a silicon oxide layer . a chem .- mech polishing of insulating layer 20 is then carried out until the upper part of resin portion 13 is exposed . in a third phase of the process of the present invention , illustrated in fig7 to 10 , a microresonator comprising a piezoelectric layer sandwiched between a lower electrode and an upper electrode is formed . in a first step , illustrated in fig7 , a conductive layer is deposited on the previously - obtained structure shown in fig6 . the entire structure comprising insulating layer 20 and resin portion 13 is thus covered with a conductive layer that may be formed of one or several superposed layers that may for example be made of platinum , gold , aluminum , molybdenum , or tungsten . this conductive layer may be coated with an upper layer used as a bonding layer for the next step . the upper layer may for example be formed of titanium / aluminum or titanium / platinum . the conductive layer is then etched to obtain a beam 30 above resin portion 13 , the ends of beam 30 resting on insulating layer 20 on either side of resin portion 13 . the beam shape in top view , not shown , is provided such that portions of resin portion 13 are exposed on either side of beam 30 . in a next step , illustrated in fig8 , a layer 40 of a material , for example , aluminum nitride , exhibiting piezoelectric characteristics at least for the layer portions deposited above beam 30 , is deposited . the portions of the aluminum nitride layer formed above beam 30 exhibit polycrystalline characteristics . those formed above insulating layer 20 are amorphous . other suitable materials which may be used to form layer 40 include zinc oxide zno , “ pzt ” ( pbzrtio 3 ), or knbo 3 . at the next step , illustrated in fig9 , one or several conductive layers , for example , made of aluminum , platinum , gold , or chromium - alloyed gold , are deposited . the conductive layer is then etched to form a conductive portion 50 positioned above beam 30 and resin portion 13 . the width of conductive portion 50 , perpendicularly to the cross - section plane of fig9 , is at most equal to that of beam 30 . preferably , and to limit interference in the microresonator , conductive portion 50 is shorter than the portion of beam 30 located above resin portion 13 . at the next step , illustrated in fig1 , layer 40 is etched to expose the parts of resin portion 13 located in top view on either side of beam 30 . for this purpose , the same etch mask as that used to form conductive portion 50 may be used to obtain a piezoelectric portion 55 of same shape as conductive portion 50 . thus , in the third phase of the process of the present invention , a microresonator comprising a piezoelectric layer 55 sandwiched between a lower electrode , i . e . beam 30 , and an upper electrode , i . e . portion 50 , has been formed . according to an alternative implementation of the third phase of the process of the present invention , a conductive layer , a piezoelectric layer , and a conductive layer are deposited above the structure illustrated in fig6 . the upper conductive layer is then etched to form the upper electrode , the piezoelectric layer is etched , after which the lower conductive layer is etched to form the lower electrode . in this embodiment , the upper conductive layer and the piezoelectric layer may for example be etched by using a first mask , and the second lower conductive layer may be etched by using a second mask . in a fourth and last phase of the process of the present invention , illustrated in fig1 , resin portion 13 is completely removed , including under the beam . the method of removal of resin portion 13 , for example , by etching , must be selective with respect to all the materials used in the preceding steps . in an alternative of the process of the present invention , an insulating support membrane may be formed under the lower microresonator electrode . for this purpose , the third phase of the process comprises an additional preliminary step consisting of forming a layer of a resistant material on resin portion 13 and on insulating layer 20 . this layer may for example be formed of an oxide layer and of a nitride layer . this layer is then etched immediately after forming of beam 30 according to the same etch mask . as a non - limiting example , the dimensions of the different elements of the microresonator obtained according to the process of the present invention are the following : thickness of the setting electrode : 0 . 5 μm spacing between the setting electrode and the lower electrode ( thickness of resin portion 13 ): from 1 to 2 μm thickness of the lower electrode : 0 . 1 μm thickness of the piezoelectric layer : 2 μm thickness of the upper electrode : 0 . 1 μm to form connections to the three electrodes of the device thus formed , additional steps may be provided in the process of the present invention . in the case where the microresonator is part of an integrated circuit , the setting electrode may be formed on an interconnect level of the integrated circuit . the setting electrode ( portion 11 ) may thus be connected to the integrated circuit elements via the interconnect network of the integrated circuit . the lower microresonator electrode ( beam 30 ) may be connected to the interconnect network by forming a conductive via in insulating layer 20 . the upper microresonator electrode ( portion 50 ) may be connected to the interconnect network by extending conductive portion 50 by a strip placed above layers 20 and 40 . before depositing the conductive layer to form the upper electrode , an opening may for example be formed in piezoelectric layer 40 , which will be covered with an insulator and which will be then filled with a conductive material . the conductive via thus formed will be placed above another via previously formed in insulating layer 20 . in the case where the microresonator is a discrete component , two contacts may be formed at the rear surface of substrate 10 by forming connection pads crossing the substrate to the setting electrode and the lower electrode . a front surface contact may be formed to have access to the upper electrode . an advantage of the method of the present invention is that it is possible in the first phase of the process of the present invention to form in a same conductive layer a conductive portion intended to form setting electrode 11 and an extension 60 of this conductive portion , such as shown in dotted lines in fig1 . extension 60 is intended to form a connection between the setting electrode and another element of the structure . resin portion 13 formed in the next step only rests on setting electrode 11 . extension 60 is then totally covered with insulating layer 20 during the last step of the first phase of the process . in the case where the microresonator is a discrete component , such a connection may for example be connected to a connection pad at the rear surface . in the case where the microresonator is formed above an integrated circuit , such a connection may be connected to an element of the integrated circuit . comparing the device obtained by the process according to the present invention illustrated in fig1 with the device illustrated in fig1 , it should be noted that the device according to the present invention differs by the presence of extension 60 of layer 11 . this feature of the device is an aspect of the present invention . of course , the present invention is likely to have various alterations , modifications , and improvements which will readily occur to those skilled in the art . 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 and 2 show by way of example an arm 10 bent to an angle so as to form two legs 11 and 12 . the outer end of the leg 11 has a narrow portion 13 with a punching or printing tip 14 preferably of hard carbide steel . the arm 10 is associated with a leaf spring 15 and is accomodated in grooves 16 and 17 therein . as shown in fig1 the groove 16 has elevated edges 18 . the leaf spring 15 comprises a central portion 19 in which the groove 17 is made . also that part of the leaf spring which has the groove 16 can be considered to belong to the central portion . at either side of the central portion 19 are two side portions 20 , each one divided into a fastener 21 with an attachment hole 22 and a reduced portion 23 which generally provides the resilient function of the leaf spring 15 . by the shape of the leaf spring , the arm and the tip will be stably positioned laterally , and this condition will prevail also after long use . as seen in fig1 and 2 , the central portion 19 of the leaf spring is bent to an angle in corresponding manner as the arm 10 . the outermost part of the central portion 19 is associated with an armature 24 , which can be fastened to the leaf spring in any suitable manner , for example by rivets . the armature of fig2 is wedge - shaped but may of course be of other suitable shape depending on the type of electromagnet to be used as operating means for the arm . when the armature 24 is attracted by an electromagnet , the arm 10 turns about the reduced portion 23 of the leaf spring so that the tip 14 moves upwards in fig2 . to ensure sufficient stiffness of the arm 10 in the direction of pivoting the arm has a reinforcing portion 25 . thus the arm can be of a thin material by which its weight will be very small . the arm can for example be of plastics reinforced by glass fibre . the arm 10 can be attached to the leaf spring 15 by any known method , for instance soldering or welding . in the embodiment according to fig3 the leaf spring 15 with the arm 10 is attached by the fastener 21 to a frame 26 connected with a magnet core 27 . as shown in the figure , screws 28 can be used for the fastening . the attachment holes can be such that it is possible by the screws 28 or other suitable attachment means to adjust the position of the tip 14 relative to a point on a surface 29 of an information carrier , for example a sheet of paper or a punch tape . the frame 26 has threaded holes 30 made in fasteners 31 for securing the device to a suitable base . the magnet core 27 has an air gap 32 the form of which corresponds to that of the armature 24 . the magnet core further has a body 33 with a winding 34 . by the electromagnet of this construction the armature 24 can be attracted for turning the arm 10 in the plane of the figure . the tip 14 strikes the surface 29 to punch a hole or make a dot forming part of a character . the device can in known manner be imparted a movement relative to the surface . when the armature under the action of the leaf spring 15 and particularly of the reduced portion 23 returns to the initial position , the arm 10 hits a damper 35 , for example a rubber cushion , attached to the frame 26 . this prevents rebounding of the arm 10 . in the shown device the arm 10 is very easily movable due to the fact that it is supported by the leaf spring , whereby there will be no friction . in the embodiment according to fig3 printing or punching is effected when the electromagnet is energized , the magnet having a pulling action . fig4 shows diagrammatically another embodiment of the invention in which the electromagnet has instead a releasing action . the device according to fig4 comprises an arm 36 and a leaf spring 37 of a construction somewhat different from the one disclosed above . the arm is attached to the leaf spring which in turn , by a fasterner 38 and a screw 39 , is attached to a support 40 , which as before can be a frame of a magnet core 27 . the arm 36 , which has a tip 14 , ia as before secured to the leaf spring by a groove 41 . between the tip 14 and the fastener 38 the leaf spring has an armature 24 coacting with the magnet core 27 , which in the same manner as above has a winding , not shown . in fig4 the device is shown in idle position which means that the armature 24 is attracted by the electromagnet , the arm 36 with the tip 14 being turned from the surface of the carrier . as before the turning occurs at a resilient , reduced portion 42 . when printing or punching is to be effected the electromagnet receives an impulse and thus releases the armature 24 . under the action of the resilient force of the leaf spring 37 the tip 14 falls unto the surface so that a dot or a hole is formed . meanwhile the electromagnet has again been energized so that the armature is again attracted to the magnet core 27 . a device according to the invention permits considerable freedom in the design of the tip 14 , which can be for instance circular , rectangular or elongated depending on the type of characters to be produced or the type of holes to be punched . also the armature 24 and the magnet core 27 can be of many different designs . also then there is great freedom in the design and thus it is possible to have a very light armature . the embodiments shown above do not limit the invention to any extent . several modifications are thus conceivable within the scope of the following claims . | 1 |
the present invention supports processing a communication signal to address isi . in an exemplary system and method , a dfe can address isi by equalizing a multi - level communication signal using a high - speed slicer that operates with a small propagation delay . while an exemplary slicer will be described in the context of a dfe operating environment , the invention can be used in other applications . a variety of applications can benefit from a multilevel slicer that exhibits small or minimal propagation delay . this invention can be embodied in many different forms and should not be construed as limited to the embodiments set forth herein ; rather , these embodiments are provided so that this disclosure will be thorough and complete , and will fully convey the scope of the invention to those having ordinary skill in the art . furthermore , all “ examples ” given herein are intended to be non - limiting , and among others supported by exemplary embodiments of the present invention . a multilevel slicer in accordance with an exemplary embodiment of the present invention can comprise an integration of certain elements or functions of a conventional adc with certain elements or functions of a conventional dac . in a back - to - back configuration , the adc elements receive the communication signal and feed the dac elements , which output a sliced signal . an adc can receive an analog communication signal having isi and output a corresponding digital signal representation of that analog signal . whereas the input analog signal may have any amplitude within an amplitude range , the digital signal representation has a discrete value selected from a finite number of possibilities . a dac can receive the digital signal representation and output a corresponding analog signal . that is , the dac sets the amplitude of its analog signal output to a specific level defined by the digital data . whereas the amplitude of the analog signal input into the adc may have essentially any value within an amplitude range , the analog signal output by the dac has a value selected from a limited number of possibilities . thus , an adc - dac pair can process an analog communication signal of variable amplitude and output an analog signal having a fixed amplitude corresponding to a digital state . a slicer in accordance with an exemplary embodiment of the present invention can be made by combining the adc with the dac and eliminating extraneous , unnecessary , or redundant circuitry of the adc and the dac . that is , integrating the adc and the dac can include removing select portions of both the adc and the dac associated with converting a signal to and from a plurality of binary signals conveying a binary representation of the multilevel signal . a single or monolithic ic chip can result from or embody this integration , for example . to better understand creating a slicer by integrating an adc and a dac , it will be useful to review the operation of a conventional flash converter , which is a type of adc . specifically , certain aspects of a conventional flash converter can serve as an architecture platform for a slicer in accordance with an exemplary embodiment of the present invention . fig3 illustrates a functional block diagram of an exemplary flash converter 310 used to receive a compensated communication signal 140 . the flash converter adc 310 takes as input the compensated multilevel signal v comp 140 . this signal 140 is split and fed to a set of n − 1 comparators 320 . the term “ comparator ” as used herein refers to a device that compares an input signal to a reference and outputs a signal 330 based on the comparison . each comparator 320 has its own distinct threshold level v n or reference that serves as the decision threshold between signal levels n − 1 and n . the set of n − 1 comparator outputs 330 thus conveys the signal level , albeit in an over - complete representation , using n − 1 bits for each symbol . the outputs 330 of the comparators 320 feed to a decoding logic block 340 that translates the information into a maximally concise binary representation using log 2 n bits . as will be appreciated by those skilled in the art , more information on flash converters can be found in the conventional art . one specific embodiment of a flash converter is described in u . s . pat . no . 6 , 816 , 101 by hietala and kim , entitled “ high - speed analog - to - digital converter using a unique gray code ,” and granted on nov . 9 , 2004 . the contents of u . s . pat . no . 6 , 816 , 101 are hereby incorporated by reference . the decision on the level of the input signal 140 is available from the comparator outputs 330 of the flash converter adc 310 in fig3 . the logic block 340 provides the signal level information in a specific binary representation . while the comparator array 320 provides a function useful for a slicer , the decoding logic can be superfluous for the slicer . thus , as will be discussed in additional detail below , a slicer can comprise the comparator array 320 or front - end of the conventional flash converter adc 310 . and , the superfluous decoding logic 340 can be eliminated . since the comparators 320 are arranged in a parallel configuration , the propagation delay through the comparator set 320 is essentially the same as the delay of a single comparator 320 a . the conventional flash converter adc 310 can be adapted to create a slicer by replacing the decoding logic 340 with a summation node . that is , adding together each of the comparator outputs 330 and bypassing or eliminating the decoding logic block 340 provides a slicing function . as will be discussed in more detail below , fig4 illustrates an exemplary slicer 400 having this configuration . referring now to fig3 , a discussion follows of the principles of operation of the flash converter 310 , its comparators 320 , and the relationships among comparator outputs 330 in the context of creating the slicer 400 that fig4 illustrates . the parallel comparator set 320 provides information on parallel lines 330 that describes the level of the input signal 140 . that is , the set of individual comparator outputs 330 a , 330 b . . . 330 c specifies the magnitude of v comp 140 within a level of precision . whereas the comparator array 320 of the flash converter 310 provides a plurality of n − 1 binary signals 330 , an exemplary slicer 400 should output a single regenerated multilevel signal . thus , the slicer 400 should have circuitry to convert the n − 1 bits into a single n - level signal in place of the flash converter &# 39 ; s dac , which conventionally converts a series of log 2 n bits into a single n - level symbol . the over - completeness of the n − 1 bit representation can be advantageous for multilevel signal regeneration . in particular , because the n − 1 bit representation is over - complete , there are well - defined dependencies among the n − 1 bits , i . e . not all permutations of n − 1 bit combinations are valid . the slicer 400 can use this property as an architectural basis . the thresholds ( v n − 1 , v n − 2 . . . v 1 ) on the comparator set 320 in fig3 can be arranged in a monotonic sequence without loss of generality . that is , one can assume that v 1 & lt ; v 2 & lt ; . . . & lt ; v n − 1 or could permute the ordering of these reference thresholds to provide an increasing sequence and adjust the decoding logic block 340 accordingly . because the same signal v comp 140 feeds all n − 1 comparators 320 , it follows that if the output of comparator n is “ true ” ( i . e . if vcomp & gt ; v n ), then the output of comparator m is also “ true ” ( i . e . v comp & gt ; v n ) for all m & lt ; n since v m & lt ; v n . a consequence of this property is that if the signal v comp lies between v n and v n + 1 , i . e . v n & lt ; v comp & lt ; v n + 1 , then the outputs of comparators 1 through n are “ true ” and the outputs of comparators n + 1 through n − 1 are “ false .” in other words , in this situation , exactly n of the comparator outputs are “ true .” recognizing that v comp falling between v n and v n + 1 can be interpreted as declaring the symbol as level n , it follows that counting the number of “ true ” comparator outputs 330 obtains the desired regenerated multilevel symbol . in other words , the identity of the multilevel symbol for the input signal 140 corresponds to the number of comparator outputs 330 that are in an “ on ” or high - voltage state . thus , the multilevel symbol can be regenerated by summing all the comparator outputs 330 . those skilled in the art will recognize that signal summation can be implemented in a manner that takes negligible time , thereby achieving a desirably small propagation delay . fig4 illustrates an exemplary slicer 400 configured to sum the comparator outputs 330 in accordance with an exemplary embodiment of the present invention . the comparator output lines 330 feed into a summation node 410 that outputs the sliced signal 160 . it may be useful to scale the comparator outputs 330 in order to prevent signal saturation in the summation node 410 . each of the comparator outputs 330 a , 330 b . . . 330 c may be attenuated by a common scaling factor , for example . such attenuation does not detract from the performance of the slicer 400 as the effect is that the multilevel slicer output 160 is also attenuated by the same factor . furthermore , this scaling can be implemented with simple passive elements that introduce negligible propagation delay . thus , in accordance with an exemplary embodiment of the present invention , the multilevel slicer 400 that fig4 illustrates can comprise the front end of a conventional flash converter , specifically a set of n − 1 comparators 320 . one of the inputs of each comparator 320 couples to the slicer input 140 , while the other input of each comparator 320 is tied to a reference or threshold v n . the threshold for the n th comparator 320 n is taken as the desired decision threshold between level n − 1 and level n of the multilevel signal . the summation node 410 adds the outputs of the n − 1 comparators 320 to regenerate the multilevel signal 160 . as discussed above , optional attenuation components ( not shown ) between the output of each comparator 320 and the summation node 410 can prevent signal saturation at the summation node 410 . the delay through the comparator set 320 as a whole is essentially the same as the delay through a single comparator 320 a , since the slicer architecture provides a parallel comparator arrangement . furthermore , the delay through the summation node 410 and any attenuation components can be negligibly small . thus , the multilevel slicer 400 operates with minimal propagation delay and thereby supports multilevel dfes with high symbol rates . it will be appreciated by those skilled in the art that the division of the system 400 into functional blocks , modules , or respective sub - modules as illustrated in fig4 ( and similarly the systems illustrated in the other figures discussed herein ) is conceptual and does not necessarily indicate hard boundaries of functionality or physical groupings of components . rather , representation of the exemplary embodiments as illustrations based on functional block diagrams facilitates describing an exemplary embodiment of the present invention . in practice , these modules may be combined , divided , and otherwise repartitioned into other modules without deviating from the scope and spirit of the present invention . turning now to fig5 , this figure illustrates a functional block diagram of an exemplary dfe 500 in accordance with an embodiment of the present invention . the dfe 500 comprises the slicer 400 that is illustrated in fig4 and discussed above . a feedback circuit 510 processes the slicer output 160 to generate isi compensation 130 in the form of feedback 130 that the summation node 190 a applies to the incoming communication signal 120 . the feedback circuit 510 adjusts the waveform in each symbol period to compensate for or remove isi on that portion of the waveform that is due to previously - received symbol periods . the propagation delay of the slicer 400 is less than or equal to the symbol period . that is , the amount of time between a signal entering and exiting the slicer 400 is less than or equal to the amount of time that each data element of the communication signal 120 occupies . in exemplary embodiments , the communication signal 120 can convey data at a rate exceeding one megabit per second , one gigabit per second , ten gigabits per second , or 100 gigabits per second , or in a range thereof . the dfe 500 can comprise a conventional dfe 110 , as illustrated in fig1 and discussed above , with the slicer 400 replacing the conventional slicer 150 . that is , in one exemplary embodiment of the present invention , a conventional dfe 110 or dfe design can be upgraded by removing the conventional slicer 150 and inserting the slicer 400 . in addition to the conventional dfe 110 illustrated in fig1 and discussed above , the slicer 400 can be applied to a wide variety of dfe systems , designs , or architectures know to those skilled in the art . furthermore , a slicer 400 in accordance with an exemplary embodiment of the present invention can enhance performance of other equalizers , equalizing devices , and communication systems . turning now to fig6 , this figure illustrates a flowchart of an exemplary process 600 , entitled slice signal , for slicing a communication signal 140 according to an embodiment of the present invention . the steps of process 600 will be discussed with exemplary reference to the slicing system 400 of fig4 , which is discussed above . certain steps in this process or the other exemplary processes described herein must naturally precede other steps for the present invention to function as described . however , the present invention is not limited to the order of the steps described if such order or sequence does not alter the functionality of the present invention . that is , it is recognized that some steps may be performed before or after other steps or in parallel with other steps without departing from the scope and spirit of the present invention . at step 610 , the first step in process 600 , a communication signal 140 conveys digital information or data in a sequence or series of symbols . designated timeslots or symbol periods each carry one of the symbols . for each symbol period , a specific signal level , selected from two or more discrete signal level possibilities , identifies or corresponds to the symbol in that symbol period . at step 615 , the sequence of symbols propagates in a physical medium or communication channel . energy transfers between or among two or more symbol periods , thus causing isi that distorts each signal level in each symbol period . at step 620 , for a current symbol period , the communication signal 140 has an amplitude or level that is between two adjacent levels in the multilevel communication scheme . that is , in response to the isi or energy transfer , the signal level for the symbol period that arrives at a receiver at a current time has shifted , varied , or deviated from its pre - transmission setting . at step 625 , circuit traces in the slicer 400 feed the communication signal 140 for the current symbol period to a set , bank , or plurality of comparators 320 . the comparators 320 are disposed in a parallel configuration so that each of the comparators 320 processes the communication signal 140 during an overlapping or essentially concurrent timeframe . at step 630 , each of the comparators 320 compares the communication signal 140 to a respective reference or threshold ( v n − 1 , v n − 2 . . . v 1 ). responsive to the comparisons , each comparator 320 outputs a comparison signal 330 that has one of two states . the comparison signal 330 a has a high state or voltage level if the comparator 320 a determines that the communication signal 140 is higher than the reference v n − 1 . on the other hand , the comparison signal 330 a assumes a low state or voltage level if the comparator 320 b determines that the communication signal 140 is lower than the reference v n − 1 . at step 635 , a summation node 410 or other summing device generates the sliced signal 160 for the current symbol period by summing each of the comparison signals 330 . the sliced signal 160 has a level set to one of the two adjacent signal levels . specifically , the chosen level is the best matching or closest level . thus , the sliced signal 160 can comprise a regenerated or reconstructed version of a degraded communication signal 140 . following step 635 , process 600 iterates steps 610 - 635 . thus , process 600 iteratively processes the communication signal 140 for each incoming symbol period in the symbol series . turning now to fig7 , this figure illustrates a flowchart of an exemplary process 700 , entitled equalize signal , for equalizing a communication signal 120 according to an embodiment of the present invention . the steps of process 700 will be discussed with exemplary reference to the dfe system 500 of fig5 , which is discussed above . the first step in process 700 is slice signal 600 , which fig6 illustrates as discussed above . process 600 outputs a sliced signal 160 having a discrete signal level for a current symbol period . at step 715 , the first delay element 170 a of a feedback circuit 510 delays the sliced signal 160 of the current symbol period . the amount of applied delay results in a timing match between the delayed signal and the next incoming symbol period of the communication signal 120 . at step 720 , the first attenuator or amplifier 180 a attenuates or scales the delayed sliced signal . the amount of applied attenuation yields a corrective signal that approximates the isi imposed on the next incoming symbol period by the signal energy of the current symbol period . at step 725 , the summation node 190 a of the feedback circuit 510 applies the attenuated and delayed sliced signal to the next incoming or first subsequent symbol period of the communication signal 120 . this compensation or correction 130 reduces the isi on that symbol period due to the current symbol period . that is , the applied corrective signal 130 comprises a corrective component produced via the first delay 170 a and the first amplifier 180 a . at step 730 , the second delay element 170 b of the feedback circuit 510 further delays the sliced signal of the current symbol period . the applied delay provides a timing match between the delayed signal and the second subsequent symbol period . at step 735 , the second amplifier 180 b attenuates the signal output by the second delay element 170 b . the applied attenuation yields an amplitude or level that matches or approximates the isi that the energy in the current symbol period imposes on the second subsequent symbol period . at step 740 , the summation node 190 a applies to the communication signal 120 a corrective component 130 that the second delay element 170 b and the second amplifier 180 b produce . specifically , that component of the corrective signal 130 addresses isi on the second subsequent symbol period due to the energy transfer from the current symbol period . following step 740 , process 700 iterates , thus applying isi correction 130 to the communication signal 120 for each symbol period , on a symbol - by - symbol basis . although a system in accordance with the present invention can comprise a circuit that addresses isi of a communication signal , those skilled in the art will appreciate that the present invention is not limited to this application and that the embodiments described herein are illustrative and not restrictive . furthermore , it should be understood that various other alternatives to the embodiments of the invention described here may be employed in practicing the invention . the scope of the invention is intended to be limited only by the claims below . | 7 |
embodiments of an inflatable seat belt apparatus according to the present invention are now described referring to the attached drawings . fig3 is a simplified perspective view showing a whole structure of the inflatable seat belt apparatus 1 . this figure illustrates for clarifying relationships between respective components of the inflatable seat belt apparatus applied to the right side front seat . in this figure , numeral 2 designates a shoulder belt . the shoulder belt 2 has an end 2a to which a tongue 3 is fixed . the shoulder belt 2 is engaged and fixed to a buckle 4 fixed to a predetermined position near the floor between the right and left front seats via the tongue 3 and has the other end 2b downwardly guided through a slip guide 5 or a pillar anchor mounted on a pillar p . the pillar anchor is adjustable in upper and lower directions . the shoulder belt is thus hung around and from the slip guide 5 to be wound up in an elr 6 arranged near the floor . a lap belt 7 has an end 7a fixed to an anchor plate 8 fixed to a mouthpiece of the tongue 3 and has the other end 7b wound in the elr 9 mounted near the floor of the door side beyond the seat cushion . the description will now be made as regard to details of the structures of the shoulder belt , peripheral components of the tongue , and the buckle , respectively . the shoulder belt 2 comprises the end 2b wound and accommodated in the elr 6 , the other end 2a connected to the tongue 3 , and a piece of webbing 10 as a through or integral member as shown in fig3 . in this embodiment , for the webbing 10 , a band shaped belt having a 50 mm width and a 1 . 6 mm thickness is used . the webbing 10 may be formed of polyester finished yarn tightly woven by twilling , plain weaving or the like . the webbing 10 is equivalent to a conventional seat belt apparatus . the webbing 10 has a section between an abdominal region and a right shoulder region which directly touches the body of an occupant , wherein the section is covered by a cylindrical cover 20 made of a cloth and formed to have a slight thickness . in the inside of the portion having the slight thickness , several kinds of envelope shape or elongated members are accommodated overlappingly . in fig4 numeral 10a shows that the webbing 10 is positioned within the cover 20 . because of the difference of the functions , this portion of the belt is called an inner belt 21 , the portion of the belt which is exposed outside and is wound into the elr is called the webbing 10 , and these portions are designated by the different numerals 10 and 21 , respectively . the inner belt 21 is inserted in a flat condition into a tube 22 formed of a thin film and made of silicone rubber as shown in fig4 . the tube 22 made of silicone rubber is cylindrical and has an end 22a fixed to a predetermined position of the inner belt 21 to maintain the airtightness as shown in fig8 ( a ). therefore , the tube 22 is inflated in a long and slender cylindrical shape as gas is introduced into the tube 22 . this tube 22 is accommodated in a cylindrical knitted textile member 23 of flat type which is knitted in a size slightly larger than the tube 22 . in this embodiment , the knitted textile member 23 is constituted by a tubular knitted textile using a polyester finished yarn ( 1500 denier ). the knitted textile member 23 of the tubular knitted textile has a characteristic which is hardly expandable in the longitudinal direction of the belt ( wrap direction of the knitted fabric ) and is easily expandable in a direction ( weft direction of the knitted fabric ) that the circumference of the cylindrical shape is increased . the cloth cover 20 as described above is arranged to wholly cover the knitted textile member 23 of a cylindrical shape . the knitted textile member 23 and the cover 20 are firmly sewn together with the inner belt 21 as shown in fig8 ( a ). preferably , a material for the cover 20 does not show the crease in the belt and is soft to the touch because the cover 20 is a portion directly touched with the hand of the occupant and directly contacts with the clothes of the occupant . in this embodiment , a tricot knit fabric knitted by warps with polyester finished yarns is employed for the cover 20 . the thick portion has the inflatable tube 22 with the inner belt 21 as a core , and the end connected to the gas generator via the tongue 3 so as to be inflated and deployed by the gas introduced in a very short period of time after a crash . therefore , the inflatable seat belt apparatus can efficiently restrain the occupant from movement . in this specification , &# 34 ; inflatable portion &# 34 ; will be denoted instead of a whole set of the inflatable member hereinafter . in addition to the embodiment described above , this invention may be accomplished by the following modified components of the inflatable portion . for the tube 22 , a rubber material which has high elasticity even against a rapid inflation and has heat - resistance because the high temperature gas is filled in the inside of the tube 22 is suitable for using . the material having rubber - like elasticity may be used for the tube 22 . the material may be , for example , various kinds of thermoplastic elastomer , urethane rubber , fluorocarbon rubber , rubber / blended rubber or the like . the knitted textile member 23 is constituted by the tubular knitted textile having no seam for forming a cylindrical shape in the above mentioned embodiment . the stitch may be plain stitch , rib stitch , pearl stitch , interlock stitch or the like . in this case , the elongation of the knitted textile member 23 in the weft direction is changeable by charging a density of weft knitted loops into the wrap direction . the knitted fabric of a flat type is made by plain weave . in this case , it is possible that 2 sheets of the knitted fabrics in a long and slender shape are overlapped and the ends of the knitted fabrics are sewn together to make a cylindrical form , and that both ends of the knitted fabric are sewn together to make a circular form . a cloth employed for the cover 20 may be a plain weave fabric using a nylon yarn or polyester yarn . besides the materials as described above , other material such as a resin film , an artificial leather or the like is considered to be employed for the cover if the material satisfies the conditions of the feel , the stiffness , the persistence and so on . fig5 is a perspective view for understanding the inside of the inflatable portion shown in fig4 when the inflatable seat belt apparatus is inflated and deployed . as shown in this figure , the tube 22 is inflated by the introduced gas , and the knitted textile member 23 constituted by the tubular knitted textile is elongated in the radial direction in a cylindrical shape . when the predetermined inner pressure is applied , a portion of the thread sewing the cloths of the cover 20 is torn . a seam 20a of the cover is then opened like a mouth , and the tube 22 covered by the knitted textile member 23 is inflated in a spindle shape to be forced out from the opening of the seam 20a . while , because a seam 20b of the cover 20 is sewn firmly at a predetermined range on the pillar anchor side of the inflatable portion 25 and at a predetermined range on the tongue 3 side , the inflation of the tube 22 is limited by a cover portion 20c of the cover 20 , so that the cover portion 20c is inflated only in a long and slender cylindrical form ( a diameter of the cylindrical form is approximately 3 . 6 cm in this embodiment ). the length in the longitudinal direction of the belt is shortened because the inflatable portion 25 is inflated in a spindle shape . at this point , because the knitted textile member 23 of the inflatable portion 25 receives a tensile force in the longitudinal direction of the belt , the inner belt 21 does not receive the tensile force , so that the inner belt 21 is loose . referring to fig6 and fig7 the description will now be made as regard to details of the fitting structure between the inflatable portion 25 and the tongue 3 provided with the gas inlet , and to a structure of a bag filter . fig6 is a perspective view showing a connecting portion between the tongue 3 and the inflatable portion 25 . in fig6 an end 25a of the inflatable portion 25 is fixed to cover an end fitting 31 made of metal which has a flat square section . furthermore , the end 25a is fixed firmly by a caulking fitting 32 so as to cover the periphery thereof so that the inflatable portion 25 is not easy to be broken away from the end fitting 31 . the end fitting 31 has a tongue pipe 33 secured to the distal end thereof . the tongue pipe 33 is inserted and engaged with a buckle body of the buckle 4 ( not shown ). the tongue pipe 33 has a gas path 34 formed inside thereof . the gas from an inflator ( not shown ) is introduced into the inflatable portion 25 through the gas path 34 and the inside of the end fitting 31 . the tongue 3 is integrally structured by a combination of the end fitting 31 , the caulking fitting 32 , and the tongue pipe 33 in this embodiment . the tongue pipe 33 has a lap belt anchor plate 8 fixed to the bottom part thereof to secure an end 7a of a lap belt 7 constituted of a normal webbing . fig7 is a longitudinal sectional view showing the inside of the inflatable portion . as shown in fig7 each component , i . e . the inner belt 21 , the bag filter 26 , the tube 22 , the knitted textile member 23 and the cover 20 , of the inflatable portion 25 is overlapped to the peripheral portion of the end fitting 31 coated by a rubber coating 31a to tightly connect with each other . the caulking fitting 32 having an inside coated by a rubber coating 32a is fixed to the peripheral portion of the inflatable portion . since the inflatable portion 25 is structured as described above , the inflatable portion 25 is maintained sealingly at the end 25a thereof and a break or a breakage of the end fitting 31 is not possible even if the reaction gas having high pressure is rapidly introduced into the inflatable portion 25 . the structure of the bag filter 26 will now be described referring to fig7 . the bag filter 26 is a filter formed of a fabric having high air permeability which is sewn in an envelope form . the filter has substantially the same width as the width of the inner belt 21 and is choked at a distal end side thereof . the bag filter 26 is inserted into the tube 22 and has an end fixed to the tongue 3 . furthermore , a skirt 27 is inserted into the bag filter and has a length which is one third of the length of the bag filter 26 . the skirt 27 is cylindrical , and opens at a distal end thereof and is formed of the same fabric of the bag filter in this embodiment . the bag filter 26 and skirt 27 are made from heat - resistant fiber in this embodiment . for example , the heat - resistant fiber may be aramid fiber . the aramid fiber is well known as a trade mark kevlar ™ fiber and has high stiffness and high elasticity . further , the aramid fiber has good heat resistance and good flame tightness and starts carbonizing at approximately 500 ° c ., so that the aramid fiber does not melt and burn even at a high temperature . though the kevlar ™ fiber employed in this embodiment is para - bond aramid fiber , meter - bond aramid fiber may , of course , be employed in view of its heat resistance . furthermore , the filter may be formed of not only a textile fabric but also a non - woven fabric . the bag filter 26 is inflated with the gas spouted from the inflator and is capable of collecting the cinders having predetermined or more bigger sizes to the inside thereof because of its air permeability . the tube is then inflated with the gas passing through the bag filter 26 . at this stage , as the gas temperature is lowered , the bag filter effectively acts as a filter and a diffuser . the skirt 27 is overlapped around the tongue to effectively display its heat resistance while considering the temperature distribution as shown in fig2 . though the aramid fiber is employed in this embodiment as described above , the fiber may be carbon fiber , alumina fiber , silicon - carbide fiber or glass fiber , each of which has high heat resistance . the carbon fiber has an extremely high heat resistance because it is made by burning and carbonizing organic fiber . therefore , the heat resistance of the carbon fiber is expected to withstand approximately 2000 ° c . if the carbon fiber is employed as a diffuser which receives no load as described in the present invention . the alumina fiber as an oxide inorganic material has also very high heat resistance and is convenient as a textile . fig8 ( a ) is a sectional view showing a structure of an end between the inflatable portion 25 and the webbing 10 , i . e . the inner belt 21 located inside the inflatable portion 25 , near a slip guide side . as the structure is now be described again , the end of the knitted textile member 23 is integrally glued to the end 20d of the cover 20 by the adhesive and is firmly sewn to the webbing 10 . the end 22a of the tube 22 made of silicon rubber is welded or glued to the inner belt 21 within the knitted textile member 23 . the end of the bag filter 26 described above is located inside the tube 22 . fig8 ( b ) shows a modification of the example shown in fig8 ( a ). the end of the knitted textile member 23 is integrally glued to the end 20d of the cover 20 by the adhesive and is firmly sewn to the webbing 10 at a predetermined position . the inner belt is cut near the end 22a of the tube 22 where the inner belt 21 is fixed to the tube 22 . only the cylindrical bag filter 26 having the same function as described above is accommodated in the tube 22 . in this embodiment , the inflatable portion 25 works as a &# 34 ; webbing &# 34 ; in a crash or the like where the gas generating means does not work . the inflatable portion 25 expands slightly in the longitudinal direction because of the elongating characteristic of the knitted textile member 23 . therefore , the inflatable portion 25 and the webbing 10 can receive a tensile force of the belt so as to restrain the occupant properly . the inflatable portion 25 is inflated in a suitable form as in the embodiment shown in fig8 ( a ) at a crash so as to restrain the occupant at the wide area of the inflatable portion 25 . fig9 - 11 are explanatory drawings showing embodiments of the buckle . the buckle 4 supports a tongue pipe 33 and has the gas generating means . the buckle 4 introduces the produced gas from the gas generating means through a gas path 34 in the tongue pipe 33 . the &# 34 ; coupling &# 34 ; between the buckle 4 and tongue 3 is achieved by engaging a tubular groove 33b disposed on the peripheral surface of a distal end of the tongue pipe 33 , to metal balls 47 inserted in tapered holes of coupling hole 44a formed in the buckle 4 . each of the metal balls 47 has a portion projecting from the inner surface of the coupling hole 44a . in fig9 numeral 41 designates a housing in which a portion of a flange plate 42 is fixed . the buckle 4 is secured by the flange plate 42 to the housing 41 near the floor of the vehicle ( not shown ). in the housing 41 , a gas generator 43 as the gas generating means is fixed to the flange plate 42 . the gas generator 43 is firmly connected to a buckle body 44 acting also as a gas passing pipe . fig9 shows a state of coupling the tongue pipe 33 to the coupling hole 44a . as shown in the figure , when the tongue pipe 33 is coupled to the coupling hole 44a of the buckle body 44 , a tongue pipe releasing ring 45 is pressed against a biasing force of the spring 46 by the tongue pipe distal end 33a in a direction of the arrow a . while , tapered holes 44b are formed at a peripheral surface of the buckle body 44 at predetermined intervals . the metal ball 47 is inserted in each tapered hole 44b to be able to move from the peripheral surface side of the buckle body 44 so that a portion of the metal ball 47 projects from the inner surface of the coupling hole 44a . when the tongue pipe 33 is coupled to the coupling hole 44a , each of the metal balls 47 is pressed from the peripheral surface side of the buckle body by a release operation ring 49 biased by a spring 48 in a direction of the arrow b . therefore , one portion of the metal ball 47 projects into the tubular groove 33b disposed on the peripheral surface of the tongue pipe 33 to press and bear the tubular groove 33b of the tongue pipe 33 , so that the tongue pipe 33 is coupled and fixed inside of the coupling hole 44a . while , release of the tongue pipe 33 is accomplished by pressing a press button 50 disposed on one portion of the housing in a direction of the arrow c as shown in fig1 . the press button 50 is an operational button of non - encircle type and has a pressing face 50a disposed at an upper front position of the housing as shown in fig1 . therefore , the occupant can operate the button 50 by one action . the description will now be briefly made as regard to a mechanism of releasing the tongue 3 from the buckle 4 . as the press button 50 is pressed in the direction of the arrow c as shown in fig1 , a protuberance portion 49a of the release operational ring 49 is pressed by an operational arm 50b mounted on the press button 50 in the direction of the arrow c , so that the release operational ring 49 slides against a biasing force of spring 48 in the direction of the arrow c to release the pressure of the metal ball 47 from the release operational ring 49 . therefore , the metal balls 47 are released from the tubular groove 33b of the tongue pipe 33 . as a result , the tongue pipe releasing ring 45 in the buckle body 44 is biased by a spring 46 in a direction of the arrow d to push out the tongue pipe 33 from the inside of the buckle body 44 and then the tongue 3 is released from the buckle 4 . fig1 ( a ), 12 ( b ) are explanatory drawings showing modified filters 26 , 26a . in the embodiment described before , to improve the heat resistance around the tongue 3 where the temperature of the spouted gas is high , the skirt 27 is mounted inside of the bag filter 26 as shown in fig7 . however , touch of the belt and feeling when wearing the belt are bad because the belt has a thick portion by the overlapping structure . the modifications as shown in fig1 ( a ) and 12 ( b ) are the bag filters structured by only one piece . for the bag filter 26 shown in fig1 ( a ), a textile having different fabric thickness which is formed of aramid fiber is employed to vary the performance of heat resistance along the longitudinal direction . for a portion around the tongue , a thick fabric 26a which has higher heat resistance is employed in order to lower the temperature of the diffuser . for the head , a sheer fabric 26b which has lower heat resistance is employed to mainly obtain a filter effect . it is possible that different kinds of heat - resistance fibers are combined and sewn . that is , a higher heat - resistance fiber may be used around the tongue and a sheer aramid fiber fabric may be used around head . fig1 ( b ) illustrates an example that a metal film coating such as aluminum is provided to an inner surface of the bag filter 26 for a range corresponding to the skirt part . though the coated range has non - air permeability , the thermal insulation effect is improved at the tongue portion . therefore , the temperature in the tube is equalized and the highest temperature around the tongue is lowered . the range to be coated is preferably set with reference to the gas flow as shown in fig1 . that is , the shoulder belt , i . e . the tube 22 , the inner belt 21 and the bag filter 26 , is curved gently around the tongue to fit to the body of the occupant d . in this state , an elbow part 26a of the bag filter 26 is hit directly and intensively by the heat flow when the gas is spouted from the inflator ( not shown ). therefore , the temperature of the elbow part 26a is raised partially to quite high temperature . since the bag filter is employed not to directly provide radiant heat in this embodiment , it is necessary to deal with such partial and continuous heating . therefore , preferably , the elbow part 26a is provided with the above described coating or 2 sheets textile fabrics are overlapped at this part . | 3 |
the present invention now will be described more fully hereinafter with reference to the accompanying drawings , in which preferred embodiments of the invention are shown . this invention may , however , be embodied in many different forms and should not be construed as limited to the embodiments set forth herein . in the drawings , the thickness of layers and regions are exaggerated for clarity . like numerals refer to like elements throughout . it will be understood that when an element such as a layer , region or substrate is referred to as being “ on ” another element , it can be directly on the other element or intervening elements may also be present . in contrast , when an element is referred to as being “ directly on ” another element , there are no intervening elements present . a tft array panel according to an embodiment of the present invention will be described with reference to fig1 and 2 . fig1 is a layout view of a tft array panel for an lcd according to an embodiment of the present invention , and fig2 is a sectional view of the tft array panel shown in fig1 taken along the line ii - ii ′. a plurality of gate lines 121 are formed on an insulating substrate 110 such as transparent glass , silicone , or plastic . the gate lines 121 transmit gate signals and extend substantially in a transverse direction . each gate line 121 includes a plurality of gate electrodes 124 projecting upward and an end portion 129 having a large area for contact with another layer or an external driving circuit . a gate driving circuit ( not shown ) for generating the gate signals may be mounted on a flexible printed circuit ( fpc ) film , which may be attached to the substrate 110 , directly mounted on the substrate 110 , or integrated onto the substrate 110 . the gate lines 121 may extend to be connected to a driving circuit that may be integrated on the substrate 110 . the gate lines 121 are preferably made of al containing metal such as al and al alloy , ag containing metal such as ag and ag alloy , au containing metal such as au and au alloy , cu containing metal such as cu and cu alloy , mo containing metal such as mo and mo alloy , cr , ti or ta . however , they may have a multi - layered structure including two conductive films ( not shown ) having different physical characteristics . one of the two films is preferably made of low resistivity metal including al containing metal , ag containing metal , and cu containing metal for reducing signal delay or voltage drop . the other film is preferably made of material such as mo containing metal , cr , ta or ti , which has good physical , chemical , and electrical contact characteristics with other materials such as indium tin oxide ( ito ) or indium zinc oxide ( izo ). good examples of the combination of the two films are a lower cr film and an upper al ( alloy ) film and a lower al ( alloy ) film and an upper mo ( alloy ) film . however , the gate lines 121 may be made of various metals or conductors . the lateral sides of the gate lines 121 are inclined relative to a surface of the substrate , and the inclination angle thereof ranges about 30 - 80 degrees . a gate insulating layer 140 is formed on the gate lines 121 . the gate insulating layer 140 is preferably made of inorganic insulator or organic insulator . examples of the inorganic insulator include silicon nitride ( sinx ) and silicon dioxide ( sio 2 ) that may have a surface treated with octadecyl - trichloro - silane ( ots ). examples of the organic insulator include maleimide - styrene , polyvinylphenol ( pvp ), and modified cyanoethyl pullulan ( m - cep ). it is preferable that the gate insulating layer 140 has good contact characteristics with organic semiconductor and small roughness . a plurality of data lines 171 and a plurality of drain electrodes 175 are formed on the gate insulating layer 140 . the data lines 171 transmit data signals and extend substantially in a longitudinal direction to intersect the gate lines 121 . each of the data lines 171 includes a plurality of source electrodes 173 projecting toward the gate electrodes 124 and an end portion 179 having a large area for contact with another layer or an external driving circuit . a data driving circuit ( not shown ) for generating the data signals may be mounted on a flexible printed circuit ( fpc ) film , which may be attached to the substrate 110 , directly mounted on the substrate 110 , or integrated onto the substrate 110 . the data lines 171 may extend to be connected to a driving circuit that may be integrated on the substrate 110 . the drain electrodes 175 are separated from the data lines 171 and disposed opposite the source electrodes 175 with respect to the gate electrodes 124 . the data lines 171 and the drain electrodes 175 are preferably made of materials having good physical , chemical , and electrical contact characteristics with the gate insulating layer 140 and organic semiconductor . in one embodiment , the data lines 171 and the drain electrodes 175 are made of a material which includes ito . ito for the data lines 171 and the drain electrodes 175 has high work function and it may be quasi - crystalline , particularly at the interface with the gate insulating layer 140 , to provide excellent contact characteristics with an organic gate insulating layer 140 . the data lines 171 and the drain electrodes 175 have smooth inclined edge profiles . a plurality of organic semiconductor islands 154 are formed on the source electrodes 173 , the drain electrodes 175 and the gate insulating layer 140 . the organic semiconductor islands 154 fully cover the gate electrodes 124 such that the edges of the gate electrodes 124 overlap the organic semiconductor islands 154 . the organic semiconductor islands 154 may include a high molecular compound or a low molecular compound that is soluble in an aqueous solution or organic solvent and in this case , the organic semiconductor islands 154 can be formed by printing . the organic semiconductor islands 154 may be made of , or formed from derivatives of , tetracene or pentacene with substituent . alternatively , the organic semiconductor islands 154 may be made of oligothiophene including four to eight thiophenes connected at the positions 2 , 5 of thiophene rings . the organic semiconductor islands 154 may be made of perylenetetracarboxylic dianhydride ( ptcda ), naphthalenetetracarboxylic dianhydride ( ntcda ), or their imide derivatives . the organic semiconductor islands 154 may be made of metallized phthalocyanine or halogenated derivatives thereof . the metallized phthalocyanine may include cu , co , zn , etc . the organic semiconductor islands 154 may be made of co - oligomer or co - polymer of thienylene and vinylene . in addition , organic semiconductor islands 154 may be made of regioregular polythiophene . the organic semiconductor islands 154 may be made of perylene , coronene or derivatives thereof with substituent . the organic semiconductor islands 154 may be made of derivatives of aromatic or heteroaromatic ring of the above - described derivatives with at least one hydrocarbon chain having one to thirty carbon atoms . a gate electrode 124 , a source electrode 173 , and a drain electrode 175 along with an organic semiconductor island 154 form an organic tft having a channel formed in the organic semiconductor island 154 disposed between the source electrode 173 and the drain electrode 175 . the gate insulating layer 140 , which is disposed between the gate electrode 124 and the organic semiconductor island 154 , may be made of material having good contact characteristics with the organic semiconductor island 154 and generating minimum leakage current in the tft . a plurality of protective members 164 are formed on the semiconductor islands 154 . the protective members 164 are preferably made of insulating material that can be dry processed and deposited under low temperature . an example of such a material is parylene that can be formed at room temperature or low temperature . the protective members 164 protect the organic semiconductor islands 154 from being damaged in the manufacturing process . the protective members 164 substantially fully cover the organic semiconductor islands 154 such that the edges of the organic semiconductor islands 154 are covered by the protective members 164 . the protective members 164 may be omitted . a passivation layer 180 is formed on the data lines 171 , the drain electrodes 175 , and the protective members 164 . the passivation layer 180 is preferably made of inorganic insulator such as silicon nitride or silicon oxide , organic insulator , or low dielectric insulator . the organic insulator and the low dielectric insulator preferably have dielectric constant less than about 4 . 0 and the low dielectric insulator includes a - si : c : o and a - si : o : f formed by plasma enhanced chemical vapor deposition ( pecvd ). the organic insulator for the passivation 180 may have photosensitivity and the passivation 180 may have a flat surface . the passivation layer 180 has a plurality of contact holes 182 and 185 exposing the end portions 179 of the data lines 171 and the drain electrodes 175 , respectively . the passivation layer 180 and the gate insulating layer 140 have a plurality of contact holes 181 exposing the end portions 129 of the gate lines 121 . a plurality of pixel electrodes 190 and a plurality of contact assistants 81 and 82 are formed on the passivation layer 180 . they are preferably made of transparent conductor such as ito or izo or reflective conductor such as ag or al . the pixel electrodes 191 are physically and electrically connected to the drain electrodes 175 through the contact holes 185 such that the pixel electrodes 191 receive data voltages from the drain electrodes 175 . the pixel electrodes 191 supplied with the data voltages generate electric fields in cooperation with a common electrode ( not shown ) of an opposing display panel ( not shown ) supplied with a common voltage , which determine the orientations of liquid crystal molecules ( not shown ) of a liquid crystal layer ( not shown ) disposed between the two electrodes . a pixel electrode 191 and the common electrode form a capacitor referred to as a “ liquid crystal capacitor ,” which stores applied voltages after the tft turns off . the pixel electrodes 190 overlap the gate lines 121 and the data lines 171 to increase aperture ratio . the contact assistants 81 and 82 are connected to the end portions 129 of the gate lines 121 and the end portions 179 of the data lines 171 through the contact holes 181 and 182 , respectively . the contact assistants 81 and 82 protect the end portions 129 and 179 and enhance the adhesion between the end portions 129 and 179 and external devices . now , a method of manufacturing the organic tft array panel shown in fig1 and 2 according to an embodiment of the present invention will be described in detail with reference to fig3 - 13 as well as fig1 and 2 . fig3 , 8 , 10 and 12 are layout views of the organic tft array panel shown in fig1 and 2 in intermediate steps of a manufacturing method thereof according to an embodiment of the present invention . fig4 is a sectional view of the tft array panel shown in fig3 taken along line iv - iv ′, fig6 is a sectional view of the tft array panel shown in fig5 taken along line vi - vi ′, fig9 is a sectional view of the tft array panel shown in fig8 taken along line ix - ix ′, fig1 is a sectional view of the tft array panel shown in fig1 taken along line xi - xi ′, and fig1 is a sectional view of the tft array panel shown in fig1 taken along line xiii - xiii ′. fig7 is a photograph illustrating a section of layers after etching an ito layer using a cr etchant . referring to fig3 and 4 , a plurality of gate lines 121 that include gate electrodes 124 and end portions 129 are formed on an insulating substrate 110 that is preferably made of transparent glass , silicone , or plastic . referring to fig5 and 6 , a gate insulating layer 140 is deposited by cvd , etc . the gate insulating layer 140 may have a thickness of about 500 - 3 , 000 å and it may be dipped in ots . thereafter , a conductive layer preferably made of ito is deposited on the gate insulating layer by sputtering , etc . the sputtering is performed at a room temperature ranging about 20 - 35 ° c . such that the sputtered ito layer is an amorphous phase and has uniform film quality from the bottom to the top . subsequently , the conductive layer is then patterned by lithography and wet etching to form a plurality of data lines 171 including source electrodes 173 and end portions 179 and a plurality of drain electrodes 175 . an example of an etchant for the wet etch includes a cr etchant containing hno 3 , ( nh 4 ) 2 ce ( no 3 ) 6 , and h 2 o , which is used for etching cr . the proportions of hno 3 , ( nh 4 ) 2 ce ( no 3 ) 6 , and h 2 o are preferably equal to about 3 - 6 w %, about 8 - 14 w %, and about 80 - 90 w %, respectively , in weight percentage . since the film quality is uniform , the etchant uniformly etches the conductive layer , thereby preventing the loss of the conductive layer caused by non - uniform etch . on the contrary , when the sputtering temperature is higher than about 100 ° c ., the sputtered ito layer includes a lower amorphous portion near the interface with the gate insulating layer 140 and a remaining quasi - crystalline portion . in this case , the amorphous lower portion having lower density than the quasi - crystalline upper portion may be etched more than the quasi - crystalline upper portion such that portions of the ito layer are unintentionally removed . the use of the cr etchant used for etching amorphous ito can reduce the damage on the gate insulating layer 140 that may be organic . on the contrary , a quasi - crystalline ito may require an etchant containing hydrochloric acid that may damage the gate insulating layer 140 . fig7 shows a section of an ito layer after being etched by a cr etchant , which shows no lost portion of the ito layer . the ito layer is shown to be well patterned to have smooth edge profile . next , the data lines 171 and the drain electrodes 175 are annealed to be quasi - crystallized . the annealing is performed preferably at a temperature higher than about 180 ° c . for about one to three hours . referring to fig8 and 9 , an organic semiconductor layer preferably made of pentacene is deposited by molecular beam deposition , vapor deposition , vacuum sublimation , cvd , pecvd , reactive deposition , sputtering , spin coating , etc ., and patterned by lithography and etching to form a plurality of organic semiconductor islands 154 . referring to fig1 and 11 , an insulating layer is dry deposited on the organic semiconductor islands 154 at low temperature or room temperature . the insulating layer may be made of parylene . the low - temperature dry deposition of the insulating layer prevents the organic semiconductor islands 154 from being damaged . the insulating layer is subjected to lithography and dry etch to form a plurality of protective members 164 . the protective members 164 fully cover the organic semiconductor islands 154 . referring to fig1 and 13 , a passivation layer 180 is deposited and patterned along with the gate insulating layer 140 to form a plurality of contact holes 181 , 182 and 185 exposing the end portions 129 of the gate lines 121 , the end portions 179 of the data lines 171 , and portions of the drain electrodes 175 , respectively . since the organic semiconductor islands 154 are fully covered by the protective members 164 , the organic semiconductor islands 154 do not be affected by the formation of the passivation layer 180 . finally , a plurality of pixel electrodes 190 and a plurality of contact assistants 81 and 82 are formed on the passivation layer 180 as shown in fig1 and 2 . at this time , the organic semiconductor islands 154 will not be affected by the formation of the pixel electrodes 190 and the contact assistants 81 and 82 since the organic semiconductor islands 154 are not exposed . as described above , since the ito layer is deposited to have uniform film quality , it is uniformly etched to prevent the loss of the ito layer . furthermore , since the ito layer is deposited in amorphous phase , it can be etched by a cr etchant that may not attack an organic layer under the ito layer . the present invention can be employed to any display devices including lcd and oled display . although preferred embodiments of the present invention have been described in detail hereinabove , it should be clearly understood that many variations and / or modifications of the basic inventive concepts herein taught which may appear to those skilled in the present art will still fall within the spirit and scope of the present invention , as defined in the appended claims . | 7 |
in the description which follows , like parts are marked throughout this description in drawings with the same reference numerals , respectively . the drawing figures are not necessarily to scale . certain features of the invention may be shown exaggerated , in scale or in schematic form , and some details of conventional elements may not be shown in the interest of clarity and conciseness . referring now to fig1 the orienting sleeve 122 , illustrated in partial cross - section , is shown substantially engaged with the sealing member 124 . in this embodiment , the orienting sleeve 122 is shown within a new wellbore 112 which extends vertically to a surface 114 . the wellbore 112 generally extends from the surface 114 through a formation region 116 where it may be desired to induce or inject fluids . the wellbore 112 , however , may extend in other non - vertical directions approaching horizontal . the orienting sleeve 122 is connected to the lower end of the casing 118 before the casing and orienting sleeve 122 are lowered into position within the wellbore 112 . generally , the casing is comprised of multiple segments which are connected at the surface 114 as the casing 118 is lowed into the wellbore 112 . preferably , one or more of the segments include an opening 208 formed in a wall of the casing 118 as shown in fig2 . the opening 208 is defined by a longitudinal position and a lateral position on the casing 118 . the opening 208 is covered by a fiberglass mesh 136 in fig1 . this material , however , may be made of any other substantially impermeable material . determining where to position the orienting sleeve 122 at an appropriate depth and lateral orientation within the wellbore 112 is accomplished by any conventional survey means such as a directional downhole survey of the formation 116 . a conventional directional survey of the wellbore 112 generally will reveal the depth ( longitudinal position ) and lateral position of each region within the formation 116 where hydrocarbons may be found . based upon the survey results , the appropriate number and location of lateral wells is determined and the segments comprising the casing 118 are made up to include one or more pre - formed openings — like the opening covered with fiberglass 136 in fig1 . each segment of the casing 118 is made up so that each opening therein may be aligned with a corresponding area in the formation 116 where a lateral well is desired . thus , the casing 118 and orienting sleeve 122 are made up and lowered into the wellbore 112 to a predetermined depth and lateral orientation which places each opening in the casing 118 in general alignment with a corresponding area in the formation 116 where a respective lateral well is desired . conversely , if openings are not included in the casing 118 , then the orienting sleeve 122 and casing 118 are made up and lowered to a predetermined depth and lateral orientation adequately below the area in the formation 116 where the lateral well furthest from the surface 114 is desired . the orienting sleeve 122 includes a longitudinal reference point which is between the first end 134 and the second end 128 of the orienting sleeve 122 , and a lateral reference point as more particularly described in reference to fig3 and 10 . the longitudinal reference point is preferably the first end 134 or the second end 128 of the orienting sleeve 122 which corresponds with the depth of the orienting sleeve 122 within the wellbore 112 . once the orienting sleeve 122 is secured , its depth and lateral orientation are recorded using the longitudinal reference point and lateral reference point as initial coordinates to locate each opening in the casing 118 and / or area in the formation 116 where a lateral well is desired . each lateral position and longitudinal position disclosed by the directional survey is measured from the lateral reference point and longitudinal reference point in the manner described in reference to fig2 to locate each opening in the casing 118 and / or an area in the formation 116 where a lateral well is desired . once positioned , the orienting sleeve 122 and casing 118 are secured within the wellbore 112 using any hardenable fluid material such as cement , which forms a cement liner 120 around the casing 118 . the cement liner 120 is prepared at the surface 114 in a conventional manner and is transferred by means of a pump through a plurality of connected tubular components forming a drill string 138 . the components comprising the drill string 138 are generally connected by a standard threaded coupling 140 . the cement liner 120 is pumped through the drill string 138 and the sealing member 124 . as the cement liner 120 exits the sealing member 124 , it enters the orienting sleeve 122 and passes through a passage 130 which extends from the first end of the orienting sleeve 134 through the second end of the orienting sleeve 128 . a float shoe 126 is connected to the second end of the orienting sleeve 128 which includes a plunger valve ( not shown ) more particularly described in reference to fig3 . after the cement liner 120 is pumped through the float shoe 126 , it is forced to the bottom of the wellbore 132 and around the orienting sleeve 122 in the direction shown by arrows 146 and 148 . pressure from the pump forces the cement liner 120 to migrate up through the wellbore 112 in the direction indicated by arrows 150 and 152 until it reaches a desired position in the wellbore 112 relative to the surface 114 . once the cement liner 120 reaches this position , it will harden over time and secure the casing 118 and orienting sleeve 122 within the wellbore 112 . the fiberglass cover 136 prevents the cement liner 120 from entering the opening 208 shown in fig2 . referring now to fig3 a detailed cross - sectional view of the orienting sleeve 122 is shown in substantial engagement with a sealing member 124 . the first end 134 of the orienting sleeve 122 includes external threads 310 for threaded engagement with the internal threads 312 of the casing 118 . similarly , the second end 128 of the orienting sleeve 122 includes external threads 314 for threaded engagement with the internal threads 316 of the float shoe 126 . the first end 134 of the orienting sleeve 122 includes a channel 318 which extends toward the second end 128 of the orienting sleeve 122 . the seat 320 supports the sealing member 124 or the orienting member 210 shown in fig2 . the sealing member 124 includes a shoulder 322 for engagement with the seat 320 . the passage 130 includes an internal diameter 324 large enough to receive at least a portion of the sealing member 124 or orienting member 210 shown in fig2 . the lower end 326 of the sealing member 124 includes a fluid passage 328 which opens into passage 130 of the orienting sleeve 122 . the drill string 138 in fig1 and passage 130 form a conduit through which the cement liner 120 is pumped . a valve 330 is secured within the passage 130 by a spring 332 which rests on support brackets 334 and 336 . a plate 338 is positioned in passage 130 . the plate 338 and brackets 334 , 336 are attached to the inside diameter 324 of the orienting sleeve . 122 by any conventional means . the plate 338 includes an opening 340 for partial receipt of the valve 330 . and , the brackets 334 , 336 include a plurality of openings ( not shown ) which allow the cement liner 120 to pass therethrough . brackets 334 and 336 support the spring 332 and allow the valve 330 to depress between the brackets 334 , 336 . the pressure of the cement liner 120 depresses valve 330 , causing the cement liner 120 to pass through opening 340 . the float shoe 126 includes an opening 344 which communicates with passage 130 . the opening 344 is large enough for receipt of a portion of the valve 342 . the pressure of the cement liner 120 causes valve 342 to depress the spring 346 , permitting the cement liner 120 to pass through opening 344 into chamber 348 . further pressure from the cement liner 120 causes cement contained in the chamber 348 to pass through openings 350 , 352 in the float shoe 126 into the wellbore 112 as described in reference to fig1 . a portion of the float shoe 126 contains a bore 354 for receipt of a lower portion of the valve once the valve 342 is depressed and compresses the spring 346 . alternatively , the second end 128 of the orienting sleeve 122 may be connected to a first end of another one of the casing segments ( not shown ). a second end ( not shown ) of the other casing segment is connected to a float shoe similar to float shoe 126 . the other casing segment thus functions as a back - up reservoir for receipt of any excess portion of the cement liner 120 which may re - enter the float shoe from the wellbore 112 . as another alternative , the second end 128 of the orienting sleeve 122 includes another valve ( not shown ) similar to valve 330 to further restrict movement of the cement liner 120 from the second end 128 to the first end 134 of the orienting sleeve 122 . each valve utilized in the orienting sleeve 122 or the float shoe 126 is a plunger valve , however , may include any other type of valve capable of performing the function thus described . a guide 360 is positioned within the orienting sleeve 122 by heating the orienting sleeve 122 , inserting the guide 360 and cooling the orienting sleeve 122 to secure the guide 360 in position . the guide 360 may , however , be secured within the orienting sleeve 122 by any other conventional means . the guide 360 includes a passage ( not shown ) for receipt of the lower end 326 of the orienting sleeve 122 . likewise , the lower end 326 is partially circumscribed by a reciprocating guide 364 . the guide 360 and reciprocating guide 364 each include an orienting surface 366 and 368 , respectively . each orienting surface 366 , 368 , commonly referred to as a muleshoe , has a curvilinear edge 367 and 369 that tapers to form a curved end 370 and 372 , respectively . the guide 360 is thus positioned within the orienting sleeve 122 to permit a portion of the fluid passage 368 to extend longitudinally beyond and below the guide 360 when the orienting surfaces 366 and 368 are substantially engaged . each curved end 370 , 372 enables the sealing member 124 and orienting sleeve 122 to rotate as each curved end 370 , 372 comes into contact with the corresponding orienting surface 366 , 368 until substantially engaged as shown in fig3 . when the guide 360 and reciprocating guide 364 are substantially engaged , the shoulder 322 of the sealing member 124 is substantially supported by the engaged seat 320 of the orienting sleeve 122 . the primary function of the guide 360 is to align the orienting member 210 and orienting sleeve 122 , as described in reference to fig5 and 7 . although not typically required , however , the sealing member 124 and orienting sleeve 122 may be aligned when the orienting surfaces 366 , 368 are substantially engaged . a pair of o - ring seals 356 and 358 are positioned between the lower end 326 of the sealing member 124 and guide 360 in order to mitigate any back - flow of the cement liner 120 between the lower end 326 and guide 360 . another o - ring seal 362 is positioned between the orienting sleeve 122 and reciprocating guide 364 in order to mitigate any back - flow of the cement liner 120 between the orienting sleeve 122 and the reciprocating guide 364 as shown in reference to fig4 . referring now to fig5 and 7 , an orienting member 210 is shown in various positions relative to a cross - sectional view of the orienting sleeve 122 . the orienting member 210 includes a flange 511 which substantially prevents rotational movement of the orienting member 210 when the flange 511 is disposed substantially within the channel 318 as shown in to fig7 in fig7 the orienting sleeve 122 and orienting member 210 are shown aligned . although it is not always necessary to restrict rotational movement of the sealing member 124 shown in fig3 a flange ( not shown ) may be attached by any conventional means to the sealing member 124 in order to restrict rotational movement of the sealing member 124 in the manner thus described . the orienting member 210 includes a stinger 513 which is used to stab and locate the orienting sleeve 122 . typically , the stinger 513 contacts the seat 320 of the orienting member 210 causing the stinger 513 to align within the passageway 130 in the first end 134 of the orienting sleeve 122 . the orienting member 210 also includes a reciprocating guide 510 which partially circumscribes the stinger 513 . the reciprocating guide 510 includes an orienting surface 512 commonly referred to as a muleshoe . the orienting surface 512 has a curvilinear edge 514 that tapers to form a curved end 516 . the curvilinear edge 514 and curved end 516 guide the orienting member 210 into alignment with the orienting sleeve 122 as shown in fig7 . the curved end 516 contacts a portion of the orienting surface 366 which causes the orienting member 210 to rotate counterclockwise as shown in fig6 . if the curved end 516 meets the curved end 370 on the guide 360 , then the orienting member 210 is forced to rotate in either direction ( clockwise or counterclockwise ) as it is forced toward the second end 128 of the orienting sleeve 122 . as the reciprocating guide 510 traverses down through the passage 130 , the stinger 513 enters passage 518 in the guide 360 shown in fig5 . in fig7 the orienting surface 512 traverses the orienting surface 366 until the guide 360 and reciprocating guide 510 are substantially engaged . once the guide 360 and reciprocating guide 510 are substantially engaged , the flange 511 will be substantially disposed within the channel 318 and a shoulder 518 on the orienting member 210 will be substantially supported by the engaged seat 320 . once the flange 511 is substantially disposed within the channel 318 , the orienting member 210 and orienting sleeve 122 are aligned and the orienting member 210 is oriented in a predetermined lateral position relative to a lateral position on the casing 118 which defines the lateral position of the opening 208 shown in fig2 . referring now to fig8 the channel 318 is slightly larger than the flange 511 which enables the flange 511 to enter the channel 318 before the guide 360 and reciprocating guide 510 are substantially engaged . consequently , nominal rotational movement of the orienting member 210 will occur once the guide 360 and reciprocating guide 510 are substantially engaged , however , will not compromise the ability to locate the lateral position of the opening 208 shown in fig2 . in fig5 - 7 , the channel 318 defines the lateral reference point and a portion of the orienting sleeve 122 between the first end 134 and the second end 128 defines the longitudinal reference point . preferably , the first end 134 or the second end 128 is chosen to define the longitudinal reference point . referring now to fig9 and 10 , another embodiment of an orienting member 910 is shown in various positions relative to another embodiment of an orienting sleeve 912 . in this embodiment , the orienting sleeve 912 includes a key 914 instead of the guide 360 shown in fig3 . the key 914 acts as a guide for the orienting member 910 . the orienting sleeve 912 is identical in all other respects to the orienting sleeve 122 in fig3 except that it includes a pair o - ring seals 916 and 918 above the key 914 which restrict the cement liner 120 from passing between the orienting sleeve 912 and the sealing member 124 described in reference to fig3 . accordingly , the orienting sleeve 912 includes a channel 920 for receipt of a flange 922 attached to the orienting member 910 by any conventional means . the orienting sleeve 912 includes a seat 924 to support the orienting member 910 when the seat 924 and a shoulder 926 on the orienting member 910 are engaged . the orienting member 910 is similar in most respects to the orienting member 210 described in reference to fig5 except that a channel forming a keyway 930 is positioned in a lower end 928 of the orienting member 910 . the lower end 928 partially circumscribes a stinger 948 . the keyway 930 includes an end stop 932 which contacts an upper surface 934 of the key 914 when the orienting member 910 and orienting sleeve 912 are aligned as shown in fig1 . the lower end 928 includes an orienting surface 936 similar to that described in reference to fig5 except that the curvilinear edge 938 tapers to form a pointed tip 940 which prevents jamming the orienting member 910 when the tip 940 meets the upper surface 934 . as shown in fig9 the curvilinear edge 938 transitions into the keyway 930 through a transition surface 942 which permits the key 914 to traverse the orienting surface 936 and keyway 930 as the orienting member 910 passes through the first end 944 toward the second end 946 of the orienting sleeve 912 . the stinger 948 is used to stab and locate the orienting sleeve 912 in order to position the orienting member 910 . in fig1 , the orienting member 910 is substantially engaged with the orienting sleeve 912 as shown by contact between the shoulder 926 and seat 924 of the orienting sleeve 912 . at this position , the orienting member 910 is aligned with the orienting sleeve 912 and substantially free from rotational movement . accordingly , the key 914 is engaged with the end stop 932 at this position . the end stop 932 is positioned at a distal end of the keyway 930 so that when the key 914 contacts the end stop 932 , the flange 922 should be substantially disposed within the channel 920 . in fig9 - 10 , the channel 920 or the key 914 defines the lateral reference point and a portion of the orienting sleeve 912 between the first end 944 and the second end 946 defines the longitudinal reference point . preferably , the first end 944 or the second end 946 is chosen to define the longitudinal reference point . referring now to fig2 an elevational view of the orienting sleeve 122 is shown in connection with the orienting member 210 and other components needed to locate the lateral position and longitudinal position of an opening 208 . once the casing 118 has been secured within the wellbore 112 , the sealing member 124 shown in fig1 is removed from wellbore 112 and replaced with the components shown in fig2 . the components shown in fig2 include a diverter 234 , an extension member 216 , and the orienting member 210 . these components are lowered into the casing 118 using the drill string 138 which is operatively and releaseably connected to the diverter 234 . because a directional survey has already been performed to position the orienting sleeve 122 at a predetermined depth and lateral orientation within the wellbore 112 , another directional survey is unnecessary . before these components are lowered into the casing 118 , the face 232 of the diverter 234 is aligned with the first lateral position and the first longitudinal position which define the opening 208 next to a desired area of the formation 214 . as described in reference to fig1 the exact longitudinal position and lateral position of the opening 208 are determined before the casing 118 is secured to the wellbore 112 . thus , the longitudinal position and lateral position of the opening 208 can be measured from the predetermined longitudinal reference point ( 128 or 134 in fig5 ) and lateral reference point ( 318 in fig5 ), respectively . the diverter 234 is aligned with the longitudinal position of the opening 208 using the extension member 216 and the face 232 of the diverter 234 is aligned with the lateral position of opening 208 using unilateral connections and a multilateral connection , in the manner described in reference to u . s . pat . no . 6 , 427 , 777 . the length of the extension member 216 can be varied by using shorter or longer components 218 , 220 and 236 . each unilateral connection 222 maintains alignment between the orienting member 210 and the face 232 of the diverter 234 in a single lateral direction . the multilateral connection 230 permits the alignment maintained by the unilateral connections to be adjusted in pre - selected increments . once the components in fig2 are made up in the manner thus described , the components are lowered into the wellbore 112 until the orienting member 210 substantially engages the orienting sleeve 122 and the face 232 of the diverter 234 is aligned with the opening 208 . an anchor 238 may be used when the extension member 216 is extremely long and needs additional support . the drill string 138 is disconnected from the diverter 234 by compressing the system . once disconnected , the probe 242 engages the face 232 of the diverter 234 causing the probe 242 to bore through the fiberglass mesh 136 , cement liner 120 and desired formation 214 . the present invention may also be used in applications where there is no opening 208 in the casing 118 and the lateral well 212 is formed in two separate runs because two different probes 240 are used . two separate runs are required because the first probe used to mill through the casing 118 must be removed at the surface 114 and replaced with another probe used to drill to drill through formation 214 . in this event , the directional survey results are used to generally determine the lateral position and longitudinal position of a desired area in the formation 214 relative to the longitudinal reference point and lateral reference point on the orienting sleeve 122 . in this manner , the face 232 of the diverter 234 can be aligned with these coordinates to begin formation of the lateral well . once the lateral well 212 is formed , the drill string 138 and probe 242 are removed from the wellbore 112 , and the orienting member 210 , extension member 216 , and diverter 234 are retrieved . the process is repeated for each desired lateral well . accordingly , another lateral well may be formed by simply adjusting the length of the extension member 216 and lateral orientation of diverter 234 . for example , if another opening ( not shown ) in the casing 118 is used to form another lateral well ( not shown ), the extension member 216 may be shortened or lengthened to align the face 232 of the diverter 234 with the longitudinal position of the new opening relative to the longitudinal reference point and the multilateral connection 230 may be adjusted to align the face 232 of the diverter 234 with the lateral position of the new opening relative to the lateral reference point . alternatively the extension member 216 may be shortened or lengthened to align the face 232 of the diverter 234 with the longitudinal position of the new opening relative to the longitudinal position of the opening 208 and the multilateral connection 230 may be adjusted to align the face 232 of the diverter 234 with the lateral position of the new opening relative to the lateral - position of the opening 208 . because the orienting sleeve 122 is designed for receipt of the sealing member 124 in fig3 and the orienting member 210 in fig5 the wellbore 112 and a lateral wellbore 212 may be completed in a more economic and efficient manner — particularly when one or more openings like the opening 208 are utilized to eliminate the step of milling through the casing 118 . moreover , the orienting sleeve 122 provides a lateral reference point and longitudinal reference point to locate the longitudinal position and lateral position of the opening 208 in the casing 118 which cannot be accurately located using other conventional methods and equipment . although the objects and advantages of the present invention have been described in detail , those skilled in the art should understand that they can make various changes , substitutions and alterations herein without departing from the spirit and scope of the present invention in its broadest form . | 4 |
fig3 shows a sectional view of a first embodiment in accordance with the present invention , in which a direct backlight module 3 has a diffuser 31 connected to a reflecting plate 32 . a chamber 35 is formed between the diffuser 31 and the reflecting plate 32 . in the chamber 35 , a plurality of light sources 34 are disposed . in this embodiment , the plurality of light sources 34 are lamps . in order to overcome deformation of the diffuser 31 due to the size of the diffuser 31 and the heat from the light sources 34 , a transparent support 33 is disposed between the diffuser 31 and the reflecting plate . in the embodiment , the transparent support 33 is integrally formed by injection molding , comprising several retaining portions 331 connected to a supporting plate 332 . the flat supporting plate 332 fixes and retains the shape of the diffuser 31 . the retaining portions 331 are arranged between the light sources 34 according to diffusion requirements , supporting the supporting plate 332 and the diffuser 31 . the transparent supports 33 comprise transparent material to not affect the brightness of the backlight module . to further aid optical uniformity , the transparent supports 33 may also comprise diffusion material or such may be coated on the surface thereof . furthermore , a first diffuser plate 36 , a prism 37 and a second diffuser plate 38 are disposed on the diffuser 31 . the first diffuser plate 36 is disposed on the diffuser 31 , the prism 37 is disposed on the first diffuser plate 36 , and the second diffuser plate 38 is disposed on the prism 37 , with amounts and sequences of disposition dictated by demand . fig4 a to 4 c show top views of a first type of transparent supports . the supporting plates 412 , 422 and 432 of the transparent supports 41 , 42 and 43 are respectively rectangular , circular and polygonal . the supporting plates 412 , 422 and 432 are integrated with the retaining portions 411 , 421 and 431 arranged thereunder . shape of the supporting plates may be designed according to the diffuser used . the area of the transparent supports may be reduced to support the diffuser . retaining portion numbers vary with demand . for example , the transparent support 42 with circular supporting plate 422 , as shown in fig4 b , has only one retaining portion disposed at the center of the supporting plate 422 . fig5 a to 5 b show top views of a second type of transparent supports . fig5 a to 5 b , the supporting plates 512 and 522 of the transparent supports 51 and 52 are , respectively , rectangular and circle hollow frames . the retaining portions 511 and 521 are arranged under the supporting plates 512 and 522 . shape of the supporting plates can vary according to the diffuser . the design of the hollow frame can reduce the area of the transparent supports and decrease the overall weight of the direct backlight module while supporting the diffuser . a majority of light is directly emitted into the diffuser without passing through the supports , such that brightness of the direct backlight module is more uniform . in the present invention , the transparent supports are not limited to an integral type , and may be combined with several supporting units . fig6 a to 6 b are top views of a second embodiment of a direct backlight module in accordance with the present invention . in fig6 a , the transparent support 60 of the direct backlight module 6 comprises two supporting units 61 . each supporting unit 61 is formed by retaining portions 611 and a supporting plate 612 . the retaining portions 611 contact the reflecting plate ( not shown ), and the supporting plate 612 contacts the diffuser 62 . the supporting units 61 are arranged in array to support the diffuser . fig6 b shows small - scale supporting units 63 arranged in array . the transparent support formed by the small - scale supporting units not only supports the diffuser but can also be conveniently transported . further , the small - scale supporting units can vary with the size of the panel with the direct backlight module to reduce costs . in the present invention , the transparent supports are not limited to an integral type , and may be combined with several different sizes of supporting units . fig7 a to 7 b are top views of a third embodiment of a direct backlight module in accordance with the present invention . in fig7 a , the transparent support 70 of the direct backlight module 7 comprises two supporting units 71 arranged in concentric circles . each supporting unit 71 is formed by retaining portions 711 and a supporting plate 712 , a hollow frame . the retaining portions 711 contacts the reflecting plate ( not shown ), and the supporting plate 712 contacts the diffuser 72 . the supporting units 71 are arranged in concentric circles to support the diffuser . in fig7 b , the supporting units 73 constituting a transparent support 70 are arranged homocentrically . the transparent support 70 comprising the different sizes of supporting units 73 supports the diffuser and prevents deformation thereof . further , the hollow design of the supporting plate not only reduces the area of the transparent supports but also weight of the direct backlight module 7 . a majority of light is directly emitted into the diffuser without passing through the supports , such that brightness of the direct backlight module is more uniform . according to the present invention , the transparent supports prevent the diffuser from deformation irrespective of the size thereof , affecting brightness . finally , while the invention has been described by way of example and in terms of the preferred embodiments , it is to be understood that the invention is not limited to the disclosed embodiments . on the contrary , it is intended to cover various modifications and similar arrangements as would be apparent to those skilled in the art . therefore , the scope of the appended claims should be accorded the broadest interpretation so as to encompass all such modifications and similar arrangements . | 5 |
referring now to fig1 , an embodiment of a drum assembly is indicated generally at 100 . the drum assembly 100 comprises a drum 102 which is operable to have a spooled device 103 wound thereupon such as , but not limited to , a logging cable , a slickline cable , and coiled tubing . the drum 102 comprises a spool 104 and a pair of opposed flanges 106 . the drum 102 is attached to a mounting location , indicated generally at 108 of a mounting base 109 , such as an offshore oil rig or the like . the mounting location 108 and mounting base 109 may further comprise a frame assembly 110 disposed above the mounting location 108 . a sprocket 112 ( best seen in fig8 ) may be mounted on an exterior surface of one of the flanges 106 and is attached , via a chain assembly 114 or the like , to a prime mover 116 , such as an internal combustion engine , an electric motor , a hydraulic motor , a combination thereof , or the like through a transmission 117 , for rotating the drum 102 during a well servicing operation with the spooled device 103 , wherein the spooled device 103 is lowered and raised into a wellbore ( not shown ). in an embodiment , the prime mover 116 is directly connected to the drum 102 such as by the sprocket 112 and chain assembly 114 or the like . such a well servicing operation performed by the spooled device 103 may comprise , but is not limited to , a logging operation , conducted by a tool 118 attached to an end of the cable 103 lowered into the wellbore 120 , a perforating operation , a completion operation , a stimulation operation , or other well servicing operation or operations , as will be appreciated by those skilled in the art . the chain assembly 114 may be a heavy - duty chain or the like having links that engage with spindles on the sprocket 112 and on the transmission 117 of the prime mover 116 , thus providing a direct drive of the drum assembly 100 for lowering and raising the spooled device 103 into and out of the wellbore 120 . the chain assembly 114 may be protected by a cover 115 , best seen in fig4 , or the like . referring now to fig6 , there is shown a connection 122 between the chain assembly 114 and the drum sprocket 112 . the connection 122 may be of a quick connect and disconnect type and may comprise , but is not limited to , a bolted disc , a clutch , a splined shaft , a keyed shaft , an elastic rubber coupling , or similar quick connect and quick disconnect connection . the connection 122 advantageously allows the prime mover 116 and transmission 117 to remain connected to the mounting base 109 when the drum assembly 100 is removed from the mounting location 108 . the connection 122 may further be mechanically assisted , such as by a hydraulic actuator , an electric actuator , a hydraulic motor , an electric motor or the like , as will be appreciated by those skilled in the art . the ability for the connection 122 to be quickly connected and disconnected may advantageously reduce the number and complexity of steps required to change the drum assembly 100 during a change - out operation , discussed in more detail below . referring now to fig1 , the drum assembly further comprises a plurality of connectors 124 between the drum assembly 100 and the mounting location 108 . the connectors 124 may be of a quick connect and quick disconnect type and may comprise , but are not limited to , those connectors utilized for intermodal containers or the like including those manufactured by the tandemloc corporation , as will be appreciated by those skilled in the art . a lifting apparatus 126 , best seen in fig2 , is operable to be attached to the drum 102 , such as by a threaded connection to the flanges 106 or by any suitable connection . the lifting apparatus 126 allows a crane ( not shown ) or similar lifting device to move the drum assembly 100 to and from the mounting location 108 ( after the connectors 124 have been disconnected ) during a change - out operation , discussed in more detail below . the drum 102 may comprise a predetermined location thereon for mounting the lifting apparatus 126 . referring now to fig5 , there is shown at least one guide member 128 adapted to be attached to the frame assembly 110 adjacent the mounting location 108 . the guide member 128 engages with the lifting apparatus 126 when the drum assembly 100 is removed from the mounting location 108 to prevent the drum assembly 100 from swinging or otherwise moving until it is fully outside of the frame assembly 110 of the mounting base 109 . such a guide member 128 may be especially advantageous when the drum assembly 100 is mounted on an offshore oil platform , as will be appreciated by those skilled in the art . the guide member 128 may define a track 130 and the lifting apparatus 126 may have wheels 132 for engaging with the track 130 when the drum assembly 100 is removed from the mounting location 108 . a portion of the guide member 128 may be substantially vertical or parallel with the frame assembly 110 and a portion of the guide member may be substantially horizontal , as will be appreciated by those skilled in the art . in a change - out operation , when the drum assembly 100 is to be changed with another drum assembly 100 , the prime mover 116 is de - energized , and the guide member or members 128 are attached to the frame assembly 110 and the lifting apparatus 126 is attached to the drum 102 . the connection 122 between the chain assembly 114 and the sprocket 112 is disconnected , and the connectors 124 between the drum assembly 100 and the mounting location 108 are disconnected . the lifting apparatus 126 is attached to a winch or the like and lifts the disconnected drum assembly 100 from the mounting location 108 . the wheels 132 engage with the guide members 128 and provide a predetermined path for moving the drum assembly 100 away from the frame assembly 110 and mounting location 108 . after the drum assembly 100 is clear of the frame assembly 110 , it is placed in a preferably secure location , the lifting apparatus 126 is detached from the drum 102 and attached to another drum 100 . the other drum assembly 100 is installed utilizing the same above - mentioned steps in a reversed order to attach the drum assembly 100 to the mounting location 108 and the chain assembly 114 , as will be appreciated by those skilled in the art . embodiments of the drum assembly 100 ease the swap of drums 102 , regardless of whether a spooled device 103 such as a logging cable , is disposed on the drum 102 for those assemblies 100 disposed either onshore or offshore . the drum assembly 100 will drastically reduce the time needed to dismount and / or install a drum , such as the drum 102 , and therefore will reduce the rig - up time for logging operations , advantageously allowing for increased efficiency at the job site . the particular embodiments disclosed above are illustrative only , as the invention may be modified and practiced in different but equivalent manners apparent to those skilled in the art having the benefit of the teachings herein . furthermore , no limitations are intended to the details of construction or design herein shown , other than as described in the claims below . it is therefore evident that the particular embodiments disclosed above may be altered or modified and all such variations are considered within the scope and spirit of the invention . in particular , every range of values ( of the form , “ from about a to about b ,” or , equivalently , “ from approximately a to b ,” or , equivalently , “ from approximately a - b ”) disclosed herein is to be understood as referring to the power set ( the set of all subsets ) of the respective range of values . accordingly , the protection sought herein is as set forth in the claims below . the preceding description has been presented with reference to presently preferred embodiments of the invention . persons skilled in the art and technology to which this invention pertains will appreciate that alterations and changes in the described structures and methods of operation can be practiced without meaningfully departing from the principle , and scope of this invention . accordingly , the foregoing description should not be read as pertaining only to the precise structures described and shown in the accompanying drawings , but rather should be read as consistent with and as support for the following claims , which are to have their fullest and fairest scope . | 1 |
the alkyl moiety in the lower alkyl group or lower alkoxy group as referred to in the present invention preferably has from 1 to 4 carbon atoms . examples of the azetidinone ( ii ) which is used as a raw material in the present invention include azetidin - 2 - one , 3 - methylazetidin - 2 - one , 3 - ethylazetidin - 2 - one , 3 - hydroxyethylazetidin - 2 - one , 3 - methyl - 4 - carboxyazetidin - 2 - one , 3 - ethyl - 4 - carboxyazetidin - 2 - one , 3 -( protected ) hydroxyethyl - 4 - carboxyazetidin - 2 - one , 4 - methylazetidin2 - one , and 4 - methoxycarbonylazetidin - 2 - one . as the protective group of the hydroxyl group , those which are generally used for protection of hydroxyl group in lactam compounds can be used . examples thereof include silyl groups ( e . g ., trimethylsilyl , triethylsilyl , tert - butyldi - methylsilyl , and diphenyl - tert - butylsilyl ), a benzyloxycarbonyl group , a p - nitrobenzyloxycarbonyl group , and an o - nitrobenzyl - oxycarbonyl group . of the above - enumerated azetidinone derivatives ( ii ), a compound in which z is a ( protected ) hydroxyethyl group , and y is hydrogen atom can be produced from a compound of formula ( iii ) which is derived , for example , from acetoacetic acid ber ., 92 , p . 1599 ( 1959 )], according to the following reaction scheme . ## str6 ## in the above reaction scheme , r 2 represents a protective group of a carboxylic acid ; r 3 represents a hydrogen atom , a lower alkyl group , a lower alkoxy group , or a phenyl or benzyloxy group which may be substituted with a lower alkyl group or a lower alkoxy group ; and r 4 represents a protective group of a hydroxyl group . that is , compound ( iii ) is subjected to enantio - selective hydrogenation using a ruthenium - optically active phosphine complex as a catalyst to give compound ( iv ), which is then hydrolyzed with a dilute acid , etc . into compound ( v ). compound ( v ) is neutralized to give compound ( vi ), which is then lactamization to obtain compound ( ii - 1 ). subsequently , the hydroxyl group of this compound ( ii - 1 ) is protected to give compound ( ii - 2 ). examples of the osmium compound used as a catalyst in the present invention are anhydrous or hydrous osmium tri - chloride , osmium tribromide , and osmium triiodide . of these , osmium trichloride is particularly preferred . the oxidizing agent used in the present invention is not especially limited . examples thereof include peroxides of various carboxylic acids , other peroxides , high - concentration bleaching powder , ozone , cyclohexene ozonide , sodium peroxide , sodium perborate , iodosylbenzene diacetate , iodosylbenzene , sodium metaperiodate , and sodium paraperiodate . specific examples of the carboxylic acid peroxides include peracetic acid , perpropionic acid , and m - chloroperbenzoic acid . these compounds may be ones which are commercially available , or they may be prepared separately from a carboxylic acid and hydrogen peroxide before the reaction . further , specific examples of other peroxides include methyl ethyl ketone peroxide , methyl isobutyl ketone peroxide , cyclohexanone peroxide , methyl - cyclohexanone peroxide , diacetyl peroxide , dipropionyl peroxide , and diisobutyryl peroxide . use of peracetic acid as the oxidizing agent is advantageous in that it is not particularly required to add acetic acid to the reaction system because acetic acid is usually incorporated in peracetic acid . it is preferred in the present invention to conduct the reaction with acetic acid in the presence of an acetic acid salt , since the presence of an acetic acid salt results in an improved yield . examples of the acetic acid salt include sodium acetate , potassium acetate , and lithium acetate . the present invention can , for example , be practiced as follows . compound ( ii ), an oxidizing agent , acetic acid , and an osmium compound are dissolved or suspended in a suitable solvent , and the solution or suspension is reacted with stirring at a temperature of - 10 ° c . to 50 ° c . for from 10 minutes to 5 hours , and preferably about 2 hours . the addition order and method of the raw material compound , catalyst , and other ingredients are not particularly limited . it is , however , desirable that the oxidizing agent be added gradually after all the other ingredients . as the solvent , organic solvents such as acetonitrile , methylene chloride , acetone , acetic acid , and acetic acid esters can be used . the amount of acetic acid used is preferably from 10 to 60 mole , and more preferably from 20 to 40 mole , per mole of compound ( ii ), while the amount of the oxidizing agent used is preferably from 1 to 8 mole , and more preferably from 2 to 3 mole , per mole of compound ( ii ). the amount of the osmium compound which is used as a catalyst is preferably from 0 . 001 to 0 . 05 mole , and more preferably from 0 . 01 to 0 . 03 mole , per mole of compound ( ii ). isolation of the desired compound from the resulting reaction mixture can be accomplished by a known means such as , for example , recrystallization and column chromatography . the process of the present invention is more advantageous in efficiently obtaining a 4 - acetoxyazetidinone derivative than the above - described method employing a ruthenium compound as a catalyst . that is , in the conventional method employing a ruthenium compound as a catalyst , the ruthenium compound should be used in an amount as large as about 10 mole % of the substrate azetidinone , whereas in the present invention , a 4 - acetoxyazetidinone can be obtained in good yield as long as the osmium compound is used even in an amount as small as about 2 mole % of the substrate . the compounds obtained by the process of the present invention are industrially useful compounds . of these , ( 1 &# 39 ;, r , 3r , 4r )- 4 - acetoxy - 3 -( 1 &# 39 ;- tert - butyldimethylsilyloxy )- ethylazetidin - 2 - one of the formula : ## str7 ## wherein t - bu is a tert - butyl group ; and ac is an acetyl group , is a particularly useful intermediate indispensable for syntheses of thienamycin and other important penem antibiotics . according to the present invention , this compound can be obtained at a diastereomer selectivity of 99 % or more . as described above , the process of the present invention can produce 4 - acetoxyazetidinone derivatives ( i ) useful as intermediates for synthesis of penem antibiotics by simple procedures with good catalytic activity and , hence , is an industrially advantageous process . the present invention will be explained below in more detail with reference to the following examples , which should not be construed to be limiting the scope of the invention . to a mixture of 200 mg ( 2 . 8 mmole ) of azetidin - 2 - one , 230 mg ( 2 . 8 mmole ) of anhydrous sodium acetate , 2 ml of acetic acid , and 17 mg ( 2 mole % based on the amount of azetidin - 2 - one ) of osmium trichloride trihydrate was added dropwise , with stirring , 1 . 56 g ( 6 . 2 mmole ) of a 30 % peracetic acid solution in ethyl acetate at room temperature over a period of 2 hours or more . the reaction mixture was poured into 50 ml of water and extracted with n - hexane . the extract was separated and purified by silica gel column chromatography ( n - hexane / ethyl acetate = 1 / 1 by volume ). thus , 280 mg ( 2 . 2 mmole , percent yield : 78 %) of 4 - acetoxyazetidin - 2 - one in a colorless oily state was obtained . the same procedures as in example 1 were repeated except that the substrate azetidinone and the amount ( mole %) of osmium trichloride trihydrate relative to the amount of the substrate were changed as shown in table 1 . as a result , the 4 - acetoxyazetidinones as shown in table 1 were obtained from the respective substrates in respective percent yields shown in the same table . table 1__________________________________________________________________________ex . synthesized 4 - oscl . sub . 3 . 3h . sub . 2 o percentno . substrate acetoxyazetidinone ( mol %) yield (%) __________________________________________________________________________ ## str8 ## ## str9 ## 2 763 ## str10 ## ## str11 ## 2 434 ## str12 ## ## str13 ## 2 925 ## str14 ## ## str15 ## 2 776 ## str16 ## ## str17 ## 2 48__________________________________________________________________________ to a mixture of 200 mg ( 0 . 87 mmole ) of ( 1 &# 39 ; r , 3s )- 3 -( 1 &# 39 ;- tert - butyldimethylsilyloxy ) ethylazetidin - 2one , 72 mg ( 0 . 87 mmole ) of anhydrous sodium acetate , 2 ml of acetic acid , and 7 mg of osmium trichloride trihydrate was added dropwise , with stirring , 1 . 91 mmole of each of the oxidizing agents as shown in table 2 at room temperature over a period of 2 hours or more . ( the oxidizing agents were used as they were or in the form of a methylene chloride solution .) each of the reaction mixtures was poured into 50 ml of water and extracted with n - hexane . the extract was distilled in vacuo and separated and purified by silica gel column chromatography ( n - hexane / ethyl acetate = 8 / 1 by volume ). thus , ( 1 &# 39 ; r , 3r , 4r )- 4 - acetoxy - 3 -( 1 &# 39 ;- tert - butyldimethylsilyloxy ) ethylazetidin - 2 - one was obtained in a percent yield shown in table 2 . table 2______________________________________example oxidizing oscl . sub . 3 . 3h . sub . 2 o percentno . agent ( mole %) yield (%) ______________________________________7 ch . sub . 3 co . sub . 3 h 2 . 3 928 mcpba . sup . 1 ) 2 . 3 739 phi ( oac ). sub . 2 . sup . 2 ) 2 . 3 7010 phio . sup . 3 ) 2 . 3 6711 mekp . sup . 4 ) 2 . 3 70______________________________________ . sup . 1 ) : mchloroperbenzoic acid . sup . 2 ) : iodosylbenzene diacetate . sup . 3 ) : iodosylbenzene . sup . 4 ) : methyl ethyl ketone peroxide to a solution prepared by mixing 500 mg ( 5 mmole ) of 3 - ethylazetidin - 2 - one , 415 mg ( 5 mmole ) of anhydrous sodium acetate , 5 ml of acetic acid , and 30 mg ( abut 2 mole % based on the amount of 3 - ethylazetidin - 2 - one ) of osmium trichloride trihydrate was added dropwise , with stirring , 2 . 8 g ( 11 mmole ) of a 30 % peracetic acid solution in ethyl acetate at room temperature over a period of 2 hours or more . the reaction mixture was further stirred at room temperature for 4 hours , subsequently poured into 80 ml of water , and then extracted thrice with 100 ml of hexane . the extract was dried over anhydrous magnesium sulfate , and the solvent was removed by evaporation under reduced pressure . the residue was separated and purified by silica gel column chromatography ( n - hexane / ethyl acetate = 1 / 1 by volume ). thus , 780 mg of 4 - acetoxy - 3 - ethylazetidin - 2 - one was obtained . the percent yield was 78 %. 1 h - nmr ( cdcl 3 ) δ ppm : 0 . 99 ( 3h , t , j = 7 . 4 hz ), 1 . 75 ( 2h , m ), 2 . 10 ( 3h , s ), 3 . 08 ( 1h , m ), 5 . 78 ( 1h , d , j = 1 . 25 hz ), 6 . 55 ( 1h , b , nh ) while the invention has been described in detail and with reference to specific embodiments thereof , it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof . | 2 |
a 70kda plasmodium falciparum exoantigen ( pf70 ) was purified from supernatant fluids of continuous in vitro p . falciparum cultures using sequential cation - exchange and high performance liquid chromatographic procedures . the purified protein was then digested with chymotrypsin and amino acid sequences determined for the resulting fragments . four peptides ( termed c2 , c3 , c5 , c10 ) were subsequently selected for synthesis , based on their predictability for antigenic sites . the individual peptides are usable to detect the presence of antibodies directed toward antigens of malarial organisms . the peptides were effectively used as a synthetic immunogen ( spf70 ) when crosslinked ( copolymerized ) with glutaraldehyde in the absence of a carrier . the synthetic peptide complex , when administered with freund &# 39 ; s adjuvant , was found to be highly immunogenic in rabbits . serologic reactivity to the peptide complex and peptides c2 and c5 was uniformly high , followed by the responses to c3 and c10 . peptide antigenicity was also assessed with human anti - p . falciparum sera from malaria - endemic regions of uganda and venezuela . elisa data showed that anti - p . falciparum antibodies were specific for and reactive to the peptides . the specificity of the rabbit anti - spf70 antibodies for p . falciparum antigen was shown by immunoprecipitation of metabolically labelled proteins and by immunoblotting . herein are described peptide sequences of a 70 kda p . falciparum exoantigen ( pf70 ), that when synthesized and constructed as a copolymer ( spf70 ), are able to induce the formation of antibodies that are reactive with the native malarial protein . the high immunogenicity and antigenic reactivity of spf70 indicate the potential use of this synthetic peptide polymer as an immunogen and diagnostic reagent . indirect fluorescent antibody ( ifa ) tests and enzyme - linked immunosorbent assays ( elisa ) were used to measure antibodies to plasmodium falciparum in patients with acute malaria from bolivar state , venezuela . antibody titers increased significantly with repeated malarial episodes . igg antibody responses to 4 synthetic peptides ( termed c2 , c3 , c5 , c10 ) derived from a 70 kda p . falciparum ( indochina i / cdc strain ) exoantigen were evaluated by a peptide - elisa with overall positivity rates of 20 %, 40 %, 20 % and 58 %, respectively . seropositivity to peptide c10 was consistently over 50 % ( range 53 - 75 %) among patients of different ages . overall igm reactivity to the respective peptides was 53 %, 30 %, 83 % and 70 %. igm reactivity was generally greater in patients with primary malarial infections . the elisa is a useful adjunct to the ifa in measuring naturally - occurring antibodies to specific parasite proteins . the present invention involves synthetic peptide - based enzyme immunoassays ( peptide - elisas ) for the early detection and quantification of p . falciparum asexual blood - stage antibodies in sera of infected individuals from bolivar state , venezuela . the majority of subjects were migrant workers and their families , employed in the gold mines of bolivar state . the nomadic activities of such individuals have made the application of malaria control programs difficult , especially in jungle regions . malariometric indicators have shown a progressive increase in malaria cases in bolivar state since 1983 . the annual parasite incidence ( api ) has steadily increased from 4 . 7 in 1984 to 27 . 4 in 1989 ( ministry of health and social assistance , venezuela ). until quite recently , p . falciparum was responsible for the majority of malaria cases in bolivar , causing 84 % of cases in 1984 . since then the situation has steadily shifted ; of a total of 26 , 418 malaria cases in bolivar in 1989 , 61 . 7 % were due to p . vivax and 38 . 3 % to p . falciparum . malaria transmission in bolivar state is typically unstable . in the present invention four peptides ( termed c2 , c3 , c5 , c10 ) were employed which were synthesized from internal chymotryptic digests of a 70 kda p . falciparum ( indochina i / cdc ) exoantigen ( pf70 ) found in high concentrations circulating in serum of infected individuals and in supernatant fluids of infected in vitro cultures ( m . a . james et al ., manuscript submitted ). the 70 kda antigen is degraded from a 120 kda precursor membrane protein in mature schizonts and increases in amount at the time of schizont rupture ( merozoite release / reinvasion ) ( shamansky et al ., 1985 ; braun - breton et al ., 1986 ). both the peptides and the native protein are highly antigenic and are conserved among diverse geographic isolates , ranging from central and south america to africa and southwest asia ( montenegro - james et al ., 1988 ). the present study was designed to determine the extent of antibody reactivity to the 4 synthetic pf70 - derived peptides among individuals with acute malaria . the 70 kda exoantigen was purified from supernatant fluids of continuous in vitro p . falciparum cultures using sequential chromatographic procedures previously described ( shamansky 1986 ; shamansky et al . 1985 ). p . falciparum parasites ( indochina i / cdc strain ) were cultured in vitro using human a + erythrocytes and 10 % human a + serum ( trager and jensen 1976 ). supernatants were collected daily from asynchronous cultures at an average parasitemia of 2 - 3 %. supernatants were stored at - 70 ° c . before use in purification procedures . exoantigens were partially purified from crude culture supernatants by sulfopropyl ( sp )- trisacryl ( crosslinked agarose with a propysulfonate ) ( pharmacia lkb biotechnology , inc ., piscataway , n . j .) cation - exchange chromatography ( thelu et al . 1985 ). briefly , supernatant fluids were thawed and pooled , concentrated 10 times by pervaporation at 4 ° c ., and then dialyzed against 60 volumes of 0 . 01m sodium acetate buffer ( ph 3 . 7 ) for 48 h at 4 ° c . subsequently , this material was placed on an sp - trisacryl column ( 50 × 200 mm ), and proteins were eluted in 0 . 01m sodium acetate buffer ( ph 3 . 7 ) with an increasing stepwise salt gradient to 0 . 3m nacl at a flow rate of 300 ml / h . antigenic fractions ( 250 ml per fraction ) were monitored by an enzyme - linked immunosorbent assay ( elisa ) using an immune human reference serum pool [ african origin ; indirect fluorescent antibody ( ifa ) titer = 1 : 5 , 120 ]. positive fractions were pooled , concentrated by lyophilization , and dialyzed against 0 . 01m phosphate - buffered saline ( pbs ) ( ph 7 . 2 ) for 48 h at 4 ° c . these fractions , enriched for the 70 kda exoantigen as determined by immunoblotting , were subsequently purified by a sequential high performance liquid chromatography ( hplc ) series . a 3 - step hplc scheme employing gel filtration ( dupont zorbax gf - 250 analytical gel filtration high performance liquid chromatography column , 9 . 4 × 250 mm ), diethylaminoethyl ( deae ) anion - exchange ( waters protein pak deae - 5 pw , 7 . 5 × 75 mm ), and phenyl hydrophobic interaction ( beckman tsk - phenyl - 5pw , 7 . 5 × 75 mm ) columns was used . chromatographic conditions were carried out according to previously described procedures ( shamansky 1986 ; shamansky et al . 1985 ). fractions were monitored by elisa and immunoblots . fractions containing the 70 kda protein were pooled , concentrated by vacuum dialysis , and then stored at - 2 ° c . for further purification . with the use of the multi - step purification scheme ( conventional cation - exchange chromatography plus sequential hplc ), the 70 kda p . falciparum exoantigen could be routinely purified to homogeneity ( confirmed by two - dimensional electrophoresis ). enzymatic digestion and gas - phase sequencing of proteolytic fragments , analysis and synthesis of peptides our strategy for the determination of amino acid sequences in the 70 kda protein was to carry out a complete enzymatic digestion using chymotrypsin , followed by isolation of the resulting peptides with reverse - phase hplc . alpha - chymotrypsin ( sigma chemical , st . louis , mo .) was used at an enzyme to protein ( w / w ) ratio of 1 : 25 to digest 500 pmoles ( approximately 35 μg / ml ) of the purified antigen according to the method of stone et al . ( 1990b ). individual peptides were isolated by analytical reverse - phase hplc ( delta pak c - 18 analytical reverse - phase high performance liquid chromatography column , 3 . 9 mm × 15 cm ) according to procedures described previously ( stone et al . 1990a ). ten peptide fragments were submitted to the genetic engineering facility at the university of illinois ( urbana - champaign , ill .) for gas - phase sequencing . peptides were sequenced by automated edman degradation on an applied biosystems model 470a protein sequencer . all sequences were analyzed for similarities to known protein sequences , both non - malarial and malarial in origin , using the swiss protein database version 2 . 0 and the malaria protein sequence database ( walter and eliza hall institute of medical research , melbourne , australia ), respectively . no significant homologies to published sequences were found . next , sequences were analyzed by the ibm dnastar software package that provided structural predictions based on computer algorithms . these included the hopp and woods ( 1981 ) and kyte and doolittle ( 1982 ) algorithms for prediction of b - cell antigenic sites ( based on hydrophilicity ), and the chou and fasman ( 1974 ) prediction of protein conformation ( associated with the α - helical propensity of t - cell epitopes ). with this information and other considerations four peptides ( termed c2 , c3 , c5 , c10 ) were selected for synthesis based on the following criteria : ( i ) peptide length , ( ii ) hydrophilicity , ( iii ) secondary structure , i . e ., α - helices , ( iv ) content of proline residues . the respective peptide sequences are detailed in table 1 . table 1______________________________________synthetic peptides . sup . 1 constructed from internal chymotrypticdigests of 70 kda p . falciparum ( indochina i / cdc ) proteinpeptide sequence . sup . 2 secondary structure (%). sup . 3fragment ( no . of aa ) α - helices β - extended β - turn______________________________________1 . c2 gqdegeeneg 60 30 70 seq id no : 1 ( 10 ) 2 . c10 grnglgantdq - 33 28 72 ddqlede seq id no : 2 ( 18 ) 3 . c5 dqffdanpnlf - 64 64 41 qllepvefded seq id no : 3 ( 22 ) 4 . c3 lvflvqqpflf - 31 69 21 vlwdqnekf - pvfmgvydp seq id no : 4 ( 29 ) ______________________________________ . sup . 1 peptides ranked according to hydrophilicity . . sup . 2 singleletter code for aminoacid residues . . sup . 3 secondary structure (% amino acids ) as predicted by choufasman algorithm in dnastar program . peptides c2 , c3 , c5 and c10 of the 70 kda p . falciparum antigen were synthesized by the merrifield ( 1963 ) method in an applied biosystems peptide synthesizer at the genetic engineering facility of the university of illinois . peptides were lyophilized and stored in a dessicator at - 20 ° c . until used . the individual peptides were finally tested by elisa for reactivity with anti - p . falciparum antibodies in sera previously collected from patients ( n = 126 ) with acute malaria from bolivar state , venezuela ( c . s . toebe et al ., in press ). overall seropositivity ( igg ) rates for peptides c2 , c3 , c5 and c10 were 20 %, 40 %, 20 % and 58 %, respectively . igm reactivity to the respective peptides was 53 %, 30 %, 83 % and 70 %. it was found that immune sera from ugandan subjects had high reactivity with the peptides ( igg seropositivity rates of 90 % for c2 , c3 , c5 and 70 % for c10 ). in order to improve on antigenicity and to overcome the restricted ( variable ) immune responsiveness to individual epitopes , the construction of a synthetic peptide hybrid was accomplished . novel approach was used for the formulation of the synthetic peptide immunogen - the copolymerization of multiple peptides in the absence of carrier molecules . this results in a product unmodified by carrier conjugation and the potential effects of epitopic suppression ( leclerc et al . 1987 ). peptides c2 , c3 , c5 and c10 were copolymerized as follows . equal molar amounts of each peptide were mixed in pbs ( ph 7 . 4 ) to affect a final protein concentration of 3 mg / ml . peptides were polymerized with 0 . 6 % ( v / v ) glutaraldehyde ( final concentration ), added dropwise while stirring at 25 ° c . three successive additions of 0 . 2 % glutaraldehyde were carried out , the first 2 steps were each for 10 min . and the final reaction step was for 30 min . finally , a sodium borohydride reduction step ( 10 mg / ml peptide solution ) was carried out for 1 h at 4 ° c . to reduce schiff bases and restore the charge to the derivatized amino groups , in effect increasing the solubility of the peptide complex ( briand et al . 1985 ). following copolymerization , the peptide solution was dialyzed against pbs for 48 h at 4 ° c . to remove free peptides and glutaraldehyde . three rabbits were given a series of 3 subcutaneous immunizations with the synthetic peptide complex spf70 . peptide doses ( 2 . 5 mg ) were administered at 4 - week intervals . the first 2 injections were given with freund &# 39 ; s complete adjuvant , while the third immunization was given with freund &# 39 ; s incomplete adjuvant . rabbits were bled 7 and 14 days after each immunization and the sera processed for analysis . the immunogenicity and antigenicity of the synthetic peptide complex was analyzed in standard microplate elisas . first , sera collected 14 days after the third immunization was pooled , serially diluted in pbs / 0 . 05 % tween 20 ( polyoxyethylene sorbitan monolaurate non - ionic detergent ) from 1 : 50 to 1 : 6400 , and reacted with the individual peptides and the peptide complex in a microplate elisa . nunc maxicorp ( denmark ) polystyrene 96 - well plates were coated with either individual peptide - bovine serum albumin ( bsa ) conjugates , the peptide copolymer ( without bsa ) or bsa alone at a protein concentration of 10 μg / ml pbs ph 7 . 4 . after a blocking / wash step with pbs / 0 . 5 % tween 20 , the sera were allowed to react for 2 h at 37 ° c . the plates were then washed three times with pbs / 0 . 1 % tween 20 , and then incubated with alkaline phosphatase ( ap )- conjugated goat anti - rabbit igg ( h & amp ; l chains ) ( kirkegaard & amp ; perry laboratories , gathersburg , md .) for 1 h at 37 ° c . after a final series of washes , anti - peptide igg reactivity ( absorbance values read at 405 nm and corrected for bsa control ) was determined in an automated elisa reader after a 30 - min reaction period with p - nitrophenyl phosphate substrate . in another experiment , the serum pool was diluted 1 : 50 and pre - incubated with the respective peptides and peptide complex at a final peptide concentration of 250 μg / ml , 25 μg / ml , 2 . 5 μg / ml , and no peptide . the final serum dilution was 1 : 100 . serum / peptides were incubated for 16 h at 4 ° c ., and immunoprecipitates removed by centrifuging at 13 , 000 rpm ( microcentrifuge ) for 20 min . supernatants containing antibodies were reacted in a standard peptide - elisa with microplates coated with the homologous peptides ( 10 μg / ml ). antigenic reactivity was measured as described above . finally , in a similar competitive inhibition elisa experiment , the antigenicity of the peptides was determined after pre - incubation with hyperimmune human serum pools containing anti - p . falciparum antibodies from malaria - endemic uganda and venezuela ( respective ifa titers = 1 : 10 , 240 ) and with a normal human serum control . these sera were kindly provided by dr . i . kakoma , university of illinois , and dr . o . noya , central university of venezuela , respectively . the final serum dilution was 1 : 100 . antigenic reactivity was measured after incubation with ap - conjugated goat anti - human igg ( h & amp ; l chains ) ( kirkegaard and perry ) and p - npp substrate as described above . in vitro cultures of the geneve / sge - 1 strain of p . falciparum were synchronized by sorbitol lysis , and late - stage parasitized erythrocytes were concentrated using percoll ( colloidal polyvinylpyrridolone coated silica for cell separation ). stage - specific labelling of schizont proteins ( approx . 70 % parasitemia ) was carried out using 35 s - methionine in rpmi 1640 plus 10 % human serum ( 1mci / 5 ml ) for 5 h according to standard procedures . schizonts were removed by centrifugation , lysed in cold 10 mm tris buffer ( ph 8 ) and solubilized in 1 % nonidet p - 40 ( octylphenol - ethylene oxide condensate ) in pbs . igg fractions ( rabbit anti - peptide complex and normal rabbit control ) were coupled to protein - a - sepharose cl - 4b ( beaded crosslinked agarose ), washed and subsequently incubated with 200 μl of labelled parasite extract . after a final washing , 100 μl of sodium dodecyl sulfate ( sds )/ dithiothreitol ( dtt ) sample buffer was added to each immunoprecipitate ( ip ), boiled for i min and centrifuged . sixty μl of each ip supernatant was loaded onto a 10 % sds - page gel and electrophoresed at 70 v for 20 - 24 h . the gels were enhanced for fluorography , and films developed by standard procedures . plasmodium falciparum ( indochina i / cdc strain ) antigens ( infected erythrocyte lysate and affinity - purified exoantigens ) from asynchronous in vitro cultures were analyzed by sds - page followed by immunoblotting . exoantigens were affinity - purified from culture supernatant fluids using monoclonal anti - peptide c3 and human anti - p . falciparum antibodies ( generously provided by dr . i . kakoma ) on reacti - gel coloumns ( activated solid support cross linked 1 1 &# 39 ; carbonylidiimidazole ) ( pierce chemical , rockford , ill ). electrophoresis was performed on 10 % acrylamide gels under non - reducing conditions . after transfer , antigens were reacted with 1 : 100 dilutions of sequentially collected rabbit antisera ( day 0 , days 7 and 14 post - first immunization , day 7 post - second immunization ) to the spf70 copolymer . the antigens were subsequently developed after incubation with horseradish peroxidase ( hrpo )- conjugated goat anti - rabbit immunoglobulins ( kirkegaard & amp ; perry ) and diamine benzidine substrate . the present study showed that a unique set of peptides ( termed c2 , c3 , c5 and c10 ), derived from a 70 kda p . falciparum exoantigen , could be effectively used as a synthetic immunogen ( spf70 ) when copolymerized with glutaraldehyde in the absence of a carrier . the synthetic peptide complex when administered with freund &# 39 ; s adjuvant was found to be highly immunogenic in rabbits . specific anti - peptide responses were analyzed by conventional peptide - elisa ( fig1 a and 1b ). serologic reactivity to the peptide complex and peptides c2 and c5 was uniformly high , followed by the responses to c3 and c10 . normal rabbit serum gave negligible background reactivity ( data not shown ). these data suggest that the most immunogenic epitopes are components of peptides c2 and c5 . the efficacy of c2 and c5 for eliciting high levels of t - dependent antibody ( igg ) may be correlated with the presence of putative t - cell epitopes as demonstrated by their respective content of alpha - helices ( table 1 ). moreover , antibodies to the peptide complex are reactive with p . falciparum schizonts as demonstrated by indirect immunofluorescence assays , with titers ranging from 1 : 320 - 1 : 640 after the third immunization . peptide antigenicity was assessed with human anti - p . falciparum sera from malaria - endemic regions of uganda and venezuela . elisa data showed that anti - p . falciparum antibodies were specific for and reactive to the peptides ( fig2 a and 2b ). with the exception of peptide c10 , all peptides demonstrated good antigenic reactivity ( particularly c3 ). normal human serum gave minimal background reactivity ( mean absorbance value = 0 . 11 ). greatest reactivity was seen with the ugandan sera . the lesser reactivity with antibodies in venezuelan immune sera may be because of strain differences or may indicate a lower level of naturally - acquired anti - 70 kda ( and anti - peptide ) antibodies in the sera . the specificity of the rabbit anti - spf70 antibodies for p . falciparum antigen was shown by immunoprecipitation of metabolically labelled proteins ( fig3 ) and by immunoblotting ( fig4 ). the major protein precipitated by anti - peptide complex ( pc ) igg was a 120 kda schizont antigen . several other minor proteins were also precipitated nonspecifically by normal rabbit igg . it appears that the 120 kda membrane protein is degraded in mature schizonts to the 70 kda exoantigen which increases in amount at the time of merozoite release / reinvasion ( braun - breton et al . 1986 ). at this point , a substantial amount of 70 kda antigen is released into the surrounding medium . hyperimmune sera collected sequentially from rabbits immunized with the synthetic copolymer reacted in immunoblots ( fig4 ) with the 70 kda antigen from ( 1 ) p . falciparum indochina i - infected erythrocyte extracts , ( 2 ) supernatant fluid , i . e ., exoantigens , from indochina i cultures affinity - purified with monoclonal antibody to peptide c3 , ( 3 ) indochina i exoantigens affinity - purified with p . falciparum - immune igg of ugandan origin . described herein are peptide sequences of a 70 kda p . falciparum exoantigen ( pf70 ), that when synthesized and constructed as a copolymer ( spf70 ), are able to induce the formation of antibodies that are reactive with the native malarial protein . the knowledge of peptide sequences allowed the construction of synthetic peptides representing immunodominant , and immunorelevant , epitopes of the native protein . if pf70 is involved in the induction of tnf production in clinical malaria , the present approach is to design and construct a synthetic immunogen that improves upon nature . with the careful selection of parasite - specific epitopes , the present invention enhances immunogenicity and induces a solid immunity against disease ( berzofsky 1991 ; good and miller 1990 ). in this phase of studies , the construction of the synthetic peptide hybrid was carried out by glutaraldehyde copolymerization ( leclerc et al . 1987 ). although glutaraldehyde copolymerization results in a relatively random - linked product , this randomized relationship of multiple parasite - specific b - cell and t - cell epitopes meets the requirements for induction of potent immune ( antibody - and t cell - mediated ) responses . the high antigenic reactivity of spf70 and the individual component peptides demonstrated the induction of t cell - dependent antimalarial antibody ( igg ) responses , and is consistent with the use of such synthetic peptide polymers as immunogens and diagnostic reagents ( together with anti - peptide antibodies for the detection of antigen ). of course , numerous other cross - linking agents are known and should be usable in place of glutaraldehyde . one of the important indicators of functional immunity to malaria is the recognition of malarial antigens or synthetic derivatives by defined sera from human populations immunized by natural exposure to p . falciparum . recent studies with epidemiologically - defined populations from indonesia , brazil and africa ( burkina faso ) have shown anti - spf70 reactivity to correlate with naturally - acquired protective - immunity . the first study was conducted by j . k . baird et al . ( unpublished data ). a total of 218 serum samples from irian jaya were analyzed for antibody to spf70 by elisa . sera were collected from individuals during a malaria epidemiologic study by baird et al . ( 1991 ). subjects were grouped according to age and immune status ( recent vs . lifelong residents ). antibody reactivity to spf70 was found to increase with age among migrant people with only 2 years exposure to hyperendemic malaria . the increased frequency and level of anti - spf70 antibody among 110 migrants was quantitatively parallel to that among 100 lifelong residents of the hyperendemic area . overall , 83 % of the people had antibodies reactive with spf70 . the proportion of people positive for anti - spf70 antibody increased from 45 % among 2 to 5 - year olds , to 95 to 100 % among adults (& gt ; 15 years of age ). the second study was conducted by c . d . ribeiro et al . in a seroepidemiologic study designed to assess the natural humoral response to various p . falciparum antigens including pf70 , the humoral immune recognition of spf70 was analyzed by elisa . sera were collected from diverse human populations , e . g ., amazonian indians and hyperimmune africans from burkina faso . seropositivity rates for antibodies reactive with spf70 were 58 % for the amazonian subjects and 85 % for the population from burkina faso . this compared with rates of 51 % and 20 %, respectively , for antibodies to a nanp 4 peptide derived from the central repeat region of the circumsporozoite protein . the present inventors provided spf samples for that study , although its structure was withheld . the above studies indicate that the target pf70 peptides are immunogenic in nature ( no obvious genetic restriction ) as 85 % of hyperimmune west african adults and 95 - 100 % of immune irian jayan adults possess antibodies to pf70 . moreover , the present results confirm the immunogenicity and antigenic reactivity of the synthetic peptide complex spf70 . detection of antibodies to a 70 kda plasmodium falciparum exoantigen in malarious subjects using synthetic peptides of the present invention serum samples ( n = 126 ) were collected between 1985 - 1989 from patients diagnosed with acute malaria attending the malaria outpatient clinics of the malariology service of the ministry of health and the hospital ruiz y paez in ciudad bolivar , bolivar state , venezuela . diagnosis was made on the basis of clinical symptoms and the detection of parasites in giemsa - stained blood films . of the 126 patients , 34 were documented as experiencing a primary malaria episode and 58 as having more than one episode . in addition , of the patients for whom definitive diagnosis of the infecting species was known , 57 were positive for p . falciparum and 28 for p . vivax . serum samples were also collected from 20 individuals with no history of malaria at charity hospital , new orleans , la ., usa . all sera were stored at - 70 ° c . prior to analysis . for the indirect immunofluorescent antibody ( ifa ) assays , thin smears of p . falciparum ( indochina i / cdc strain )- infected monkey erythrocytes were prepared as antigen slides and fixed in acetone for 15 min . serum samples were diluted in phosphate - buffered saline ( pbs ) ( initial dilutions 1 : 20 and 1 : 40 ) and allowed to react with antigen for 30 min at 37 ° c . the slides were then washed twice in pbs and once in distilled h 2 o ( 5 min each ). commercial fluorescein - conjugated anti - human igm and igg ( cappel laboratories , malvern , pa ., u . s . a .) were used as second antibodies diluted 1 : 40 in pbs . two - fold dilutions of test sera were also titered for igg and igm antibodies ( initial dilution 1 : 80 ) using heavy chain - specific fluorescein - conjugated anti - human igg and igm ( cappel laboratories ) for determination of total anti - asexual blood - stage antibody levels . an enzyme - linked immunosorbent assay ( peptide - elisa ) adapted from the method of deloron et al ., ( 1989 ) was used to determine antibody reactivity to synthetic peptides . peptides were conjugated to bovine serum albumin ( bsa ) at a molar ratio of 25 : 1 ( peptide to bsa ) with glutaraldehyde in pbs . after passage over a g - 25 sephadex column ( dextran cross linked with epichlorohydrin ), peptides were stored frozen and used at a final concentration of 5 μg / ml . as control antigens , bsa - glutaraldehyde was prepared at 2 . 5 μg / ml and p . falciparum ( venezuelan strain )- infected erythrocyte lysate at 200 μg / ml . flat - bottom , 96 - well immulon ii , polystyrene ( dynatech laboratories , alexandria , va ., u . s . a .) plates were coated with antigens for 2 h at 37 ° c ., blocked / washed twice for 10 min each in pbs containing 0 . 5 % tween - 20 ( pbs - t ) and rinsed with distilled h 2 o . sera were diluted 1 : 100 in pbs - t containing 5 % non - fat dry milk and 0 . 3 % bsa - glutaraldehyde ( blotto - g ) and applied to duplicate wells for 2 h at 37 ° c . and then washed in pbs - t as before . alkaline phosphatase - conjugated anti - human igg or igm were added at a 1 : 750 dilution in blotto - g and incubated for 1 h at 37 ° c . after a final wash , 100 μl of p - nitrophenol phosphate substrate was added and allowed to react for 1 h at room temperature . absorbance values were measured by reading the optical density ( od ) at a wavelength of 405 nm . test sera were considered antibody - positive when the absorbance value was greater than the mean od + 2 standard deviations obtained with control sera . all of the patients ( n = 126 ) diagnosed with acute malaria were positive at screening dilutions of 1 : 20 and 1 : 40 for anti - p . falciparum asexual blood - stage igg antibodies as determined by the ifa . of these , 105 ( 83 %) were also positive for anti - malarial igm antibodies . all positive sera were subsequently titrated using two - fold dilutions ( initial dilution 1 : 80 ) for igg and igm antibodies , respectively . there was a trend toward higher igg titers with increasing age ( not shown ) but correlations between antibody levels and age were complicated as subjects less than 20 years old attending the clinic were under - represented . patients known to have experienced more than one malarial episode ( n = 58 ) had significantly higher mean igg levels ( p & lt ; 0 . 05 ) than those with primary malaria infections ( n = 34 ) ( table 2 ). table 2______________________________________antibody responses and exposure to malaria geometric mean ifa titer . sup . a ( standard deviation ) exposure n = 92 igg igm______________________________________primary 34 7 . 76 ( 2 . 72 ) 6 . 90 ( 2 . 55 ) repeated . sup . b 58 8 . 96 ( 2 . 51 ) 6 . 61 ( 2 . 92 ) ______________________________________ . sup . a the geometric mean ifa titer of igg antibodies to p . falciparum ( indochina i / cdc strain ) asexual bloodstage antigens increased significantly with more than one malarial episode ( b ) ( p = 0 . 035 , by anova ). although igm levels were higher in individuals experiencing their first malarial episode , the difference was not statistically significant . the respective cut - off values ( mean od level + 2 standard deviations ) of the 20 control sera used in peptide - elisas was 0 , 065 for c2 , 0 . 066 for c3 , 0 . 009 for c5 , 0 . 020 for c10 and 0 . 486 for the p . falciparum lysate antigen . of the patients with acute malaria , 123 ( 97 . 6 %) reacted with the p . falciparum lysate , reflecting a high correlation with ifa reactivity . each of the three patients that tested negative had low igg titers (≦ 320 ) by ifa . overall seropositivity rates of the subjects to the respective peptides were c2 = 20 %, c3 = 40 %, c5 = 20 % and c10 = 58 %. the results of igg reactivity by ifa and elisa are summarized in fig5 . due to the limited number of subjects under 20 years old , a relationship between peptide reactivity and age could not be determined . however , c10 showed the greatest reactivity , ranging from 53 to 75 % seropositivity among different age groups of malarious subjects ( n = 104 ) ( fig6 ). selected sera , categorized on the basis of primary or repeated exposure to malaria , were tested for igm antibody reactivity in peptide - elisas . preliminary results indicated that except for c3 , overall igm reactivity to each peptide was relatively high with maximal reactivity to c5 ( 83 %). igm reactivity was generally greater in patients with primary malaria infections . this pattern was more distinct among sera with higher igm titers and for sera reacting to c5 and c10 ( table 3 ). table 3______________________________________percentage of sera positive by peptide - elisafor igm ( μ chain - specific ) antibody peptides ( percent positive ) igm titer . sup . a exposure c2 c3 c5 c10______________________________________high p 80 20 80 100 r 40 0 60 60medium p 80 20 100 100 r 40 80 80 60low p 20 20 80 40 r 60 40 80 40total reacti - 53 . 3 30 83 . 3 70vity : ( n = 30 ) ______________________________________ . sup . a reciprocal igm titers determined by ifa ( range : low = 40 - 1 , 280 , medium = 2 , 560 - 5 , 120 , high = 10 , 240 - 40 , 960 ). p = primary malarial infection . r = repeated malarial infection . five sera were assessed in each group . cutoff values ( mean od + 2 standard deviations of control sera ) for determining positive reactions were as follows : c2 = 0 . 122 , c3 0 . 029 , c5 = 0 . 019 , and c10 = 0 . 051 . the present study was designed to characterize the antibody responses of subjects with acute malaria from bolivar state , venezuela to synthetic peptides derived from a 70 kda p . falciparum ( indochina i / cdc strain ) exoantigen . all patients had asexual blood - stage antibodies to the indochina i strain as determined by ifa . igg titers were correlated with exposure to malaria . a large proportion ( 83 %) of subjects also possessed igm antibodies as determined by ifa , indicative of the early course of infection . the overall level of igg reactivity to synthetic peptides derived from pf70 was c2 = 20 %, c3 = 40 %, c5 = 20 % and c10 = 58 %. seropositivity to peptide c10 was consistently over 50 % ( range 53 - 75 %) among patients of different age groups . in the present study , preliminary investigations with selected sera from patients with anti - malarial igm antibodies indicated that , with the exception of c3 , the level of reactivity to peptides was generally high : c2 = 53 %, c5 = 83 % and c10 = 70 %. reactivity was generally greater in individuals with a primary malaria episode . given the fact that igm levels wane much sooner than igg during a malarial infection , igm - specific reactivity may serve as a useful indicator of recent exposure to the parasite for diagnostic purposes ( shehata et al ., 1988 ). this and previous studies in the inventors &# 39 ; laboratory have demonstrated that the pf70 peptides do not cross - react with non - malaria parasites , although they are reactive with p . vivax antibodies ( montenegro - james et al .). this point is advantageous from the standpoint of early diagnosis as a general ` malaria `- specific peptide would not only be useful but desirable for initial screening prior to speciation ( chiodini and moody , 1989 ). as mentioned , malaria transmission in bolivar is unstable and the majority of individuals in this study were migrant workers and their families who were only intermittently exposed to malaria in gold - mining areas of the state . sanchez et al . ( 1990 ) noted that in such subjects elisa values for serological reactions to crude p . falciparum asexual blood - stage antigens are often low or negative . in addition , all of the subjects in this study were suffering from acute malaria . in such patients , other investigators have observed low seropositivity rates and antibody levels to various blood - stage antigens suggestive of disease - induced immunosuppression ( deloron et al ., 1989 ; petersen et al ., 1989 ). seroepidemiologic surveys that have used other malarial antigens have shown that antibody levels fall rapidly in the absence of repeated infections ( tapchaisri et al ., 1985 ; mendis et al ., 1992 ) and that antibody responses vary among people at equal risk of exposure to malaria ( rosenberg and wirtz , 1990 ) which may be explained in part by genetic restriction ( chizzolini et al ., 1988 ). the limited number of epitopes on a given peptide may also fail to be recognized by a number of subjects with intermittent experience of malaria . a study conducted by mendis et al . ( 1992 ) in sri lanka , where malaria transmission is also unstable , found that antibodies to the cs protein of either p . vivax or p . falciparum were present in less than 20 % in the population as a whole , despite a life - long exposure to p . vivax . thus , it was concluded that in such areas , seropositivity may reflect differences in exposure to inoculation versus a cumulative experience of malaria . one skilled in the art can see that the antibodies induced to the circulating malarial antigens of the present invention can , in turn , be purified and used as a reagent for assaying the level of circulating malarial antigens in a patient . these prepared antibodies are affixed to a surface and incubated with a biological sample from the patient to allow immunoreaction to occur . the detection of circulating malarial antigens is accomplished by contacting the immunoreacted product with an indicator antibody directed to the malarial antigens bound to the affixed antibodies . the biological sample from the patient may be serum or plasma , in particular , human serum or plasma . the indicator antibody may be an enzyme linked antibody , a fluorescent tagged antibody or a radiolabeled antibody . the use of composite immunogen spf70 as a vaccine in humans the spf70 protein will be reconstituted ( if lyophilized ) in 0 . 9 % saline solution and adsorbed onto alum hydroxide at a concentration of 4 mg of synthetic protein and 2 mg of ai ( oh ) 3 / ml . the vaccine will be kept at 4 ° c . before use . a dose of 2 mg spf70 in 0 . 5 ml will be injected subcutaneously for each adult individual . children less than 5 years old will receive half this dosage . the vaccination schedule will consist of 3 doses administered on days 0 , 30 , and 180 . in conclusion , the synthetic peptides employed in this study , representing epitopes of a native 70 kda p . falciparum exoantigen can be used for the detection of asexual blood - stage antibodies in malaria - endemic regions and in epidemiological settings which measure their relative antigenicity , specificity and conservation between p . falciparum strains . further investigations described herein demonstrate the antigenic use of these peptides as a hybrid molecule ( spf70 ), thereby increasing the number of epitopes available for immune reactivity ( see example 1 ). baird et al . ( 1991 ). age - dependent acquired protection against plasmodium falciparum in people having two years exposure to hyperendemic malaria . am j trop med hyg 45 : 65 - 76 . bate et al . ( 1990 ). malaria exoantigens induce t - independent antibody that blocks their ability to induce tnf . immunology 70 : 315 - 320 . berzofsky j . a . ( 1991 ). mechanisms of t cell recognition with application to vaccine design . mol immunol 28 : 217 - 223 . braun - breton , et al . in vivo time course of synthesis and processing of major schizont membrane polypeptides in plasmodium falciparum . mol . biochem . parasitol . 20 ( 1986 ) 33 - 43 . briand et al . ( 1985 ). synthetic peptides as antigens : pitfalls of conjugation methods . j immunol meth 78 : 59 - 69 . campbell , et al . use of synthetic and recombinant proteins in the study of host - parasite interactions in the malarias . amer . j . trop . med . hyg . 37 ( 1987 ) 428 - 444 . chiodini , et al . techniques for the detection of malaria parasites . j . roy . soc . med , suppl . 17 , 82 ( 1989 ) 41 - 43 . chizzolini , et al . natural antibodies against three distinct and defined antigens of plasmodium falciparum in residents of a mesoendemic area in gabon . amer . j . trop . med . hyg . 39 ( 1988 ) 150 - 156 . chizzolini , et al . age - related prevalence of antibody response against three different , defined plasmodium falciparum antigens in children from the haut - ogooue province in gabon . trans . roy . soc . trop . med . hyg . 83 ( 1989 ) 147 - 151 . chou et al . ( 1974 ). prediction of protein conformation . biochemistry 13 : 222 - 245 . deloron , et al . antibodies to plasmodium falciparum ring - infected surface antigen and p . falciparum and p . malariae circumsporozoite proteins : seasonal prevalence in kenyan villages . amer . j . trop . med . hyg . 41 ( 1989 ) 395 - 399 . deloron , et al . antibodies to the reng - infected erythrocyte surface antigen and the circumsporozoite protein of plasmodium falciparum in a rural community from burkina faso . trans . roy . soc . trop . med . hyg . 84 ( 1990 ) 191 - 195 . esposito , et al . prevalence and levels of antibodies to the circumsporozoite proteins of plasmodium falciparum in an endemic area and their relationship to resistance against malaria infection . trans . roy . soc . trop . med . hyg . 82 ( 1988 ) 827 - 832 . good et al . ( 1990 ). t - cell antigens and epitopes in malaria vaccine design . curr top microbiol immunol 155 : 65 - 78 . grau et al . ( 1989 ). tumor necrosis factor and disease severity in children with falciparum malaria . new engl j med 320 : 1586 - 1591 . hopp et al . ( 1981 ). prediction of protein antigenic determinants from amino acid sequences . proc natl acad sci usa 78 : 3824 - 3828 . james et al . ( 1985 ). induction of protective immunity to plasmodium falciparum in saimiri sciureus monkeys with partially purified exoantigens . infect immun 49 : 476 - 480 . karunaweera et al . ( 1992 ). dynamics of fever and serum levels of tumor necrosis factor are closely associated during clinical paroxysms in plasmodium vivax malaria . proc natl acad sci usa 89 : 3200 - 3203 . kwiatkowski et al . ( 1989 ). tumour necrosis factor production in falciparum malaria and its association with schizont rupture . clin exp immunol 77 : 361 - 366 . kwiatkowski et al . ( 1990 ). tnf concentration in fatal cerebral , non - fatal cerebral , and uncomplicated plasmodium falciparum malaria . lancet 336 : 1201 - 1204 . kyte et al . ( 1982 ). a simple method for displaying the hydropathic character of a protein . j mol biol 157 : 105 - 132 . leclerc et al . ( 1987 ). a synthetic vaccine constructed by copolymerization of b and t cell determinants . eur j immunol 17 : 269 - 273 . mendis , et al . anti - circumsporozoite protein antibodies measure age related exposure to malaria in kataragama , sri lanka . parasite immunol . 14 ( 1992 ) 75 - 86 . mendis k . n . ( 1992 ). contrasting clinical disease in plasmodium vivax and plasmodium falciparum malaria , and the association of both with cytokines . bull inst pasteur 90 : 3 - 9 . merrifield r . b . ( 1963 ). solid phase peptide synthesis . i . the synthesis of a tetrapeptide . j am chem soc 85 : 2149 - 2154 . molyneux m . ( 1990 ). cerebral malaria in children : clinical implications of cytoadherence . am j trop med hyg 43 , suppl . : 38 - 41 . montenegro - james et al . abstr . annu . meet . am . soc . trop . med . hyg . 1988 , 175 , pg . 154 . petersen , et al . an epidemiological study of humoral and cell - mediated immune responses to the plasmodium falciparum antigen pf155 / resa in adult liberians . amer . j . trop . med . hyg . 41 ( 1989 ) 386 - 394 . playfair et al . ( 1991 ). don &# 39 ; t kill the parasite : control the disease . acta leid 60 : 157 - 165 . playfair et al . ( 1990 ). the malaria vaccine : anti - parasite or anti - disease ? immunol today 11 : 25 - 27 . ribeiro et al ., ( 1991 ) proc . iv intl . cong . malaria & amp ; babesiosis , abstr . 2 . 22 . rosenberg , et al . intrinsic individual differences in circumsporozoite antibody response at a hyperendemic malaria focus . trans . roy . soc . trop . med . hyg . 84 ( 1990 ) 206 - 208 . sanchez , et al . malaria in the amazon . prevalence of plasmodium falciparum antibodies in amerindians inhabiting the venezuelan amazon . ann . trop . med . parasit . 84 ( 1990 ) 307 - 312 . scuderi et al . ( 1986 ). raised serum levels of tnf in parasitic infections . lancet ii : 1364 - 1365 . shamansky l . m . ( 1986 ). purification and characterization of soluble antigens from the human malaria parasite plasmodium falciparum . ph . d . thesis , university of illinois , urbana - champaign , ill . shamansky , et al . purification and characterization of culture - derived exoantigens of plasmodium falciparum mol . biochem . parasit . 17 ( 1985 ) 299 - 310 . shehata , et al . reversed enzyme - linked immunosorbent assay for detection of specific anti - plasmodium falciparum immunoglobulin m antibodies . bull . wld , hlth . org . who / mal / 88 . 1050 ( 1988 ) 1 - 9 . stone et al . ( 1990a ). reversed - phase high - performance liquid chromatography for fractionation of enzymatic digests and chemical cleavage products of proteins . meth enzymol 193 : 389 - 412 . stone et al . ( 1990b ). enzymatic digestion of proteins and hplc peptide isolation in the sub - nanomole range . in : fini c ., floridi a ., finelli v . n ., ( ed ) laboratory methodology in biochemistry . crc press , boca raton , pp . 181 - 205 . tapchaisri , et al . antibodies against malaria sporozoites in patients with acute uncomplicated malaria and patients with cerebral malaria . amer . j . trop . med . hyg . 34 ( 1985 ) 831 - 836 . taverne et al . ( 1990a ). two soluble antigens of plasmodium falciparum induce tumor necrosis factor release from macrophages . infect immun 58 : 2923 - 2928 . taverne et al . ( 1990b ). human and murine macrophages produce tnf in response to soluble antigens of plasmodium falciparum . parasite immunol 12 : 33 - 43 . thelu et al . ( 1985 ). purification and immunochemical study of plasmodium falciparum exoantigens . j parasitol 71 : 542 - 546 . trager w , et al . ( 1976 ). human malaria parasites in continuous culture . science 193 : 673 - 675 . who scientific group . the use of synthetic antigens for diagnosis of infectious diseases . who . tech . rep . ser . 784 ( 1989 ) 59 - 64 . wilson et al . ( 1969 ). antigens associated with plasmodium falciparum infections in man . lancet ii : 201 - 205 . __________________________________________________________________________sequence listing ( 1 ) general information :( iii ) number of sequences : 4 ( 2 ) information for seq id no : 1 :( i ) sequence characteristics :( a ) length : 10 amino acid residues ( b ) type : amino acid ( d ) topology : linear ( xi ) sequence description : seq id no : 1 : glyglnaspgluglygluglua snglugly1510 ( 2 ) information for seq id no : 2 :( i ) sequence characteristics :( a ) length : 18 amino acid residues ( b ) type : amino acid ( d ) topology : linear ( xi ) sequence description : seq id no : 2 : glyargasnglyleuglyalaasnthraspgl naspaspglnleuglu151015aspglu ( 2 ) information for seq id no : 3 :( i ) sequence characteristics :( a ) length : 22 amino acid residues ( b ) type : amino acid ( d ) topology : linear ( xi ) sequence description : seq id no : 3 : aspglnphepheaspalaasnproasnleupheglnleuleuglupro151015valglupheaspgluasp20 ( 2 ) information for seq id no : 4 :( i ) sequence characteristics : ( a ) length : 29 amino acid residues ( b ) type : amino acid ( d ) topology : linear ( xi ) sequence description : seq id no : 4 : leuvalpheleuvalglnglnpropheleuphevalleutrpaspgln15101 5asnglulyspheprovalphemetglyvaltyrasppro2025 | 2 |
the present invention includes a user friendly apparatus and method for replenishing spent dispersant material . in one embodiment one pulls out a dispensing compartment in the manner one pulls out a drawer . once open the dispensing material can be placed in the dispensing drawer and the drawer closed to bring the system to dispensing condition . in anther embodiment a dispensing compartment can be hung from the side of the container and in a further embodiment a fountain like dispenser that allows one to place the dispersant material into the fountain like dispenser so the dispensable material can be flow carried throughout the system . fig1 is a cutaway view showing a dispenser system 10 with an outer housing 11 having an inner container 11 a partially filled with a fluid such as water 25 . typically , system 10 can be used in a pool , spa or other fluid container where fluid treatment is required . for example , the system can be used for the water that is used either for work , pleasure or for drinking . in the embodiment shown the container 11 a is configured in a spa mode with an inlet 30 positioned to draw water into an inlet pipe 29 through a pump 27 . pump 27 increases the pressure of the water and forces the water in fluid conduit 28 on the outlet side of the pump to discharge under high pressure as a high pressure jet at underwater port 28 a . the high pressure fluid jet can provide multiple functions , for example , in a hot tub , the high pressure fluid jet produced by the pump system circulates the water in the hot tub thus ensuring that the water purification materials are dispersed throughout the tub . in addition , the high pressure jet produced by the pump system can also provide a water massages as a user sits in the tub . a further use of a portion of the stream of fluid can occur when fluid is diverted to a dispensing housing to allow the fluid to flows past a dispersant material that is contained in the dispenser housing . in the present invention the high pressure line 28 is in fluid communication with a dispenser 19 which is mounted in the housing 11 . dispenser 19 comprises a housing that contains a dispenser inlet 14 with a fluid restriction 15 in the form of a small aperture with a cross sectional flow diameter on the order of 0 . 010 of an inch while the cross sectional flow diameter of the line 28 and nozzle outlet 28 a may be two inches or more . it will be appreciated that the cross sectional area or size of the aperture 15 and the cross sectional area or size line 28 can be scaled up or down to accommodate various flow conditions but that the ratio of the difference in cross sectional area produces a low pressure region in the dispenser . thus , in the present invention , a purpose of the restriction 15 is to limit the volume flow of high pressure water into chamber 16 in the dispenser 19 but still provide for flow of water at a lower pressure through chamber 16 . in the embodiments shown in fig1 the dispenser 19 contains an open dispersant chamber 16 for placing or retaining dispersant materials therein . that is , cap 13 can be removed and typical materials such as bromine sticks 17 can be dropped in chamber 16 . located in the bottom portion of chamber 16 in dispenser 19 are the water purification materials 17 or other fluid treatment materials . in one embodiment dissolvable materials 17 such as halogens and particularly halogens such as bromine or chlorine tablets are placed directly into chamber 16 by removal of cap 13 which threadingly engages a male thread on dispenser 19 . in operation of the system of fig1 , the top inlet 14 of dispenser 19 receives water under high pressure but low volume flow since only a small amount of water can flow through the restriction 15 . with the cap 13 on dispenser 9 the pressure in the chamber 16 rises sufficient to force water to flow , albeit at a slow velocity , through the dispenser chamber 16 and into the container 11 a through outlet 21 . as shown in fig1 dispenser 19 includes an air pocket 16 a above the water line 18 of the water in the dispenser 19 . it should be understood that the top end 19 a of dispenser is located above the water line 26 in the container 11 a and that the bottom discharge port offers little resistance to fluid returning to container 11 a . consequently , if the cap 13 is not on the dispenser 13 the water will not flow out of dispenser 19 but will seek its own level , namely the level indicated by water line 26 in container 11 a since there is little resistance to flow of water out of the port 21 in dispenser 19 . a further feature of the invention is that the liquid level in the dispenser 19 , which is indicated by reference numeral 18 and the air pocket 16 a combine to provide a reservoir or chamber for fluid . that is , the water flows in the directions indicated by arrows in fig1 . the water flows through chamber 16 and out passage 20 and is discharged into container 11 a through port 21 which is located below the water line 26 . the egress passage 20 is characterized by having a substantially larger diameter than the diameter of the restrictor 15 so as not to impede the flow of water therethrough . as a result , the high pressure low volume flow of water entering the dispenser 16 is forced through the dispenser 19 and into the bottom of the container 11 a where the discharge pressure is primarily determined by the depth of the water “ h ” below the water line . the presence of the air pocket 16 a ensures that if the cap is removed it will be air that escapes from the dispenser rather than the fluid in the chamber . the maintenance of an air pocket in the dispenser housing insures that the fluid level in the system will be below the top of the dispenser housing so that removal of cap 13 will not cause fluid to spill from the housing . thus in the present system the water discharges into a low pressure region in the bottom of container 11 a . if someone should accidentally remove cap 13 the pressure of water entering into the dispenser arrives at a low volume flow with the stream of water directed away from the top opening 19 a to prevent any water or dispenser materials from being blown back at the person as the cap 13 is removed . in addition , the air pocket 16 a can provide a reservoir chamber to absorb water flowing into the dispenser 19 . that is , even with the outlet 21 blocked there is a time lag of several minutes before the water would flow out the top of dispenser 19 thus giving a person time to shut off the recirculation system . in normal operation , the pressure in air pocket 16 a may rise slightly due to the fluid circulation resistance through the dispenser 19 and cause the air pocket 16 a to compress slightly , however , once the cap 13 is removed the water level 18 in the dispenser 19 may rise slightly but under normally conditions the flow will continue to circulate through the dispenser since the fluid resistance to water discharging out the top 19 a of the dispenser 19 is maintained at greater fluid resistance than the fluid resistance to water flowing though the dispenser 19 and back into the container 11 a . in other words , the inlet 15 and the outlet 20 are sized such that if the water under pressure continues to come into the dispenser chamber 16 when the cap 13 is removed the water in the dispenser 19 will not rise over the top of the dispenser housing and spill out of the dispenser 19 . that is , even though a slight increase in the water level 18 can occur water continues to flow through dispenser 19 and back into the container 11 a thereby ensuring that unnecessary spills are avoided . in an alternate embodiment of the invention a removable cartridge or removable cartridges are placed in a cartridge holder that is removably positioned in a dispenser housing . fig2 shows a front view of a cartridge dispenser 40 for receiving a typical fluid treatment material such as water purification material . cartridge 40 comprises an outer sleeve 41 that is rotatable positioned with respect to an inner container 42 which contains a dispersant 39 . a pair of elongated openings 41 a allow fluid to flow enter container 42 through the openings 43 a . located in the bottom of container 42 is a dispersant material 39 such as minerals or the like which are used to treat water . minerals 39 are different from chlorine or bromine tablets and the like which dissolve as they are used as minerals which do not dissolve need to be removed once the minerals have been spent . thus the cartridge 40 comprises a dispersant holder that can be removed from a dispenser housing and replaced with a fresh cartridge . if desired cartridge 40 can be provided with a flotation chamber 45 that is attached directly to the cartridge 40 so the cartridge will float to the top of the dispenser chamber 16 for easy access and thus removal . in another embodiment of the invention a cartridge dispenser is carried by a cartridge holder . fig3 shows a cartridge carrier or cartridge holder 50 for holding one or more cartridges in an end to end condition . cartridge carrier 50 includes a handle 51 and an open body skeleton housing 60 having elongated flexible circumferential edges or ears 60 a and 60 b as part of the skeleton housing . the purpose of the skeleton housing is to allow water to flow through the skeleton housing and into and out of the cartridge held therein while at the same time provide a convenient tool for holding the cartridges in position in the dispenser housing and for removing the cartridges from the dispenser housing . carrier 50 contains a first circumferential lip 50 a that is spaced from a second circumferential lip 50 b with a resilient sealing member such as an o - ring 45 located between the lips to allow one to seal the top of the cartridge carrier 50 to the inside of a dispenser housing to prevent flow past the top of the dispenser housing . fig4 shows a side view of cartridge carrier 50 revealing two ears 56 and 56 a for locking the cartridge carrier 50 into a dispenser locating housing cam 65 , which is shown in fig1 . cartridge career 50 is preferable made from a polymer plastic that is flexibly thin yet sufficiently rigid to hold dispensing cartridges therein . carrier 50 contains side openings 60 f , 60 e , 60 g and 60 h to permit ingress or egress of fluid through the skeleton housing 60 . while only one cartridge dispenser 40 is shown in cartridge holder 50 additional cartridges holder can be placed in the cartridges holder to provide for different dispersants . fig5 shows a sectional view of the cartridge carrier 50 taken along lines 55 to show the cylindrical open body skeleton housing 60 with ears 60 a and 60 b being resiliently displaceable radially outward ( see arrows ) to allow lateral insertion of the cartridge 40 therein . a lower stop 43 c extends around the bottom of the skeleton housing to hold the cartridge in position . in order to hold a plurality of dispenser cartridges in a fixed position in the cartridge holder 50 reference should be made to fig3 which shows internal circumferential bands that form a protruding partial circumferential ridge . that is , a top circumferential ridge 44 a holds the top cartridge dispenser 40 , a second identical partial circumferential ridge 44 b can hold a second cartridge dispenser and a third identical partial circumferential ridge 44 c located on skeleton housing 60 can hold a third dispensing cartridge therein . a circumferential mating stop , such as a mating circumferential recess 40 a located on cartridge 40 allow one to maintain the cartridge 40 in the proper axial location in skeleton housing 60 . the flexible ears 60 a and 60 b and the skeleton body 60 which flex radially outward can be configured to provide a slight frictional fit between the outer surface of the cartridge and the inner surface of the skeleton holder 60 to thereby hold the cartridge in position during insertion and removal of the cartridge from the dispensers as well as to avoid movement of the cartridge in the housing due to changing water conditions in the dispenser housing which could cause unnecessary noise . fig1 shows an exploded view of the portion of the dispensing system that is fixedly attached to a panel 70 and fig6 - 10 show the unassembled components for forming a dispensing system in either an existing fluid system or a new fluid system . the cartridge holder of fig3 is placeable directly into the housing 61 shown in fig6 and an isolated cross sectional view of the flow around the skeleton housing and the cartridge 12 is shown in general detail in fig1 . in order to illustrate the attachment and operation of the system with dispersant cartridges reference should be made to the dispersant housing components illustrated in fig6 - 10 . the dispersant housing 61 shown in fig1 contains an upper end collar 61 a for securement to a housing head , a circumferential inlet port 61 b , a central chamber 61 d with a dispenser 40 therein and a lower outlet 61 c . dispenser housing 61 is mountable below a panel on a water system and is connected to the inlet and outlets as illustrated in fig1 . dispenser housing collar 61 a includes an internal cylindrical surface 61 e for mating with a dispenser housing head and an alignment notches 61 f for engaging with alignment members in the dispenser housing head 62 . fig7 is a pictorial view of the dispenser housing head 62 that is securable to the dispenser housing 61 through an adhesive or solvent bonding or the like . that is , in the preferred embodiment dispenser housing 61 and dispenser housing head 62 can be made from materials such as a polymer plastic and can permanently secured to each other through adhesives or the like . dispenser housing head 62 includes a circumferential lip 62 a for securing above a panel to support the dispenser housing head thereon . located along the body of dispenser housing head 62 is a set of external threads 62 b , an alignment member 62 d and a male cylindrical mating surface 62 c for insertion into the female cylindrical surface 61 e on dispenser housing 61 . located within housing head 62 is a set of internal threads 62 f for engagement with a removable cover . the use of a separate dispenser housing 61 with a collar permits one to assembly the unit on a system through placement of parts above and below the panel of the unit that is receiving the dispensing system of the present invention . fig8 is a pictorial view of a dispenser housing securement nut 63 having a set of internal threads 63 c , a set of hexagon lands 63 b to allow one to rotate the nut 63 and a flange 63 a for abutment against a bottom side of a panel on a circulation system . fig9 is a pictorial view of a decorative cap 64 having a set of circumferentially spaced finger grips 64 a . cap 64 includes a flange 64 b for abutting attachment to the top of the dispenser housing head 62 and a set of external male threads 64 c for engaging female threads 62 d on dispenser housing head 62 . fig1 is a pictorial view of the dispenser housing locking cam collar 65 that is mounted in dispenser housing head 62 to enable one to lock a dispenser cartridge carrier 50 in position . cam collar 65 includes a cylindrical body 65 a with openings 65 b on each side . openings 65 b includes a vertical slot region 65 c and a lateral slot 65 d with a lip 65 e extending therein to lock a dispenser carrier therein . that is one pushes the cartridge carrier 50 ( see fig1 ) down with ears 56 and 56 a located in alignment with the vertical ; slot region 65 c and an identical vertical slot region on the opposite side . once lowered the cartridge carrier is rotated to cause the ears 56 and 56 a engage lateral stops 65 b and 65 c to retain the cartridge carrier therein . fig1 shows a pictorial exploded view of a panel 70 and a dispensing cartridge housing 61 to reveal the members 64 , 65 and 62 are located above the panel 70 and the nut 63 and dispenser housing 61 are positioned below the panel for the in situ assembly of the unit in a fluid circulation system . a feature of the invention is that the system can be assembled on site as an after market item or can be mounted on original equipment during manufacture of the water circulation system using conventional techniques . fig1 shows that in the first step the dispenser housing head 62 is inserted though an opening 74 in a top panel 70 . once inserted the external threaded section 62 b extends through the panel 70 . once threaded section 62 b extends through the opening in panel 70 the housing nut 63 can be positioned on threads 62 b and tightened to firmly secure the housing head 62 to panel 70 . thus the housing head 62 and housing nut 63 are sandwiched around panel 70 . one is now in a position to complete the installation of the dispensing system . with the housing head 62 secured to panel 70 the remaining components can be secured thereto from above and below the panel . that is , the dispenser housing 61 , which is located below the panel 70 , has internal mating surface 61 e , which is securable to the external dispenser housing head cylindrical mating surface 62 c , which extends through the panel . preferably , the dispenser housing and dispenser housing head are formed of pvc pipe and can be joined together through the use of solvent cement or the like . by permitting the securement of the dispenser housing to the dispenser housing head below the panel , as shown in fig5 , one can maintain a minimum size opening in the panel yet permit lateral extension 61 b on dispenser housing 61 since the dispenser housing 61 need not pass through the opening 71 in the panel 70 . once the dispenser housing 61 and dispenser housing head 62 are secured to each other the dispenser housing locking collar 65 can be secured into the dispenser housing head 62 , preferably through solvent cement or the like . the dispenser housing is now in a condition for receiving a cartridge carrier 50 and for locking the cartridge carrier in position therein . in order to close the dispenser housing the dispenser cap 64 is secured to the female threads 62 in the dispenser housing head 62 though male threads 64 c thereon . a sealing member such an is o - ring located beneath lip 64 b to prevents fluids from escaping there past . accordingly , a feature of the present invention is that the dispenser housing can be assembled in situ and secured to a fluid circulation system either in the field or as part of a manufacturing process through the steps of forming a hole in a panel , inserting a dispenser housing head therein , securing the dispenser housing head with a lock nut , securing the dispenser housing to the dispenser housing head while the dispenser housing head is secured to the panel . if a locking system for the cartridge carriers is required a locking collar can be secured to dispenser housing from above the panel 70 . to close off the system a dispenser cap can be rotatable secured into the dispenser housing head to prevent leakage . a feature of the present invention is that it can be incorporated into a fluid system either during the manufacture of the system or as an after market item . fig1 shows an exploded view of the dispenser housing proximate a panel on a water system and fig6 - 10 show individual components of an embodiment of the present invention . fig1 shows a partial top view of the cartridge carrier 50 that includes a handle 51 and a cylindrical body having a first tab 56 and a second tab 56 for forming locking engagement with the locking cam collar 65 ( fig1 ). fig1 shows a cross sectional view of housing 61 with a cartridge carrier 50 and a cartridge dispenser 40 coaxially positioned therein . a circumferential positioned port 61 b directs the fluid between the peripheral surface 61 g and the inner cartridge carrier 50 and cartridge dispenser 40 . the introduction of the fluid circumferentially induces a downward vertical flow between upper entry port 61 b and lower discharge port 61 c . the arrows indicate the general circular flow around the dispenser housing 61 and dispenser cartridge 42 to allow the dispersant to be dispersed into the fluid in the container 10 . it has been found that by introducing fluid tangentially one can produce a stable uniform flow pattern , i . e . the fluid flows uniformly past the openings 46 and 41 a even if the flow rates are changed . by maintaining a stable flow pattern past the openings 46 and 41 a it allows one to predictably control the dispersant rate by changing the flow rate . that is , the faster the flow rate past the cartridge 40 the greater the dispersant rate and conversely the slower the flow rate the slower the dispersant rate . a feature of the present invention is that not only can one predicable determine the dispersant rate by changing the flow rate but it has been found that as the number of openings are made available in the cartridge dispenser the concentration of the dispersant in the housing increases in a predictable manner . fig1 illustrates the concentration of the dispersant on the ordinate axis and with time on the abscissa axis . three different curves 80 , 81 , and 82 are shown to illustrate the dispersant rate under different size access areas in the dispersant cartridges . that is , curve 80 is the dispersant level as a function of time for a first number of access openings in cartridge 40 , the curve 81 is the dispersant level as a function of time for a larger number of access opening in cartridge 40 and curve 82 is the dispersant level as a function of time for a yet larger number of access opening in cartridge 40 . thus one way to control the amount of dispersant is to increase the area of the openings into the dispersant cartridge . in still another method one can increase the flow rate through the dispersant housing which also results in an increased dispersant level . while it is not fully understood it is believed that use of a circumferential input eliminates instability in flow patterns that can occur when fluid streams impinge on objects . as a result if the flow pattern remains stable one can uniformly increase or decrease the flow rate to correspondingly increase or decrease the dispersant rate . fig1 shows a portion of a fluid circulation system 99 for a fluid container such as found in spas , hot tubs , jetted bath tubs or swimming pools and the like . the fluid circulation system includes a fluid inlet 101 and a fluid outlet 102 located in a housing 100 having a chamber 110 therein . a cylindrical dispensing drawer 104 is slidable mounted in cylindrical chamber 110 in housing 110 with dispensing drawer 104 having a dispensing compartment 115 for holding a dispensable material 117 . located on the exterior surface of dispensing drawer 104 is a set of elastomer sealing members 105 , 106 and 107 for maintaining the dispensing drawer 104 and the housing 100 in a sealed condition with respect to one anther to prevent fluid flow past the dispensing drawer when the dispensing drawer is in an either an open or closed condition . fig1 shows the dispensing drawer 104 in the closed condition . in the closed condition a fluid or liquid , such as water , enters fluid inlet 101 and flows into chamber 115 , through the dispersal material 117 in chamber 115 and out the end of drawer 104 through a one way flap valve 118 . in this condition fluid circulates through the chamber 115 to enable the dispensing material therein to be dispensed into the fluid stream in response to the fluid flowing through the dispensing drawer 104 . fig1 shows the dispensing drawer 104 as the dispensing drawer is pulled partially outward from chamber 110 . in this condition the one way valve 118 closes and fluid flows from inlet 101 into fluid outlet 102 but is prevent from flowing into the dispensing chamber 115 in dispensing drawer 104 by the sealing member 107 engaging fluid outlet 102 . fig1 a shows an end view of dispensing drawer 104 with the one way flap valve 118 extending over openings 104 a , shown as dashed lines , to seal the openings 104 a . the top portion 118 a of flap valve is secured to drawer 104 to permit flap 118 to flex in a cantilevered fashion so that fluid can flow out of drawer 104 when fluid enter through top port 104 b . flap valve 118 is preferably a resilient material such as an elastomer . fig1 shows the dispensing drawer 104 in the open condition . in the open condition one can place a fresh charge of dispensable material in the dispensing compartment 115 . as can be seen in fig1 fluid bypass drawer 104 is held within housing 102 by a stop 120 comprising a flexible chain that has one end secured to drawer plate 109 and the other secured to housing 100 . stop 120 prevents the dispensing drawer 104 from being forced out of chamber 102 in the event the fluid in chamber 110 remains under pressure . when the dispensing drawer 104 is in an open condition the dispensing material 117 a is placed in chamber 115 . the dispersant drawer 104 is then pushed in to a closed condition wherein the dispensing material therein can be dispensed into the fluid circulation system as illustrated in fig1 . thus in the embodiment of fig1 - 17 one can quickly reposition spent dispersant by pulling out a dispensing drawer , placing the dispersant in the drawer and then closing the drawer . the dispensing drawer can be mounted on either a high pressure side of a fluid circulation system or a low pressure side of a fluid circulation system . fig1 shows a dispensing drawer 141 , which is mounted in a low pressure portion of the system . drawer 141 can be pulled out to allow a dispersant to be placed in the drawer 141 and the dispensing drawer than closed to allow the dispersant material to be dispersed into the system . fig1 also shows a partial view of a fluid system 130 having a pump 131 for circulating fluid from container 133 into inlet 132 and then directing the fluid through a outlet 132 into a drawer housing 140 which cause the fluid to flow through the dispensing drawer 141 and into a spill or return conduit 142 which delivers the fluid into container 133 . the fluid interface between the atmosphere and the liquid is identified by reference numeral 135 . the embodiments of fig1 and fig1 are extremely user friendly . that is practically everyone is familiar with the operation of a drawer and the placement of articles in the drawer . consequently , a user can periodically replenish the dispersant material by merely opening a drawer , placing the dispersant material in the drawer and closing the dispensing drawer . fig1 shows a perspective view of a slidable dispensing drawer 141 for use in the embodiment of fig1 . dispensing drawer 141 includes a set of lateral extension members 142 , 143 , 144 and 145 extending upward from a bottom member 147 to form an open top compartment . bottom member 147 has a plurality of openings 147 a therein to permit flow of fluid therethrough . a front member 149 and a rear member 150 complete the compartment for holding the dispensing material therein . a handle 153 allows one to pull dispensing drawer from the fluid system housing 130 much like one opens a conventional sliding drawer . once dispensing drawer 149 is open , the user can place dispensable materiel in the dispensing drawer 141 much like one places an article in a drawer . in order to prevent withdrawal of the dispensing drawer when the pump is operating a limit switch ( not shown ) can be connected to the drawer so that when the drawer is pulled outward the power to the pump 131 is shut off thereby prevent flow of fluid into the dispensing drawer or a bypass can be used to divert the fluid back into the container fig2 shows an example of a type of dispensing cartridge 156 that can be used with the present invention . cartridge 156 includes a set of openings 157 to permit fluid access to the contents 158 therein , which can typically be an ion yielding material such as silver chloride or the like . fig2 shows that other dispensable materials such as a solid bromine stick 160 can be placed in the dispensing drawer 150 . fig2 shows the sectional view taken along lines 5 - 5 to show the compartments 161 , 162 and 163 located behind front panel 149 to show the compartments with the upright extension for confining the dispensable material . therein . thus the dispensing drawers of fig1 - 22 disclose a user friendly method of adding dispersant to a fluid system such as a hot tub , spa , jetted bath tub , swimming pool or the like wherein the user merely pulls out a drawer and drops the dispersant into the drawer and then closes the drawer . in one embodiment the drawer can be placed in the pressurized fluid circulation system without shutting down the system and in the other embodiment the system can be automatically shut down as the drawer is opened to prevent fluid from escaping . fig2 shows a partial sectional view of an alternate embodiment of a dispensing member for use in fluid systems including spas , hot tubs , jetted bath tubs swimming pools and the like . in the embodiment shown the system 170 includes a container 171 with a fluid 169 therein . the fluid is directed upward through conduit 172 into a funnel shaped member 174 that directs the fluid through a porous member 173 that permits fluid to flow therethrough but prevents the dispensing material 166 , 167 , and 168 from falling through . in operation of the system 170 the fluid flows upward like a fountain and flows gently around or through the dispersant to bring the dispersant into the body of fluid . the path of the fluid is indicted by the arrows . in the embodiment shown a cover 176 is hinged over the top of the fountain like dispenser to isolate the dispensing unit form contact . however , in an alternate embodiment the cover 176 need not be used to enable the dispersant to be readily accessible . in this embodiment one can readily observe the condition of dispersant in the system and can replenish the dispersant when the dispersant is spent or in a low condition . thus , the embodiment of fig2 includes a method of replenishing a dispersant in a spa , hot tub , jetted bath tub or pool therein comprising the steps of directing a liquid through a fountain with a tray 173 having a spill chute 173 a for returning the liquid to a body of recreation liquid 169 under the influence of gravity ; and placing a fresh charge of dispersant such as dispersant 166 , in the tray 173 to allow the liquid to flow over the charge of dispersant 166 , 167 or 168 to thereby carry the dispersant into the body of recreational liquid 169 . fig2 and fig2 show hanging dispenser 200 comprising a support member 201 having a top member 201 a with a lip 201 b for engaging a portion 210 such as a side wall of a fluid system . in the embodiment shown the top member 201 a is located above a fluid line such as liquid gas interface 202 with a dispenser housing 203 carried by member 201 having a compartment 214 herein for receiving a dispersant material located below the fluid line 202 to permit the fluid in the system to come into contact with the dispensable material therein . a pivotal lid 212 can be placed on top of the dispenser housing 202 to enable a user to quickly place a dispersing cartridge , bulk dispersant material or dispenser cartridges in the compartment 214 in the dispersant housing . in the embodiment shown the dispenser housing 203 includes a plurality of openings 207 therein to permit ingress and egress of fluid therethrough . the dispenser housing is shown in fig2 with two dispensing cartridges 205 , 206 located in the compartment 214 in housing . an example of a dispensing cartridge 205 or 206 is the dispensing article 40 shown in fig1 . in operation of the hanging dispenser of the top member 201 a extends laterally from member 201 to engage a ledge 210 a on a fluid container in the system with the top member 201 a including a ridge or lip 201 b to prevent the top member 201 a from accidentally slipping off the ledge 210 a . thus the present invention includes the method of replenishing a dispersant in a spa , hot tub , jetted bath tub or pool therein comprising : removing a cover located above a water line in a container of recreational water ; placing a charge of dispersant in a liquid line ; and placing the cover on the liquid line to thereby enable the dispersant to be delivered to the recreational water in the container to render the recreational water suitable for body immersion . the present invention also includes the method of replenishing a dispersant in a spa , hot tub , jetted bath tub or pool therein comprising sliding a drawer having an open chamber normally positioned in a liquid media at least partially out of a drawer housing located in a fluid circulation system ; placing a fresh charge of dispersant in the drawer ; and closing the drawer to permit the dispersant to be carried into the liquid media . | 2 |
referring now to the drawings by reference characters , and particularly fig1 - 5 , there is shown a motor 7 having a drive shaft 9 with a pulley 11 thereon . mounted parallel to the drive shaft 9 is a driven shaft 13 . the driven shaft 13 has a pulley 15 thereon which rotates freely with respect to shaft 13 and which is driven by belt 17 from the pulley 11 acting on the driving face 16 of pulley 15 . an arm 19 directly connected to the shaft 13 so that if the arm 19 moves , the shaft 13 moves with it . arm 19 has a segment member 21 attached thereto , said segment member closely overlying a small portion of the driving face 16 of pulley 15 and being normally spaced slightly therefrom so that the member 21 is normally not in contact with the face 16 of pulley 15 . since the belt 17 is normally in contact with about 180 ° of the pulley face 16 ( i . e ., slightly more or less than 180 ° depending upon the relative sizes of pulleys 11 and 15 ), the segment 21 will have an arcuate length of somewhat less than 180 ° and may be very substantially less . in any event , as will be later apparent , the segment must normally lie between the tangent portions of belt 17 without touching the belt . arm 19 has a pin 23 extending therefrom which is connected to a spring 25 which biases arm 19 in the direction of rotation of pulley 15 . shaft 13 carries a pin 27 which is normally in contact with a stop 29 . thus , spring 25 urges shaft 13 in the direction of rotation of pulley 15 , but the stop 29 normally prevents the shaft from rotating . stop 29 is provided with a means for withdrawing it from contact with the pin 27 which can conveniently take the form of a solenoid 31 , having an armature 33 attached to stop 29 . pin 27 can be eliminated and the stop made to act on pin 23 . in some instances , the spring can be eliminated since friction or gravity , if the rotation direction is reversed , will serve as the bias means . the use of a spring is preferred to bring the segment rapidly up to speed as well as insuring positive action and preventing rebound . the operation of the device can now be readily appreciated by reference to fig2 through 5 . in the normal condition , the parts are in the position shown in fig2 and 3 wherein the pulley 11 is continously driving the pulley 15 through the belt 17 . stop 29 , acting on the pin 27 , prevents any rotation of shaft 13 . now if one energizes solenoid 31 , stop 29 is removed from contact with pin 27 so that spring 25 urges segment 21 into contact with belt 17 as is shown in fig4 and 5 . the motor acting through the belt against segment 21 now rotates shaft 13 . if solenoid 31 is pulsed only momentarily , as shaft 13 makes one revolution , stop 29 again engages pin 27 so that shaft 13 is again at rest and the parts are in a position for a repetition of the operation . if the stop is released for a longer period of time , more than one revolution of shaft 13 is obtained . in the structure thus far described , segment 21 is a rigid structure and at no time comes into contact with the face 16 of the pulley 15 as is shown in fig5 . in accordance with the embodiment shown in fig6 the segment 21 is replaced with a springy member 35 , suitably a resilient plastic , the springiness normally holding the member out of contact with the face 16 of the pulley . however , since the member 35 is engaged by the belt as soon as arm 19 is released , member 35 will be drawn down into contact with the pulley face 16 and will maintain contact during the one or more revolutions through which the clutch operates . after shaft 13 stops , the segment 35 will again flex back out of contact with the pulley face 16 . the member 35 may be provided with a friction surface to ensure that there will be no slippage between the pulley face 15 and the member 35 . in this embodiment of the invention , advantage is taken of the inertia of pulley 15 as well as that of pulley 11 and belt 17 so that the maximum amount of energy can be taken from shaft 13 for a motor of given size . in fig7 another embodiment of the invention is shown wherein a flexible belt having teeth thereon is employed . belt 40 has teeth 42 formed integrally therewith and the drive pulley 44 as well as the idler pulley 46 have complimentary teeth . the segment 48 has complimentary teeth 49 and is attached to shaft 50 as previously described . the parts not numbered in this drawing have exactly the same function as the parts of fig1 . as can be seen from fig8 when the solenoid is pulsed , the segment 48 engages the teeth 42 as previously described and causes shaft 50 to revolve . in some applications , it is desirable to take two intermittent motions from a single motor . for instance , in a terminal printer , it would be highly desirable to derive the character feed and line feed motions from the same motor . thus , referring to fig9 and 10 , there is shown a motor 52 driving shaft 54 which is keyed to pulley 56 . a second shaft 58 is free to revolve with respect to shaft 54 and is concentric therewith . shaft 58 is supported near its outer end by bearing 59 . shaft 58 carries arm 60 to which segment 62 is attached . shaft 58 is normally prevented from rotation by means of detent 64 while spring 66 biases arm 60 in the direction of rotation and against the detent 64 . the driven pulley 68 is mounted on shaft 70 but is free to rotate with respect thereto . belt 67 drives pulley 68 from pulley 56 . arm 72 , carrying segment 74 , is fixed to shaft 70 while detent 76 normally prevents shaft 70 from rotating and spring 78 biases arm 72 in the direction of rotation . if it is desired that shaft 70 turn , detent 76 is pulsed and the operation is exactly as was described in connection with fig1 . when it is desired that shaft 58 rotate , detent 64 is pulsed , whereupon the segement 62 is urged into contact with the belt 67 causing shaft 58 to rotate . since the intervention of the segment 62 between the belt and the pulley tends to reduce the ability of the pulley to drive the belt , preferably the segment 62 does not overlie the entire face width of the pulley but only about half of it . thus , as can be seen at the bottom portion of fig1 , during the driving cycle the belt is driving both segment 62 and pulley 56 . of course , if the segment 62 is made shorter , so that it extends only a few degrees over the face of pulley 56 , there will be less tendency for the pulley to be free from the belt , in which case this overlapping relationship of the belt over both the pulley and segment becomes less necessary . still another embodiment of the invention is shown in fig1 wherein shaft 80 is keyed to a pulley 82 . the pulley is provided with a notch 84 and a belt 86 lies in this notch with a portion of the belt 88 being unsupported by the pulley and held in an extended position by the combination of the stiffness of the belt material and the notch 84 . an arcuate segment member 90 lies substantially on the same plane as that of the notch 88 . segment 90 is supported on arm 92 which corresponds with the arm 60 of fig9 . now , when the shaft is released , the belt couples the pulley to the segment . in this embodiment of the invention , the belt is not distorted , as is in the previous embodiments but merely serves as a coupling element between the segment and the pulley face which lie on the same plane . further , with this embodiment of the invention the drive pulley is fully in contact with the belt at all times and the segment does not tend to decouple the drive pulley from the belt . of course , if one wishes to take two independent drives from a single motor it is not necesssary to employ the structure of fig9 and a single motor can drive two or more integral clutches of the type shown in fig1 by providing the drive motor with a plurality of drive pulleys . although certain specific embodiments of the present invention have been illustrated , it will be obvious to those skilled in the art that many variations can be made without departing from the spirit of this invention . | 8 |
a typical arrangement of a rotary joint having an external compensator is shown in fig1 and this arrangement is very similar to that shown in the assignees u . s . pat . no . 3 , 874 , 707 . the rotary joint is generally indicated at 10 and includes a housing 12 having a conduit inlet port 14 . the housing includes an inner wall plate 16 attached to the housing by bolts , and at its other axial end the housing is closed by the outer wall plate 18 also attached to the housing by bolts . the housing wall 18 also includes a syphon housing 20 whereby syphon structure , not shown , may communicate with the housing 12 . internally , the housing 12 is mounted upon the rotating tubular nipple 22 which is coaxially connected to the rotating heat exchanger drum for rotation therewith , not shown , receiving the pressurized medium introduced into the rotary joint 10 through the inlet port 14 . sealing structure is located within the housing 10 interposed between the nipple 22 and the housing and such seals are of an annular configuration including collars 24 and 26 , at least one of which may be axially displaceable on the nipple , and an annular sealing ring 28 is located between collar 24 and inner wall 16 while the annular seal 30 is located between collar 26 and outer wall 18 . a compression spring 32 biases the collars 24 and 26 into engagement with the associated sealing ring and sealing surfaces exist between the collars and their associated sealing rings , and between the sealing rings and their associated housing end wall plates . as will be appreciated , as the housing sealing structure is directly exposed to the pressurized medium , usually steam , within the housing 10 significant internal pressures exist within the housing that are also imposed upon the sealing structure causing the engaging surfaces of the seals and collars to firmly engage . the rotary joint housing 10 is supported upon a pair of radially extending arms 34 which have holes at their outer ends for slidable association with the support rods 36 which are attached to fixed support structure adjacent the rotary drum , not shown . the support rods 36 are threaded at their outer ends for providing support for the compensating external expansible chamber device or motor 38 as later described . the aforedescribed rotary joint structure is known and fully described in the assignees u . s . pat . no . 3 , 874 , 707 . the construction of the compensating expansible chamber motor 38 is best appreciated from fig2 . the compensator comprises an expansible chamber motor 38 having a housing defined by an outer cover plate 40 , an annular spacer plate 42 , and a body plate 44 . these three plates are maintained in assembled relationship by eight threaded bolts 46 having heads bearing against the cover plate 40 , and threads which thread into holes defined in the body plate 44 . as will be appreciated from fig2 plates 40 and 42 are each provided with an internal cylindrical surface of equal diameters to define the cylindrical chamber 48 of the compensator motor . the plate 44 includes a pair of radially extending arms 50 having threaded nuts 52 affixed thereto and by the use of lock nuts 54 , the axial position of the compensator motor 38 to the support rods 36 , and to the joint housing 12 , can be accurately determined and maintained . it is to be appreciated that the rotary joint arms 34 are supported upon the support rods 36 for axial displacement of the housing 12 relative thereto , while the compensator 38 is axially fixed with respect to the support rods and the joint housing . the compensator 38 includes a piston 56 axially extending through the center of the body plate 44 through a bushing 58 , and internally , a circular rigid head 60 is mounted upon the piston by bolt 62 . a flexible diaphragm 64 formed of a high temperature resistent elastomer and fabric , such as commercially known under the trademark viton , is mounted upon the piston head by a lip retainer 66 held in position by the bolt 62 , and at its outer region the flexible diaphragm is received between the joining surfaces of the cover plate 40 and the spacer plate 42 so that the outer circumference of the diaphragm is sealed with respect to the compensator housing . a compression spring 68 circumscribing to the boss 70 formed on the cover plate bears against the lip retainer 66 to bias the piston head and piston to the right , fig2 ., into engagement with the anvil 72 defined on the rotary joint syphon housing 20 . an inlet port 74 , fig2 is formed in the cover plate and is tapped with a 1 / 2 &# 34 ; pipe thread for receiving the air supply tube 76 , fig1 . with reference to fig4 the circuitry and operation of the external rotary joint bearing compensator of the invention will be explained . the pressurized medium , such as high temperature steam , supplied to the rotary joint 10 through the port 14 is supplied from a header 78 . a transmitter 80 is in communication with the header 78 sensing the pressure within the header . the transmitter 80 produces a signal proportional to the pressure within the header and this signal is transmitted to the multiplier 82 . the multiplier 82 in turn produces a signal fed to the amplifying relay 84 which is in the form of a compressed air regulator receiving compressed air through supply conduit 86 the pressure of the compressed air from the regulator 84 is determined by the signal received from the multiplier 82 , and the regulated compressed air is supplied through conduit 88 to the compensator expansible chamber motor 38 through tube 76 , and accordingly , the pressure within the compensator chamber 48 will be determined by the regulator 84 and the axial force imposed on the rotary joint housing 12 by the piston 56 is accurately determined by the value of the compressed air within the compensator 38 . in fig4 a plurality of compensators 38 are shown as being controlled in parallel by the compressed air from regulator 84 , and it will be appreciated that a plurality of rotary joints 10 may be controlled by a single regulator or each rotary joint may have its own regulator . it will be appreciated from the above description that the compressed fluid medium used to control the compensator expansible chamber motor 38 is separate and distinct from the pressurized fluid medium within the header 78 and joint 10 . as the preferred control pressurized medium is compressed air , and as compressed air will be relatively cool , no significant deterioration of the flexible diaphragm 64 will occur due to the compensator medium , and as will be appreciated from fig2 the &# 34 ; fold &# 34 ; of the diaphragm may be significantly long to permit sufficient piston travel to accommodate the entire range of movement required for compensation as the seals wear without necessitating adjustment of the compensator upon the support rods 36 . in the disclosed control circuitry shown in fig4 the transmitter 80 and multiplier 82 are air controlled , and compressed air is supplied to the transmitter and multiplier through the compressed air conduit 90 . the transmitter 80 may be a foxboro pressure transmitter and the multiplier may also be a foxboro pneumatic computer multiplier while the amplifying relay regulator may be a standard model manufactured by moore products . as the transmitter 80 receives a steam pressure signal from the header , the transmitter produces an air pressure signal corresponding to the steam pressure and the pneumatic computer multiplier 82 produces an air pressure signal proportional to the amount of compensation force needed . this air pressure signal from the multiplier 82 is then supplied to the amplifying relay regulator 84 where it is boosted to provide the necessary pressure for the compensator 38 . while , in the enclosed embodiment , the sensing and control of the air pressure supplied to the compensator utilizes air controlled devices , it will be appreciated that electronically operated transmitter and multiplier devices may be used and the amplifying relay would constitute an electrically controlled compressed air regulator . the computer multiplier 82 , or transmitter 80 , or both , include readily adjustable controls so that the air pressure supplied to or through the conduit 88 may be very accurately regulated merely by adjusting such controls . thus , the practice of the invention permits the amount of load bearing compensation of the rotary joints to be very accurately regulated to accommodate the particular conditions present . to obtain maximum seal ring life the force exerted on the seal rings 28 and 30 and the temperature of the seal rings must be maintained at a minimum . however , the axial sealing force on the seal rings must be sufficient to produce effective sealing . excessive force on the seal rings causes faster than normal wear and high temperature causes rapid deterioration . the axial force on the seal rings is determined by the pressure of the medium within the rotary joint , and the temperature of the seal rings is determined by both the temperature of the medium within the joint and the heat generated by contact between the seal rings and the associated collars and plates . while the temperature of the medium within the joint cannot be regulated , the degree of seal friction can be controlled by the compensation provided by the practice of the invention , and by regulating the output signals of the transmitter and multiplier the degree of axial compensating force imposed on a rotary joint may be very accurately regulated and varied if desired . such &# 34 ; customized &# 34 ; adjustment has not been previously available with either external or internal compensated rotary joints . by utilizing compressed air as a control pressurized medium for the compensator expansible chamber motor problems previously encountered due to condensate within the expansible chamber motor compensating motor are eliminated , the seal structure within the compensator is not exposed to high temperatures , and sufficient axial piston movement can be achieved with 100 % effective sealing between the piston and chamber by the use of the diaphragm is present as compared to the limited metal diaphragm movement of prior art devices , and with the practice of the invention the ability of an exteriorly compensated rotary joint to handle nonconcentric installations is maintained while simultaneously providing a degree of control of compensation not heretofore achievable . it is appreciated that various modifications to the inventive concepts may be apparent to those skilled in the art without departing from the spirit and scope of the invention . | 8 |
referring now to fig1 this invention is a direct development of the prior art taught in thomas , et al . fig1 is a simplified side view of the nozzle housing assembly shown in fig3 of u . s . pat . no . 3 , 997 , 111 . accordingly , the teachings of thomas , et al . show a nozzle housing 10 holding a mounting ring 12 and a nozzle element 14 . high - pressure fluid enters the system in the direction shown by the arrow in fig1 and is collimated upstream of the arrow to form a high - pressure jet . nozzle 14 has an opening 16 to receive the high - pressure fluid . the nozzle is conventionally fashioned from sapphire and is held in place by a mounting ring 12 formed of an elastically deformable material . this mounting ring is set in the nozzle housing 10 to define seal areas between the corresponding elements accordingly , a first seal area 18 is defined annularly between the elastic ring and the nozzle 14 . a second concentric seal area 20 is defined between the mounting ring 12 and nozzle housing 10 , and a third transversely extending seal area 22 is defined perpendicular to the nozzle opening 16 . an exit port 24 is utilized to discharge the thusly formed high - pressure stream . as previously indicated , the nozzle mount shown in the prior art fig1 has shown a propensity to leak under the nozzle area -- that is , in the area of seal 22 . additionally , the deformable mounting ring 12 has tended to , under pressure , extrude into the seal area 20 thereby reducing the area of seal between the nozzle element 14 shown as seal 18 . moreover , deformation of elastic material has caused displacement of the nozzle element 14 relative to the discharge opening 24 . turning now to fig2 a first preferred embodiment of this invention is shown which eliminates the deformable mounting ring 12 . as shown in fig2 the nozzle housing 26 is secured in a support 28 . the support has a threaded portion 30 for threading of the support and allied internal structure into an upstream pipe not shown . the housing 26 can be fashioned of a steel material , such as 300 series cres . a first high - pressure seal is formed between the nozzle housing and the threaded support element 26 along surface 32 . this seal is applied by the use of a mounting nut , not shown , which is threaded onto an upstream pipe 34 which contains the nozzle housing . the nozzle element itself , 36 , fashioned typically from sapphire , is a disc of approximately 0 . 090 inches . it may typically range from 0 . 050 - 0 . 150 inches and has an internal bore constituting a jet shaping port 38 . the diameter of that shaping port is in the range of approximately 0 . 003 - 0 . 015 inches . a nozzle mount 40 is used to position and seat the nozzle 36 in the housing 26 . the nozzle mount is formed from a material which , although relatively hard , tends to yield slightly under the influence of high pressure . accordingly , with the application of fluid pressure in the range of 60 , 000 psi , the nozzle 36 tends to be impressed upon the mount 40 creating a seal about the surface 42 . because the nozzle mount 40 is set in the housing 26 and this element is of a harder material than the mount 40 , a support is formed for the mount by the harder material which will withstand the sliding contact forces applied during installation . a suitable material for the mount is one which has a yield strength in proportion to the working pressure of the fluid . such an element allows firm placement of the nozzle element in the mount , yet provides for a good sealing surface . in view of the relatively small size of the nozzle element , the increased size of the mount provides an adequate technique for handling of those elements when not in the mount itself . additionally , because the nozzle mount has a section 44 disposed immediately downstream of the nozzle element 36 , a sealing surface of compatible yielding material is provided along surface 42 backed up by nozzle housing 26 without the problems of deformation and elastic recovery in the prior art . this section eliminates the problem of the washer extruding into the seal area . also , the use of the harder steel material in the nozzle mount 26 provides a third sealing area 44 between the housing mount 26 and the nozzle housing 40 . a small radial clearance shown as surface 39 in fig2 typically of the order of 0 . 001 - 0 . 003 inch , is provided between the nozzle element 36 and the nozzle mount 40 to prevent cracking or other structural damage to the nozzle element due to radial yielding deformation of the nozzle mount when subjected to the high - pressure fluid . in operation , high - pressure fluid in the realm of 40 , 000 - 60 , 000 psi is fed to the nozzle element via upstream pipe 34 . the nozzle element 36 , having a flat surface to contact its housing , is forced down by liquid pressure providing an adequate high - pressure seal such that no liquid will flow around the nozzle element . in this example , a material such as free - machining brass , having a yield strength of about 50 , 000 psi , can be used for the housing 40 . this minimizing of leakage reduces wetting of the material being cut . additionally , because the housing not only surrounds at surface 39 but additionally provides a yielding bearing surface 42 , firm placement of the nozzle element against lateral shifting or displacement is facilitated . the nozzle element 36 in intimate contact with the nozzle mount 40 prevents leaks which would tend to form in the prior art , for example , between the nozzle element 14 and the housing 10 along the common surface wall 22 as shown in fig1 . in this invention , the elimination of contact between the nozzle and the nozzle housing improves control of the liquid jet by eliminating all leaks along that surface . hence , as shown in fig2 the surface 46 between the nozzle mount and its housing 26 does not in any way involve contact of the nozzle element 36 . additionally , repeated and rapid duty cycling by means of an upstream valve resulting in the cycling of high - pressure liquid through the orifice 38 will not dislodge the nozzle element 36 as is a tendency in prior art designs . referring now to fig3 another preferred embodiment is shown wherein the same basic concept -- namely , of having the nozzle element bear against a mount for it as opposed to direct contact with the nozzle housing -- is shown . in fig3 as in other designs , a support 28 is screwed into a pipe section 50 by means of thread elements 30 . the nozzle element 36 has an axial bore 38 aligned with a complementary bore 52 in the mounting plate 40 . this alignment is self - centering during operation . a high - pressure seal is formed along surface 32 between the support 28 and the pipe 50 . high - pressure cutting fluid in source 34 tends to press the nozzle element 36 into contact along surface 42 with the mounting plate 40 . a small amount of grease on surface 42 will hold element 36 in position during assembly . accordingly , a high - pressure seal is formed between the nozzle element 36 and the support 40 during cutting . as in the prior examples , the nozzle support plate 40 shown in fig3 is fashioned from a material which will withstand sliding forces applied to it , but will yield slightly under the influence of the fluid pressure . fig4 shows a variation of the fig2 embodiment wherein the nozzle element 36 is disposed in the housing 40 in the same manner as shown in fig2 . additionally , however , a mounting plate 54 is utilized and interposed between the nozzle housing and the housing mount 28 . this plate 54 extends the full circumferential width of the chamber 34 to provide , in a manner shown in fig3 adequate seating for the nozzle housing against the support 28 . as in prior examples , the nozzle element 36 has a surface 42 bearing against its mount 40 to provide sealing contact , thereby preventing leakage . referring now to fig5 yet another preferred embodiment is shown . in this embodiment , the support pipe element 50 is threaded by internally extending threads 56 to couple the support housing 26 directly to the pipe . the threads 56 extend to the upper surface where the housing joins in forming a common surface with the nozzle element mount 40 . a high - pressure seal 32 is formed between the pipe 50 and the support housing 26 in a manner described hereinabove . the nozzle element 36 has a portion raised above the surface 56 defined by the top walls of the support housing 26 and the nozzle mount 40 . in this embodiment , the use of a lower support plate 28 is eliminated and the nozzle housing extends contiguous to the outer pipe 50 and is threaded into it by threads 56 . as in the prior embodiments , the nozzle element itself , 36 having orifice 38 , is disposed in a pressure transfer relationship with the mount 40 . referring now to fig6 a , there is shown a first preferred fluid jet nozzle configuration , and in fig6 b a plot of energy density for the nozzle of fig6 a as a function of cross - section . the nozzle 36 has an orifice 38 with a bevel section either radiused or conical in shape . the angle of the taper is generally in the range of 10 - 20 °. the nozzle , typically fashioned from sapphire , has a height t in the range of 0 . 030 - 0 . 040 inches and the radius of the taper 60 is approximately 0 . 5 t to a depth of 0 . 005 inches . the ratio of length / diameter ( l / d ) for the orifice 38 is in the range of 1 . 5 - 2 . 5 . as shown in fig6 b , the energy density ( ed ) is plotted as a function of cross - section of the nozzle . the nozzle of fig6 a will produce a well - collimated beam having a dispersion rate of 1 . 0 - 1 . 2 diameters at 100 diameters nozzle length . at a working pressure of 40 , 000 - 60 , 000 psi , an optimum cutting speed is about 13 inches per second . because the beam is well shaped , it is suited for low - ply fabrics , homogeneous solids and hard materials . fig7 a shows a second preferred embodiment of the nozzle element 36 . the nozzle of this configuration will produce a more dispersed beam having areas of spray as shown in the shaded portions of the energy density plot shown in fig7 b . such a nozzle will be usable for fibrous goods , loose - woven materials and low - density laminates . the jet produced has a high energy density during the center portion of the beam with residual areas at the outside of the jet to sever threads or fibers that are not rigidly held in place by the interior properties of the material . such a jet can be accomplished by using the taper configuration of fig6 a with an l / d ratio reduced to 0 . 7 - 1 . 0 . the taper 60 is primarily for purposes of reducing nozzle wear at the upstream section but plays a role in jet shaping . accordingly , the depth of the taper t 1 can be increased from 0 . 005 to approximately 0 . 010 - 0 . 015 . in such a configuration , the l / d ratio is in the range of 1 . 5 - 1 . 8 . a nozzle fasioned in accordance with the above - referenced parameters will also produce the beam having the energy density shown in fig7 b . fig8 a shows a third nozzle configuration having a broad energy density configuration shown in fig8 b . as in the case of fig7 b , the area of spray is shown as the shaded portion of fig8 b . such a jet is suitable for very loose - weave materials , multiple ply cutting and elements that tend to move on the cutting table . although a large degree of dispersion occurs , so long as the jet strength is greater than four times the tensile strength of the material to be cut , adequate cutting will take place . the depth of the taper t 1 is approximately 0 . 015 inches and the l / d ratio is in the range of 0 . 2 - 1 . 5 . as shown in fig8 a , the depth of taper is deep relative to the orifice 38 . a wide beam of relatively uniform energy density in the cutting region is produced . since cutting occurs at the edge of the stream as it moves across the material , the jet produced by the nozzle of fig8 b will having a relatively longer duration of cutting time per cut to insure complete severing of the goods . it is readily apparent that other configurations and embodiments are present without departing from the essential aspects of this invention . so long as the nozzle element bears directly against a mounting element to provide sealing contact under pressure between those elements , a well - collimated beam will result without the attendant problems of leakage around the nozzle . | 1 |
the present invention is directed to an instruction folding mechanism , a method for performing the instruction folding mechanism and a pixel processing system employing the instruction folding mechanism to fold instructions with data independency into reduced instructions for generating a new program . furthermore , the instruction folding mechanism is used to fold instructions having an identical target register and outputs data to different components of the target register to save the hardware cost of pixel processing system . it should be noted that the instruction folding mechanism is also suitable for vertex shader , geometric shader or a combination of the two . fig5 is a block diagram of a pixel processing system having an instruction folding mechanism according to one preferred embodiment of the present invention . the pixel processing system comprises an instruction folding mechanism 500 and a pixel shader 502 . the instruction folding mechanism 500 folds a plurality of first instruction in a first program 504 to generate a second program 506 having at least one second instruction which is a combination of the first instruction . the pixel shader connected to the instruction folding mechanism 500 fetches the second program 506 to decode at least the second instruction having the combination of the first instruction to execute the second program 506 . fig6 is a block diagram of an example program applied to the instruction folding mechanism in fig5 according to one embodiment of the present invention . the data of instruction “ mul ” is independent in the first program 504 from that of instruction “ mov ”, and the data output of “ mul ” and “ mov ” is stored in an identical register , i . e . “ r 1 ”, but in different components . in one embodiment , the total number of source operands of the data is three , i . e . “ r0 ”, “ t0 ”, and “ r0 . a ”, and it can easily be performed by the instruction folding mechanism to create a new instruction , e . g . “ mul_mov ”, as in the second program 506 . therefore , a decoder can easily decode the new “ folded ” instruction . since the instruction of the pixel shader is able to cover the total number of the source operands , an additional operand capacity of the instruction is not required to expand in order to save hardware cost of the pixel shader . however , in the prior art of a co - issue architecture , additional decoders for operators , operation pipelines , register write ports and register read ports for the operator are necessary to be prepared . furthermore , instructions should be provided with many processing abilities , e . g . component selections , format transformations , source code modifications , and instruction modifications of source and target operands . therefore , it is important to reduce the number of the operands . fig7 is a detailed block diagram of the instruction folding mechanism in fig5 according to one embodiment of the present invention . the instruction folding mechanism 500 comprises an instruction scheduler 700 , a folding rule checker 702 , and an instruction combiner 704 . the instruction scheduler 700 connected to the folding rule checker 702 is used to scan the first instruction according to static positions to schedule the first instruction in the first program 504 . preferably , the instruction scanner 700 successively scans the first instruction . the folding rule checker 702 checks the first instruction according to a folding rule whether the first instruction has data independency . the instruction combiner 704 connected to the folding rule checker 702 can combine the first instruction having the data independency to generate at least the second instruction in the second program 506 . specifically , in one preferred embodiment of the present invention , a general formula of folding rule is represented as following items : opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , where opc 1 and opc 2 are arbitrary operators and opc 1 _opc 2 is a new combination operator indicating an operation instruction which performs opc 1 in components ( r , g , b ) and opc 2 in component “ a ”. the target operands , tgt . [ r | g | b ] and tgt . a , of opc 1 and opc 2 are in a same register , i . e . register “ tgt ”, but in different components of “ tgt ”. for example , component “ a ” is located in opc 1 and opc 2 at the same time . additionally , the representation [ r | g | b ] means that components “ r ”, “ g ”, and “ b ” are not necessarily present but not limited to their presence src 0 , src 1 , and src 2 are source operands and have arbitrary component ( s ), where opc 1 is defined as a binary operator having two operands , including operands src 0 and src 1 , or defined as a unary operator including operand src 0 only . the formula of tgt . [ r | g | b ]∩ src 2 = φ . represents data independency in viewing of opc 1 and opc 2 , which the operation results of opc 1 are irrelevant to that of opc 2 . in one embodiment , instruction opc 1 is not required to be adjacent to opc 2 but only if the data of opc 1 is independent from that of opc 2 . while taking the orders of instruction opc 1 and opc 2 into consideration , the formula of the folding rule also can be represented as follows : opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , where while instruction opc 1 is a unary operator and opc 2 is a binary operator , the formula of folding rule also can be represented as follows : opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , where opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , where when opc 2 is defined as a unary operator in the representation , operand includes src 1 only . in one preferred embodiment of the present invention , component “ a ” is operated alone and the result is then moved by instruction “ mov ” while component “ a ” is a “ transparency ” or coordinates of fourth dimension in the graphic effect applications . component “ a ” is operated by instruction “ rsq ” to calculate the result of ( 1 /√ x ) while component “ a ” is a distance or an angle from the light source in the lighting effect applications . while component “[ r | g | b ]” represents colors or coordinates , instructions “ mov ”, “ mul ”, “ add ”, “ mad ”, and “ dp3 ” are usually used , for example . as a result , in one embodiment , when opc 1 is instructions “ mov ”, “ mul ”, “ add ”, “ mad ”, or “ dp3 ” and opc 2 is “ mov ” or “ rsq ”, the combination of opc 1 _opc 2 can be instructions “ mov_mov ”, “ mul_mov ”, “ add_mov ”, “ dp3_mov ”, “ mov_rsq ”, “ mul_rsq ”, “ add_rsq ”, or “ dp3_rsq ”. in the present invention , a decoder in the hardware is additionally able to decode these instructions of opc 1 _opc 2 or other combinations of opc 1 and opc 2 to increase the capability of the pixel shader . in another preferred embodiment of the present invention , the operands of new instructions of folding rule are four , src 0 , src 1 , src 2 , src 3 , and instruction “ mad ” can be used . although , a register read port and source modifier in the hardware can be added , its cost - effectiveness is better than that of a co - issue mechanism . the general formula of folding rule is represented as follows : opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , src 3 , where taking the order of instructions opc 1 and opc 2 into consideration , the formula of folding rule also can be represented as follows : ( 6 ) opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , src 3 , where when opc 1 is defined as a unary operator , its operand includes src 0 only , and when opc 1 is defined as a binary operator , its operands include src 0 and src 1 . when opc 1 is defined as a unary operator and opc 2 is a triple operator , additional folding rule is described as follows : opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , src 3 , where tgt . [ r | g | b ]∩( src 1 ∪ src 2 ∪ src 3 )= φ . ( 7 ) opc 1 — opc 2 tgt . [ t | g | b ] a , src 0 , src 1 , src 2 , src 3 , where when opc 2 is defined as a unary operator , its operand includes src 1 only , and when opc 2 is defined as a binary operator , its operands include src 1 and src 2 . when opc 1 is defined as a binary operator and opc 2 is a binary operator also , additional folding rule is described as follows : opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , src 3 , where tgt . [ r | g | b ] ∩( src 2 ∪ src 3 )= φ . ( 9 ) opc 1 — opc 2 tgt . [ r | g | b ] a , src 0 , src 1 , src 2 , src 3 , where when opc 1 is defined as a unary operator , its operand includes src 0 only , and when opc 2 is defined as binary operator , its operands include src 1 and src 2 . as a result , in one embodiment , when opc 1 is the instruction “ mad ” and opc 2 is the instructions “ mov ” or “ rsq ”, the combination of opc 1 _opc 2 can be instructions “ mad_mov ” and “ mad_rsq ”. in the relationship of data independency between two adjacent first instructions , the source register of the later first instruction is different from a target register of the former first instruction . in other words , both the source register of the later first instruction and the target register of the former first instruction have a null set , e . g . “ tgt . [ r | g | b ]∩ src 2 = φ ” in the above - mentioned item ( 1 ). the data of the two adjacent first instructions is outputted into different components in the target register . in one embodiment , the total number of the source operands of the first and second instructions is within a predetermined threshold value , e . g . 3 , 4 , or more , so that the decoder can decode the combination of the first instructions . when the first instructions comprise at least two adjacent first instructions having data dependency , one instruction is written into the second program and the other is checked with a next first instruction according to the folding rule . referring to fig5 again , the pixel shader comprises an instruction memory 508 , a fetcher 510 , a decoder 512 , an arithmetic logic unit ( alu ) 514 , a register port 516 , and a register unit 518 . the instruction memory 508 is used to store the second instructions of the second program 506 . the fetcher 510 connected to the decoder 512 fetches the second instructions stored in the instruction memory 508 according to a program counter . the decoder 512 decodes a control signal from the second instructions having the combination of the first instructions . the alu 514 connected to the decoder 512 performs an operation of a plurality of register components of the second instructions according to the control signal . the register port connected to the alu 514 is used to select the register components to transform operand formats of the second instructions . the register unit 518 connected to the register port 516 is employed to store data of the register components of the second instructions . it should be noted that instruction folding mechanism 500 can be implemented in the forms of software or hardware . if implemented in software , the instruction folding mechanism 500 is a software tool kit running in an operating system ( os ), a program loader or a part of a device driver attached to a latter part of a compiler . furthermore , if implemented in a hardware , the instruction folding mechanism 500 is preferably connected to an instruction fetch unit or a decode unit , i . e . before the instruction queue unit and decoder of the pixel shader in the preferred embodiment , or may be built in a pixel shader . fig8 shows a flow chart of performing a pixel processing system according to the present invention . starting at step s 800 , a plurality of first instructions in a first program is folded by an instruction folding mechanism to generate a second program having at least one second instruction which is a combination of the first instructions . in step s 802 , the second instructions are fetched according to a program counter . a control signal is decoded from the second instructions having the combination of the first instructions by a decoder , as shown in step s 804 . then , in step s 806 , an operation of a plurality of register components of the second instructions is performed according to the control signal by an alu . finally , the register components are selected to transform operand formats of the second instructions by a register port in step s 808 . fig9 shows a flow chart of performing an instruction folding mechanism of the pixel processing system in fig8 according to the present invention . during the step s 800 , the first instructions are scanned according to static positions to schedule or rearrange the first instructions in the first program or to rearrange the first instructions with data independency in step s 900 . then , in step s 902 , the first instructions are checked by a folding rule checker according to a folding rule depending on whether the first instructions are data independent . in step s 904 a , when the folding rule checker checks the first instructions by way of two adjacent first instructions and the two adjacent first instructions have data independency , one instruction and the other are combined to generate the second instruction to be written into the second program . in step s 904 b , when the folding rule checker checks the first instructions by way of two adjacent first instructions and the two adjacent first instructions have data dependency , one instruction is written into the second program and the other is checked with a next first instruction according to the folding rule . at step s 906 , the last first instruction is not processed and step s 902 is proceeded again . the second program is then ready to be executed at step s 908 . preferably , during the step s 900 , the instruction scheduler builds a dependence graph ( dg ) to determine whether the result of the former instruction is employed by the later one to indicate data dependency relationship between the first instructions , where each of the instruction is a node , as shown in step s 910 . specifically , in the dependence graph , when the node is connected by an edge sign , the instruction is dependent . on the contrary , if the instruction is independent , then the folding rule checker can scan the dg . in the relationship of data independency between two adjacent first instructions , the source register of the later first instruction is different from a target register of the former first instruction . in other words , both the source register of the later first instruction and the target register of the former first instruction have a null set . preferably , the data of the two adjacent first instructions are outputted into different components in the target register . the total number of the source operands of the first and second instructions is within a predetermined threshold value to be decoded by the decoder . the advantages of the present invention include : ( a ) folding instructions with data independency into reduced instructions for generating a new program ; ( b ) folding instructions having an identical target register and output data to different components of the target register to save the hardware cost of pixel processing system ; and ( c ) providing a folding mechanism applied to a pixel processing system to improve the performance of the pixel processing system . as is understood by a person skilled in the art , the foregoing preferred embodiments of the present invention are illustrative rather than limiting of the present invention . it is intended that they cover various modifications and similar arrangements be included within the spirit and scope of the appended claims , the scope of which should be accorded the broadest interpretation so as to encompass all such modifications and similar structures . | 6 |
various approaches were taken in the pursuit of a stable solution of posaconazole that would be useful as an intravenous formulation of sufficient bioavailability and other pharmaceutically desired characteristics . cyclodextrins , and their derivatives , are known to display the characteristic of enhancing the aqueous solubility of certain compounds , as taught in u . s . pat . no . 5 , 134 , 127 . however , this reference is silent as to whether or not cyclodextrins can enhance the aqueous solubility of posaconazole , or any related azole compounds . example 32 of u . s . pat . no . 7 , 635 , 773 purports to teach the stabilization of posaconazole with sulfobutyl ether - β - cyclodextrin ( sbe 66 - β - cd ) that had undergone single or double treatment with activated carbon . captisol ® is the trade name for a sulfobutyl ether - β - cyclodextrin shown below , and marketed by cydex pharmaceuticals , inc ., lenexa , kans . the chemical structure of captisol ® is as follows : in an effort to evaluate the range of posaconazole solubilities that could be achieved at feasible ph &# 39 ; s , a series of solutions was prepared with a fixed captisol ® concentration . utilizing an acidic solution of 20 % captisol ® ( w / v ), the solubility of posaconazole was increased more than 1000 times and it was determined that a target concentration of 5 mg / ml could be achieved . table 2 displays posaconazole solubilities in 20 % captisol ® solutions at various ph values . posaconazole solubility was also evaluated in acidified solutions with different captisol ® concentrations . as shown in fig1 , posaconazole solubility increases with ph , as well as captisol ® concentration . however , fig1 also shows that at each ph the increase in posaconazole solubility is non - linear with respect to the captisol ®, and at ph 3 . 0 and 4 . 5 , there is a greater than linear increase in posaconzole concentration . therefore , at some ph values , as the captisol ® concentration increases , the ratio of captisol ® to solubilized posaconazole will decrease . based on this solubility effect , a formulation could be developed whereby for the same posaconazole daily dosage , the daily dose of captisol ® could be decreased . for example at a ph of 3 . 1 , the posaconazole solubility in 20 % captisol ® was calculated to be 7 . 8 mg / ml ( see table 2 ), whereas in 40 % captisol ®, the solubility was determined to be 22 . 5 mg / ml . in this case the captisol ® concentration was increased by a factor of 2 whereas , the posaconazole solubility was increased by a factor of 2 . 9 . however , if increasing captisol ® concentration has a greater than linear effect on posaconazole solubility , the opposite effect would also be expected , i . e ., dilution of captisol ® solutions containing posaconazole at or near posaconazole equilibrium solubility should result in precipitation of posaconazole . this effect is of significance in that the preferred delivery of the posaconazole formulation is dilution with either normal saline or 5 % dextrose , followed by infusion . surprisingly however , following dilution of the posaconazole / captisol ® formulation , no precipitation was seen for at least 24 hours . hydrochloric acid was used as an acidifier in the posaconazole formulation . however , several additional acidifiers ( i . e ., citric , sulfuric , maleic , phosphoric , acetic , l - tartaric , d - tartaric , dl - tartaric , methanesulfonic , naphthalenesulfonic , p - toluenesulfonic , lactic , l - lactic , l - ascorbic and malic acid , as well as , glycine hydrochloride ) were also evaluated in regard to posaconzole solubilization . however , at the same ph , no improvement in solubility was seen with these acidifiers . in an effort to explore further improvements to the formulation , the effects of various co - solvents and non - ionic surfactants , on the solubility of posaconazole in a 100 mm captisol ® solution , were examined . the captisol ® solutions were adjusted with hcl to ph 4 . 5 and an appropriate amount of co - solvent was added . an excess amount of posaconazole was added to the ph - adjusted cyclodextrin / co - solvent solution and the solutions were allowed to equilibrate for a period of three days . the contents of the vials were then centrifuged and the supernatant was assayed for posaconazole . table 3 shows the impact of the various co - solvents and several surfactants ( 0 . 1 % 0 . 2 % v / v poloxamer f - 68 , tween 20 or tween 80 ) on the solubility of posaconazole . the surfactants that were tested did not enhance the solubility of posaconazole , and the co - solvents decreased the solubility . the solubilities of posaconazole in each of several modified β and γ - cyclodextrins were evaluated . solubilization of posaconazole was tested with three gamma cyclodextrins ; sbe ( 5 . 2 )- gamma , sbe ( 5 . 2 ) et ( 3 . 9 )- gamma and sbe ( 5 . 2 ) et ( 4 . 9 )- gamma cyclodextrin , ( cydex , inc .). at cyclodextrin concentrations of 100 mm and ph 4 . 5 , the highest posaconazole solubility achieved was 0 . 189 mg / ml , approximately 8 fold less than the 1 . 51 mg / ml achieved with captisole , sbe ( 6 . 5 ) − β cyclodextrin , under similar conditions ( see fig2 ). on the other hand , some changes in β - cyclodextrin substitutions did lead to greater solubilization . utilizing 100 mm cyclodextrin solutions at ph 4 . 5 , solubilization of posaconazole with sbe ( 4 . 6 ) − β , sbe ( 4 . 6 ) − et ( 3 . 5 ) − β and sbe ( 4 . 6 ) − et ( 8 . 5 ) − β cyclodextrins , versus captisol ®, was evaluated . the sbe ( 4 . 6 ) − et ( 3 . 5 ) − β and sbe ( 4 . 6 ) − et ( 8 . 5 ) − β cyclodextrins solubilized 2 . 6 and 6 . 6 fold more posaconazole ( respectively ) than did captisol ® ( see fig2 ). however , the extensive captisol ® safety information outweighed the potential benefits of greater solubilization and , for this reason , formulations with other sulfobutyl ether cyclodextrins were not further developed . finally , stability screening studies also showed that captisol ® formulations of posaconazole undergo color changes under accelerated conditions . solutions of 10 mg / ml posaconazole , in 40 % captisol ® at ph 3 . 0 , were prepared , both with and without 1 mg / ml edta , and with and without nitrogen overlay . after 20 days at 40 ° c ., the solutions were evaluated for color changes with a colorimeter , whereby color formation is indicated by a “ b *” value ( solutions with a b * value of 3 or greater appear yellow ). as shown in table 4 , the development of color was minimized by both edta and nitrogen overlay . however , in the solution containing edta , no additional improvement was seen by inclusion of a nitrogen overlay . based on these studies , as well as further formulation screening , edta is used in the current formulation at level of 0 . 2 mg / ml , which is suitable for parenteral delivery . in addition , although posaconazole is stable in acidified captisol ® solutions under room temperature and accelerated conditions , as described below , a storage temperature of 5 ° c . is suggested in order to further minimize development of yellow color . a set of studies was conducted to explore the stability of posaconazole solutions of varied composition and ph . the accelerated stability of 10 mg / ml posaconazole in a 200 mm captisol ® solution at ph 3 . 0 was examined over a period of three months . posaconazole was added to a ph - adjusted solution of 200 mm captisol ® and mixed for 24 hours . the solution was then filtered and placed on stability at 4 ° c ., 25 ° c ./ 60 % rh , and 40 ° c ./ 75 % rh . the sample did not contain a chelating agent and was not sparged with nitrogen . results are shown in fig3 . the temperature had minimal impact on the degradation of posaconazole over the three month time period . however , the solution became pale yellow within two weeks and grew darker with time . thus , it was concluded that the chelating agent is important to obtain compositions according to the present invention . a similar time study of the stability of posaconazole ( 5 mg / ml ) in 100 mm captisol ® solution at ph 3 . 0 was conducted over a period of three months . posaconazole was added to a ph - adjusted solution of 100 mm captisol ® and mixed for 24 hours . the solution was then filtered and placed on stability at 4 ° c ., 25 ° c ./ 60 % rh , and 40 ° c ./ 75 % rh . the sample did not contain a chelating agent and was not sparged with nitrogen . results are shown in fig4 . the temperature had minimal impact on the degradation of posaconazole over the three month time period . however , the solution became pale yellow within two weeks and grew darker with time . a study of the stability of posaconazole ( 18 mg / ml ) in 400 mg / ml captisol ® solution at ph 3 . 0 was also conducted over a period of nine months . the sample was manufactured using the most current clinical manufacturing process . edta was dissolved in water for injection . captisol ® was then dissolved in the edta solution and the solution was then acidified with hcl . posaconazole was then added and dissolved . additional hcl was added to the solution , as necessary to adjust the ph . the solution was also sparged with nitrogen during the entire process . the prepared solution was then aspetically filtered , filled into vials , and placed on stability under different storage conditions . as shown in fig5 , the temperature had minimal impact on the degradation of posaconazole over the nine month time period . several prototype formulations , based on either solutol hs 15 ( macrogol ® 15 hydroxysterate ph . eur .) or cyclodextrins , were also evaluated . these formulations were found to have sufficient physical and chemical stability to support further development but , as described below , toxicological testing showed unexpectedly superior results for the 40 % captisol ® formulation . six prototype formulations , reflected in tables 5 and 6 , were prepared . table 5 displays the composition of three solutol ® based formulations ( nos . 1 - 3 ) and table 6 displays the compositions of another three cyclodextrin based formulations ( nos . 4 - 6 ). these six formulations were the subject of a toxicological screening study using the suspension formula as a control . the formulations were dosed to rats via intravenous infusion for 15 min . over a period of 2 weeks . the posaconazole dose for all animals was 10 mg / kg . in addition , the hemolytic potential of each formula was tested in vitro prior to dosing . the 30 % solutol formulation that was directly injected ( formula no . 1 ) produced hemolysis in the in vitro screening and showed severe local intolerance . and in vivo hemolysis was indicated . this study was stopped before completion and the animals were sacrificed . the 30 % solutol formulation that was diluted 1 : 5 before infusion ( formula no . 2 ) produced hemolysis in vitro , similar to that produced by formula no . 1 . based on this result , animals were not dosed . the 75 % solutol formulation that was diluted 1 : 5 before infusion ( formula no . 3 ) showed some evidence of hemolysis in vitro ( time dependent ). in addition , clinical signs of local intolerance were seen in some animals . similar results were seen for both the 20 % hpβcd formulation , diluted 1 : 5 before infusion ( formula no . 4 ), and the 20 % captisol ® formulation , diluted 1 : 2 . 5 before infusion ( formula no . 5 ). for both formulations , the in vitro hemolysis testing showed no hemolysis but , slight effects on rat kidney tubule cells were seen . in addition , animal studies have suggested that hpβcd sterile dosage forms have significant toxicological potential . the 40 % captisol ® formulation ( formula no . 6 ) was diluted 1 : 10 before infusion . this formulation did not produce hemolysis in vitro and showed no clinical signs of toxicity or effects on clinical pathology parameters . thus , only the 40 % captisol ® formulation had no toxicological findings and , interestingly , this formulation was also superior to the 20 % captisol ® formulation . the reason for this difference is assumed to be that , for an equivalent posaconazole dose , the 20 % formulation requires twice as much captisol ® as that of the 40 % formulation . the final formulation , based on the 40 % captisol ® solution , included modifications to ensure posaconazole solubilization over any potential variability in the formulation . for example , both a target ph and an acceptable ph range are required for manufacturing , and the formulation must be stable over the entire specified range . in order to meet these criteria , the concentration of posaconazole was reduced slightly , from 20 mg / ml to 18 mg / ml , and the ph was reduced from 3 . 0 to 2 . 6 . the clinical composition of intravenous posaconazole solution formulation is shown in table 7 . a dilution study was conducted in order to evaluate the likelihood of precipitation during dilution prior to administration to a patient . a ten percent excess of the required amount posaconazole was weighed into an amber vial . captisol ® solution adjusted to the target ph using hcl was added to the vial . the vial was capped and gently mixed at room temperature for 24 hours . after 24 hours , the test vials were filtered through 0 . 22 micron millipore pvdf millex - gv ® filter . a portion of the filtered sample ( 10 ml ) was added to a 100 ml volumetric flask . the sample was diluted to the 100 ml mark with either 0 . 9 % sodium chloride injection usp ( normal saline ) or 5 % dextrose injection usp (“ d5w ”). samples were observed for 24 hours at 4 ° c . and ambient temperature . the results of using normal saline and d5w as diluents are summarized in tables 8 and 9 . solid precipitate was visually observed in the following formulations of posaconazole 24 hours after dilution with normal saline : 20 mg / ml posaconazole in 200 mm captisol ® at ph 3 , 3 mg / ml posaconazole in 100 mm captisol ® at ph 4 , and 5 mg / ml posaconazole in 150 mm or 200 mm captisol ® at ph 4 . all of the other diluted samples were clear after 24 hours . solid precipitate was visually observed in the following formulations of posaconazole 24 hours after dilution with d5w : 5 mg / ml posaconazole at ph 3 , 10 mg / ml posaconazole at ph 3 , 20 mg / ml posaconazole in 200 mm captisol ® at ph 3 , 3 mg / ml posaconazole in 100 or 200 mm captisol ® at ph 4 , and 5 mg / ml posaconazole in 150 mm captisol ® at ph 4 . all of the other diluted samples were clear after 24 hours . this experiment indicates that it is possible to prepare posaconazole formulations that will not precipitate out when diluted for delivery to the patient . in order to further evaluate the potential for precipitation during infusion of the diluted solution into a vein , a dynamic precipitation study was performed by using a yalkowsky et al . method ( j . l . h . johnson , y . he , s . h . yalkowsky , validation of an in vitro model for prediction of in vivo phlebitis , aaps , 2002 , poster # 14919 ) with small modifications . the flow rate of isotonic sorenson &# 39 ; s phosphate buffer ( ispb ) was 5 ml / min which is comparable to that of human blood flow in readily accessible veins . a peristaltic pump ( master flex ® model 7518 - 10 ) provided flow of an aqueous phase at a rate of 5 ml / min through flexible tubing ( cole - parmer &# 39 ; s l / s 14 silicone ( platinum ) which has an internal diameter of 1 . 6 mm ), then through a uv flow - cell . the aqueous phase served as a blood surrogate and consisted of isotonic sorenson &# 39 ; s phosphate buffer ( ispb ) at ph 7 . 4 . the sample solution was injected into the tubing through a needle inserted 30 cm upstream of the flow cell . a syringe pump was used to control the rate of sample injection . the injection rate varied from 0 . 05 to 10 ml / min . the appearance of a precipitate was detected by beckman du - 7 spectrophotometer at 540 nm . this study was conducted at room temperature . the filtered test sample was diluted 1 : 10 with normal saline or d5w before injection . results of the dynamic precipitation study for samples injected at 1 . 0 ml / min are illustrated in table 10 . the results of dynamic precipitation study suggest that various formulations can be prepared and diluted without resulting in precipitation . less precipitation was also seen in samples injected at rates less than 1 . 0 ml / min . filter an appropriate volume of edta + sbe - β - cyclodextrin solution through a clarifying filter into the main compounding vessel . the total filtered volume of edta + sbe - β - cyclodextrin solution is dependent on the mixing efficiencies of the equipment used during compounding . add 1n hcl to vessel in order to acidify the filtered solution . add posaconazole into the filtered solution . when compounding with equipment that provides sufficient agitation , posaconazole may be charged as a powder . when compounding with equipment that provides limited agitation pre - wet the posaconazole in wfi in a separate vessel using a ratio of one part posaconazole to five parts water ( 1 : 5 ratio ) and mix until a homogeneous suspension is formed . add pre - wetted posaconazole suspension to main vessel and mix until dissolved . add any additional 1n hcl or 1n naoh in order to adjust the ph to the appropriate level . q . s . ad water for injection to obtain the final batch volume and mix to obtain a homogenous solution . aseptic filter pharmaceutical composition through a 0 . 22 μm filter . package filtered product into 6rdin glass vials . stopper and crimp cap . during the development of the manufacturing method , different manufacturing procedures were evaluated including optimizing the posaconazole : wfi ratio , changing the order of excipient addition , and charging the powder excipients concurrently . based on the development studies , the above detailed manufacturing method provides the optimal manufacturing process for the solution . a three vessel manufacturing process was used for the 200 l commercial - scale batches . to ensure adequate mixing , overhead mixers were utilized to help dissolve the captisol and posaconazole . nitrogen sparging was utilized during the compounding process . fig6 displays the process flow diagram for the commercial scale developmental batches , which process is summarized as follows : the edta and captisol are dissolved in nitrogen - sparged water for injection ( wfi ) in the first vessel . the edta + captisol solution is then filtered through a 0 . 22 μm clarifying membrane filter into the drug product compounding vessel . in the drug product compounding vessel , the filtered edta + captisol solution is acidified with hydrochloric acid , and the api is charged into the acidified solution . the solution is mixed until the api dissolves . the ph is then adjusted to 2 . 6 using hydrochloric acid and / or sodium hydroxide as necessary , and the product is brought to final volume . the drug product is then filtered through a 0 . 22 μm bioburden reducing membrane filter into a receiving vessel . from the receiving vessel , the solution is sterilized through an in - line 0 . 22 μm sterilizing filter and aseptically filled and stoppered into sterile , depyrogenated glass vials in a grade a filling area . the diluted intravenous solution ( admixture ) for infusion can be prepared according to the following procedure : the following concentrations and dose ranges bracket the lower and upper levels of the rising single dose study defined in the clinical protocol . allow the posaconazole injectable solution , 18 mg / ml drug product to equilibrate to room temperature . gently invert the drug product vial ten times . remove an appropriate volume of diluent ( 0 . 9 % nacl or 5 % dextrose ) from admixture bag so that 142 ml of diluent remains in the bag . withdraw 8 . 4 ml of posaconazole injectable solution , 18 mg / ml with an appropriately sized syringe and inject the entire amount of drug product into the iv bag . mix the contents of the bag with ten gentle inversions . allow the posaconazole injectable solution , 18 mg / ml drug product to equilibrate to room temperature . gently invert the drug product vial ten times . remove an appropriate volume of diluent ( 0 . 9 % nacl or 5 % dextrose ) from admixture bag so that 125 ml of diluent remains in the bag . withdraw 25 ml of posaconazole injectable solution , 18 mg / ml with an appropriately sized syringe and inject the entire amount of drug product into the iv bag . mix the contents of the bag with ten gentle inversions . a phase 1 , single - site , randomized , evaluator - blind ( within dose level ) placebo - controlled , single - dose study was conducted to evaluate the pharmacokinetics , safety and tolerability of posaconazole intravenous solution when administered as single dose and as multiple doses . the first group , received a single dose of posaconazole 200 mg . posaconazole intravenous was admixed in 150 ml of 5 % dextrose to provide a final concentration of approximately 1 . 33 mg / ml of posaconazole in solution for the 200 mg dose , and was infused in a peripheral vein in the arm over 90 minutes . although central line administration is generally recommended to infuse low ph formulations , the lack of signal in nonclinical toxicology studies supported the use of posaconazole intravenous solution administered via peripheral lines in this study . a cohort of 12 subjects ( 9 active and 3 dextrose placebo ) received a single infusion of posaconazole intravenous solution on day 1 . six out of 9 subjects experienced post - infusion local reactions , manifested as erythema , induration and tenderness . one subject had extravasation and resulting arm swelling . the events were reported between 4 and 24 hours post - infusate . local intolerability is likely due to the irritation caused by the low ph of the infusate , administered slowly via peripheral lines . the local intolerability observed prompted the discontinuation of this trial in healthy volunteers that received posaconazole intravenous via peripheral infusion . alternative infusion strategies ( rapid or slow infusion via peripheral lines ) will be explored in healthy volunteers . formulations with low ph are better tolerated if infused via central lines . therefore , a strategy was designed to continue the program in patients with central lines . the pharmacokinetic profile of posaconazole intravenous was typical of an intravenous drug ( see fig7 ) with low variability . median t max was 1 hour , mean c max 1470 ng / ml , mean auc ( 0 - 24 ) 13 , 500 hr · ng / ml , ( estimated c avg 563 ng / ml ) and variability for all parameters around 25 % or less . table 11 displays mean ( cv %) posaconazole plasma pharmacokinetic parameters of posaconazole following single dose , 200 mg intravenous solution of posaconazole to healthy adult volunteers ( all subjects included ). c max and t max were observed pharmacokinetic parameters . individual plasma concentration data were used to estimate the following pharmacokinetics parameters : auc ( tf ), auc ( i ), t 1 / 2 , vd / f , and c avg . the terminal phase rate constant ( k ) was calculated as the negative of the slope of the log - linear terminal portion of the plasma concentration - time curve using linear regression . the t 1 / 2 was calculated as : t 1 / 2 = ln ( 2 )/ k . the auc ( tf ) was calculated using the linear trapezoidal method and extrapolated to infinity , auc ( i ), as follows : auc ( i )= auc ( tf )/ cest tf / k , where cest tf is the estimated concentration at the time of the last measurable sample , determined from the linear regression of the terminal portion . as shown in table 11 , the c avg range following 200 mg single dose is anticipated to be about 900 to about 1900 ng / ml that meets the target c avg targeted for bridging with posaconazole oral suspension . therefore , the likely dose is 200 mg qd , provided patient pharmacokinetic data are no different than the healthy volunteer data and no non - linearity is observed upon the multiple dosing . fig8 displays a summary of observed posaconazole steady - state exposures and the projected exposure distribution for the posaconazole intravenous solution . each box represents 25th to 75th percentiles , the line inside the box represents median value , whiskers represent 10th and 90th percentile , and points beyond whiskers represent outlier values ; outliers not shown for projected exposure distribution . thus , in some embodiments of the invention , the composition is one that delivers 200 mg of posaconazole to a patient , wherein administration of such a dose results in a c max of about 1470 ng / ml and an auc last of about 27 , 000 hr * ng / ml . bioequivalent doses and formulations are within the scope of the invention . for systemically absorbed drugs , bioavailability is commonly defined as displaying relevant pharmacokinetic parameters ( e . g ., c max and auc ) of between 80 % and 125 % of the reference drug . thus , in some embodiments of the invention , the composition is one that delivers 200 mg of posaconazole to a patient , wherein administration of such a dose results in a c max of between about 1176 and about 18375 ng / ml , and an auc last of between about 21 , 600 and about 33 , 750 hr * ng / ml . the present invention encompasses methods of prevention and treatment of a variety of infection caused by a broad spectrum of infectious agents . the term “ infection ” is understood to include , but not be limited to , those disease state caused by molds , yeasts , and other infectious agents such as : candida , dermatophytes , dimorphics , dematiaceous , ( e . g ., alternaria and bipoiaris ), aspergillus , acremonium , basidiomycetes , bjerkandera , coprinus , paecilomyces , microsporum , trichophyton , pseudallescheria , schizophyllum , crytococcus , histoplasma , blastomyces , coccidioides , fusarium , exophiala , zygomycocetes ( e . g ., absidia , mucor , rhizopus , and rhizomucor ), kluyveromyces , saccharomyces , yarrowia , pichia , epidermophyton , paracoccidioides , scedosporium , apophysomyces , curvularia , penicillium , fonsecaea , wangiella , sporothrix , pneumocystis , trichosporon , cladophialophora , ramichloridium , syncephalastrum , madurella , scytalidium , or protozoa such as leshmania , trichomononas and trypanosoma . the present invention is intended to treat both opportunistic and non - opportunistic infections , where the term “ opportunistic ” as used herein denotes those infections caused by organisms capable of causing a disease only in a host whose resistance is lowered , e . g ., by chemotherapy or hiv . posaconazole can be used to treat the progression of invasive fungal infections including prophylaxis , empiric , pre - emptive , primary , and refractory treatments . in particular , posaconazole is useful in the prevention and / or treatment of the following disease states : initial ( first line ) treatment of oropharyngeal or esophageal candidiasis ; salvage therapy of azole - refractory oropharyngeal and esophageal candidiasis ( e . g . in patients who have failed oral fluconazole and / or intraconazole ); initial treatment of invasive aspergillosis , candidiasis , fusariosis , scedosporiosis , infections due to dimorphic fungi ( e . g ., cryptococcosis , coccidioidomycosis , paracoccidioidomycosis , histoplasmosis , blastomycosis ), zygomycosis , and invasive infections due to rare molds and yeasts ; salvage therapy for invasive mycoses in patients who are refractory to or intolerant of other therapies ( e . g ., amphotericin b , lipid formulations of amphotericin b , fluconazole , caspofungin , micafungin , anidulafungin , voriconazole and / or intraconazole ); prevention of invasive candidiasis , invasive mold infections ( including zygomycosis and aspergillosis ) in patients at high risk , including patients who have undergone intensive chemotherapy and / or radiation therapy for hematologic malignancies , bone marrow or peripheral stem cell transplant conditioning regimens , and patients receiving combination immunosuppressive therapy for the treatment of acute or chronic graft - versus - host disease or prevention of solid organ transplantation ; chagas disease ( trypanosomiasis due to t . cruzi ) including acute and chronic forms ; and leishmaniasis , including visceral and localized forms . in some embodiments , the invention encompasses a method of treating or preventing an infection in an animal in need thereof which comprises administering to said animal an effective amount of the formulation . in some embodiments , the animal is a mammal , a bird , a fish , or a reptile . in some embodiments , the animal is a mammal , including , but not limited to a human . in some embodiments , the infection is caused by a fungus or parasite . in some embodiments , the invention encompasses a method wherein said formulation is administered intravenously . immuno - suppressant therapy ( e . g . chemotherapy , radiation therapy , myeloablative conditioning regimens ) often results in one of more of the above - referenced infections . the present invention encompasses the administration of a posaconazole formulation adjunctive to immuno - suppressant therapy , wherein the posaconazole formulation functions prophylactically with regard to opportunistic infections including the above - referenced disease states . the present invention encompasses a variety of modes of administration to any part , organ , interstice of cavity of an animal &# 39 ; s body that is subject to and infection . a non - limiting set of examples of modes by which the posaconazole formulations of the present invention may be administered includes : intravenously , intramuscularly , via inhalation , or intravascularly . co - formulation or co - administrations comprising combinations of posaconazole and at least one other active ingredient are also within the scope of the present invention . non - limiting examples of such active ingredients include : antifungals such as echinocandins ( including caspofungin , micafungin , and anidulafungin ) and azoles ; amphotericin b ; deoxycholate amphotericin b ; flucytosine ; and terbinafine . also within the scope of this invention are combinations with an antibacterial , antiviral , steroid , or nonsteroidal anti - inflammatory drugs (“ nsaids ”), chemotherapeutics , and / or anti - emitics . similarly , co - administration of posaconazole with at least one of the above active ingredients , aside from within a single formulation , is also within the scope of the present invention . in certain embodiments , the pharmaceutical compositions described herein may be administered to a patient in need thereof at a dose of 100 mg to 400 mg every 12 to 24 hours . in certain such embodiments , a dose may comprise at least one intravenous dosage form . in certain embodiments , the pharmaceutical compositions described herein may be administered to a patient in need thereof at a dose of 100 mg to 400 mg every 12 to 24 hours . in some preferred embodiments , the composition is administered in an amount sufficient to deliver a dose of between about 180 and about 220 mg posaconazole to the patient . in some more preferred embodiments , this dose is about 200 mg posaconazole . the administration may occur once per day or twice per day . the pharmaceutical compositions of the present invention are administered to a patient according to a dosing regimen . it should be understood that the specific dosing regimen for any particular patient will depend on a variety of factors , including species , age , body weight , body surface area , height , general health , sex , diet , time of administration , rate of excretion , drug combination , specific disease being treated , the severity of the condition , the renal and hepatic function of the patient , the particular active ingredient employed , and the judgment of the treating physician . other features and embodiments of the invention will become apparent by the following examples which are given for illustration of the invention rather than limiting its intended scope . unless defined otherwise , all technical and scientific terms used herein have the same meaning as those commonly understood by one of ordinary skill in the art to which this invention belongs . although methods and materials similar or equivalent to those described herein can be used tin the practice or testing of the present invention , suitable methods and materials are described below . the materials , methods and examples are illustrative only , and are not intended to be limiting . all publications , patents and other documents mentioned herein are incorporated by reference in their entirety . as used herein , the phrase “ small - volume parenteral unit ” refers to a single - dose or multiple - dose small - volume injection labeled as , or actually containing 100 ml or less . as used herein , the term “ injectable ” means adapted to parenteral administration . as used herein , the term “ fungus ” includes but is not limited to one of the diverse morphologic forms of yeasts and molds . fungi include organisms in the following groups or genera : candida , dermatophytes , dimorphics , dematiaceous , ( e . g ., alternaria and bipolar &# 39 ; s ), aspergillus , acremonium , basidiomycetes , bjerkandera , coprinus , paecilomyces , microsporum , trichophyton , pseudallescheria , schizophyllum , crytococcus , histoplasma , blastomyces , coccidioides , fusarium , exophiala , zygomycocetes ( e . g ., absidia , mucor , rhizopus , and rhizomucor ), kluyveromyces , saccharomyces , yarrowia , pichia , epidermophyton , paracoccidioides , scedosporium , apophysomyces , curvularia , penicillium , fonsecaea , wangiella , sporothrix , pneumocystis , trichosporon , cladophialophora , ramichloridium , syncephalastrum , madurella , scytalidium , or protozoa such as leshmania , trichomononas and trypanosome . as used herein , the term “ dematiaceous ” means dark - walled conidia and / or hyphae , and includes as non - limiting examples : alternaria , and bipolaris . phaeohyphomycosis is an example of a dematiaceous fungal infection . as used herein , the term “ parasite ” means an organism that lives on or in another and draws its nourishment from them . parasites include leishmania , trypanosoma , and trichomonas , among others . as used herein , the term “ auc ” is the area under the plasma concentration - time curve from time zero to a certain time period of the sample . for example , auc ( 4 h ) means the area under the plasma concentration - time curve from time zero to 4 hours . the term “ patient ” refers to an animal including a mammal ( e . g . human ). the term “ pharmaceutically acceptable excipient ” refers to a non - toxic excipient that may be administered to a patient , together with the weakly basic and poorly - aqueous soluble azoles as describe herein , which does not destroy the pharmacological activity thereof . the term “ treating ” or “ treatment ” is intended to mean prophylactic use to prevent disease or mitigating or alleviating the symptoms of the recited condition , disease or disorder in a mammal such as a human . the term “ pharmacokinetics ” refers to the process by which a drug is absorbed , distributed , metabolized and eliminated by the body . pharmacokinetic parameters include , but are not limited to “ maximum plasma concentration ” or “ c max ”, “ area under the plasma concentration time curve or “ auc ”, and “ time to c max ” or “ t max ”. as used herein , the term “ t 1 / 2 ” refers to the half - life of the drug . the present invention is not to be limited in scope by the specific embodiments describe herein . indeed , various modification of the invention in addition to those described herein will become apparent to those skilled in the art from the foregoing description . such modifications are intended to fall within the scope of the appended claims . | 0 |
preferred embodiments of the present invention will now be described in detail in accordance with the accompanying drawings . fig1 is a block diagram showing the configuration of printing system using a color laserbeam printer to which a first embodiment of the present invention is applied . in fig1 , reference numeral 200 denotes a host computer which outputs print information including print data and control code via an interface ( i / f ) 203 to a printer 100 . the host computer 200 is a computer system having a keyboard 210 as an input device , a mouse 211 as a pointing device and a display monitor 220 as a display device . further , when a scanner 300 is connected to the host computer , image data obtained by optically reading an original image from the scanner 300 can be inputted into the host computer . the host computer 200 operates by a basic os such as windows nt and windows 95 ( 98 ) ( trademarks by microsoft corporation ). on the host computer 200 side , the functions on the basic os regarding the present embodiment are briefly classified into application software 201 and a graphic subsystem 202 . the application software 201 is , e . g ., application software which operates on basic software such as a word processing program or a spreadsheet program . as shown in fig2 , the graphic subsystem 202 has a graphic device interface ( hereinafter gdi ) 2021 as a part of the functions of the basic os and a printer driver 2020 as a device driver dynamically linked from the gdi 2021 . the printer driver 2020 is called from the gdi 2021 via a device driver interface ( ddi ), and performs processing in accordance with a device upon each drawing object . the processing system of the printer driver 2020 divides into a pdl mode type 2023 and a image mode type 2024 , and one of them is selected in correspondence with input data . the pdl mode type is provided for a printer having a controller capable of processing a control command called pdl ( page description language ). as soon as the printer driver 2020 converts the print information forwarded via the ddi into a pdl command , it transmits the command via the gdi 2028 to the printer 100 . as the processing by the printer driver 2020 in the pdl mode type is merely generating a command from the data from the ddi , it can be considered that this processing is light - loaded processing for the driver . the feature of the pdl mode type is that if the printer 100 has high performance to interpret the pdl command , the printer driver 202 can receive data with high degree of extraction from the gdi 2021 and send the data to the printer 100 , therefore , in normal page printing , the data size to be transferred can be small regardless of resolution and output tonality . however , in the pdl mode type , in drawing gradation - processed figure or the like by graphic application software or outputting high - resolution / high tonality image , a large print command is generated , therefore , the processing speed is often extremely lowered . on the other hand , in the image mode type , a print image is mapped on memory space ensured on the printer driver 2020 side , to avoid high - level drawing processing on the printer 100 side , and the print image is converted into data which can be directly printed by the printer 100 , then sent to the printer 100 . as the processing by the printer driver 2020 in the image mode type , the image mode printer driver 2024 performs drawing processing , using print information inputted via the ddi from the gdi 2021 as in the case of the pdl mode type , on a band memory 2027 , and transmits bitmap data generated on the band memory 2027 via the gdi 2028 to the printer 100 . the feature of the image mode type is that drawing processing can be performed on high - resolution color image data and complicated graphic data at a high speed . on the other hand , even in case of drawing characters and / or simple figures , the image data in the entire drawing area is generated in the output resolution and output tonality and transmitted as a print command , therefore , when high - resolution / high tonality characters / graphics are printed at a high speed , the processing time is increased . hereinbelow , counterfeit judgment processing will be described about the pdl mode type processing system and the image mode type processing system in the printer driver 2020 as pdl driver 2023 and image driver 2024 . the pdl driver 2023 and the image driver 2024 have counterfeit judgment units 2025 and 2026 respectively , and perform the counterfeit judgment processing by detecting pre - embedded electronic watermark information from image data which satisfies a predetermined resolution condition among print information received from the ddi . the print information includes three attributes , “ text ” indicative of font data , “ graphics ” indicative of figure vectors , gradation information or the like , and “ image ” indicative of read photographic image or the like , and different functions are called for the respective attributes . further , as “ image ” attribute data includes information on the numbers of pixels in vertical and horizontal directions , the output image size and the like , it is easy to extract only data having the “ image ” attribute ( hereinafter , simply referred to as “ image data ”) satisfying the above resolution condition when print information has been received from the ddi and process the data . hereinbelow , the counterfeit judgment processing by the counterfeit judgment unit 2025 in the pdl driver 2023 will be described with reference to the flowchart of fig3 . note that as the counterfeit judgment processing by the counterfeit judgment unit 2026 in the image driver 2024 is the same as that in the pdl driver 2023 except that bitmap data is generated on the printer driver 2020 side , the explanation of the processing by the counterfeit judgment unit 2026 will be omitted . in fig3 , first , at step s 301 , print information is inputted from the ddi . as the print information , image data obtained by reading an original by the scanner 300 , image data pre - stored in a storage medium such as a hard disk ( not shown ) or the like , as well as image data generated by the application 201 , may be inputted . next , at step s 302 , it is determined whether or not the input print information represents image ( image attribute image ) and satisfies a predetermined resolution condition . generally , when a bank note or negotiable instrument is to be duplicated , an original image read by the scanner 300 or the like is to be reproduced with fidelity , image data to be processed has a resolution equal to or higher than a predetermined level . accordingly , the resolution condition is set to a certain level at which sufficient precision cannot be obtained in a printed output as a counterfeit bank note or negotiable instrument . more specifically , if data resolution upon output is equal to or less than 100 dpi ( dot / inch ), it can be considered from the output image quality that the obtained output is insufficient as a counterfeit . accordingly , there is a low probability that image data having resolution equal to or less than 100 dpi is counterfeit data . in the present embodiment , 100 dpi is set as the resolution condition . at step s 302 , if it is determined that the input print information is image data having a resolution equal to or less than 100 dpi , the process proceeds to step s 306 , at which the pdl driver 2023 converts the print information into a pdl command as in normal processing , and the process ends . on the other hand , if the input print information is image data having a resolution over 100 dpi , the process proceeds to step s 303 , at which electronic watermark detection processing is performed . hereinbelow , the electronic watermark detection processing at step s 303 will be described . in the present embodiment , if particular electronic watermark information indicating duplication prohibition is detected from input image data having resolution over 100 dpi , it is determined that the image data is based on a particular original and there is a high probability that the print processing is made for the purpose of counterfeiting . next , a method for extracting the electronic watermark information in the present embodiment will be described . note that the present invention is not limited to this method but any other well - known extraction method can be employed . first , the input image data is divided into blocks , and fourier transform is performed on each block to extract a frequency component . the image data in obtained frequency area is separated into amplitude spectrum and phase spectrum , and a registration signal included in the amplitude spectrum is detected . generally , according to human visual perception characteristics , a signal embedded in a low frequency component is usually recognized as noise in comparison with a signal embedded in a high frequency component . further , since irreversible compression such as jpeg processing has an effect similar to that of low - pass filter , the high frequency component is eliminated by jpeg compression / expansion processing . the registration signal is embedded as an impulse signal to an intermediate frequency area with a level equal to or less than a first frequency level at which the signal is hardly recognized by human eye and equal to or higher than a second frequency level at which the signal is not eliminated by irreversible compression / expansion . accordingly , the registration signal is detected by extracting an impulse signal included in the amplitude spectrum in a frequency area at the intermediate level . then the scaling factor of the digital image data is calculated based on coordinates of the extracted registration signal ( impulse signal ). in the counterfeit judgment unit 2025 , in the object image which has not been scaling - processed , a frequency component where the impulse signal is embedded is previously determined . accordingly , the scaling factor is calculated by the ratio between this frequency and a frequency where the impulse signal has been detected . for example , assuming that the previously - determined frequency is a , and the frequency where the impulse signal has been detected is b , it is determined that a / b scaling has been performed , which is characteristic of the well - known fourier transform . then , a pattern size to detect the electronic watermark information included in the image data is determined , and convolution using the pattern is performed , thereby the electronic watermark information can be detected . as a result of the electronic watermark detection processing ( s 303 ) as described above , if electronic watermark information indicating duplication prohibition has not been detected ( s 304 ), the pdl driver 2023 performs normal pdl command conversion processing at step s 306 . note that in this case , as the print information is image data , predetermined header information is added to the image data , and the data is converted into the print command . on the other hand , if electronic watermark information indicative of duplication prohibition has been detected at step s 304 , the pdl driver 2023 performs counterfeit prevention processing at step s 305 . hereinbelow , the counterfeit prevention processing in the present embodiment will be described with reference to the flowchart of fig4 . first , at step s 401 , the pdl driver 2023 notifies the os that the duplication prohibition data is included in the input data . in response to the notification , the os side displays a warning dialog as shown in fig5 for a user to notify that there is a possibility that the current print processing is made as counterfeiting , i . e ., a crime . next , at step s 402 , if the user has selected “ no ” (= stop printing ) in response to the warning dialog , the pdl driver 2023 stops the printing operation based on the data , and the process ends . on the other hand , if the user has selected “ yes ” (= continue printing ) in response to the warning dialog , the operation history is stored in a hard disk device ( not shown ) or the like in the host computer 200 , and processing to fill the image with black color or the like is performed as counterfeit prevention ( s 403 ), and the routine of the counterfeit prevention processing ( s 305 ) ends . note that the above image filling is merely an example of the counterfeit prevention processing . any other processing may be used as long as it degrades image quality of image data , i . e ., it disturbs reproduction of input image with fidelity . if the print operation has not been stopped , the print information outputted from the pdl driver 2023 is inputted into the printer 100 in fig1 via a host i / f 111 . the printer 100 is divided into a formatter controller 110 which interprets the print information inputted from the host computer 200 and generates a print image ( bitmap image data ), and at the same time , controls the overall printer 100 , and a printer engine 140 which receives the print image and forms a visible image on a print sheet . the formatter controller 110 is connected to an operation panel 120 having switches and led display device and the like for the user &# 39 ; s operation and for notifying the user of printer statuses . the operation panel 120 is provided as a part of exterior components of the printer 100 . hereinbelow , the formatter controller 110 in the printer 100 will be described with reference to fig6 . the formatter controller 110 is a part generally referred to as a pdl controller or the like . the formatter controller 110 has the host interface ( i / f ) 111 as connection means for connection with the host computer 200 , a reception buffer 1121 as storage means for temporarily storing and managing reception data and the like from the host computer 200 , a transmission buffer 1122 as storage means for temporarily storing and managing transmission data and the like to the host computer 200 , a command interpreter 113 which interprets print data , a print controller 114 , a drawing processor 115 , a page memory 116 , an output controller 130 and the like . the host interface 111 which is communication means for transmission / reception of print data with the host computer 200 enables communication in conformance with the ieee - 1284 protocol . note that the present invention is not limited to this communication protocol , but connection by various protocols may be performed via the network . further , the interface 111 may be communication means in conformance with ieee - 1394 protocol , usb communication protocol or the like . the print data received via the host interface 111 is sequentially stored in the reception buffer 112 , and read and processed by the command interpreter 113 or the drawing processor 115 in accordance with necessity . the command interpreter 113 comprises a control program in conformance with the pdl command system and print job control languages . the command interpreter 113 provides instructions to the drawing processor 115 based on the result of interpretation of the print data regarding character printing , figure and image drawing , and provides instructions to the print controller 114 regarding commands for paper selection , reset and the like other than drawing commands . the drawing processor 115 has a function as a renderer of sequentially mapping the respective drawing objects of characters and images on the page memory 116 . the output controller 130 converts the content in the page memory 116 into a video signal vdo , and transfers the video signal vdo via a video i / f 150 to the printer engine 140 . the printer engine 140 is a printing mechanism to form a permanent visible image on a print sheet based on the received video signal . hereinbelow , the operation of the printer engine 140 will be described with reference to fig7 showing the construction of the printer engine 140 . in fig7 , one end of print sheet p supplied from a paper cassette 161 is held by a gripper 154 f , and held on the outer periphery of transfer drum 154 . respective color latent images formed by an optical unit 170 on an electrostatic drum 151 are developed by respective developers dy , dm , dc and db for yellow ( y ), magenta ( m ), cyan ( c ) and black ( b ) colors , then transferred plural times onto the print sheet on the periphery of the transfer drum , thus a multi - color image is formed . thereafter , the print sheet p is separated from the transfer drum 154 , then the image is fixed onto the print sheet by a fixing unit 155 , and the print sheet p is discharged from a paper discharging unit 159 onto a paper discharge tray 160 . the developers for colors , dy , dm , dc and db respectively have a rotation shaft on both ends . the developers are held by a developer selection mechanism 152 such that they are rotatable on the shafts . in this arrangement , as shown in fig7 , the positions of the respective developers dy , dm , dc and db can be maintained constant even when the developer selection mechanism 152 rotates on its rotation shaft 152 a . in the developer selection mechanism 152 integrated with the developers , when a selected developer has been moved to a developing position , a selection mechanism holding frame 153 is drawn toward the electrostatic drum 151 by a solenoid 153 a , with a support 153 b as the center , thus the developer selection mechanism 152 is moved toward the electrostatic drum 151 , and developing processing is performed . next , the electrostatic drum 151 is uniformly charged to a predetermined polarity by a charger 156 . the image data vdo mapped as a print image by the formatter controller 110 is converted into a video signal of corresponding pattern , and outputted to a laser driver to drive a semiconductor laser 141 . a laser beam emitted from the semiconductor laser 141 is on / off controlled in accordance with the input image data ( video signal ) vdo , further , the laser beam is swayed in left and right directions by a polygon mirror rotated at a high speed by a scanner motor 143 , to scan - expose the electrostatic drum 151 via a polygon lens 134 and a reflection mirror 144 . thus a latent image of the image pattern is formed on the electrostatic drum 151 . next , for example , an m ( magenta ) color electrostatic latent image is developed by the m ( magenta ) developer dm , then a first toner image in m ( magenta ) color is formed on the electrostatic drum 151 . on the other hand , the print sheet p is fed at predetermined timing , and a transfer bias voltage of an opposite polarity to that of the toner ( e . g ., plus polarity ) is applied to the transfer drum 154 . then the first toner image on the electrostatic drum 151 is transferred onto the print sheet p , and at the same time , the print sheet p is electrostatically attracted to the surface of the transfer drum 154 . thereafter , the residual m ( magenta ) color toner is removed by a cleaner 157 from the electrostatic drum 151 , in preparation for the latent image formation and development for the next color . then , the second toner image of c ( cyan ) color , then the third toner image of y ( yellow ) color , and the fourth toner image of bk ( black ) color are transferred in similar procedures . note that upon transfer of each color image , a bias voltage higher than the previous transfer is applied to the transfer drum 154 . when the front end of the print sheet p where the four color toner images are overlap - transferred approaches a separation position , a separation claw 158 comes into contact with the surface of the transfer drum 154 , to separate the print sheet p from the transfer drum 154 . the print sheet p is conveyed to the fixing unit 155 , then the toner images on the print sheet are fixed to the print sheet , and the print sheet is discharged on the paper discharge tray 160 . the printer engine 140 of the present embodiment enables image output up to 600 dot / inch ( dpi ) resolution through the above image formation process . as described above , according to the present embodiment , in the printer driver 2020 , the electronic watermark detection processing is performed only on image data having a resolution over a predetermined resolution . since the execution of electronic watermark detection processing can be minimized , the counterfeit prevention function against counterfeiting bank notes , negotiable instruments and the like can be realized while suppressing reduction of total throughput . further , in the present embodiment , the resolution as a criterion as to whether or not the electronic watermark detection processing is performed , i . e ., whether or not the counterfeit judgment processing is performed , is 100 dpi . generally , the resolution of data frequently transferred on the internet or the like for image print - output is equal to or less than 100 dpi . accordingly , to skip the counterfeit judgment processing for image data having a resolution equal to or less than 100 dpi is effective in reduction of processing time . note that in use of another resolution as the criterion of counterfeit judgment processing , there is no change in subject matter of the present invention . in the above - described embodiment , the counterfeit judgment processing is performed in accordance with whether an output resolution is over a predetermined value , however , in addition to the output resolution , an output image size may be added to the criterion . for example , if the size of output image is small even though the output resolution is high , the printed output based on the image data is not used as a counterfeit . accordingly , the counterfeit judgment processing can be skipped if the output image size is less than a predetermined value ( e . g ., within 5 cm × 5 cm ). in this manner , the counterfeit judgment processing is performed only if image data has a size equal to or greater than a predetermined size , in addition to a resolution equal to or higher than a predetermined resolution , thereby processing time can be further reduced . hereinbelow , a second embodiment of the present invention will be described . since the second embodiment is executed in a similar system to that in the first embodiment , constituent elements corresponding to those in the first embodiment have the same reference numerals and the detailed explanations of the elements will be omitted . in the above - described first embodiment , the electronic watermark detection processing is performed only on image data representing image and having a resolution higher than a predetermined resolution . in the second embodiment , the electronic watermark detection processing is performed on image data representing image without any condition . as in the case of the first embodiment , print information inputted from the ddi has three attributes , “ text ” indicative of font information , “ graphics ” indicative of figure vector , gradation information and the like , and “ image ” indicative of read photographic image or the like , and different functions are called for the respective attributes . accordingly , it is easy to extract only the “ image ” attribute data upon reception of print information from the ddi and process the extracted data . it can be considered that generally , in a case where a bank note , a negotiable instrument or the like is to be duplicated , in order to reproduce an original image read by the scanner 300 or the like with fidelity , image data as the object of processing is inputted as “ image ” attribute data . in the second embodiment , it can be considered that if the counterfeit judgment processing is performed only on input image data , counterfeit prevention can be sufficiently realized . next , the counterfeit judgment processing in the second embodiment will be described with reference to the flowchart of fig8 . in fig8 , process steps corresponding to those in fig3 described in the first embodiment have the same step numbers , and the detailed descriptions of the steps will be omitted . note that the counterfeit judgment processing is performed in the counterfeit judgment unit 2025 in the pdl driver 2023 or in the counterfeit judgment unit 2026 in the image driver 2024 , in the printer driver 2020 . in fig8 , at step s 802 , it is determined whether or not the input print information is image data . if the input information is image data , the process proceeds to step s 303 at which the electronic watermark detection processing is performed , while if the input information is not image data , the process proceeds to step s 306 , at which normal print processing is performed . note that the counterfeit prevention processing in the second embodiment is the same as that as shown in fig4 in the first embodiment . as described above , according to the second embodiment , the electronic watermark detection processing is performed only on image attribute data in the printer driver 2020 . by this arrangement , as the execution of the electronic watermark detection processing can be minimized , the counterfeit prevention function against counterfeiting bank notes , negotiable instruments and the like can be realized while preventing reduction of total throughput . in the second embodiment , the counterfeit judgment processing is performed in accordance with whether or not input data is image data , however , the judgment reference can be further limited . fig9 shows a flowchart of the counterfeit judgment processing in the counterfeit judgment unit 2026 in the pdl driver 2023 according to the present modification . the flowchart of fig9 is different from the flowchart of fig3 in that the determination as to whether or not the electronic watermark detection processing is performed is made at two steps s 902 a and s 902 b . that is , if it is determined at step s 902 a that the input data is image data , the amount of information per pixel ( the number of bits ) is checked at step s 902 b . only if the amount of information is equal to or greater than that of respectively 8 - bit rgb data , 24 bits , the process proceeds to step s 303 to perform the electronic watermark detection processing . generally , even in case of image data , if the number of representable colors is small , i . e ., the image data is indicative of monochrome image , 16 - color image , 256 - color image or the like , the probability of image data for counterfeiting is very low . accordingly , the counterfeit judgment processing is omitted regarding image data with small number of representable colors , i . e ., small amount of information , thereby processing time can be further reduced . note that in the above - described first and second embodiments and the modifications , the present invention is applied to a color laser - beam printer , however , the printer to which the present invention is applicable is not limited to the color laser - beam printer , but the invention is applicable to other color printers such as an ink - jet printer and a thermal printer to form an image on a print medium based on other printing methods . further , the criteria of judgment for execution of the counterfeit judgment processing is not limited to the above - described image data resolution , the image size , the image attribute or the information amount . any other judgment reference can be employed as long as it can be used for judging whether or not input image data is in high quality for obtaining a printed output as a counterfeit . the present invention can be applied to a system constituted by a plurality of devices ( e . g ., a host computer , an interface , a reader and a printer ) or to an apparatus comprising a single device ( e . g ., a copy machine or a facsimile apparatus ). further , the object of the present invention can be also achieved by providing a storage medium ( or recording medium ) storing software program code for realizing the functions of the above - described embodiments to a system or an apparatus , reading the program code with a computer ( e . g ., cpu , mpu ) of the system or apparatus from the storage medium , then executing the program . in this case , the program code read from the storage medium realizes the functions according to the embodiments , and the storage medium storing the program code constitutes the invention . furthermore , besides aforesaid functions according to the above embodiments are realized by executing the program code which is read by a computer , the present invention includes a case where an os ( operating system ) or the like working on the computer performs a part or entire actual processes in accordance with designations of the program code and realizes functions according to the above embodiments . furthermore , the present invention also includes a case where , after the program code read from the storage medium is written in a function expansion card which is inserted into the computer or in a memory provided in a function expansion unit which is connected to the computer , cpu or the like contained in the function expansion card or unit performs a part or entire actual process in accordance with designations of the program code and realizes functions of the above embodiments . as many apparently widely different embodiments of the present invention can be made without departing from the spirit and scope thereof , it is to be understood that the invention is not limited to the specific embodiments thereof except as defined in the appended claims . | 6 |
referring to fig1 , a motor vehicle seat assembly according to one embodiment of the invention is generally indicated at 8 . the seat assembly 8 includes a cushion 13 for supporting an occupant above a floor . the seat assembly 8 also includes a first seat back 12 and a second seat back 14 each capable of supporting a torso of the occupant seated on the seat cushion 13 . at least one of the seat backs 12 , 14 is pivotally coupled to the cushion 13 for movement between a plurality of back support positions and / or a forwardly folded flat position . each seat back 12 , 14 includes a side surface 18 , 19 . the side surfaces 18 , 19 of the seat backs 12 , 14 face each other and are generally parallel to each other . a gap 16 is formed between the side surfaces 18 , 19 of the seat backs 12 , 14 due largely to the at least one of the seat backs 12 , 14 being pivotally coupled to the seat cushion 13 . described in greater detail below , the seat assembly 8 includes a side shield or cover 10 for concealing a lower area of the gap 16 . referring to fig2 - 3 , the cover 10 includes a main wall 20 that is generally parallel with the side surfaces 18 , 19 of the seat backs 12 , 14 . a rib lattice 22 is integrally formed on at least one side of the main wall 20 to reinforce the cover 10 . a first flange 23 extends arcuately along a leading edge 25 of the main wall 20 . the first flange 23 is generally orthogonal to the main wall 20 . the first flange 23 extends toward the side surface 18 of the first seat back 12 . a bottom portion 24 of first flange 23 is integrally formed with the main wall 20 . the main wall 20 and the bottom portion 24 of the first flange 23 are substantially rigid . the main wall 20 and the bottom portion 24 of the first flange 23 may be formed of any suitable plastic material and formed , for example , in an injection molding process . an upper portion 26 of the first flange 23 is formed of a different material than the bottom portion 24 of the first flange 23 . more specifically , the upper portion 26 of the first flange 23 is formed from a flexible material . in one embodiment , the upper portion 26 is formed of an elastomeric or rubber material , so as to be flexible relative to the substantially rigid portions of the cover 10 , i . e . the main wall 20 and the bottom portion 24 . a second flange 34 extends arcuately along the leading edge 25 of the main wall 20 . the second flange 34 is generally orthogonal to the main wall 20 . the second flange 34 extends toward the side surface 19 of the second seat back 14 . in one embodiment , the second flange 34 is formed of an elastomeric or rubber material , so as to be flexible relative to the bottom portion 24 of the first flange 23 and the main wall 20 . in another embodiment , the upper portion 26 of the first flange 23 and the second flange 34 are integrally formed from the same flexible material . the relatively flexible portions of the cover 10 , i . e . the upper portion 26 of the first flange 23 and the second flange 34 , may be formed integrally with the substantially rigid portions 20 , 24 of the cover 10 in a two - shot injection molding process , in which the substantially rigid portions 20 , 24 of the cover 10 are formed in one part of an injection molding tool using a resin or plastic material and the relatively flexible portions 26 , 34 of the cover 10 are formed in a subsequent step in the same injection molding tool using a flexible elastomeric or rubber based material . alternatively , the rigid 20 , 24 and flexible 26 , 34 portions of the cover 10 may be formed separately and assembled in a subsequent assembly step , such as by fasteners or heat staking . the rigid portion 20 , 24 of the cover 10 may also include a third flange 32 extending generally orthogonally from the main wall 20 . the third flange 32 may include mounting holes 38 for mounting the cover 10 to other components of the seat assembly 10 , such as the seat cushion 13 . the cover 10 may also include ribs 36 for minimizing flexing of the third flange 32 relative to the main wall 20 . by this arrangement , the first 23 and second 34 flanges conceal portions of the gap associated with respective seat backs 12 , 14 , thereby eliminating the need for individual conventional covers that are otherwise typically used for covering the same portions of the gap . further , the flexible portions 26 , 34 of the cover 10 flex to prevent pinching of or uncomfortable hard points being felt by the occupant . the invention has been described in an illustrative manner . it is , therefore , to be understood that the terminology used is intended to be in the nature of words of description rather than of limitation . many modifications and variations of the invention are possible in light of the above teachings . thus , within the scope of the appended claims , the invention may be practiced other than as specifically described . | 1 |
fig1 - 9 and the following description depict specific embodiments of the invention to teach those skilled in the art how to make and use the best mode of the invention . for the purpose of teaching inventive principles , some conventional aspects have been simplified or omitted . those skilled in the art will appreciate variations from these embodiments that fall within the scope of the invention . those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple embodiments of the invention . as a result , the invention is not limited to the specific embodiments described below , but only by the claims and their equivalents . fig1 illustrates communication network 100 in an embodiment of the invention . communication network 100 includes communication system 110 in communication with communication network 150 over link 7 . communication system 110 is also in communication with node 120 over link 6 . node 120 is in communication with node 130 over link 3 . node 120 is also in communication with end point 144 over link 5 , and end point 143 over link 4 . node 130 is in communication with end point 141 over link 1 , and with end point 142 over link 2 . in this embodiment , communications are transferred to and from the various end points to communication system 110 . similarly , communications are transferred to and from communication network 150 to communication system 110 . communication network 150 could be , for example , a packet based communication network , such as an internet or intranet . communication network 150 could also be , for example , a circuit switched network , such as the public switched telephone network ( pstn ). communication network 150 could also be a wireless communication network . further in this embodiment , communication system 110 could be any communication system capable of handling communication sessions between elements of communication network 150 and end points 141 - 144 . end points 141 - 144 could be , for example , user devices , customer premise equipment , soft switches , or proxy servers , as well as other types of network end points . nodes 120 and 130 could be network elements , such as routers , that handle session traffic between the various end points and communication system 110 . in this embodiment , communication system 110 manages sessions between the various end points and each other , as well as with communication network 150 . for instance , communication system 110 sets up voice or video sessions for the end points . in addition , communication system 110 could interwork session traffic between various formats and protocols required by the end points and communication network 150 . fig2 illustrates the operation of communication network 100 in an embodiment of the invention . to begin , communication system 110 receives a session setup request ( step 210 ). such a request could be in the form of a session initiation protocol ( sip ) message or an h . 323 setup message , as well as in other forms . based on the request message , communication system 110 determines an end point for the session ( step 220 ). the end point could be determined from end points 141 - 144 . next , communication system 110 determines a resource group associated with the selected end point ( step 230 ). any particular end point could be associated with one or more resource groups . a resource group is a collection of one or more network resources to be managed or allocated based upon a shared identity or commonality . for example , elements of a resource group could be related by connectivity . a network element could be a hardware component , such as a router or soft switch , as well as a link . each resource group could have one or more profiles . a profile describes the constraints of the resource group and how the constraints should be applied to the resource group . upon determining the resource group , communication system 110 access the current profile for that resource group . upon accessing the profile , communication system 110 determines whether or not the requested session would violate the resource profile if the session were to be setup ( step 240 ). if yes , the session is rejected ( step 250 ). if not , communication system 110 further processes the request message to determine if there are anymore resource groups associated with the end point ( step 260 ). if so , step 240 is repeated for the next resource group and its current profile . if not , the session setup process is completed ( step 270 ). the above illustrated steps could be performed in a different order than that described . fig3 is an illustration of a resource table 300 used by communication system 110 is the above described processes . table 300 has three columns . the first column indicates the name of the resource group . the second column illustrates the commonality that provides the relationship between the elements of the resource group . the third column illustrates the elements of the resource group . in fig3 , the resource groups are allocated elements based upon their common connectivity to a node . for example , resource group a includes end point 141 related to link 1 because link 1 connects end point 141 to node 130 . in contrast , resource group c has two members — end point 141 and end point 142 — included because of their common relationship to link 3 , which provides both end points with connectivity to node 120 . resource group f has four members in its resource group — end point 141 , end point 142 , end point 143 , and end point 144 — based on their common relationship to link 6 , which provides connectivity to communication system 110 . a profile is then created for each resource group a - f . the profile holds the constraints to be applied to the members of the resource groups . for example , the profile for resource group a could indicate a constraint , such as maximum bandwidth , associated with link 1 . adding end point 141 is only allowed so long as the resulting bandwidth does not exceed the maximum bandwidth allowed for link 1 . this could occur if , for instance , end point 141 is a high - bandwidth device and if the requested service requires a high bandwidth . in that case , the requested service could be rejected . in another example , the profile for resource group c could indicate a maximum bandwidth constraint to be applied to link 3 . end points 141 and 142 are part of resource group c . end point 141 is also part of resource group a . thus , the constraints of two profiles for both resource groups must be satisfied in order to allow a service request that implicates both resource groups . in an illustrative example , assume a session request is received by communication system 110 for a voice over packet ( vop ) session between end point 141 and a user device in communication network 150 . further assume that communication network 150 is the pstn . in this example , communication system 110 processes a session request 110 to select end point 141 . communication system 110 would then access table 300 to determine any resource groups associated with end point 141 . in this example , end point 141 is associated with resource groups a , c , and f . next , communication system 110 determines if the requested session would violate a profile for resource group a . assuming the session would not violate the profile for resource group a , communication system 110 then determines whether the session would violate the resource group for resource group c . again , assuming the session would not violate the profile for resource group c , communication system 110 then determines whether or not the session would violate the profile for resource group f . if the session would violate the profile for any of the resource groups , the session could be rejected . the profiles could , for example , set a maximum number of calls that can be handled by any one resource group at a given time . assuming again that the session would not violate any of the profiles for the various resource groups , the session setup would continue . once the session is completely setup , session traffic can be transferred to and from end point 141 and communication network 150 . in this example , communication system 110 would interwork the traffic between an asynchronous packet format and a synchronous format for communication network 150 . communication system 110 could also include link 7 in determining if the session should be setup . however , in this example , communication network 150 is the pstn . link 7 would therefore likely be a synchronous trunk line . thus , if the trunk is available , then it can be assumed that the bandwidth profile for the trunk would not be exceeded by the session . advantageously , communication network 100 provides an improved way to allocate network resources . in contrast to the prior art , the individual bandwidth requirements of various links and devices involved in a session can be accounted for prior to setting up a session . in this manner , quality of service requirements can be enforced without the risk of service degradation or cessation . furthermore , the concept of resource groups and resource profiles provides a flexible and efficient mechanism for managing network resources . fig4 illustrates communication network 400 in an embodiment of the invention . communication network 400 includes service provider 410 in communication with pstn 460 . service provider 410 includes call controller 412 , border controller 411 , and gateway 413 . call controller could also be referred to as a gateway controller . gateway 413 interworks asynchronous packet traffic to and from a synchronous format for pstn 460 . the traffic is exchanged over link 407 . border controller 411 is in communication with router 421 over link 406 . router 421 is in communication with intermediate access device ( iad ) 441 through router 422 and via links 401 and 403 . similarly , router 421 is in communication with private branch exchange ( pbx ) 443 through router 423 via link 404 . router 521 is also in communication with soft switch 444 through router 424 and via link 405 . lastly , router 421 is in communication with iad 442 through router 422 and via links 402 and 403 . in operation , service provider 410 provides services to end users 451 and 452 . in addition , service provider 410 provides services to end users ( not pictured for the sake of clarity ) of pbx 443 and soft switch 444 . services could be , for example , voice or video over packet ( vop ) services . in addition , services could be , for example , data services , as well as other types of services . further in operation , the various links 401 - 406 are capable of providing a finite amount of bandwidth for traffic . similarly , routers 421 - 424 are also capable of providing a finite amount of bandwidth . soft switch 444 can also only handle a certain amount of traffic , and therefore can have an associated bandwidth . pbx 443 also typically can handle only a certain number of simultaneous calls . end users 451 and 452 typically utilize particular codec schemes , and therefore use a certain amount of bandwidth per call . as such , it is important that service provider 410 allocate and manage the bandwidth associated with all the various network elements and links . fig5 illustrates the operation of communication network 400 in an embodiment of the invention . to begin , call controller 412 receives a vop call setup request ( step 510 ). such a request could be in the form of a session initiation protocol ( sip ) message or an h . 323 setup message , as well as in other forms . based on the request message , call controller 412 determines an end point for the session ( step 520 ). in this example , it is assumed that end user 451 is an end point for the call . next , call controller 412 determines a resource group associated with the selected end point ( step 530 ). any particular end point could be associated with one or more resource groups . each resource group could have one or more profiles . in this example , the path to be used for the session from end user 451 to service provider 410 follows link 401 , link 403 , and link 406 through routers 422 and 421 . a first resource group for end user 451 would therefore be link 401 . a second resource group for end user 451 would be link 403 . a third resource group for end user 451 would be link 406 . the first resource group would have a profile of the bandwidth requirements of link 401 . the profile could indicate a maximum amount of calls allowed on link 401 using a particular codec type . another profile for the same resource group could indicate a combination of two or more maximum numbers of calls using two or more types of codecs . another profile for the same resource group could indicate a maximum weight allowed for the link . the maximum weight could be determined by allocating a weight for each type of codec . depending upon the current utilization of the link , adding a new weight to the current weight could be allowed under the maximum weight . the other remaining resource groups would also have profiles as illustrated for the first resource group . upon determining the resource group , call controller 412 accesses the current profile for that resource group . upon accessing the profile , call controller 412 determines whether or not the requested session would violate the resource profile if the session were to be setup ( step 540 ). if yes , the session is rejected ( step 550 ). if not , call controller 412 further processes the request message to determine if there are anymore resource groups associated with the end point ( step 560 ). if so , step 440 is repeated for the next resource group and its current profile . if not , the session setup process is completed ( step 570 ). the above illustrated steps could be performed in a different order than that described . fig6 further illustrates the operation of communication network 400 in an embodiment of the invention . at step 540 in fig5 , call controller 412 accesses the current profile for the resource group . the profile could be a codec profile for the resource group . in such as case , call controller 412 retrieves the codec profile ( step 610 ). next , call controller 412 determines whether or not the call violates the codec profile ( step 620 ). the codec profile could describe , for example , a maximum number of calls allowed over the resource group from devices using a particular codec scheme , such as g . 711 or g729 . for example , 100 calls using the g . 711 codec could be allowed on the resource group . if the current call is call number 101 using g . 711 , the call would be rejected ( step 630 ). if the call is less than the one - hundredth call using g . 711 , the call would be allowed ( step 640 ). fig7 further illustrates the operation of communication network 400 in an embodiment of the invention . here , a profile range is utilized . a profile range is a range of different profiles that can be applied to a resource group . to begin , call controller 412 retrieves a profile for a resource group ( step 710 ). next , call controller 412 determines whether or not the call would violate the current profile for the resource group ( step 720 ). if not , the call can be completed ( step 730 ). if so , call controller 412 then determines if there are any other profiles available for the current resource group ( step 740 ). if so , the next profile is retrieved ( step 710 ). if not , the call is rejected as the current profile would be violated by the call , and no other profiles exist for the resource group ( step 750 ). fig8 further illustrates the operation of communication network 400 in an embodiment of the invention . here , a profile having a codec weight is utilized . a codec weight profiles utilizes weights for each codec type to create a ratio and normalize calls to a single unit of bandwidth utilization . the maximum number of calls is based on the normalized unit . to begin , a call setup request is received by call controller 412 ( step 810 ). next , the codec for the call is determined ( step 820 ). a weight for the codec is determined ( step 830 ) and incorporated into a determination of whether there is enough bandwidth to handle the call ( step 840 ). if not , the call is rejected ( step 850 ). if so , call setup can continue for completion of the call ( step 860 ). for example , a g . 729a codec could have a weight of one , and a g . 711 codec could have a weight of six . this means that g . 711 calls use six times the bandwidth of a g . 729a call . a new g . 711 call adds six to the total number of simultaneous calls , while a g . 729a call adds only one . advantageously , the codec weight profile is very efficient and flexible . in an alternative , codecs could be prioritized . under a prioritization scheme , calls using a first type of codec could receive priority over calls using a second type of codec . the first type of codec could be , for example , more desirable than the second type . fig9 illustrates computer system 900 in an embodiment of the invention . computer system 900 includes interface 920 , processing system 930 , storage system 940 , and software 950 . storage system 940 stores software 950 . processing system 930 is linked to interface 920 . computer system 900 could be comprised of a programmed general - purpose computer , although those skilled in the art will appreciate that programmable or special purpose circuitry and equipment may be used . computer system 900 may use a client server architecture where operations are distributed among a server system and client devices that together comprise elements 920 - 950 . interface 920 could comprise a network interface card , modem , port , or some other communication device . signaling interface 920 may be distributed among multiple communication devices . interface 930 could comprise a computer microprocessor , logic circuit , or some other processing device . processing system 930 may be distributed among multiple processing devices . storage system 940 could comprise a disk , tape , integrated circuit , server , or some other memory device . storage system 940 may be distributed among multiple memory devices . processing system 930 retrieves and executes software 950 from storage system 940 . software 950 may comprise an operating system , utilities , drivers , networking software , and other software typically loaded onto a general - purpose computer . software 950 could also comprise an application program , firmware , or some other form of machine - readable processing instructions . when executed by the processing system 930 , software 950 directs processing system 930 to operate as described for communication system 100 and call controller 412 . also when executed by the processing system 930 , software 950 directs processing system 930 to operate as described for communication networks 100 and 400 . | 7 |
a rotary vibrator 10 , as seen in fig1 has an exterior defined by a tubular housing or casing 12 and a cap 14 which is detachably connected to the casing 12 by mating threads 15 . the casing 12 is formed from a metal tube 16 and two flanges 17 and 18 , with the flanges 17 and 18 welded to opposite ends of the metal tube 16 . the casing 12 , as well as the components 16 , 17 and 18 , could also be machined from solid bar of an appropriate cross section . the casing 12 has an open chamber 19 and the cap 14 has a cantilevered stub - shaft 20 which extends from the cap 14 into the chamber 19 . a rotating assembly 22 is mounted on the stub - shaft 20 for rotation about an axis 23 and includes an eccentric weight 24 , a bearing assembly 26 , a conventional lip seal 28 adjacent the base of the stub - shaft 20 , a bearing retainer 30 adjacent the end of the stub - shaft 20 , plug / bearing retainer 32 , a retaining ring 34 for the bearing assembly 26 , and a retaining ring 36 for the lip seal 28 . the cap 14 and the rotating assembly 22 may be removed from the casing 12 as a subassembly 37 by simply unscrewing the cap 14 from the casing 12 . this feature allows the rotating assembly 22 to be removed from the vibrator 10 in a simple and efficient manner with no need for the time consuming extraction of individual components from the casing . additionally , because the rotating assembly 22 is maintained as a single subassembly 37 with the cap 14 , there is no risk during the removal from the casing that individual component parts will inadvertently fall from the rotary vibrator 10 and become lost or damaged . further , this feature allows for simplified maintenance because a pre - assembled subassembly 37 can be quickly and easily substituted for the subassembly 37 currently in the vibrator 10 . finally , this feature allows the rotating assembly 22 to be removed from the vibrator 10 without having to disconnect the vibrator 10 from its power source . as best seen in fig1 the eccentric weight 24 has a mass section 38 which extends along the axis 23 from a first terminal end 40 to a step 42 . as best seen in fig2 and 3 , the eccentric weight 24 is also provided with a bearing bore 44 having a first internal cylindrical surface 46 extending the length of the mass section 38 to an annular rib 47 , and a second internal cylindrical surface 48 which extends from the annular rib 47 to an internal thread 49 of the eccentric weight 24 . as best seen in fig2 the bearing assembly 26 includes a sealed or shielded , deep groove ball bearing 52 which acts as a thrust bearing for reacting axial loads . an outer race 54 of the ball bearing 52 is mounted within the second cylindrical surface 48 of the eccentric weight 24 . as shown in fig1 the bearing assembly 26 further includes three needle roller bearings 55 which extend along the axis 23 for reacting radial loads . as best seen in fig3 outer races 56 of the bearings 55 are mounted within and press fit against the first cylindrical surface 46 of the eccentric weight 24 . as seen in fig1 the bearing 52 is retained within the bearing bore 44 by the plug / bearing retainer 32 which is detachably connected to a second terminal end 58 of the eccentric weight 24 by mating threads 60 . as best seen in fig2 the outer race 54 of the bearing 52 is trapped between the annular rib 47 and a first terminal end 64 of the bearing retainer 32 . the bearing 52 is retained to the stub - shaft 20 by the bearing retainer 30 which has a shoulder 72 abutting an inner race 74 of the bearing 52 and forcing the inner race 74 against a terminal end 75 of the stub - shaft 20 . the bearing retainer 30 is detachably connected to the stub - shaft 20 by mating threads 76 . the bearings 55 are retained within the bearing bore 44 by the retaining ring 34 . as best seen in fig3 the retaining ring 34 is mounted in an annular groove 77 formed in the eccentric weight 24 adjacent the first terminal end 40 . the outer races 56 of the bearings 55 are trapped between the retaining ring 34 and the annular rib 47 . however , it should be noted that , in some instances , it may be preferable to omit the retaining ring 34 and to use the lip seal 28 for retaining the bearings 55 . an outer surface 78 of the stub - shaft 20 acts as the inner race for the bearings 55 . thus , radial loads generated by the eccentric weight 24 during rotation are reacted directly through the bearings 55 to the outer surface 78 of the stub - shaft 20 . axial loads generated by the rotation of the eccentric weight 24 are reacted against the outer race 54 of the bearing 52 by the annular rib 47 and the first terminal end 64 of the bearing retainer 32 . the axial loads are transferred through the bearing 52 to the stub - shaft 20 by the inner race 74 which abuts the terminal end 75 of the stub - shaft 20 and by the bearing retainer 30 which abuts the inner race 74 and is threadably connected to the stub - shaft 20 . as best seen in fig3 the lip seal 28 is mounted in the first cylindrical surface 46 adjacent the terminal end 40 for retaining lubricant within the bearing bore 44 and the bearings 55 . the lip seal 28 is trapped between the retaining rings 34 and 36 . the retaining ring 36 is mounted in an annular groove 79 formed in the eccentric weight 24 adjacent the terminal end 40 . thus , the lip seal 28 and the sealed or shielded bearing 52 retain lubricant within the bearing chamber 44 . as best seen in fig1 the rotating assembly 22 is rotationally driven by a hydraulic motor 80 through a flexible drive shaft 82 that includes a non - circular drive - tang 84 extending into the bearing retainer 32 with an axially sliding fit . the motor 80 is mounted in a fitting 86 which is threadably engaged with the casing 12 . the flexible drive shaft 82 includes a flex shaft 88 , a coupling 90 crimped to the flex shaft 88 and operably engaged with a drive shaft 92 of the hydraulic motor 80 through a conventional woodruff key 94 , and a coupling 96 that is crimped to the flex shaft 88 and the drive - tang 84 . the drive - tang 84 slides freely in the bearing retainer 32 and the coupling 90 slides freely on the shaft 92 along the axis 23 for purposes of assembly . this allows the subassembly 37 to be removed from the rotary vibrator 10 without removing the hydraulic motor 80 . the mating threads 60 between the bearing retainer 32 and the eccentric weight 24 are configured such that they tend to engage when the eccentric weight 24 is driven by the flexible shaft 82 . the hydraulic motor 80 is connected to a hydraulic power source by hydraulic supply and return lines 98 and 100 which are connected to the hydraulic motor 80 by hydraulic fittings 102 . the hydraulic lines 98 and 100 are surrounded by a sheath or rubber hose 104 which is clamped to a hose barb 105 on a bracket 106 by a hose clamp 107 . the bracket 106 is threadably engaged to the hydraulic vibrator 10 through the fitting 86 . the sheath 104 serves to protect the hydraulic lines 98 and 100 and to allow manipulation of the rotary vibrator 10 by an operator . any suitable power source and drive means can be substituted for the hydraulic power source and hydraulic motor 80 . appropriate power transfer means can also be substituted for the hydraulic supply and return lines 98 and 100 , as well as the hydraulic fittings 102 . for example , a high cycle electric motor can be substituted for the hydraulic motor 80 , with an appropriate electric power source and electrical cables substituted for the hydraulic power source and the hydraulic supply and return lines 98 and 100 . packings or seals 108 are provided between the fitting 86 and the casing 12 and between the cap 14 and the casing 12 to prevent fluid from entering the vibrator 10 during operation . in the event of a bearing failure or for routine maintenance , the cap 14 is unthreaded from the casing 12 . the cap 14 and the rotating assembly 22 are then removed as the subassembly 37 from the rotary vibrator 10 and a replacement subassembly 37 is installed . to replace the bearings 52 and 55 , the plug / bearing retainer 32 is unthreaded from the eccentric weight 24 and then the bearing retainer 30 is unthreaded from the stub - shaft 20 . this frees the rotating assembly 22 from the stub - shaft 20 , thereby allowing the rotating assembly 22 to be removed from the stub - shaft 20 . the bearings 52 and 55 may then be removed from the eccentric weight 24 and replaced as required . reassembly of the rotary vibrator 10 is accomplished in reverse order of the steps for disassembly . because the cap 14 and the rotating assembly 22 are removable as the subassembly 37 from the terminal end of the vibrator 10 , the bearings 52 and 55 can be replaced without disconnecting and the sheath 104 and the hydraulic lines 98 and 100 from the vibrator 10 . additionally , if necessary , subassembly 37 allows the bearings 52 and 55 to be removed from the vibrator 10 while the vibrator 10 remains within the work environment , without the fear of inadvertently dropping loose components . thus , the bearings 52 and 55 may be quickly and easily replaced whenever bearing failure occurs . by spacing the needle roller bearings 55 along and directly under the mass section 38 , the radial loads generated by the mass section 38 are distributed equally to each bearing 55 . this is advantageous because the radial loads can be equally distributed between more than two bearings , thereby minimizing the operating loads on each of the bearings . additionally , because the bearings 55 are placed inside the bearing bore 44 of the eccentric weight 24 , there is no additional length required for the mounting of the bearings 55 . the material removed from the eccentric weight 24 to form the bearing bore 44 has a minimal impact on the magnitude of vibrational forces generated by the rotary vibrator 10 because the mass at the larger diameters has a far greater impact on the magnitude of the vibrational forces . thus , more of the length of the rotary vibrator 10 can be devoted to the mass section 38 of the eccentric weight 24 when compared to a standard straddle - mounted design , thereby providing a rotary vibrator 10 which can generate higher vibratory forces for a given rotational speed . further , because the axial loads are transferred through the ball bearing 52 , the bearings 55 do not have to perform double duty and need only transfer radial loads . this allows for the bearings 55 to be roller bearings which typically have a greater dynamic load rating than ball bearings of a comparable frame size . thus , bearing failures are further reduced when compared to standard straddle mount designs which commonly employ ball bearings at either end of the eccentric weight to transfer both radial and axial loads . it will be understood that the invention may be embodied in other specific forms without departing from the spirit or central characteristics thereof . the present examples , therefor , are to be considered in all respects as illustrative and not restrictive , and the invention is not to be limited to the details given herein . | 1 |
while the present invention is susceptible of embodiment in various forms , there is shown in the drawings and will hereinafter be described a presently preferred embodiment with the understanding that the present disclosure is to be considered an exemplification of the invention and is not intended to limit the invention to the specific embodiments illustrated . referring generally to fig1 - 3 , a woven retractor sleeve 100 for providing access to a surgical site is illustrated . the woven retractor sleeve 100 is constructed to include a central portion 12 , a base end 10 and a proximal portion 14 . the retractor sleeve is generally tubular in cross sectional shape and can be made in a variety of sizes for different types of percutaneous surgical procedures . the base portion 10 is preferably provided with at least one , and more preferably a plurality of anchor members 16 . in general , the anchor members include a sloped side 18 and a catch side 20 . the anchor members are preferably constructed from a relatively rigid or spring like material to allow the directional engagement of the sleeve through the tissue or bone surrounding the surgical site while the anchors engage tissue and / or bone to secure the sleeve at the desired location . however , it should also be noted that the anchor members may be constructed from the same or similar material as the sleeve without departing from the scope of the invention . in this manner , the sleeve can be incrementally advanced to the surgical site . alternatively , the sleeve may be moved to the desired location and the anchors may be directly engaged to the tissue surrounding the surgical site . in one non - limiting embodiment , the anchor members 16 each include a v - shaped cross sectional shape , a sloped side 18 and a catch side 20 . the anchor members 16 may be secured at various locations along the retractor sleeve 100 by stitching , adhesive , weaving , fasteners or any suitable combination thereof . the proximal portion 14 of the retractor sleeve is preferably larger in diameter than the base end and may include at least one , and more preferably a plurality of apertures 22 sized and shaped to cooperate with one or more cage members 24 ( fig6 - 11 ). the apertures may also be utilized in conjunction with a drawstring member 26 ( fig4 ) to secure the retractor sleeve 100 to an insertion probe 28 as shown in fig4 . still referring to fig1 - 3 . the sidewall 30 of the retractor sleeve 100 is constructed from a fabric , e . g . woven and / or knit material , to provide properties not found within rigid retraction devices . it will be appreciated by those skilled in the art that , in the fabric produced in the weaving or knitting process , the longitudinal fibers 36 and the circumferential fibers 38 may not be distributed in discrete layers in the fabric . however , in the preferred embodiment of the instant invention , the fibers of one yarn are predominantly located on the technical front 32 of the fabric and the other yarn fibers are predominantly located on the technical back 34 of the fabric . this construction provides numerous advantages with respect to rigid type retractors . the fabric material allows the retraction sleeve to be reduced significantly in size or changed in shape for insertion . the woven construction permits the use of fibers or yarns having different properties extending through the fabric in longitudinal and circumferential directions . this will allow the retractor sleeve to expand in diameter beyond its static diameter for passage of an implant or tool providing shorter term retraction of tissue , nerve roots etc . to minimize trauma to the patient . the fabric may also include one of a variety of surface or face finishing including caustic reduction , napping , brushing , sueding , and shearing to increase surface filament count to increase surface acceptance of fluids . alternatively or in addition to the surface finishing , the fabric may be coated with a coagulant to increase surgeon visibility of the site by limiting blood flow into the surgical site . in at least one embodiment , the technical back includes fibers that extend primarily in the longitudinal direction , e . g . longitudinal fibers 36 . this construction allows implants and tools to be more easily slid across the surface of the retractor sleeve while the predominantly circumferential fibers on the outside of the sleeve provide gripping to the adjacent tissue to resist movement . the longitudinal fibers are preferably constructed from a high performance material / fabric , such as a ballistic resistant material / fabric , a high tensile strength material / fabric , nylon , an aramid material such as kevlar , spectra , twaron , dyneema , another synthetic material or any mixture of these . these materials provide some rigidity to the overall length of the retractor sleeve while resisting punctures and tears . in some embodiments , radio opaque fibers 40 extend along the length or portions of the length of the retractor sleeve for cooperation with surgical radiography to aid the surgeon in locating the device in the surgical site . the circumferential fibers 38 can be manufactured from a variety of fibers including cellulosic fibers , such as cotton , or synthetic petrochemical fibers , such as polyester . the fibers may be used in 100 % form , or from blended fibers , including cellulosic fiber in combination with synthetic fibers , either in mechanical or intimate blends . spandex ( such as lycra ® manufactured by dupont ), monofilament , rubber , or elastomerics may be utilized or introduced to the fabric construct to create an expandable diameter sleeve . referring to fig4 and 5 , the retractor sleeve 100 is illustrated in a first compact configuration cooperating with an insertion probe 28 . in fig4 the retractor sleeve is wrapped about an insertion probe 28 having a central shaft 42 . the central shaft includes a sharp distal end 44 for ease of tissue penetration . the insertion probe is preferably constructed of a biocompatible material and may be constructed to transfer electrical current to a neuro - monitoring device to aid the surgeon in avoiding nerve structures . a drawstring 26 may be provided to secure the retractor sleeve in place about the insertion tool . the sleeve can , after insertion be released by pulling or cutting the drawstring to release the retractor . fig5 illustrates an alternative embodiment of the insertion probe 28 . in this embodiment , the central shaft is a hollow shaft 46 and may include a deployment window 48 for deploying the retraction sleeve . referring to fig6 - 11 , various types of cage members are illustrated . in general , the cage members are constructed and arranged to hold the retractor sleeve in a second open position . the cage members may include spikes 50 that project through the retractor sleeve to engage tissue or bone . the cage members may be constructed from various materials that may be rigid , resilient or elastic in nature . in some embodiments , the cage member may include telescoping joints 52 that may be used alone or in combination with spring and / or rigid materials . it is to be understood that while certain forms of the invention are illustrated , it is not to be limited to the specific forms or arrangements herein described and shown . it will be apparent to those skilled in the art that various changes may be made without departing from the scope of the invention and the invention is not to be considered limited to what is shown and described in the specification and any drawings / figures included herein . one skilled in the art will readily appreciate that the present invention is well adapted to carry out the objectives and obtain the ends and advantages mentioned , as well as those inherent therein . the embodiments , methods , procedures and techniques described herein are presently representative of the preferred embodiments , are intended to be exemplary and are not intended as limitations on the scope . changes therein and other uses will occur to those skilled in the art which are encompassed within the spirit of the invention and are defined by the scope of the appended claims . although the invention has been described in connection with specific preferred embodiments , it should be understood that the invention as claimed should not be unduly limited to such specific embodiments . indeed , various modifications of the described modes for carrying out the invention which are obvious to those skilled in the art are intended to be within the scope of the following claims . | 0 |
fig1 is a conceptual diagram of a route search system that is an embodiment of the present invention . in fig1 , a route supply server 20 and three cellular phones 10 _a , 10 _b , and 10 _c are illustrated . at least a partial section on the cellular phones 10 _a , 10 _b , and 10 _c side is wirelessly connected to the route supply server 20 . in reality , the cellular phones 10 _a , 10 _b , and 10 _c wirelessly communicate to each base station ( not illustrated ). there are many base stations and internet networks or the like between each of the base stations and the route supply server 20 . however , to simplify the diagram , only elements necessary for describing the present embodiment are illustrated . fig2 is a perspective view of an appearance of one cellular phone representing three cellular phones illustrated in fig1 . ina cellular phone 10 illustrated in fig2 , an upper case 10 a and a lower case 10 b are connected to each other so as to be foldable via a hinge 10 c . the upper case 10 a is pressed to a user &# 39 ; s ear during talk and the lower case 10 b is held by the user &# 39 ; s hand . on the upper case 10 a , there provided a menu screen , an lcd panel 11 on which a photo image and the like is displayed , an internal speaker ( see fig3 ), an earpiece 12 to output a sound from the speaker . also , on a side of the upper case 10 a , a talk switch 13 is provided that is pressed at the time of talking to use a voice broadcasting function . on the lower case 10 b , there provided a selection button 15 used as a button to select various kinds of functions or used as a shutter button for photographing , a push button to enter phone numbers or the like , an internal microphone ( see fig3 ), and a mouthpiece 17 for sending a voice to the microphone . fig3 is an internal block diagram of the cellular phone of which appearance is illustrated in fig2 . fig3 illustrates a cpu 101 , a ram 102 , a microphone device 103 , a speaker device 104 , a camera device 105 , an infrared device 106 , a media controller 107 , a rom 108 , a non - volatile memory 109 , a display device 110 , a key device 111 , a clock 112 , a communications device 113 , and a gps device 114 . these elements are connected to one another via a bus 115 . the cpu 101 has a function to run various types of programs and controls the entire cellular phone 10 . the rom 108 stores the various types of programs and various kinds of constants necessary for the cpu 101 to run the various types of programs . the cpu 101 runs the programs stored in the rom 108 by using the ram 102 as a working area . the non - volatile memory 109 stores various kinds of information that may be possibly overwritten , like address book and received emails . the microphone device 103 is a microphone to pick up a voice of a user as well as a functional block to process the voice picked up by the microphone . the speaker device 104 is a speaker to output a voice to the user as well as a functional block to generate a voice signal for driving the speaker . the camera device 105 is a block to collect image data by photographing . the display device 110 is a block to display an image on the lcd panel 11 ( see fig3 ). the key device 111 is a block to detect various kinds of key operations by the user . the clock 112 is a block to obtain a current time . the infrared device 106 transmits an image and a telephone number to an external device located in a close range via infrared communications without going through a base station . the media controller 107 reads data from a mounted recording medium 107 a as well as writes image data or the like generated by the camera device 105 into the recording medium 107 a . further , the communications device 113 realizes a communications function such as talk or packet communications ( emailing and so on ). in addition , the gps device 114 detects geographical location of the cellular phone 10 based on a signal from a satellite . fig4 is an internal block diagram of a route supply server . this block diagram is of a general computer . the route supply server includes a computer and a program that is run in the computer and that causes the computer to perform processing illustrated in fig6 . the route supply server 20 illustrated in fig4 is equipped with a cpu 201 that runs various types of programs , a main memory 202 in which a program stored in a hard disk device 203 is read and expanded to be run by the cpu 201 , the hard disk device 203 that stores various types of programs and data , a cd / dvd drive 207 which accesses a cd - rom 210 or a dvd mounted therein , a communications interface 208 that is connected to communications line to communicate with the cellular phones 10 _a , 10 _b and 10 _c illustrated in fig1 , and an image display device 204 that displays various kinds of images . all the elements are connected to one another via a bus 209 . in the hard disk device 203 , a route map database is constructed . the route map database stores map information associated with latitude and longitude , and a route map including a railroad map such as trains and subways , station names , timetable at each station . fig5 is a schematic diagram illustrating an example of services to be performed by the route supply system that has been described with reference to fig1 to 4 . in fig5 , two train routes x , y are illustrated . these two train routes x , y cross each other at a station e , allowing users to change the line . a user a carrying one cellular phone plans to meet a user b carrying the other cellular phone . generally , the user a makes a call to the user b or exchanges email with the user b to talk about a meeting place and a meeting time . in this case , however , the meeting will take place to be described below . fig6 is a diagram illustrating communications sequence in the route search system illustrated in fig1 . it is assumed that the users a , b carry the cellular phone 10 _a , 10 _b , respectively , among the three cellular phones 10 _a , 10 _b and 10 _c . the cellular phones 10 _a and 10 _b are equipped with gps devices 114 _a and 114 _b , respectively ( see fig3 ). in the following , explanation is made about a case in which the user a carrying the cellular phone 10 _a requests searching of route . so the cellular phone 10 _a is called a request terminal 10 _a , and other terminal that is a target of the request is called other terminal 10 _b . additionally , in the route supply server 20 , a route map database 203 a is constructed in the hard disk device 203 ( see fig4 ). the user a carrying the request terminal 10 _a operates the request terminal 10 _a to specify the other terminal 10 _b , based on information such as the telephone number , and at the same time obtains positional information of the user a ( request terminal 10 _a ) by using the gps device 114 _a to transmit its positional information to the route supply server 20 . in this way , the user a requests the route supply server 20 to search a meeting point with the user b carrying the other terminal 10 _b and also a moving route to the meeting point ( step a ). upon receipt of the request , the route supply server 20 notifies the other terminal 10 _b of the request from the request terminal 10 _a and asks to transmit positional information of the other terminal 10 _b ( step b ). when the other terminal 10 _b transmits its positional information to the route supply server 20 in response to the request ( step c ), the route supply server 20 receives the positional information of the other terminal 10 _b and searches the route map database 203 a based on the positional information of the request terminal 10 _a and the other terminal 10 _b to determine a meeting point of the user a and the user b as well as moving routes to the meeting point for the users a and b , respectively ( step d ). in this case , a station where the user a and the user b can meet in a shortest time is searched for as the meeting point and moving routes to the station are determined for the respective users a and b . in the example illustrated in fig5 , the meeting point is station e . for the user a , a walking route from the current location of the user a to station c nearest from the current location , a train route from the station c to the station e , and estimated arrival time at the station e are obtained . for the user b , a walking route from the current location of the user b to station d nearest from the current location , a train route from the station d to the station e , and estimated arrival time at the station e are obtained . as a result of searching the route map database in the route supply server 20 , when the meeting point and the moving routes of the respective users a and b from the current locations to the meeting point are obtained , the request terminal 10 _a is notified of the meeting point and the moving route of the user a which are searched results ( step e 1 ), and the other terminal 10 _b is notified of the meeting point and the moving route of the user b ( step e 2 ). the request terminal 10 _a having received the notification displays contents of the notification ( step f 1 ), and similarly , the other terminal 10 _b having received the notification displays contents of the notification as well ( step f 2 ). fig7 is a flowchart of a route supply program run in the route supply server 20 . firstly , positional information of the request terminal 10 _a is received ( step s 01 ). the current location of the request terminal 10 _a is indicated by a latitude a 1 , a longitude a 2 . secondly , positional information of the other terminal 10 _b is received ( step s 02 ). the current location of the other terminal 10 _b is indicated by a latitude b 1 , a longitude b 2 . next , in the route map database , station c that is the nearest from the current location of the user a ( the request terminal 10 _a ) is searched for ( step s 03 ). in this case , to be more specific , the current location of the request terminal 10 _a ( latitude a 1 , longitude a 2 ) is compared with positional information of stations in the database , thereby a station having the nearest latitude and longitude is extracted . similarly , in the route map database , station d that is the nearest from the current location of the user b ( other terminal 10 _b ) is searched for ( step s 04 ). to be more specific , the current location of the other terminal 10 _b ( latitude b 1 , longitude b 2 ) is compared with positional information of stations in the database , thereby a station having the nearest latitude and longitude is extracted . thereafter , based on the positional information of the two stations c and d , and railroad information , station e that is located in between these two stations , c and d is found ( step s 05 ). a line name of the station e , a name of the station e , and a moving route to the station e , which have been found in this way are transmitted to the request terminal 10 _a and the other terminal 10 _b ( step s 06 ). in the above example , between the request terminal 10 _a and the other terminal 10 _b , a meeting point and moving routes are searched for and notified to these two cellular phones . however , a meeting point and moving routes may be searched for and notified to three and more cellular phones . additionally , although in the above description , railroad routes such as train and subway have been used , bus routes and bus stops may also be included . according to the route search system of the present invention , current positions of plural mobile terminals are obtained , a meeting point is determined for plural users carrying each of the mobile terminals , and the plural users are notified of the meeting point and routes to guide to the meeting point , respectively , thereby providing route guidance that utilizes positional information of the plural mobile terminals comprehensively . all examples and conditional language recited herein are intended for pedagogical purposes to aid the reader in understanding the invention and the concepts contributed by the inventor to furthering the art , and are to be construed as being without limitation to such specifically recited examples and conditions , nor does the organization of such examples in the specification relate to a showing of the superiority and inferiority of the invention . although the embodiments of the present invention have been described in detail , it should be understood that the various changes , substitutions , and alterations could be made hereto without departing from the spirit and scope of the invention . | 6 |
the embodiment will be specifically explained on the basis of the drawings below . fig1 illustrates an example of an entire constitution of a communication system of the embodiment . the communication system of the embodiment includes a management server 10 and a plurality of communication apparatuses 20 a , 20 b and so forth being nodes to be managed by the management server 10 which are coupled to one another through a communication network 5 such as the internet or a wan in such a way as to be enabled to communicate with one another . the management server 10 is a server which collects and manages asset data individually stored in the communication apparatuses 20 a , 20 b and so forth . the communication apparatuses 20 a , 20 b and so forth are various kinds of apparatuses equipped with communication functions such as a personal computer , a server , a mobile phone , a mobile data terminal , etc . asset data such as data related to specific hardware , data related to software or user data is stored individually in the communication apparatuses 20 a , 20 b and so forth . the communication network 5 is being layered . let the management server 10 be a node of a 0 - th layer , and connect the communication apparatuses 20 a and 20 b being nodes of a first layer to the management server 10 . the communication apparatuses 20 c , 20 d , . . . , 20 h being nodes of other layers are similarly placed in such a way that a node of an n - th layer ( n is an integer and is one or more ) is coupled to a node of an ( n − 1 )- th layer being its immediately upper node . the communication apparatuses 20 a , 20 b and so forth of the respective nodes each manage data of a period of time in which communication is enabled as described later , and reserve transmission of asset data for a period of time with an upper node including the management server 10 . if a reservation is made , the communication apparatuses of the respective nodes each transmit the asset data in the relevant period of time . the communication apparatuses 20 a , 20 b and so forth of the respective nodes of the embodiment each autonomously reserve transmission with an upper node and transmits the asset data in a period of time specified by the reservation for transmission so as to attempt load distribution on the communication network 5 . fig2 illustrates an example of a hardware constitution of the communication apparatus 20 a . the communication apparatus 20 a has a cpu 201 , a rom 202 , a ram 203 , a communication interface 204 , a hard disk drive 205 , an optical disk drive 206 , a keyboard 207 and a display monitor 208 . a computer program for controlling operations of the respective hardware portions is stored in the rom 202 . further , a computer program for implementing the communication method of the application is stored in a hard disk 205 d . the cpu 201 reads and runs the computer program stored in the rom 202 or the hard disk 205 d at the right time so as to control operations of the respective hardware portions described above and to make the communication apparatus 20 a work as the communication apparatus of the application . the cpu 201 is an example of a processor which executes a the computer program . the processor is a hardware to carry out operations based on at least one program ( such as the computer program ) and control other hardware , such as the cpu 201 , a gpu ( graphics processing unit ), fpu ( floating point number processing unit ) and dsp ( digital signal processor ). the ram 203 is a type of memory , e . g ., a dram ( dynamic ram ), an sram ( static ram ) or a flash memory , etc . various data generated when the cpu 201 runs the computer program ( e . g ., operation results or various kinds of parameters ) is temporarily stored in the ram 203 . the communication interface 204 communicates with other communication apparatuses 20 b , 20 c and so forth or the management server 10 through the communication network 5 . the hard disk drive 205 controls operations for writing and reading data to and from the hard disk 205 d , which is a type of memory . the hard disk drive 205 writes data accepted through the keyboard 207 , received by the communication interface 204 , read from an optical disk 206 d by the optical disk drive 206 and so forth to the hard disk 205 d , so as to store various data in the hard disk 205 d . the optical disk drive 206 controls operations for writing data to the optical disk 206 d and reading data recorded on the optical disk 206 d . incidentally , although it is supposed as to the embodiment that the computer program for implementing the communication method of the application is stored in the hard disk 205 d , the computer program may be stored in the optical disk 206 d and provided . the keyboard 207 accepts an operation and a character input , e . g ., done by a user of the communication apparatus 20 a . the display monitor 208 displays data that the user is notified of . if the communication apparatus 20 a may be remotely operated through the communication network 5 , the optical disk drive 206 , the keyboard 207 , the display monitor 208 and so forth may be omitted . the other communication apparatuses 20 b , 20 c and so forth and the management server 10 may each have a same hardware constitution as that of the communication apparatus 20 a , and have , e . g ., a cpu , a rom , a ram , a communication interface , a hard disk drive , etc . fig3 illustrates a functional constitution of the communication apparatus 20 a . the communication apparatus 20 a has a node data storing unit 21 , a connection end list managing unit 22 , a transmission reserving unit 23 , a request for reservation processing unit 24 , a transmitter 25 , a receiver 26 and an asset data storing unit 27 . for example , the cpu 201 runs the computer program stored in the rom 202 or the hard disk 205 d and controls the respective hardware portions illustrated in fig2 , so as to implement respective functions by means of the node data storing unit 21 , the connection end list managing unit 22 , the transmission reserving unit 23 and the request for reservation processing unit 24 . for example , the communication interface 204 is implemented functions of the transmitter 25 and the receiver 26 . for example , the ram 203 , the hard disk 205 d or optical disk 206 d implemented function of asset data storing unit 27 . node data is stored in the node data storing unit 21 for carrying out communication with an upper node coupled to the communication network 5 . fig4 illustrates an example of the node data . a row of a self - node address includes an address allotted to the self - node ( self - apparatus ) on the communication network 5 . a row of an upper node address includes an address allotted to an apparatus of an upper node coupled to the self - node on the communication network 5 . a row of a transmission deadline includes a deadline for transmission of the asset data of the self - node to the management server 10 , and is defined beforehand by an operation policy . a row of an expected arrival date and time includes a date and time when the asset data transmitted from the self - node arrives at the management server 10 . obtain data related to the expected arrival date and time that an apparatus of an upper node keeps from the upper node . incidentally , if no upper node to be coupled to is defined , a same date and time as the transmission deadline is set to the expected arrival date and time . a row of layer data includes data indicating on which layer the self - node relays transmitted data . identify the layer of the self - node from a layer of a node that the connection end list is obtained from . as the embodiment is constituted in such a way that the connection end list is obtained from an upper node , the layer of the self - node is n + 1 if the layer of the node that the connection end list is obtained from is n . a row of the number of nodes that may be relayed includes the number of nodes enabled to be relayed in a frame of a reservation . the node data storing unit 21 calculates the number of nodes that may be relayed by using a following method for calculation . the number of nodes that may be relayed in a frame of a reservation , n , is calculated by division of a schedule unit of a communication - enabled period of time ( a time length of a frame of a reservation : e . g ., ten minutes ) by a time length for transmission per one node ( e . g ., 5000 msec ). the time length of a frame of a reservation mentioned here is a preset time length . further , let a time length required for transmission last time , a last time transmission size and an average size of the asset data per one node be t , sa and sb , respectively , and the time length for transmission per one node is then calculated by t × sb / sa . as data of the time length required for transmission last time , t , or the last time transmission size sa cannot be obtained if there is no transmission record , the communication apparatus 20 a may be configured to make a transmission record beforehand . transmit a packet for survey use of a specific size to an upper node , e . g ., and detect a response data rate so that a time length required for transmission may be calculated with respect to the size of the transmitted packet . further , the average size of the asset data sb is an average of the sizes of the asset data attached to the connection end list . if the average size of the asset data sb cannot be obtained , a size of asset data of the self - node may be used instead . a row of the average size of the asset data per one node includes a value calculated by the management server 10 . as having collected the asset data that the communication apparatuses 20 a , 20 b and so forth each keep , the management server 10 may calculate the average size of the asset data per one node . the nodes which directly transmit the asset data to the management server 10 ( e . g ., the communication apparatuses 20 a and 20 b ) each obtain the data of the average size calculated by the management server 10 . further , the other nodes ( e . g ., the communication apparatuses 20 c , 20 d and so forth ) each obtain the data of the average size as included in the connection end list from the upper node . a row of communication - enabled periods of time data includes a period of time in which communication is enabled by means of the self - node . indicate periods of time in which communication is not enabled , communication is enabled , a reservation for receiving is accepted from a lower node and a reservation for transmission is made with an upper node as “ 0 ”, “ 1 ”, “ 2 ” and “ 3 ”, respectively , e . g ., and indicate condition in every period of time by using one of numerals “ 0 ” through “ 3 ”. let the period of time be ten minutes in length , and the communication - enabled periods of time for 24 hours may be indicated by a value of 144 digits . incidentally , suppose that a lower node reserves one node per one period of time ( per one frame ) as explained below . as the number of nodes that may be relayed is not limited to one , though , the lower node may reserve a plurality of nodes per one frame of a reservation depending upon management of conditions as to whether the respective nodes may each afford to receive asset data from more nodes . the node data storing unit 21 updates the communication - enabled periods of time data included in the node data if the self - node reserves transmission with another node or consents to a reservation for transmission requested by another node . the connection end list managing unit 22 makes a connection end list to be distributed to a lower node and obtains a connection end list distributed by an upper node . a connection end list includes data related to communication - enabled periods of time of an upper node , the self - node and a lower node . further , the connection end list includes a transmission deadline , an expected arrival date and time , the number of nodes that may be relayed and an average size of asset data transmitted by one node . the connection end list managing unit 22 merges node data included in a connection end list obtained from an upper node , node data of the self - node and node data of a lower node having reserved connection with the self - node , so as to make a new connection end list . remove a node placed higher than the lower node by three layers or more and not on a transmission and receiving path at this time . the connection end list having been made in this way includes node data on a transmission and receiving path from a node to which the list is distributed to the management server 10 . fig5 illustrates an example of making a connection end list . fig5 illustrates a list on which node data included in a connection end list obtained from an upper node , node data of the self - node and node data of a lower node having reserved connection with the self - node are merged . node data of an upper node illustrated in fig5 is included in a connection end list obtained from an upper node that the self - node is coupled to ( the node having an address of “ 12 . 345 . 67 . 92 ”). add data of the self - node and a coupled lower node to the data of the upper node so as to make a connection end list to be distributed to a lower node . remove a node not put on a transmission and receiving path and placed higher than the lower node by three layers or more at this time . nodes not put on the transmission and receiving path from the lower node to the management server 10 in fig5 are four nodes having addresses “ 12 . 345 . 67 . 93 ” and “ 12 . 345 . 67 . 95 ” on the third layer , “ 12 . 345 . 67 . 91 ” on the second layer and “ 12 . 345 . 67 . 88 ” on the first layer . a node placed three layers or more apart from the lower node is the one having the address “ 12 . 345 . 67 . 88 ” on the first layer , thus remove this node and make a connection end list . the transmission reserving unit 23 reserves transmission with an upper node so as to transmit the asset data of the self - node . the request for reservation processing unit 24 accepts a reservation for transmission requested by a lower node . further , the request for reservation processing unit 24 decides whether to consent to or turn down the request having been accepted , and notifies the node having requested the reservation of the decision . what is processed by the transmission reserving unit 23 and the request for reservation processing unit 24 will be described later in detail . the transmitter 25 transmits the asset data stored in the asset data storing unit 27 to an upper node that transmission is reserved with in accordance with the communication - enabled periods of time data included in the node data in the node data storing unit 21 . further , the receiver 26 receives asset data transmitted from a lower node , etc . the asset data of the lower node received by the receiver 26 is stored in the asset data storing unit 27 . the functional constitution of the communication apparatus 20 a has been explained with reference to fig3 . functional constitutions of the other communication apparatuses 20 b , 20 c and so forth are same as that of the communication apparatus 20 a . further , the management server 10 has functional portions including a node data storing unit , a connection end list managing unit , a request for reservation processing unit , a transmitter , a receiver and an asset data storing unit ( not illustrated ) similarly as the communication apparatus 20 a . incidentally , although receiving and processing a request for reservation for transmission from a lower node , the management server 10 does not reserve transmission with an upper node and thus may lack a functional constitution corresponding to the transmission reserving unit 23 of the communication apparatus 20 a . further , the node data and the connection end list may lack data related to an upper node . a method for reserving transmission of asset data with an upper node and a method for processing a reservation requested by a lower node will be explained below . in order to reserve transmission of asset data with an upper node , compare the communication - enabled periods of time data of the upper node included in the connection end list with the communication - enabled periods of time data of the self - node so as to reserve transmission . the communication - enabled periods of time data of the self - node may be made , e . g ., as follows . let a schedule unit of a period of time in which communication is enabled be ten minutes in length . sample load conditions ( e . g ., a cpu usage rate ) at ten - minute intervals as required , and add up the samples for the latest five days . let the cpu usage rate be zero percent in a period of time in which the self - node is powered off , suspended or put on standby , though . fig6 illustrates an exemplary added - up result . suppose that communication is enabled and not enabled if the cpu usage late for the latest five days is lower than ten percent and is not lower than ten percent , respectively . as average values of the cpu usage rate are lower than ten percent in periods of time 9 : 00 - 9 : 10 , 9 : 10 - 9 : 20 , 9 : 20 - 9 : 30 and 9 : 30 - 9 : 40 as illustrated in fig6 , e . g ., set those periods of time communication - enabled . meanwhile , as the cpu usage rates are not lower than ten percent in periods of time 9 : 40 - 9 : 50 and 9 : 50 - 10 : 00 , set those periods of time communication - disabled . fig7 a and 7b illustrate conditions of communication - enabled periods of time . fig7 a illustrates a table on which communication - enabled periods of time are defined from average values of the cpu usage rates in the respective periods of time . a communication - disabled period of time and a communication - enabled period of time are indicated by “ 0 ” and “ 1 ”, respectively . the node data storing unit 21 stores in itself data of the periods of time for 24 hours from 0 : 00 to 24 : 00 as a 144 - digit value ( see fig7 b ). incidentally , the data of the periods of time stored in the node data storing unit 21 is updated as required . upon consenting to a reservation requested by a lower node , update a digit of a relevant period of time to “ 2 ”. upon making a reservation with an upper node , update a digit of a relevant period of time to “ 3 ”. fig8 a and 8b illustrate diagrams for comparing exemplary periods of time data between the self - node and an upper node . periods of time from 11 : 00 to 12 : 40 are excerpted and illustrated in fig8 a and 8b . communication - enabled periods of time common to the self - node and the upper node are 11 : 30 - 11 : 40 and 11 : 50 - 12 : 00 as illustrated in fig8 a . reserve a transmission for transmitting the asset data in the period of time 11 : 50 - 12 : 00 which is closer to a period of time in which the upper node expects transmission ( 12 : 30 - 12 : 40 ). if transmission is reserved with the upper node , the self - node and the upper node each update the communication - enabled periods of time data . the self - node having reserved transmission with the upper node rewrites the data in the period of time 11 : 50 - 12 : 00 from “ 1 ” to “ 3 ” as illustrated in fig8 b . further , the upper node having accepted the reservation for transmission made by the lower node similarly rewrites the data in the period of time 11 : 50 - 12 : 00 from “ 1 ” to “ 2 ”. fig9 a and 9b illustrate diagrams for comparing exemplary periods of time data between the self - node and the management server 10 . the periods of time from 11 : 00 to 12 : 40 are excerpted and illustrated in fig9 a and 9b , as well . communication - enabled periods of time of the self - node are 11 : 30 - 11 : 40 , 11 : 50 - 12 : 00 and 12 : 00 - 12 : 10 as illustrated in fig9 a . meanwhile , the management server 10 has reserved transmission or is in communication - disabled condition in those periods of time . in this case , reserve transmission for the latest one of the communication - enabled periods of time of the self - node ( 12 : 00 - 12 : 10 ) in which the management server 10 has set itself communication - disabled , though . if transmission is reserved with the management server 10 , the self - node and the management server 10 each update the communication - enabled periods of time data . the self - node having reserved transmission with the management server 10 rewrites the data in the period of time 12 : 00 - 12 : 10 from “ 1 ” to “ 3 ” as illustrated in fig9 b . further , the management server 10 having accepted the reservation for transmission made by the lower node similarly rewrites the data in the period of time 12 : 00 - 12 : 10 from “ 0 ” to “ 2 ”. although it is supposed that one lower node makes a reservation per one period of time according to the embodiment , reservations may be accepted from a plurality of nodes per one period of time as described above . in this case , the nodes each may be configured to manage the number of reservations having been made and to choose a period of time of the smallest number of the reservations so as to reserve transmission . fig1 illustrates a procedure of processing for transmitting asset data . the transmission reserving unit 23 of the communication apparatus ( e . g ., communication apparatus 20 c ) reserves transmission of asset data with an upper node ( s 11 ). then , the transmitter 25 decides whether a period of time for which the reservation for transmission is made has come ( s 12 ). if not ( s 12 : no ), the transmitter 25 waits until the period of time for which the reservation for transmission is made comes . upon deciding that the period of time for which the reservation for transmission is made has come ( s 12 : yes ), the transmitter 25 reads the asset data from the asset data storing unit 27 and transmits the asset data to an upper node that the self - node is coupled to ( s 13 ). then , the node data storing unit 21 updates the communication - enabled periods of time data included in the node data ( s 14 ). then , the connection end list managing unit 22 obtains a latest connection end list from the upper node that the self - node is coupled to ( s 15 ), and chooses to which node the self - node is coupled from the obtained latest connection end list ( s 16 ). then , the connection end list managing unit 22 decides whether the node that the self - node is coupled to is changed ( s 17 ). if changed ( s 17 : yes ), the flow returns to the s 11 . unless changed ( s 17 : no ), the flow returns to the s 12 . then , a procedure for reserving transmission with an upper node which may transmit asset data to the management server 10 before the transmission deadline comes will be explained . a procedure of processing explained below is run as required before a node that the self - node is coupled to is chosen , upon the self - node being notified that the reservation for transmission made with the upper node is turned down , or immediately after the asset data is transmitted . fig1 illustrates an example of a procedure of processing for reserving transmission . before the transmission reserving unit 23 requests a reservation for transmission , the request for reservation processing unit 24 adjusts the number of reservations that the self - node relays . the request for reservation processing unit 24 calculates the number of nodes that the self - node may relay ( s 21 ). the number of nodes that may be relayed may be calculated by division of a schedule unit of a period of time in which communication is enabled ( a time length of a frame of a reservation : e . g ., ten minutes ) by a time length for transmission per one node ( e . g ., 5000 msec ) as described above . the request for reservation processing unit 24 decides whether the present number of reservations is above the number of nodes that may be relayed ( s 22 ). upon deciding that the present number of reservations is above the number of nodes that may be relayed ( s 22 : yes ), the request for reservation processing unit 24 notifies the lower node that the reservation is turned down and cancelled ( s 23 ). at this time , the request for reservation processing unit 24 adjusts the number of the nodes so that the present number of reservations is not above the number of nodes that may be relayed . incidentally , as the reservation for transmission of the self - node may be possibly updated in an earlier period of time , the request for reservation processing unit 24 notifies the lower nodes that the reservations are turned down in late order of periods of time for which the reservations are made . if the request for reservation processing unit 24 adjusts the number of the reservations , the node data storing unit 21 updates the communication - enabled periods of time data of the self - node included in the node data . if the request for reservation processing unit 24 decides that the present number of reservations is not above the number of nodes that may be relayed ( s 22 : no ) or notifies the lower nodes that the reservations are turned down at the s 23 , the transmission reserving unit 23 refers to the connection end list obtained from the upper node and the node data stored in the node data storing unit 21 so as to narrow down connection end candidates ( s 24 ). the transmission reserving unit 23 narrows down connection end candidates on the grounds , e . g ., ( a ) that the asset data may be transmitted before the preset transmission deadline comes , ( b ) that a communication - enabled period of time exists on the connection end , ( c ) that the number of nodes that may be received is above the number of nodes that may be relayed on the connection end , ( d ) that the asset data reaches the management server 10 at an earlier date and time than a connection end having been determined , and ( e ) that the node has never been chosen since a process for choosing an upper node starts . then , the transmission reserving unit 23 selects the upper node to be the connection end from the narrowed - down result ( s 25 ). if the result of narrowing down the connection end candidates is zero and the connection end has already been selected , the transmission reserving unit 23 runs a process following a s 26 . if no connection end has been selected , the transmission reserving unit 23 checks the transmission deadline of the asset data . before the transmission deadline comes , the transmission reserving unit 23 turns down one reservation requested by the lower node in late order of periods of time and returns to narrowing down the connection end candidates at the s 24 . if the transmission deadline has come , the transmission reserving unit 23 forcibly transmits the asset data to the management server 10 through the transmitter 25 . if a reservation has been requested by the lower node at this time , the request for reservation processing unit 24 notifies the lower node that the reservation is turned down and cancels itself from being a relay node . if the result of narrowing down the connection end candidates is one or more , the transmission reserving unit 23 chooses a node whose asset data reaches the management server 10 at the earliest date and time . if there is a plurality of nodes whose asset data reaches the management server 10 at the earliest date and time , a node of the minimum number of nodes that may be received or a node of the longest communication - enabled period of time may be chosen . then , the transmission reserving unit 23 decides whether the new selected connection end contributes to conditions ( s 26 ). if none of the conditions improves in a case where a connection with an upper node has already been reserved ( s 26 : no ), end the process according to the flowchart as the present reservation is kept and used . if the new selected connection end contributes to the conditions ( s 26 : yes ), e . g ., transmission may be reserved for an earlier period of time , a node of the minimum number of nodes that may be received may be chosen and so forth , the transmission reserving unit 23 requests a reservation for transmission from the upper node selected at the s 25 ( s 27 ). then , the receiver 26 receives a notification to accept or turn down the request for the reservation for transmission ( result of request ) and a new connection end list ( s 28 ). the node that the reservation has been requested from transmits the notification and the connection end list . the transmission reserving unit 23 decides whether the notification received by the receiver 26 is to consent to the request or not ( s 29 ). if the notification is not to consent to the request ( notification to turn down the request ) ( s 29 : no ), the process returns to the s 24 . upon receiving a notification to consent to the request for a reservation for transmission ( s 29 : yes ), the node data storing unit 21 updates the communication - enabled periods of time data included in the node data of the self - node ( s 30 ). fig1 illustrates an example of a procedure of processing in a case where a request for a reservation for transmission is received from a lower node . if a request for a reservation for transmission is received from a lower node , the request for reservation processing unit 24 obtains node data of the node having been requested the reservation ( s 41 ). the request for reservation processing unit 24 compares communication - enabled periods of time data included in the obtained node data of the node having been requested the reservation with the communication - enabled periods of time data included in the node data of the self - node ( s 42 ), and decides whether the request for the reservation is consented to ( s 43 ). if the request for the reservation is consented to ( s 43 : yes ), the node data storing unit 21 updates the communication - enabled periods of time data included in the node data of the self - node ( s 44 ). further , the connection end list managing unit 22 makes a new connection end list to be distributed to the node having been requested the reservation ( lower node ) ( s 45 ). the connection end list managing unit 22 merges the node data included in the connection end list obtained from the upper node , the node data of the self - node and the node data of the lower node having reserved a connection with the self - node so as to make the connection end list ( s 45 ). the connection end list managing unit 22 distributes a new connection end list to the node having requested the reservation if the request for the reservation is turned down ( s 43 : no ), as well . thus , the connection end list managing unit 22 makes a connection end list to be distributed similarly as in the case where the request for the reservation is consented to ( s 45 ). then , the request for reservation processing unit 24 notifies the lower node that the request is consented to or turned down ( result of request ), and transmits the new connection end list having been made ( s 46 ). then , a procedure for deciding whether there is a reservation slot being in time for the transmission deadline from node data of both ends of a connection so as to select a reservation slot for communication will be explained . the procedure for processing explained below will be run after a connection end candidate for next time is selected from the connection end list , or in order to decide whether a request having been made from a lower node for a reservation for transmission is consented to or not . fig1 illustrates an example of a procedure for selecting a reservation for connection . the request for reservation processing unit 24 obtains a transmission deadline of asset data from node data of a connection root ( s 51 ), and obtains a date and time when transmission to an upper node is expected from node data of a connection end ( s 52 ). then , the request for reservation processing unit 24 decides whether the transmission deadline of the asset data is set earlier than the transmission - expected date and time of the connection end ( s 53 ). if the transmission deadline of the asset data is set later than the transmission - expected date and time of the connection end ( s 53 : no ), the request for reservation processing unit 24 decides that there is no reservation slot as the asset data may possibly fail to reach the management server 10 before the deadline even if the connection end is used as a relay node ( s 54 ). if the transmission deadline of the asset data is set earlier than the transmission - expected date and time of the connection end ( s 53 : yes ), the request for reservation processing unit 24 searches the periods of time being earlier than those for which the connection end has reserved connection and communication - enabled on the connection root from the final ( latest ) one in upstream order ( s 55 ). a period of time having been searched is excluded , though . then , the request for reservation processing unit 24 decides whether a communication - enabled period of time is obtained at the s 55 ( s 56 ). if a communication - enabled period of time is obtained ( s 56 : yes ), the request for reservation processing unit 24 obtains a status of the connection end in the obtained period of time ( s 57 ). the request for reservation processing unit 24 decides whether the obtained status represents being communication - enabled ( s 58 ). if the status represents being communication - enabled ( s 58 : yes ), the request for reservation processing unit 24 selects the period of time as a reservation slot ( s 59 ). upon deciding that the obtained status does not represent being communication - enabled ( s 58 : no ), the request for reservation processing unit 24 makes the process go back to the s 55 . further , upon deciding that no communication - enabled period of time is obtained ( s 56 : no ), the request for reservation processing unit 24 searches communication - enabled periods of time on the connection end from the final ( latest ) one in upstream order ( s 60 ). then , the request for reservation processing unit 24 decides whether a communication - enabled period of time is obtained ( s 61 ). if a communication - enabled period of time is obtained ( s 61 : yes ), the request for reservation processing unit 24 selects the period of time as a reservation slot ( s 62 ). upon deciding that no communication - enabled period of time is obtained ( s 61 : no ), the request for reservation processing unit 24 decides that there is no reservation slot ( s 54 ). the respective communication apparatuses 20 a , 20 b and so forth each make a reservation for transmission with an upper node according to the processing procedure described above , so that a transmission path on which asset data may reach the management server 10 before the deadline may be built . fig1 illustrates a transmission path from the self - node to the management server 10 . periods of time from 11 : 00 to 12 : 40 are excerpted and illustrated in fig1 . let the deadline for the asset data reaching the management server 10 be 12 : 40 in fig1 . an upper node on the third layer that the self - node is coupled to ( upper 3 ) has reserved transmission with an upper node on the second layer ( upper 2 ) for a period of time 11 : 30 - 11 : 40 . the upper node on the second layer has reserved transmission with an upper node on the first layer ( upper 1 ) for a period of time 12 : 20 - 12 : 30 . thus , if the self - node reserves transmission with the upper node on the third layer for a period of time before 11 : 30 , the asset data will reach the management server 10 before the deadline . see the periods of time data illustrated in fig1 here . as the period of time 11 : 20 - 11 : 30 is communication - enabled for both the self - node and the upper node on the third layer , the self - node reserves transmission for this period of time . the asset data that the self - node transmits in the period of time for which transmission is reserved reaches the management server 10 via the upper node on the third layer , the upper node on the second layer and the upper node on the first layer . as the number of reservations for each of the periods of time is limited according to the embodiment ( e . g ., limited to one node ), connections to a certain node never concentrate on a particular period of time , and the load may be suitably distributed . according to the embodiment described above , a path on which data is transmitted and a period of time in which data is transmitted may be set in accordance with load conditions of the management server 10 and the respective communication apparatuses 20 a , 20 b and so forth and the deadline for data to be transmitted ( asset data ) reaching a destination . further , even if one node cannot relay asset data because of a failure or a pause , another node may relay the asset data instead , so as to reduce risks of failing to collect the asset data because of a failure , etc . further , cases where the asset data of the respective devices does not reach the management server before the deadline may be made occur less frequently . all examples and conditional language recited herein are intended for pedagogical purposes to aid the reader in understanding the invention and the concepts contributed by the inventor to furthering the art , and are to be construed as being without limitation to such specifically recited examples and conditions , nor does the organization of such examples in the specification relate to a showing of the superiority and inferiority of the invention . although the embodiment of the present invention has been described in detail , it should be understood that the various changes , substitutions , and alterations could be made hereto without departing from the spirit and scope of the invention . | 7 |
an exploded view of the invention is shown in fig1 . a display 5 has a first sheet 10 with a first substrate 12 which can be a clear transparent material such as kodak estar film base formed of polyester plastic and has a thickness of between 20 and 200 microns . in the exemplary embodiment , the first substrate is a 80 micron thick sheet of polyester film base . other clear polymers , such as polycarbonate can also be used . first substrate 12 has a first surface 12a that supports a light sensitive , metal forming layer 14 . in the preferred embodiment , the light sensitive , metal forming layer 14 is an emulsion of silver halide grains in gelatin . alternatively , other light sensitive , metal forming materials can be used such as gold or copper salts . in the case of silver halide emulsions , high concentrations of silver halide salts in gelatin are used to improve conductivity over conventional imaging emulsions . conductive additives such as fine indium - tin - oxide or fine silver with diameter between 0 . 5 and 2 . 0 microns are added to emulsion to improve conductivity of photographically produced metallic silver . the second surface of first substrate 12b supports a color filter array 40 . color filter array 40 can be a single layer printed on first substrate 12 before first light sensitive layer 14 is applied to first substrate 12 . alternatively , color filter array 40 can be three layers of silver halide , color dye forming chemistry , each layer forming a separate color of color filter array 40 . an example of such a multilayered array can be found in u . s . pat . no . 5 , 462 , 822 . that invention sputters a transparent electrically conductive coating of indium - tin - oxide ( ito ) under high temperature over the color filter array . in this invention , the conductive layer is metallic traces disposed on the a side of first substrate 12 opposite from color filter array 40 . in the case of a multilayered , light sensitized dye - forming cfa , a red filter layer 50 is a silver halide emulsion layer that has been exposed and developed to create red filter dyed areas 52 and red filter undyed areas 54 . a second green filter layer 60 is a silver halide emulsion layer that has been exposed and developed to form green filter dye areas 62 and green filter undyed areas 64 . a blue filter layer 70 is a silver halide emulsion that has been exposed and developed to form blue filter dyed areas 72 and blue filter undyed areas 74 . the exposure and development of a multilayered color filter array can be done before application of first light sensitive conductive layer 14 . the exposure mask that forms traces in first light sensitive layer 14 is aligned to color filter array 40 to align horizontal traces 16 to color filter array 40 . in a different embodiment , both color filter array 40 and first light sensitive layer 14 are coated simultaneously . an additional layer of light absorbing material 75 is coated on one or both sides 12a and 12b of first substrate 12 . light absorbing material 75 can be formulations well known in the art that provide anti - halation layers on silver halide films . light absorbing material 75 permit independent exposure of the layers on the two surfaces of first substrate 12 . light absorbing material 75 is soluble in the solutions used to develop the light sensitive layers so that substrate 12 is optically transmitting after the sheet has been processed . a second sheet , 20 has a second clear substrate 22 formed of a clear polymer with properties similar to first substrate 12 . a second light sensitive layer 24 is applied on a surface of second substrate 22 . light sensitive layer 24 is similar in nature to first light sensitive layer 14 . light sensitive layer 24 is exposed through a mask to form non - conducting areas 26 and conducting areas 28 . first sheet 10 and second sheet 20 are oriented so that conductive traces 14 and 28 are aligned . a light modulating material layer 30 is disposed between the first sheet 10 and second sheet 20 and the two sheets are pressed against light modulating material layer 30 . light modulating material layer 30 can be a liquid crystal 32 of conventional design and contain spacer beads 34 that provide a calibrated distance between first sheet 10 and second sheet 20 . in another embodiment , a liquid crystal material is homogenized in a polymeric binder such as gelatin . the gelatin emulsion is applied to one of the two sheets and the other sheet is pressed against the polymer dispersed liquid crystal ( pdlc ). upon drying , the gelatin acts as a binder to hold the two sheets together . other light - modulating , electrically operated materials can also be applied between the two sheets such as a ferroelectric ( flc ) material . a completed display 5 , is shown in fig3 . for sake of clarity , it is assumed that the light modulating material has been driven to a transparent state . vertical traces 28 in second sheet 20 are on the top layer . light modulating material layer 30 is transparent in the drawing . horizontal traces 16 are formed in first light sensitive layer 14 . red filter dye area 52 , green filter dye area 62 and blue filter dye area 72 are formed into pixels 80 to create color filter array 40 . in this preferred embodiment , display 5 is designed to display images according to video standard smpte 274m . horizontal traces consist of 1080 traces that are 100 microns wide with 400 micron gaps between lines . there are 1920 vertical traces 28 which are 100 microns wide with 400 micron gaps between lines . clear aperture is 400 microns square in a 500 square micron pixel . fig4 and fig5 detail a conductive structure that is formed within each pixel 80 . horizontal traces 16 and vertical traces 28 are opaque and frame each pixel in this embodiment . a clear aperture 82 acts as the light modulating area for each pixel . horizontal traces 16 have a vertical filament grid 84 across clear aperture 82 . vertical filament grid 84 can be composed of two sets of filaments 5 microns wide and pitched 15 microns apart that are orthogonal to each other and pitched a 45 degree angle . horizontal filament grid 86 are similar in structure to vertical filament grid 84 and run horizontally from each vertical trace 28 . the intersection of two sets of filaments across a clear aperture spread electrical charge from traces 16 and 28 across clear aperture 82 . stated differently , the vertical and horizontal first and second conductive traces are aligned so that when a potential is applied between them , a field is produced which operates upon the light modulating material layer 30 to selectively transmit light which passes through the second transparent substrate 22 , the light modulating layer 30 , the second transparent substrate 12 , and the color filter array 40 so that a displayed image is produced . in an alternative embodiment , the pixel is defined as the four quadrants around the intersection of the traces as shown in fig3 . filament grids 84 and 86 are disposed into each of the four quadrants . this alternative structure has the advantage that an electrical field is stretched less than half way across clear aperture 82 . this reduces field loss across grids 84 and 86 by reducing the distance that the filament grids 84 and 86 spread charge . the areas between filament grids 84 and 86 can be exposed to a level of radiation that causes limited metallic silver to be deposited in the clear areas between the filaments . alternatively , non - photosensitive , electrically conductive particles such as fine indium - tin oxide between 0 . 5 and 2 . 0 microns in diameter can be incorporated in layers 14 and 24 to spread the electrical field across openings between the filaments . in another embodiment , indium - tin oxide is sputter coated on substrates 12 and 22 before light sensitive layers are applied to either surface . in the pre - sputtered embodiment , the ito material acts to spread charge on the filaments across opening between filaments . some light striking each pixel is blocked by the opacity of the traces 16 and 28 and filament grids 84 and 86 , and the remainder is controlled by the electrically field between processed first light sensitive layer 14 and processed second light sensitive layer 24 . fig6 is a schematic representation of how conductive traces are formed in light sensitive layers 14 and 24 in accordance with a modification to u . s . pat . no . 3 , 033 , 765 and u . s . pat . no . 3 , 464 , 822 . in fig6 a , photo - mask 90 selectively blocks a source of light that strikes and activates exposed silver halide 94 while unexposed silver halide 92 remains inactivated . in the preferred embodiment , unexposed silver halide 92 is the light sensitive material . in fig6 b , display 5 has been photographically developed to convert exposed silver halide 94 to metallic silver 96 . in fig6 c , a conventional photographic fixing step has removed unexposed silver halide 92 . in fig6 d , the metallic silver 96 has been rehaliginated by a bleach to form re - halogenated silver 98 . in fig6 e , rehalogenated silver 98 has been redeveloped to form redeveloped silver 100 . metallic salts in the developer deposits additional metal 102 to improve conductivity . in an alternative process , the silver metal particles in gelatin are subjected to a first plating bath to deposit palladium metal onto the silver grains . a final plating bath of copper salts adds additional conductor to improve the conductivity of the traces . electrical connection to display 5 is shown in fig7 a and 7b . horizontal traces 16 and vertical traces 28 terminate in a staggered pattern of conductive pads 114 . pins 110 having a piercing point 112 and are disposed in a rigid non - conductive substrate . the pins arc pressed into display 5 so that piercing point 112 is driven through the pads 114 at the end of each trace . the piercing action provides electrical interconnect for traces 16 and 18 of display 5 . alternatively , areas of sheets 10 and 20 outside of the intersection of traces 16 and 28 do not overlap each other . the non overlapping areas are connected to drive electronics using conventional interconnect techniques , such as conductive bumps or wire bonding between traces 16 and 28 and drive electronics . 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 . ______________________________________ 5 display10 first sheet12 first substrate 12a first substrate first surface 12b first substrate second surface14 first light sensitive , metal forming layer16 horizontal traces20 second sheet22 second substrate24 second light sensitive layer26 second sheet non - conducting areas28 second sheet conducting areas ( vertical traces ) 30 light modulating layer32 liquid crystal34 spacer beads40 color filter array50 red filter layer52 red filter dye area54 red filter undyed area , 60 green filter , layer62 green filter dye area64 green filter undyed area70 blue filter layer72 blue filter dyed area74 blue filter undyed area75 light absorbing material80 pixel82 clear aperture84 vertical filament grid86 horizontal filament grid90 photo - mask92 unexposed silver halide94 exposed silver halide96 developed metallic silver98 re - halogenated silver100 redeveloped silver102 additional metal110 pins112 piercing point114 pads______________________________________ | 6 |
pioneer brand hybrid 3082 is a single cross , yellow endosperm , flint - dent maize hybrid which is high yielding with good test weight and good roots . hybrid 3092 also demonstrates good husk cover and good stalks . this unique hybrid combines low kernel row number and a small cob with exceptional grain yield and good test weight . grain from hybrid 3082 tends to be a yellow - orange color . hybrid 3082 has above average resistance to northern leaf blight and southern leaf blight . hybrid 3082 is approximately 124 relative maturity based on the comparative relative maturity rating system for harvest moisture of grain . this hybrid has the following characteristics based on the data collected primarily at johnston , iowa . table 1__________________________________________________________________________variety description informationvariety = 3082__________________________________________________________________________ 1 . type : ( describe intermediate types in comments section ): 4 1 = sweet 2 = dent 3 = dent - like 4 = flint dent 5 = flint - like 6 = flint 7 = flour 8 = pop 9 = ornamental 2 . maturity : heatdays units69 1 , 471 from emergence to 50 % of plants in silk70 1 , 499 from emergence to 50 % of plants in pollen6 138 from 10 % to 90 % pollen shed68 1 , 381 from 50 % silk to harvest at 25 % moisture standard sample 3 . plant : deviation size303 . 0 cm plant height ( to tassel tip ) 24 . 04 2147 . 0 cm ear height ( to base of top ear node ) 12 . 73 216 . 1 cm length of top ear internode 2 . 97 102 average number of tillers 0 . 71 21 . 0 average number of ears per stalk 0 . 00 21 . 0 anthocyanin of brace roots : 1 = absent 2 = faint 3 = moderate 4 = dark standard sample 4 . leaf : deviation size10 . 5 cm width of ear node leaf 0 . 99 1086 . 3 cm length of ear node leaf 3 . 25 107 . 7 cm number of leaves above top ear 0 . 42 1021 . 0 degrees leaf angle ( measure from 2nd leaf 2 . 83 2 above ear at anthesis to stalk above leaf ) 3 leaf color dark green ( munsell code ) 7 . 5gy341 . 5 leaf sheath pubescence ( rate on scale from 1 = none to 9 = like peach fuzz ) 7 . 0 marginal waves ( rate on scale from 1 = none to 9 = many ) 5 . 5 longitudinal creases ( rate on scale from 1 = none to 9 = many ) standard sample 5 . tassel : deviation size8 . 1 number of primary lateral branches 1 . 27 1080 . 0 branch angle from central spike 0 . 00 27 . 5 pollen shed ( rate on scale from 0 = male sterile to 9 = heavy shed ) 7 anther yellow ( munsell code ) 2 . 5yr461 glume color light green ( munsell code ) 7 . 5gy582 . 0 bar glumes ( glume bands ): 1 = absent 2 = present 6a . ear ( unhusked data ): 9 silk color ( 3 days after emergence ) salmon ( munsell code ) 10rp461 fresh husk color ( 25 days after 50 % silking ) light green ( munsell code ) 5gy5621 dry husk color ( 65 days after 50 % silking ) buff ( munsell code ) 2 . 5y841 position of ear at dry husk stage : 1 = upright 2 = horizontal 3 = pendent upright6 . 5 husk tightness ( rate of scale from 1 = very loose to 9 = very tight ) 2 husk extension ( at harvest ): 1 = short ( ears exposed ) 2 = medium (& lt ; 8 cm ) medium 3 = long ( 8 - 10 cm beyond ear tip ) 4 = very long (& gt ; 10 cm ) standard sample 6b . ear ( husked ear data ): deviation size21 . 2 cm ear length 1 . 6970 1045 . 6 mm ear diameter at mid - point 2 . 2627 10211 . gm ear weight 40 . 870 1015 . 6 number of kernel rows 1 . 1313 102 kernel rows : 1 = indistinct 2 = distinct distinct1 row alignment : 1 = straight 2 = slightly curved 3 straight12 . 2 cm shank length 1 . 9798 102 ear taper : 1 = slight 2 = average 3 = extreme average standard sample 7 . kernel ( dried ): deviation size12 . 6 mm kernel length 0 . 5656 108 mm kernel width 0 . 2828 104 . 8 mm kernel thickness 0 . 5656 1012 . 6 % round kernels ( shape grade ) 2 . 9407 21 aleurone color pattern : 1 = homozygous 2 = segregating homozygous8 aluerone color yellow - orange ( munsell code ) 5yr71410 hard endosperm color pink - orange ( munsell code ) 7 . 5yr6143 endosperm type : normal starch 1 = sweet ( su1 ) 2 = extra sweet ( sh2 ) 3 = normal starch 4 = high amylose starch 5 = waxy starch 6 = high protein 7 = high lysine 8 = super sweet ( se ) 9 = high oil 10 = other33 gm weight per 100 kernels ( unsized sample ) 2 . 8284 2 standard sample 8 . cob : deviation size22 . 5 mm cob diameter at mid - point 2 . 1213 1014 cob color red ( munsell code ) 10r5121 cob strength 1 = weak 2 = strong 9 . disease resistance ( rate from 1 ( most susceptible ) to 9 ( most resistant ); leave blank if not tested ; leave race or strain options blank if polygenic ): a . leaf blights , wilts , and local infection diseases anthracnose leaf blight ( colletotrichum graminicola ) common rust ( puccinia sorghi ) common smut ( ustilago maydis ) eyespot ( kabatiella zeae ) 8 goss &# 39 ; s wilt ( clavibacter michiganense spp . nebraskense ) 4 gray leaf spot ( cercospora zeae - maydis ) helminthosporium leaf spot ( bipolaris zeicola ) 6 northern leaf blight ( exserohilum turcicum ) 7 southern leaf blight ( bipolaris maydis ) 4 . 5 southern rust ( puccinia polysora ) 4 stewart &# 39 ; s wilt ( erwinia stewartii ) other ( specify ) b . systemic diseases 2 corn lethal necrosis ( mcmv and mdmv ) head smut ( sphacelotheca reiliana ) maize chlorotic dwarf virus ( mdv ) maize chlorotic mottle virus ( mcmv ) 3 maize dwarf mosaic virus ( mdmv ) sorghum downy mildew of corn ( peronosclerospora sorghi ) other ( specify ) c . stalk rots 3 anthracnose stalk rot ( colletotrichum graminicola ) diplodia stalk rot ( stenocarpella maydis ) fusarium stalk rot ( fusarium moniliforme ) gibberella stalk rot ( gibberella zeae ) other ( specify ) d . ear and kernel rots aspergillus ear and kernel rot ( aspergillus flavus ) diplodia ear rot ( stenocarpella maydis ) 6 fusarium ear and kernel rot ( fusarium moniliforme ) gibberella ear rot ( gibberella zeae ) other ( specify ) 10 . insect resistance ( rate from 1 ( most susceptible ) to 9 ( most resistant ); ( leave blank if not tested ): banks grass mite ( oligonychus pratensis ) corn worm ( helicoverpa zea ) leaf feeding silk feeding mg larval wt . ear damage corn leaf aphid ( rhopalosiphum maidis ) corn sap beetle ( carpophilus dimidiatus ) european corn borer ( ostrinia nubilalis ) 4 . 8 1st generation ( typically whorl leaf feeding ) 7 . 1 2nd generation ( typically leaf sheath collar feeding ) stalk tunneling cm tunneled / plant fall armyworm ( spodoptera fruqiperda ) leaf feeding silk feeding mg larval wt . maize weevil ( sitophilus zeamaize ) northern rootworm ( diabrotica barberi ) southern rootworm ( diabrotica undecimpunctata ) southwestern corn borer ( diatreaea grandiosella ) leaf feeding stalk tunneling cm tunneled / plant two - spotted spider mite ( tetranychus urticae ) western rootworm ( diabrotica virgifrea virgifera ) other ( specify ) agronomic traits : 6 staygreen ( at 65 days after anthesis ) ( rate on a scale from 1 = worst to excellent ) 0 . 7 % dropped ears ( at 65 days after anthesis ) % pre - anthesis brittle snapping % pre - anthesis root lodging 5 . 8 post - anthesis root lodging ( at 65 days after anthesis ) 10 , 940 kg / ha yield ( at 12 - 13 % grain moisture ) __________________________________________________________________________ comparisons of characteristics for pioneer brand hybrid 3082 were made against pioneer brand hybrids 3140 , 3163 and 3167 . table 2a compares pioneer hybrid 3082 and pioneer hybrid 3140 . the results show that hybrid 3082 is significantly higher yielding than hybrid 3140 . both hybrids demonstrate good resistance to root lodging , stalk lodging , northern leaf blight and southern leaf blight . hybrid 3082 demonstrates better seedling vigor , better early stand count , better staygreen and better resistance to second generation european corn borer than hybrid 3140 . table 2b compares pioneer hybrid 3082 and pioneer hybrid 3163 . the results show that hybrid 3082 is significantly higher yielding than hybrid 3163 and that both hybrids demonstrate good resistance to northern leaf blight , southern leaf blight , root lodging and stalk lodging . hybrid 3082 demonstrates significantly better staygreen , better grain appearance , better resistance to fusarium ear rot and better resistance to second generation european corn borer than hybrid 3163 . table 2c compares pioneer hybrid 3082 to pioneer hybrid 3167 . the results show that hybrid 3082 is significantly higher yielding than hybrid 3167 and that both hybrids demonstrate above average staygreen and above average resistance to root lodging . both hybrids also demonstrate good resistance to northern leaf blight and southern leaf blight . hybrid 3082 demonstrates better resistance to stalk lodging and better resistance to second generation european corn borer than hybrid 3167 . hybrid 3082 also demonstrates significantly better seedling vigor than hybrid 3167 . table 2a__________________________________________________________________________variety # 1 = 3082variety # 2 = 3140__________________________________________________________________________ prm bu bu tst sdg est gdu prm shd acr acr mst wt vgr cnt shd abs abs abs % mn % mn abs % mn % mn % mn__________________________________________________________________________total sum 1 128 121 176 . 6 116 121 56 . 2 105 107 105 2 119 118 149 . 9 98 101 55 . 6 89 101 102 locs 5 4 56 56 56 6 17 13 4 reps 5 4 67 67 67 9 24 16 4 diff 10 3 26 . 7 17 20 0 . 6 16 5 2 pr & gt ; t . 000 # . 156 . 000 # . 000 # . 000 # . 446 . 011 + . 077 * . 066 * __________________________________________________________________________ gdu stk plt ear rt sta stk brt glf slk cnt ht ht ldg grn ldg stk spt % mn % mn % mn % mn % mn % mn % mn % mn abs__________________________________________________________________________total sum 1 104 104 103 107 107 130 105 103 4 . 0 2 103 100 101 105 105 114 102 103 5 . 4 locs 2 66 12 13 20 19 29 1 7 reps 2 84 16 17 22 27 32 3 11 diff 1 4 2 2 2 16 3 0 1 . 4 pr & gt ; t . 180 . 004 # . 034 + . 178 . 534 . 085 * . 638 . 018 + __________________________________________________________________________ nlf slf gos stw ant hd mdm fus blt blt wlt wlt rot smt cln cpx ers abs abs abs abs abs abs abs abs abs__________________________________________________________________________total sum 1 5 . 8 6 . 9 7 . 5 3 . 5 3 . 4 100 . 0 2 . 0 3 . 0 6 . 4 2 6 . 7 6 . 1 8 . 0 3 . 5 4 . 9 100 . 0 3 . 0 3 . 0 5 . 7 locs 3 4 1 1 4 1 1 1 5 reps 6 7 2 2 8 2 2 3 7 diff 0 . 8 0 . 8 0 . 5 0 . 0 1 . 5 0 . 0 1 . 0 0 . 0 0 . 7 pr & gt ; t . 199 . 432 . 046 + . 296__________________________________________________________________________ com sou ecb ecb rst rst 1lf 2sc abs abs abs abs__________________________________________________________________________ total sum 1 4 . 5 4 . 5 4 . 8 8 . 5 2 6 . 5 7 . 0 4 . 0 4 . 5 locs 2 2 2 1 reps 3 4 4 2 diff 2 . 0 2 . 5 0 . 8 4 . 0 pr & gt ; t . 000 # . 000 # . 795__________________________________________________________________________ * = 10 % sig + = 5 % sig # = 1 % sig table 2b__________________________________________________________________________variety # 1 = 3082variety # 2 = 3163__________________________________________________________________________ prm bu bu tst sdg est gdu prm shd acr acr mst wt vgr cnt shd abs abs abs % mn % mn abs % mn % mn % mn__________________________________________________________________________total sum 1 126 120 168 . 0 112 116 56 . 8 110 104 103 2 118 117 159 . 1 105 98 56 . 9 96 104 101 locs 35 12 280 280 287 25 92 42 15 reps 35 12 302 302 309 28 101 44 15 diff 8 3 8 . 9 6 18 0 . 0 14 0 3 pr & gt ; t . 000 # . 000 # . 000 # . 000 # . 000 # . 999 . 000 # . 999 . 000 # __________________________________________________________________________ gdu stk plt ear rt sta stk brt grn slk cnt ht ht ldg grn ldg stk app % mn % mn % mn % mn % mn % mn % mn % mn % mn__________________________________________________________________________total sum 1 105 102 102 105 105 121 102 84 106 2 101 100 99 99 103 108 103 82 97 locs 6 325 72 75 60 141 130 7 6 reps 6 356 83 86 61 161 136 9 6 diff 3 1 3 6 2 13 2 3 8 pr & gt ; t . 007 # . 001 # . 000 # . 000 # . 539 . 000 # . 277 . 755 . 025 + __________________________________________________________________________ drp glf nlf slf gos stw ant hd ear spt blt blt wlt wlt rot smt cln % mn abs abs abs abs abs abs abs abs__________________________________________________________________________total sum 1 99 4 . 0 5 . 9 6 . 6 7 . 5 3 . 5 3 . 4 100 . 0 2 . 0 2 100 4 . 9 6 . 2 6 . 3 7 . 5 4 . 5 3 . 3 100 . 0 4 . 0 locs 10 7 4 9 1 1 4 1 1 reps 10 11 9 12 2 2 8 2 2 diff 1 0 . 9 0 . 3 0 . 3 0 . 0 1 . 0 0 . 1 0 . 0 2 . 0 pr & gt ; t . 511 . 045 + . 252 . 506 . 836__________________________________________________________________________ mdm fus com sou ecb ecb cpx ers rst rst 1lf 2sc abs abs abs abs abs abs__________________________________________________________________________ total sum 1 2 . 8 6 . 6 5 . 1 4 . 5 4 . 8 8 . 5 2 3 . 0 4 . 7 5 . 9 3 . 5 4 . 0 6 . 5 locs 2 9 15 1 2 1 reps 6 11 16 2 4 2 diff 0 . 3 1 . 8 0 . 7 1 . 0 0 . 8 2 . 0 pr & gt ; t . 500 . 001 # . 000 # . 742__________________________________________________________________________ * = 10 % sig + = 5 % sig # = 1 % sig table 2c__________________________________________________________________________variety # 1 = 3082variety # 2 = 3167__________________________________________________________________________ prm bu bu tst sdg est gdu prm shd acr acr mst wt vgr cnt shd abs abs abs % mn % mn abs % mn % mn % mn__________________________________________________________________________total sum 1 126 120 170 . 9 111 116 58 . 4 109 103 103 2 123 120 152 . 2 99 109 58 . 0 82 101 103 locs 36 9 288 288 292 10 104 59 10 reps 36 9 309 309 313 10 109 62 10 diff 3 0 18 . 7 12 7 0 . 4 27 2 0 pr & gt ; t . 000 # . 999 . 000 # . 000 # . 000 # . 633 . 000 # . 035 + . 999__________________________________________________________________________ gdu stk plt ear rt sta stk brt grn slk cnt ht ht ldg grn ldg stk app % mn % mn % mn % mn % mn % mn % mn % mn % mn__________________________________________________________________________total sum 1 103 102 101 104 106 124 103 94 105 2 105 99 96 97 103 130 100 104 114 locs 2 328 82 83 69 132 140 4 3 reps 2 356 95 96 72 150 144 6 3 diff 2 3 6 7 3 6 2 10 9 pr & gt ; t . 055 * . 000 # . 000 # . 000 # . 400 . 056 * . 052 * . 446 . 184__________________________________________________________________________ drp glf nlf slf gos stw ant hd ear spt blt blt wlt wlt rot smt cln % mn abs abs abs abs abs abs abs abs__________________________________________________________________________total sum 1 100 3 . 6 5 . 8 6 . 6 7 . 5 3 . 5 3 . 4 100 . 0 2 . 0 2 100 5 . 6 6 . 8 5 . 4 8 . 0 5 . 5 4 . 4 100 . 0 2 . 5 locs 4 5 3 9 1 1 4 1 1 reps 4 9 6 12 2 2 8 2 2 diff 0 2 . 0 1 . 0 1 . 2 0 . 5 2 . 0 1 . 0 0 . 0 0 . 5 pr & gt ; t . 999 . 025 + . 074 * . 014 + . 016 + __________________________________________________________________________ mdm fus com sou ecb ecb cpx ers rst rst 1lf 2sc abs abs abs abs abs abs__________________________________________________________________________ total sum 1 2 . 8 6 . 6 5 . 1 4 . 5 4 . 8 8 . 5 2 3 . 3 6 . 4 8 . 6 4 . 0 3 . 8 7 . 5 locs 2 9 15 2 2 1 reps 6 11 16 4 4 2 diff 0 . 5 0 . 2 3 . 5 0 . 5 1 . 0 1 . 0 pr & gt ; t . 000 # . 608 . 000 # . 500 . 295__________________________________________________________________________ * = 10 % sig + = 5 % sig # = 1 % sig comparison data was collected from strip tests that were grown by farmers . each hybrid was grown in strips of 4 , 6 , 8 , 12 etc . rows in fields depending on the size of the planter used . the data was collected from strip tests that had the hybrids in the same area weighed . the moisture percentage was determined and bushels per acre was adjusted to 15 . 5 percent moisture . the number of comparisons represent the number of locations or replications for the two hybrids that were grown in the same field in close proximity and compared . comparison strip testing was done between pioneer brand hybrid 3082 and pioneer brand hybrids 3167 and 3163 . the comparisons come from all the hybrid &# 39 ; s adapted growing areas in the united states . these results are presented in table 3 . hybrid 3082 demonstrates a 5 . 5 bushel per acre and $ 11 . 07 per acre advantage over 3167 . hybrid 3082 has a weighted average one percentage point stand advantage and a 0 . 5 pound per bushel test weight advantage over the other hybrids . table 3__________________________________________________________________________1995 performance comparison report for corn1 year summary of all standard test types . income / pop stand roots testbrand product yield moist acre k / acre (%) (%) wt__________________________________________________________________________pioneer 3082 168 . 0 18 . 5 409 . 22 22 . 7 88 87 57 . 7pioneer 3167 162 . 5 17 . 8 398 . 15 22 . 0 86 86 57 . 0advantage 5 . 5 - 0 . 7 11 . 07 0 . 7 2 1 0 . 7number of comparisons 44 44 44 20 17 17 42percent wins 75 25 68 55 29 23 64probability of difference 99 99 98 81 82 61 99pioneer 3082 152 . 8 20 . 1 367 . 41 22 . 8 94 94 57 . 6pioneer 3163 160 . 4 16 . 9 395 . 18 22 . 8 93 94 57 . 1advantage - 7 . 6 - 3 . 2 - 27 . 77 0 . 0 1 0 0 . 5number of comparisons 105 105 105 75 66 41 97percent wins 30 2 23 40 34 17 54probability of difference 99 99 99 0 75 91 99pioneer 3082 157 . 3 19 . 7 379 . 76 22 . 7 93 92 57 . 6weighted avg 161 . 0 17 . 1 396 . 05 22 . 6 92 92 57 . 1advantage - 3 . 7 - 2 . 6 - 16 . 29 0 . 1 1 0 0 . 5number of comparisons 149 149 149 95 83 58 139percent wins 43 9 36 43 33 18 57probability of difference 99 99 99 45 87 94 99__________________________________________________________________________ note : the probability values are useful in analyzing if there is a &# 34 ; real &# 34 ; difference in the genetic potential of the product involved . high values are desirable , with 95 % considered significant for real differences . characteristics of pioneer hybrid 3082 are compared to pioneer hybrids in table 4 . the values given for most of the traits are on a 1 - 9 basis . in these cases , 9 would be outstanding , while 1 would be poor for the given characteristics . these values are based on performance of a given hybrid relative to other pioneer commercial , precommercial and competitive hybrids that are grown in research strip test trials . these performance based values are determined using several factors such as research data , experience the trained corn researchers had in the field , and the sales experience with the hybrids in strip tests in the field . these values reflect the hybrid &# 39 ; s relative performance to other hybrids for the characteristics listed . table 4 shows hybrid 3082 is high yielding , demonstrates good test weight and has a good protein to yield rating . hybrid 3082 also exhibits above average resistance for stalk lodging while also exhibiting above average plant and ear height . table 4__________________________________________________________________________hybrid patent comparisons - characteristicspioneer hybrid 3082 vs . pioneer hybrids 3167 and 3163__________________________________________________________________________ silk phy gdu gdu h / l / varietycrm crm crm silk phy yld pop pop d / d s / l r / l__________________________________________________________________________3082 124 119 120 1490 2930 9 5 6 53167 124 120 121 1500 2960 7 4 7 5 7 43163 119 117 118 1450 2880 9 7 9 7 5 7__________________________________________________________________________ sta tst plt ear brtvariety grn d / t wt e / g ht ht d / e stk pro p / y__________________________________________________________________________3082 8 7 5 7 7 4 5 93167 8 8 5 3 4 4 5 5 4 63163 8 7 4 6 5 6 5 3 4 8__________________________________________________________________________ this invention includes hybrid maize seed of 3082 and the hybrid maize plant produced therefrom . the foregoing was set forth by way of example and is not intended to limit the scope of the invention . as used herein , the term plant includes plant cells , plant protoplasts , plant cell tissue cultures from which maize plants can be regenerated , plant calli , plant clumps , and plant cells that are intact in plants , or parts of plants , such as embryos , pollen , ovules , flowers , kernels , ears , cobs , leaves , seeds , husks , stalks , roots , root tips , anthers , silk and the like . duncan , williams , zehr , and widholm , planta , ( 1985 ) 165 : 322 - 332 reflects that 97 % of the plants cultured which produced callus were capable of plant regeneration . subsequent experiments with both inbreds and hybrids produced 91 % regenerable callus which produced plants . in a further study in 1988 , songstad , duncan & amp ; widholm in plant cell reports ( 1988 ), 7 : 262 - 265 reports several media additions which enhance regenerability of callus of two inbred lines . other published reports also indicated that &# 34 ; nontraditional &# 34 ; tissues are capable of producing somatic embryogenesis and plant regeneration . k . p . rao , et al ., maize genetics cooperation newsletter , 60 : 64 - 65 ( 1986 ), refers to somatic embryogenesis from glume callus cultures and b . v . conger , et al ., plant cell reports , 6 : 345 - 347 ( 1987 ) indicates somatic embryogenesis from the tissue cultures of maize leaf segments . thus , it is clear from the literature that the state of the art is such that these methods of obtaining plants are , and were , &# 34 ; conventional &# 34 ; in the sense that they are routinely used and have a very high rate of success . tissue culture of maize is described in european patent application , publication 160 , 390 , incorporated herein by reference . maize tissue culture procedures are also described in green and rhodes , &# 34 ; plant regeneration in tissue culture of maize ,&# 34 ; maize for biological research ( plant molecular biology association , charlottesville , va . 1982 , at 367 - 372 ) and in duncan , et al ., &# 34 ; the production of callus capable of plant regeneration from immature embryos of numerous zea mays geneotypes ,&# 34 ; 165 planta 322 - 332 ( 1985 ). thus , another aspect of this invention is to provide cells which upon growth and differentiation produce maize plants having the genotype of 3082 . maize is used as human food , livestock feed , and as raw material in industry . the food uses of maize , in addition to human consumption of maize kernels , include both products of dry - and wet - milling industries . maize , including both grain and non - grain portions of the plant , is also used extensively as livestock feed , primarily for beef cattle , dairy cattle , hogs , and poultry . industrial uses of maize include production of ethanol , maize starch in the wet - milling industry and maize flour in the dry - milling industry . the industrial applications of maize starch and flour are based on functional properties , such as viscosity , film formation , adhesive properties , and ability to suspend particles . the maize starch and flour have application in the paper and textile industries . other industrial uses include applications in adhesives , building materials , foundry binders , laundry starches , explosives , oil - well muds , and other mining applications . plant parts other than the grain of maize are also used in industry . stalks and husks are made into paper and wallboard and cobs are used for fuel and to make charcoal . the seed of the hybrid maize plant and various parts of the hybrid maize plant can be utilized for human food , livestock feed , and as a raw material in industry . although the foregoing invention has been described in some detail by way of illustration and example for purposes of clarity and understanding , it will be obvious that certain changes and modifications may be practiced within the scope of the invention , as limited only by the scope of the appended claims . applicant has made a deposit of at least 2500 seeds of hybrid maize line 3082 with the american type culture collection ( atcc ), rockville , md . 20852 usa , atcc deposit no . 209330 . the seeds deposited with the atcc on october 6 , 1997 were taken from the deposit maintained by pioneer hi - bred international , inc ., 700 capital square , 400 locust street , des moines , iowa 50309 - 2340 since prior to the filing date of this application . this deposit of the hybrid maize line 3082 will be maintained in the atcc depository , which is a public depository , for a period of 30 years , or 5 years after the most recent request , or for the enforceable life of the patent , whichever is longer , and will be replaced if it becomes nonviable during that period . additionally , applicant has satisfied all the requirements of 37 c . f . r . §§ 1 . 801 - 1 . 809 , including providing an indication of the viability of the sample . applicant imposes no restrictions on the availability of the deposited material from the atcc ; however , applicant has no authority to waive any restrictions imposed by law on the transfer of biological material or its transportation in commerce . applicant does not waive any infringement of its rights granted under this patent . | 0 |
the invention will now be described with reference to fig1 to 7 . it is to be noted that the fig1 to 7 are not drawn to scale with respect to the relative thicknesses of the closures , sleeves and the substrate to which they are applied , or with respect to the thicknesses of the layers comprising the closures and the sleeves . [ 0023 ] fig1 and 2 illustrate a preferred closure 10 according to the present invention . as shown in fig1 closure 10 comprises a backing layer 12 , a layer of adhesive 14 applied to the backing layer , and a release film 16 applied to the adhesive layer 14 . closure 10 preferably has an elongate , rectangular shape for application along the length of an overlapping joint formed by the ends of a wraparound sleeve . the backing layer 12 is comprised of a fibrous material and has a first surface 18 and an opposed second surface 20 . the backing layer 12 has sufficient dimensional stability such that , during heat shrinking of the wraparound sleeve to which the closure will be applied , the backing layer will resist substantial deformation which would result in pulling apart of the overlapping joint formed by the ends of the wraparound sleeve . furthermore , the backing layer possesses sufficient resistance to heat such that it will retain its integrity and dimensional stability when it is heated during application to a wraparound sleeve . preferably , the backing layer should be of a composition able to resist the heat and flame of a torch for a time sufficient to allow the closure to be applied to the underlying wraparound sleeve . preferably the backing layer is comprised of an inorganic fibrous material , such as glass fibers ( also referred to herein as “ fiberglass ”). the fibrous material may comprise either a woven or non - woven material . where it is non - woven , it is preferably in the form of a random mat . most preferably , the backing layer comprises a woven mat , having either an open weave or a closed weave . an open weave may be more preferred where the substrate to which the wraparound sleeve is applied has a small diameter or an irregular shape , or where there is some axial shrinkage of the sleeve , since a fabric with an open weave may be more flexible and therefore better able to conform to the contours of the sleeve and the underlying substrate . one example of a suitable backing layer comprises a 10 ounce or 14 ounce woven fiberglass fabric . the backing layer may preferably be coloured , for example by incorporation of a colourant such as a dye , or by including other types of fibers in the backing layer for colouring purposes . the adhesive layer 14 is applied to the first surface 18 of backing layer 12 , preferably by lamination , such that it is in direct contact with the fibrous material comprising backing layer 12 . the adhesive comprising layer 14 has sufficient shear resistance such that it resists slippage of the closure 10 relative to the wraparound sleeve during heat shrinking of the sleeve , and so as to resist creeping of the closure relative to the sleeve after heat shrinking of the sleeve is completed . the adhesive preferably has sufficient tack ( pressure sensitivity ) at ambient temperatures so that it can be applied to the contours of the wraparound sleeve prior to heating of the closure . as used herein , the term “ ambient temperature ” refers to the temperatures at which the closure is applied to a heat shrinkable sleeve , the lower limit of the ambient temperature being at least as low as about 0 ° c . furthermore , the adhesive also has sufficient pressure - sensitivity at elevated temperature such that it forms a permanent bond between the backing layer and the wraparound sleeve upon application of sufficient heat . the pressure - sensitive adhesive comprising layer 14 can be selected from one or more adhesive materials selected from the group comprising iso - butylene polymers such as polyisobutylene , polybutene and butyl rubber . these polymers are preferably at least partially crosslinked in order to increase their shear strength , particularly at elevated temperatures . other preferred adhesive materials include silicones . one particularly preferred pressure - sensitive adhesive is the partially crosslinked butyl mastic rsl - 091 manufactured by rpd inc . of evansville , ind . this adhesive is preferably applied to the fibrous backing layer 12 in a thickness of about 0 . 03 inches . the release film 16 preferably comprises a self supporting strippable polymer film which is removed prior to use of the closure 10 . thus , immediately prior to application of the closure 10 to a wraparound sleeve , the adhesive layer 14 has an exposed surface 22 which is available for adhesion to the sleeve , the area of the exposed surface 22 being substantially equal to the total area of the adhesive layer 14 . the following is a description of a preferred method of applying a close - fitting protective covering to an article , and in particular a method of applying a heat - shrinkable wraparound sleeve 24 to a joint at which two lengths of pipe 26 are connected , as illustrated in fig3 to 6 . it will be noted that details of the pipe 26 are omitted from fig4 to 6 , as are details of the layers of material comprising the wraparound sleeve 24 . the heat - shrinkable sleeve comprises a flexible sheet 28 having a first surface 30 , an opposed second surface 32 , a first end portion 34 and a second end portion 36 , the end portions being spaced from one another in a longitudinal direction ( when the sheet is laid flat ). the flexible sheet 28 is comprised of a dimensionally heat unstable material , preferably a polymer , the material having been stretched in the longitudinal direction from an original heat stable form to a dimensionally heat unstable form capable of moving in the longitudinal direction toward its original heat stable form by the application of heat . as used herein , the term “ longitudinal direction ” refers to the direction along an axis extending between the end portions 34 and 36 of the flexible sheet 28 . the flexible sheet 28 is wrapped around the pipe 26 by laying the sheet 28 against the pipe 26 and overlapping the first end portion 34 of the sheet 28 over the second end portion 36 . this is illustrated in fig3 and 4 . next , the closure 10 is applied to the overlapped end portions 34 , 36 of flexible sheet 28 . the closure 10 , with the release film 16 removed , is applied to the overlapped end portions 34 , 36 with the exposed surface 22 of adhesive layer 14 directly contacting the sleeve 24 . as mentioned above , the adhesive has sufficient pressure sensitivity at ambient temperature such that it initially adheres to the sleeve 24 prior to application of heat . the closure 10 has a first edge 38 which is applied to the first end portion 34 of sheet 24 , and an opposed second edge 40 which is applied on the underlapping second portion 36 of the flexible sheet 28 . this is illustrated in fig5 . after application of the closure 10 to the sleeve 24 , the closure 10 is heated for a sufficient time and to a sufficient temperature to cause the adhesive layer 14 to bond the closure 10 to the first and second end portions 34 , 36 of the flexible sheet 28 . as illustrated in fig6 heat is preferably applied directly to the second surface 18 of backing layer by a flame from a torch , from example a propane torch . after the closure 10 is bonded to the sheet 28 , the flexible sheet 28 is heated , causing it to shrink in the longitudinal direction toward its original heat stable form and into close - fitting relation with the underlying pipe 26 . preferably , the first surface of the flexible sheet 28 is provided with a functional coating 42 to improve contact between the flexible sheet 28 and the underlying substrate and to fill any voids . the functional coating preferably comprises a hot - melt adhesive or a mastic . as mentioned above , the adhesive layer 14 has sufficient shear resistance to prevent substantial slippage and creeping of the closure 10 relative to the flexible sheet 28 during and after heating thereof , and the dimensional stability of the backing layer is sufficient to resist substantial deformation in the longitudinal direction during and after heating of the flexible sheet . the closure discussed above with reference to fig1 to 6 is in the form of an elongate strip which is applied to the sleeve 24 after it is wrapped around pipe 26 . fig7 illustrates an alternate type of closure in which the closure is attached to the sleeve before the sleeve is wrapped around the substrate . the sleeve / closure 100 illustrated in fig7 comprises a closure strip 110 and a flexible sheet 128 . the closure strip 110 has a first edge 138 which is disposed on the first end portion 134 of the flexible sheet 128 . the second edge 140 of closure strip 110 comprises a free edge extending beyond the first end portion 134 . in the embodiment shown in fig7 a release film 116 ( shown partially peeled from adhesive layer 114 ) is provided between the free edge 140 and the first end portion 134 of flexible sheet 128 , thereby preventing premature adhesion of adhesive layer 114 to the second end portion 136 of flexible sheet 128 . as with sleeve 24 described above , the flexible sheet 128 has a first surface 130 and a second surface 132 , wherein a functional coating 142 is provided on the first surface 130 . although the invention has been described by reference to certain preferred embodiments , it is not to be limited thereto . rather , the invention is intended to include all embodiments which may fall within the scope of the following claims . | 2 |
a system for preventing corrosion in a dry fire sprinkler system ( dry fss ) is disclosed . this system offers several advantages over conventional dry fss treatment systems by utilizing chemicals , instead of foams , salts , gasses , and other treatments known in the art . by treating these systems with chemicals , the present invention protects and maintains the longevity of the dry fss , preventing damage to the dry fss system and enhancing the operation characteristics of the dry fss system . referring to fig1 , dry fire sprinkler system 10 includes main line pipe 12 , branch line pipes ( not shown ), drip leg pipes ( not shown ), sprinkler head pipes ( not shown ), etc . dry fire sprinkler system 10 includes an air compress ( not shown ), first tee 14 , input ball valve 16 and second tee 18 . the remainder of the dry sprinkler system 10 is of a conventional configuration and is not shown . interconnected with the dry fire sprinkler system 10 is corrosion inhibitor system 110 . the corrosion inhibitor system 110 is interconnected with the fire sprinkler system 10 at first tee 14 through ball valve 112 and third tee 122 . the corrosion inhibitor system 110 includes coupon rack 120 before the third tee 122 , and after the ball valve 112 , includes dewater separator 130 , deoil separator ( or oil coalescing filter ) 140 , union 142 , desiccant filtration apparatus 150 , humidity eye 152 , filtration ball valve 160 , fill valve 165 , filter feeder apparatus 170 , flush valve 190 , fourth tee 192 , output ball valve 194 and second coupon rack 196 . the corrosion inhibitor system 110 is connected back to the fire sprinkler system 10 at second tee 18 . air from air compressor ( not shown ) in the dry fire sprinkler system 10 enters the corrosion inhibitor 110 where it goes into corrosion coupon rack 120 which can record corrosion by loss of weight . the air then goes through dewater separator 130 which can include a centrifuge to remove water vapor from the air . the dry air then goes through deoil separator 140 where any oils , such as oils from the compressor , are removed from the air to protect the desiccant from interacting with trace amounts of oil in the air . next , the air flows through desiccant filtration apparatus 150 where the air flows through desiccant and loses moisture . thereafter , the air flows through the humidity eye 152 . the humidity eye 152 indicates when the desiccant is used up . the humidity eye can be treated paper having a surface containing cobalt chloride which indicates when the air does not include any moisture , allowing improved absorption for chemicals . ball valve 160 allows for shutting the corrosion inhibitor system 110 to change / reload desiccant filtration apparatus 150 . after the air flows through chemical filter feeder 170 the air and chemicals are broken into small bubbles , for maximizing contact of the chemical inhibitor to the surfaces of the air particles , before entering the dry fire sprinkler system 10 . essentially , the air flow is disrupted to turbulent flow through the chemicals , and the chemicals are dispersed on one or more filters to maximize contact with air to create an aerosol - like flow . after leaving the chemical filter feeder 170 , the air and chemicals flows through blr flush valve 190 to flush out chemicals and then flows to coupon rack 196 and through fourth tee 192 and ball valve 194 into the dry fire sprinkler system 10 . referring now to fig2 a and 2b , the filter feeder apparatus 170 is shown . a top 172 , shown in fig2 a , may include gauge port 173 . the apparatus 170 further includes outer body 174 , outlet 176 , inlet 178 , ports 180 , optional stand 182 , and drain 184 . apparatus 170 also includes inner body 186 . the filter apparatus 170 could be any suitable size , such as , for example , a tube approximately three feet long . fig3 a , 3b and 3c show another aspect of the filter feeder apparatus 270 . the apparatus 270 includes an outer body 274 and a top 272 . as shown in fig3 b , apparatus 270 also includes an inner body 286 . as shown in fig3 c , the bottom of the inner body 286 includes a plurality of apertures 287 for fluid flow . referring to fig2 a , 2b , 3a , 3b and 3c , as well as fig1 , it can be seen that chemical filter feeder 170 , 270 includes an inner chamber 186 , 286 that can be supported within outer body 172 , 272 , by spring 173 which pushes inner body 186 , 286 up against air o - ring at the upper end of inner body 186 , 286 to seal the upper end of the inner body 186 , 286 at an up end . the inner chamber 176 , 286 houses a steel mesh filter media and a liquid chemical . the dried air enters the apparatus 170 , 270 at an upper end , flows down the sides of the inner chamber 186 , 286 to the bottom and then flows s back up through apertures 287 into the inner chamber 186 , 286 pushing through the liquid chemical and filter media to pick up chemical vapors . fig4 a , 4b and 4c show filter media for use in inner body 186 . as shown the filter medium , is contained within the inner body 186 through which the compressed air flows , absorbing chemical product ingredients and carrying them into dry fire sprinkler systems . various grades of filter media can be used , such as steel wool 302 . beads , fibers of wood or plastic , can also be used . appertured plates 312 can also be used . the inner body 186 has an opening on the top for exiting of the vapors , and a slotted opening on the bottom for entrance of the air and / or product . the pressure pushing the air down and into the bottom slots of the interior tube , forces the air through the slots and through the filter media and starts breaking down the air and the chemical product into smaller and smaller bubbles as it moves upward through the filter media . the smaller bubbles allow greater surface areas between air and chemical allowing maximum absorption between chemical and air . there could be a wetted filter with chemical and larger surface area allows for more vapor pick up in dried air . the air then exits of the inner body 186 and flows into the fire sprinkler system . the vapors coat the metal of the dry fire sprinkler system , and if water is present , dissolve into the water and coat the underwater metal stopping corrosion both above and below the water . the corrosion inhibitor composition is comprised of one or more chemical product ingredients and may include an amine , a carboxylate , a carboxylate amine , and combinations thereof . in some aspects , the corrosion control composition may include a compound having the formula hn ( ch 2 ch 2 oh ) n , where n is 1 , 2 , or 3 . in some aspects , the corrosion inhibitor composition may include a primary amine , such as monoethanolamine . in some aspects , the corrosion inhibitor composition may include a secondary amine , such as morpholine . in some aspects , the corrosion inhibitor may include a tertiary amine , such as triethanolamine . in some aspects , the corrosion inhibitor composition may include a carboxylic acid , having the formula hooc —( ch2 ) n - cooh , wherein n is 0 - 13 . in some aspects , the carboxylic acid is undecanedioic acid , dodecanedioic acid , neodecanoic acid , sebacic acid , c4 - c9 dibasic acids , or other dibasic acids . in some aspects , the corrosion inhibitor composition may include a combination of monoethanolamine , morpholine , triethanolamine , and / or neodecanoic acid . in some aspects , the corrosion inhibitor composition may include heterocyclic compound . in some aspects , the heterocyclic compound may include a heterocyclic alkyl and an amine . in some aspects , the heterocyclic compound may have the formula r —( c 6 h 4 )— n 2 nh , wherein r is hydrogen or a c 1 - c 10 alkyl . in some aspects , the heterocyclic compound may include benzotriazole . in some embodiments , the corrosion inhibitor composition may include tolytriazole . in some aspects , the corrosion inhibitor composition may include water . in some aspects , the corrosion inhibitor composition may include benzotriazole and tolytriazole . in some aspects , the corrosion inhibitor composition may further include a diol , such as propylene glycol . in some aspects , the amine corrosion inhibitor may include any class of amines ; including ammonia , primary amines , secondary amines , tertiary amines , cyclic amines , quaternary ammonium salts , and / or amino acids and zwitterions . in greater detail , amines may include : ammonia a compound of nitrogen and hydrogen with the formula nh 3 . contains zero carbons . and , or : primary amines — primary amines arise when one of three hydrogen atoms in ammonia is replaced . these have two hydrogen atoms and one non - hydrogen group attached to the nitrogen to form the amine or amino group — nh 2 . important primary alkyl amines include methylamine , ethanolamine ( 2 - aminoethanol ), and the buffering agent tris , while primary aromatic amines include aniline . additional primary amine examples include but are not limited to : aliphatic amines : methylamine ( aminomethane ), ch 5 n ; ethylamine ( aminoethane ), c 2 h 7 n ; propylamine , ( 1 - aminopropane ), c 3 h 9 n ; 2 - aminopropane ; butylamine , ( 1 - aminobutane ), c 4 h 11 n ; 2 - aminobutane ; 1 - aminopentane ( pentylamine ), c 5 h 13 n ; 2 - aminopentane ; 3 - aminopentane ; 1 - aminohexane ( hexylamine ), c 6 h 15 n ; 2 - aminohexane ; 3 - aminohexane . examples of primary diamines : 1 , 2 - diaminoethane , c 2 h 8 n 2 ; 1 , 3 - diaminopropane , c 3 h 10 n 2 ; 1 , 4 - diaminobutane , c 4 h 12 n 2 ; 1 , 5 - diaminopentane , c 5 h 14 n 2 ; 2 , 3 - diaminopentane ; 2 , 4 - diaminopentane ; 1 , 4 - diaminohexane , c 6 h 16 n 2 ; 1 , 6 - diaminohexane . examples of primary cyclo - amines : e . g . cyclopentylamine ; aminocyclopentane , c 5 h 11 n 2 ; aminocyclohexane ; cyclohexylamine , c 6 h 13 n 2 ; benzylamine , c 7 h 9 n . aromatic amines , where the amino or amine group is directly attached to the aromatic benzene ring : e . g . phenylamine , c 6 h 7 n , c 6 h 5 nh 2 ; 1 , 3 - diaminobenzene , c 6 h 8 n 2 ; 3 - aminobenzoic acid ; 2 - methylphenylamine ; methyl - 2 - phenylamine ; 1 - amino - 2 - methylbenzene . many ‘ amino acids ’ are ‘ primary ’ amines . and , or : secondary amines — secondary amines have two non - hydrogen groups , such as organic substituents ( alkyl , aryl or both ) bound to n together with one hydrogen ( or no hydrogen if one of the substituent bonds is double ). important representatives include dimethylamine and methylethanolamine , while an example of an aromatic amine would be diphenylamine . these have one hydrogen atom and two alkyl or aryl groups attached to the nitrogen . additional secondary include but are not limited to : aliphatic amines : dimethylamine ; ethylmethylamine ; diethylamine ; methylpropylamine ; ethylpropylamine ; dipropylamine . examples of cyclo - secondary amines : e . g . piperidine , c 5 h 11 n ; n - methylcyclopentylamine , c 6 h 13 n . aromatic amines : n - methylphenylamine , c 7 h 9 n ; n - ethylphenylamine , c 8 h 11 n ; and diphenylamine , c 12 h 11 n . and , or : tertiary amines — in tertiary amines , all three hydrogen atoms are replaced , such as by organic substituents . examples include trimethylamine , which has a distinctively fishy smell , or triphenylamine . these have no hydrogen atom and three alkyl or aryl groups attached to the nitrogen . additional tertiary amines include but are not limited to : aliphatic amines : trimethylamine ; ethyldimethylamine ; diethylmethylamine ; and triethylamine . cyclo - tertiary amines : n - methylpyrrolidine , and n - methylpiperidine , tertiary aromatic amines : n , n - dimethylphenylamine ; n , n - diethylphenylamine ; and triphenylamine and , or : cyclic amines — cyclic amines are either secondary or tertiary amines . examples of cyclic amines include the 3 - member ring aziridine and the six - membered ring piperidine . n - methylpiperidine and n - phenylpiperidine . and , or : quaternary ammonium salts — it is also possible to have four organic substituents on the nitrogen . these species are not amines but are quaternary ammonium cations and have a charged nitrogen center . quaternary ammonium salts exist with many kinds of anions . if all for hydrogens of an ammonium ion are replaced , such as with alkyl or aryl groups , then an ionic quaternary salt is formed . the simplest is tetramethylammonium chloride , ( ch 3 ) 4 n + cl − ; tetrapropylammonium chloride , ( ch 3 ch 2 ch 2 ) 4 n + cl − ; and the r groups can be mixed e . g . [( ch 3 ch 2 ch 2 ) 3 nc 6 h 5 ] + cl − and , or : amino acids and zwitterions — the primary suffix name for an aliphatic carboxylic acid is based on the “ longest carbon chain name *” for the — cooh bond system e . g . ethanoic acid , propanoic acid etc . the amino group — nh 2 , with its c - atom position number , is added as a prefix . [* without the end ‘ e ’] many amino - acids in aqueous solution , or in the crystalline state , exist as ‘ zwitterions ’ where the proton migrates from the acidic — cooh group to the basic — nh 2 group to form the ionic groups — nh 3 + and — coo − but within the same ‘ molecule ’. additional amino acids include but are not limited to : aminoethanoic acid , c 2 h 5 no 2 ; 2 - aminopropanoic acid , c 3 h 7 no 2 ; and 3 - aminopropanoic acid . in a range , the corrosion inhibitor composition may be prepared according to table 1 : in a preferred embodiment , the corrosion inhibitor composition may be prepared according to table 1 : the initial mix of monoethanolamine , morpholine , triethanolamine and neodecanoic acid may be combined with equal portions of benzotriazole and tolytriazole in the same proportional volume as the initial mix . propylene glycol may be added to dilute the final mix to whatever consistency desired . it should be understood that the following is a listing of the components shown fig1 and they are shown simply by way of example and not by way of limitation : bypass valve sized to plant air line air line tee reduced to ¾ inch going to and from feed system ¾ inch nipple to air line tee ¾ inch valve shut off going to above nipple ¾ inch nipple to valve to feed system ¾ inch union ¾ inch nipple from union to tee ¾ inch tee to nipple ¾ inch brass or steel corrosion plug on end of tee corrosion coupon ¾ inch nipple on end of tee ½ inch male bushing to connect to ¾ female thread s . s . 5 inch × 24 inch air filter 1 . 5 inch male thd × ½ inch female thd s . s . bushing ½ inch × short nipple ¼ inch 316 l s . s . valve drain 4 . 5 inch blue pvc × 20 inch internal casing tube 10 lbs desiccant material 1 . 5 inch male thd × ½ inch female thd s . s . bushing ½ inch × short nipple ½ × ½ × ½ tee ½ indicating site glass ½ inch × short nipple ½ valve ½ inch union 5 inch × 24 inch ½ inch × short nipple 1 . 5 inch male thd × ½ inch female thd s . s . bushing s . s . 5 inch × 24 inch air filter 4 . 5 inch blue pvc × 20 inch internal casing tube 0000 aught steel wool filtering medium ¼ inch 316 l s . s . valve drain gallon “ proguard air ” 1 . 5 inch male thd × ½ inch female thd s . s . bushing ½ inch × short nipple ½ × ½ × ½ inch s . s . tee ½inch boiler valve ( 2 each ) ½ to ¾ inch expanding bushing ¾ inch × short nipple ¾ × ¾ × ¾ inch tee corrosion coupon ¾ corrosion coupon plug ¾ inch nipple on top end of tee ¾ inch union ¾ inch nipple to valve to feed system ¾ inch valve shut off going to above nipple ¾ inch nipple to air line tee air line tee reduced to ¾ inch going to and from feed system in order to chemically treat the fire sprinkler system , the operator closes the os & amp ; y (“ outside stem and yoke ”) or control valve and then drains the system . the drain ( not shown ), is located in the downstream portion of the fire sprinkler system . this permits all of the air in the fire sprinkler system to be evacuated . the drains are then closed and the two ball valves are then opened , which permits the air to flow through the corrosion inhibition system . referring to fig5 , another aspect of the corrosion inhibitor system 410 is shown . the corrosion inhibitor system 410 is interconnected with the fire sprinkler system 10 by tee 14 through valve 412 to tee 422 , and includes a first coupon rack 420 , a dewater separator 430 , deoil separator 444 ), union 442 , desiccant filtration apparatus 454 ), humidity eye 552 , filtration ball valve 460 , fill valve 465 , filter feeder apparatus 470 , fourth tee 492 , output ball valve 494 and second coupon rack 496 . the corrosion inhibitor system 410 is connected back to the dry fire sprinkler system 10 at second tee 18 . the system 410 further includes a tee 499 , such as a two inch mechanical tee , with a hose 500 to float level control 510 , such as a magnetic float switch , for turning a chemical metering pump on and off . float level control 510 receives power from plug 530 and is connected by hose 520 to the filter feeder apparatus 470 . a metering pump 554 ), such as a four gallon per day metering pump , also receives power from plug 530 and is connected to a tank 540 , such as a five gallon container , of the corrosion inhibitor chemical ingredients and can inject the chemical ingredients into the feeder apparatus 470 through injector 560 based on feedback from the float level control 510 . this allows for automatic control and maintenance of the chemical level in the feeder apparatus 470 . the fire sprinkler corrosion monitoring station ( fscms ) can be installed on the system riser or on a main connected to the riser to monitor internal corrosion conditions in a water based fire protection system . the fire sprinkler system can be continuously monitored so that activities such as filling and draining are also experienced by the fscms . in buildings where more than one fire sprinkler system being fed from a common riser , the fscms can be installed on the system side of the control valve on each of the individual systems . the fscms is designed to simulate conditions where internal corrosion may develop within the system . the fscms can be safely isolated from the system riser or main and easily accessed for servicing and monitoring of test specimens , ( corrosion coupons or corrosion monitoring probes ) without taking the fire protection system out of service . corrosion coupons can be installed in the corrosion monitoring station by the use of a di - electric coupon holder . the corrosion monitoring station can be provided as two components , to allow for quick installation . the main assembly could include the corrosion monitoring station with ball valve . the second component could include the dielectric coupon holder . the procedure for the installation of the corrosion monitoring station can be as follows : a 1 ″ npt connection into the sprinkler system riser or supply main is provided as may be detailed by the designer . 2 . the threaded nipple closest to the bail valve is screwed into the 1 ″ npt connection to the system . teflon tape and / or ptfe paste may be used on this threaded connection . the fscms is positioned in a vertical format where the dielectric coupler is at the bottom of the assembly . the corrosion monitoring station should not be installed in any configuration that could cause trapped water within the unit or the piping to the unit that will not drain when draining the fire sprinkler system . 2 . remove the di - electric coupon holder slowly to release any remaining pressure from the coupon holder . 3 . once the di - electric coupler is removed , connect the coupon sample to the wand with the holding screw . 4 . apply teflon tape to the threaded portion of the di - electric coupler . 6 . slowly open the isolation ball valve to fill the chamber with water . leave the ball valve in the open position so system water floods the assembly . it should be verified that all valves are in the correct position and the corrosion monitoring station is free of any leaks . while the invention has been described in detail and with reference to specific examples thereof , it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof . | 5 |
fig1 illustrates from left to right , a reactor 11 for heat treatment of wood / pulp / cellulose - containing material . in the reactor 11 is the mass is heated under pressure in the presence of water vapor and air . the mixing ratio between water vapor and air may vary and the filling level of the reactor can likewise vary . temperature and residence time in the reactor may vary and are typically in the range from 160 to 300 ° c . and from 1 to 15 minutes . higher temperatures and longer processing time are as controlling elements actually undesirable because it provides greater degradation , more mass loss and problems in operating the downstream process in the form of undesirable amounts of non - condensable gases , gases with strong odors , etc . the reactor typically comprises equipment and devices for controlling and monitoring the process , including valves to control pressure , means for heating and cooling of the reactor respectively , etc . this is not illustrated since it is not key to the process run in the reactor 11 . container 12 is a pressure release vessel into which the reaction mixture is released at end of treatment . at least a portion of the pressure in the reactor 11 is released abruptly , thereby expelling the reaction mixture from the reactor into the pressure release container 12 . the skilled artisan will appreciate that gases other than steam and air may be present in the reactor , provided that they do not interfere negatively with the process quantities . for example , the ratio between oxygen and nitrogen in the reactor be different from what is the case in air , e . g . through the addition of oxygen enriched air or oxygen consumed during the process . on completion of reaction treatment the reaction mixture is expelled from the reactor 11 to pressure release tank 12 via conduit 21 . this is performed in a manner known in the art . the solid with a certain quantity of moisture is moved into the pressure release tank 12 and transferred via conduit 22 to after - treatment in any suitable manner known in the art . the gas containing condensable components as well as components which are not condensable within the prevailing conditions , passes through conduit 23 at or near the top of the pressure release tank 12 and is led therefrom directly to at least a heat exchanger 13 . the heat exchanger 13 cools the gas flow and ensures that the condensable components of the gas are condensed , so as to thereby reduce the volume of the gas flow . the heat of condensation received by the refrigerant is utilized as energy in any suitable manner within or outside the current process . typically , this energy is used to preheat the air for a drying unit or for combustion . the condensate from the heat exchanger 13 contains , in addition to water , components which should be removed before the water is discharged or recycled for reuse . the condensate is discharged through conduit 25 , while the gas passes to the next step in the process through conduit 26 . as regards the heat exchanger or heat exchangers 13 this or these can be indirect heat exchangers where the refrigerant is kept separate from the vent gases or it can be direct heat exchangers where cooling water is mixed with the vent gases . it can also be a combination , where the heat exchange mainly is indirect , but where water 24 at a limited rate is sprayed into the flow of discharge gases into the heat exchanger 13 to cause a quenching of the discharge gases 23 to thereby more easily condense all condensable components in the subsequent indirect step of heat exchange . if one chooses to use only direct heat exchange , a much larger volume of fluid needs to be handled downstream of the heat exchanger . it is therefore preferred that the heat exchange at least partially is conducted as indirect heat exchange . the next step of the process utilizes a container 14 with flexible volume , typically a “ balloon ”, which like other balloons has soft walls and is dimensioned so that it is able to receive the “ puff ” of non - condensable gases resulting from expulsion from a batch reactor operated under normal operating conditions . in fig1 , the reaction mixture is still enclosed in the reactor 11 and container 14 with flexible volume is therefore substantially empty , as is shown in the figure . referring now to fig2 , which shows the same as fig1 except that here the pressure in the reactor has just been released so that the reaction mixture has been expelled into the pressure release tank 12 while the gas is blown on to the container 14 with flexible volume through the heat exchanger 13 and conduits 23 and 26 . within a few seconds after the pressure is released , the container 14 is inflated by non - condensable gases as shown in fig2 . the container 14 will typically be oversized in relation to the need that can be calculated based on a single batch . in addition , a safety valve can ensure that the container 14 does not burst even in case of extreme amounts of non condensable gases . the container 14 will , for each batch , for a short period of time , occupy the entire amount of non - condensable gases without thereby causing any significant overpressure , and then slowly and in a controlled manner release the gas via conduit 27 to at least one chamber 15 for after - treatment of the gases , ensuring that the gases do not escape to the atmosphere untreated . here any flammable components may be burned and the combustion heat may be taken care of through appropriate cooling of the chamber and / or of the exhaust gases . after - treatment can be conducted in multiple chambers 15 , arranged in series , parallel or a combination of series and parallel . this is not essential to the inventive concepts . what is important is what takes place in the form of heat exchange in heat exchanger ( s ) 13 and temporary accumulation of non - condensable gases in a container 14 with flexible volume . this combination is unique and indicates that the heat energy that one previously was not able to take care of in this type of batch processes , now is possible to recover in order to achieve a process with a lower net energy consumption and thereby a more profitable process . in addition one achieves the bonus that gases with harmful or unpleasant odors are taken care of . it is furthermore possible to reduce the load on the heat exchanger by placing a container with flexible volume upstream thereof , to reduce the rate at which released gases pass through the heat exchanger . the disadvantage of this is that all “ unclean ” components will still be present in the gas and parts of these will adhere to the walls of the container 14 with the flexible volume . with regard to the need for dimensioning , a typical reactor for the purpose in question can have a volume of 10 m 3 and with a pressure of 25 bars , the pressure release will produce up to approx . 250 m 3 gas that needs to be taken care of . in practice , the amount of gas will be somewhat less because part of the reactor volume is occupied by the biomass and because some of the pressure can be vented out carefully prior to the sudden pressure release . by appropriately controlling of the process , the volume which is discharged in one quick pressure surge lasting approximately for 5 seconds , may be decreased to approximately 70 m 3 . the specific heat of vaporization of water is 242 kj / mole or 13 . 45 mj / kg . if 50 % of these 70 m 3 is water vapor ( about 1 kg / m 3 ), the immediate need for heat transfer in heat exchangers will amount to : provided all available vapors will condense . the processes can naturally be controlled so that this need larger or smaller , the figures given as an example of sizing needs , but also to shed light on the challenges of success in managing such energy - rich “ impacts ”. if condensation capacity is not sufficient a pressure build - up will take place . the prerequisite for respite and escape out through the condensing unit is that the capacity is so large that the pressure drop does not increase excessively . the part of the reduction of the steam impact caused by introduction / self - production of volatile gases , means that the impact of non - condensable gases is increased to a volume of from 25 to 150 m 3 per ton biomass or up to 30 m 3 per second . this must be considered a large useless volume in relation to the reactor size . this pressure impact is large and must be collected and then passed on as a continuous flow . to collect a large quantity of gas in a short time at such a low pressure , is a demanding task which according to the present invention is solved by the container with the flexible volume . after - treatment must also be performed on both water and gas . this is made according to known technology once the process is carried out in accordance with the disclosure . if the desired reactor is 10 m 3 and this is supplied with 5 m 3 of biomass ( wood chip or similar ) then that corresponds to a ton of mass . dry matter 400 600 700 900 kg spec heat 0 . 65 0 . 65 0 . 65 0 . 65 kcal / kg wood mass diff temp 145 145 145 145 degrees celsius enthalpy 37700 56550 65975 84825 kcal water 600 400 300 100 kg spec heat 1 1 1 1 kcal / kg water diff temp 145 145 145 145 degrees enthalpy 87000 58000 43500 14500 kcal sum kcal 124700 114550 109475 99325 sum kcal required 514 . 8 472 . 9 451 . 9 410 . 0 gj / ton energy & amp ; 0 % 10 % moisture moisture energy 514 . 8 410 . 0 gj / t requirement enthalpy 1870 1870 evaporation enthalpy water 920 920 sum 2790 2790 uses 1870 1870 eq kg steam 275 . 274 219 . 259 suppl . amount steam vs . material moisture in addition , steam is needed to provide a desired vapor pressure . filling level 50 % means that approximately 70 % of the volume is filled with steam to provide steam pressure , and at a reduction / expulsion pressure of 10 bars , there will be 75 kg steam in the reactor . 75 % of the volume * 10 bar * 1 kg / m 3 = 75 kg volume of the puff and volume of non - condensable gases can thereafter be calculated . per ton mass supplied this means that for a typical volume and operation range 180 - 235 ° c ., the condensable volume is 25 - 35 times the reactor volume and the non - condensable gases corresponds to the mass loss in the reactor , ranging from 0 - 30 times the reactor volume . both volumes are slightly changed when it turns out that the mass loss becomes both water and non - condensable gases depending on the pressure / time / temperature in the reactor . the example shows that the immediate impact is huge . | 2 |
with reference to the figures , the coupling in accordance with the invention comprises a body given overall reference 1 that is of tubular shape defining an internal channel 2 , and that is arranged to connect the internal channel 2 to two pipes , e . g . forming parts of members of a fluid circuit , such as pipework , a manifold , an actuator , a tank . the channel 2 has an end chamber forming a housing 19 for one end 100 of one of the pipes . the housing 19 is stepped , and it possesses a minimum diameter that is greater than the diameter of the internal channel 2 ( the minimum diameter of the housing 19 is slightly greater than the outside diameter of the pipe end 100 ), and a maximum diameter beside its inlet . the body 1 comprises first and second body parts given respective overall references 4 and 3 . the first body part 4 and the second body part 3 thus define respective segments of the internal channel 2 . the body part 3 possesses a first end portion 5 arranged as a female connection portion for connection to the pipe end 100 for connecting said pipe to the internal channel 2 , and at its opposite end , it possesses a second end portion 6 arranged as a male connection portion for connection to the body part 4 . the housing 19 extends over the entire length of the body part 3 and opens to the outside beside the end portion 5 via its maximum - diameter portion that presents an inlet orifice for admitting the pipe end 100 into the coupling . the end portion 5 is provided with connection means that are themselves known and that here comprise a radially - movable latch for co - operating with an external portion in relief on the pipe end 100 . the end portion 6 is formed by a tubular wall having four through openings 7 that are disposed symmetrically at 90 ° from one another so as to open out transversely into the housing 19 . the body part 4 possesses a first end portion 8 arranged as a male connection portion for connection to the end of the other pipe in order to connect said pipe to the internal channel 2 , and at its opposite end , it possesses a second end portion 18 arranged at a female connection portion for connection to the body part 3 . the first body part 4 has a bend such that the male end portion 8 is at an angle of 90 ° relative to the end portion 18 . the end portion 8 is provided with connection means , here outwardly - projecting christmas tree - shaped teeth , and it is arranged to be forcibly engaged in said end of said pipe . the end portion 18 defines the end 19 . 1 of the housing 19 that is connected to the channel 2 via a shoulder that forms an abutment for the pipe end 100 and that also defines a chamber 10 for receiving the end portion 6 . the housing 19 receives sealing elements 23 beside the end portion 8 , which sealing elements serve to clamp onto the pipe end 100 that is to be retained by the connection means of the body part 3 . the wall of the end portion 18 defining the chamber 10 is provided with two through openings 9 , disposed symmetrically at 180 ° from each other . the coupling of the invention also includes a clip element 20 having a locking portion 21 of annular shape and two diametrically - opposite lugs 22 . more precisely , the clip element 20 is in the form of an elongate element shaped to define the two lugs 22 of u - shape with branches that are rounded towards the outside and that are joined together to form the locking portion 21 . the locking portion 21 has an outside diameter substantially equal to the inside diameter of the end portion 6 , and an inside diameter that is slightly smaller than the outside diameter of the pipe end 100 . the locking portion 21 is elastically deformable from a rest state in which the outside diameter is substantially equal to the inside diameter of the end portion 6 , and a flattened state in which the transverse dimension of the clip element ( measured perpendicularly to a middle axis passing through the lug 22 ) is no greater than the dimension of the openings 7 , 9 ( measured perpendicularly to the central axis of the coupling ). assembling the coupling amounts to engaging the end portion 6 axially into the chamber 10 , while causing the openings 7 and the opening 9 to correspond ( fig2 ). the clip element 20 is then put into place . to do this , the cocking portion 21 of the clip element is flattened to enable it to be inserted in the housing 19 by passing through an opening 9 and a facing opening 7 . once it has passed through the openings , the locking portion 21 returns to its previous shape and extends transversely inside the housing 19 ( fig3 and 4 ). the lugs 22 are received in two pairs of facing openings 7 , 9 , said pairs being diametrically opposite . the clip element 20 thus constitutes an element for pinning the coupling parts to each other . when the pipe end 100 is inserted into the coupling , the pipe end 100 engages in the locking portion 21 and thus prevents said locking portion from flattening , thereby opposing extraction of the clip element 20 . the pipe end 100 is engaged by force in the locking portion 21 . the clip element is thus constrained against the body and against the pipe end , which is deformed thereby , thus enabling assembly clearances to be accommodated and possibly ensuring electrical conductivity between the pipe end and the coupling . more precisely , by comparing fig5 a ) and 5 b ) it can be seen that engaging the pipe end 100 by force causes the branches of the lugs 22 to be spaced apart and thus to be pressed against the two opposite side walls of the openings 7 , 9 , thus ensuring contact . this putting onto contact serves to eliminate operating clearances and thus ensures electrical continuity assuming that the clip element , the body parts , and the pipe ends are made of electrically conductive materials ( e . g . conductive polymer or metal ), thereby enabling any electrical charge that might accumulate in the fluid transport circuit to be dissipated . the first body part 4 has a bend so that the male end portion 8 is at an angle of 90 ° relative to the end portion 18 . it can be understood that the symmetrical arrangement of the openings 7 at 90 ° to one another makes four orientations possible for the body parts relative to each other , thus making it possible to select the orientation of the latch in the second body part 3 relative to the male end portion 8 of the second body part 4 so as to enhance accessibility to the latch as a function of the surroundings of the coupling . naturally , the invention is not limited to the embodiments described , but covers any variant coming within the ambit of the invention as defined by the claims . in particular , the number and the positions of the openings 7 , 9 could be different from those described above . the number and the positions of the lugs and of the grooves could also be modified , e . g . as a function of the number of possible angular orientations that it is desired to have between the body parts . other connection means could be used , and in particular optionally quick - connection means , means for forced mutual engagement , or clip - fastener means , a toothed washer , an attachment clamp . the coupling may have two male ends or two female ends . the connection between the first body part and the second body part may be made either upstream from the sealing elements 20 as described above (“ upstream ” relative to the insertion direction of the pipe end into the chamber of the first end portion ), or else downstream from said sealing elements , but it is then necessary to provide additional sealing elements between the first body part and the second body part . the clip element may be of a shape that is different from that shown , and for example it may be in the shape of a hairpin . the clip element then has one lug from which two diverging branches extend so as to form the locking portion . the branches are elastically deformable towards a release state in which they are parallel to each other so as to allow the locking portion into the openings . when the pipe end is engaged in the coupling , the two branches are held captive between the wall of the coupling and the pipe end , thereby preventing the branches from being deformed towards their release state . in a variant , the locking portion 21 could be plastically deformable or it could be hinged so as to be movable between its two states . as it is anticipated that certain changes may be made in the present invention without departing from the precepts herein involved , it is intended that all matter contained in the foregoing description shall be interpreted in as illustrative rather than in a limiting sense . all references including any priority documents cited herein are expressly incorporated by reference . | 5 |
fig1 which is a simplified schematic diagram , shows a four transistor differential amplifier operated from three current sources , 10 , 12 , and 13 . to achieve balance , current sources 12 and 13 produce equal currents . input transistor 16 is operated from current source 12 as a common emitter driver directly connected to the emitter of common base transistor 17 . thus the collector current in transistor 16 and hence the collector current in transistor 17 , which is directly driven by transistor 16 , will follow the input voltage on line 8 . the output voltage on line 19 will be the inverted (-) function of the voltage at input line 8 . similarly on the other half of the circuit , which is intended to be a mirror image of the section just described , an input on line 9 will be applied to the base of transistor 22 which acts as a common emitter amplifier and is directly coupled to the emitter on transistor 23 . thus the current in transistor 22 , and hence the current in transistor 23 , will follow the voltage at input 9 to produce an output at line 24 . the two halves of the circuit are made to fully interact by virtue of the common direct connections . the bases of transistors 17 and 23 are connected together and operated at point 30 which is the terminal of constant current source 10 . this source operates from the + 15 volt power supply line . ( note that two power supplies are indicated , a + 15 volt supply and a - 15 volt supply , both referenced to ground or neutral potential .) point 30 is returned to point 31 by means of resistor 32 . point 31 represents the average potential of the emitters of transistors 16 and 22 as determined by equal value resistors 33 and 34 . since the emitters of transistors 16 and 22 are operated from constant current sources 12 and 13 respectively which provide equal currents from the - 15 volt power supply , the emitter voltages will follow their respective base voltages . therefore transistors 16 and 22 float , from a voltage standpoint , at a value determined by the common mode input voltage . the so called common mode input voltage refers to the voltages applied equally to lines 8 and 9 . so long as 8 and 9 are at the same voltage there will be no response at output terminals 19 and 24 . this occurs because output transistors 17 and 23 have their bases connected together and returned by way of resistor 32 to point 31 which represents the average potential at the emitters of transistors 16 and 22 . since this average potential will follow the common voltage at inputs 8 and 9 , any common mode signal voltage applied to the emitters at transistors 17 and 23 will be offset by the same change in voltage at the bases at point 30 . this action tends to maintain a constant collector to emitter voltage across each of transistors 16 and 22 , thereby keeping them at the same operating point and reducing common mode signal amplification due to dissimilarities of the devices . if a differential voltage appears between input lines 8 and 9 . a quite different action occurs . the voltage at the bases of transistors 16 and 22 will no longer be the same therefore the currents fed to transistors 17 and 23 will be different . however since the bases of transistors 17 and 23 are still returned to the average voltage at the emitters of transistors 16 and 22 the outputs at lines 19 and 24 will fully respond to the difference in input voltages while transistors 17 and 23 fluctuate around the same operating point . since the differences in input will produce a directly related output , whereas a common mode input will not , the circuit essentially rejects the common mode input . the term common mode rejection is the ratio of signal output for a differential input to the signal output for the same signal value applied to the two inputs in common . since such a ratio is dimensionless it is expressed in db . for example a common mode rejection of 20 db means that a 1 - volt differential input will produce the same output response as a 10 - volt common mode signal . thus it can be seen that the common mode rejection is a function of how well the two halves of the circuit are balanced . the advantage of the above described circuit lies in its high common mode rejection while using parts that do not need to be carefully selected . in effect the circuit is highly self balancing . this is due to the high degree of coupling between the two halves of the circuit and the means employed to make the circuit responses independent of device parameters . fig2 shows the elements of fig1 with emitter follower isolation added . input 18 is applied to emitter follower transistor 15 , the emitter of which is supplied from constant current source 11 . input 20 is applied to emitter follower transistor 21 , the emitter of which is supplied from constant current source 14 . to achieve circuit balance , sources 11 and 14 are made to have equal currents . since transistors 15 and 21 are operated from constant current emitter sources 11 and 14 , these emitter followers will have very close to unity gain independent of the transistor characteristics . since transistors 16 and 22 have their emitters supplied from constant current sources 12 and 13 these common emitter stages will also have very close to unity gain . the common base connected stages using transistors 17 and 23 are emitter driven from high impedance drivers so that they too have very close to unity gain . it will be noted that in each stage the characteristics of the transistor will have practically no influence on the gain value . fig3 is a complete schematic diagram of a practical circuit using the invention . it will be noted that the circuit elements described in connection with fig1 and 2 employ the same numbers . transistor 40 along with its biasing resistors 41 - 43 comprises constant current source 10 operating from the + 15 volt power supply . matched transistors 44 and 45 comprise constant current sources 12 and 13 respectively . since the transistors have a common biasing source , made up of diode - connected transistor 46 and resistor 47 , the currents will be equal . matched transistors 48 and 49 comprise constant current sources 11 and 14 respectively . since they have a common biasing source , made up of diode - connected transistor 50 and resistor 51 , the currents will be equal . the above described current equalities and their application to the associated transistor emitters is responsible in part for the excellent common mode rejection . the circuit of fig3 was constructed using the following components : transistors 15 , 21 , 48 , 49 and 50 -- rca ca3046 ( 5 - npn transistors ) transistors 16 , 22 , 44 , 45 and 46 -- rca ca3046 ( 5 - npn transistors ) transistors 17 and 23 -- 2n2369 ( npn ) resistor 32 -- 1 . 5 k ohmsresistors 33 and 34 -- 150 ohms ( matched pair ) transistor 40 -- 2n2907 ( pnp ) resistor 41 -- 2 . 2k ohmsresistor 42 -- 5k ohmsresistor 43 -- 10k ohmsresistor 47 -- 3k ohmsresistor 51 -- 7 . 5k ohmsresistors 52 and 53 -- 300 ohms ( matched pair ) no particular effort was made to select parts except for the matched resistor pairs 33 and 34 and 52 and 53 . the 5 - transistor ic &# 39 ; s were employed because it was convenient to do so and the common substrate construction places the transistors close together and tends to make their characteristics similar . this made the circuit less temperature sensitive because , as temperature changes , the transistor characteristics tend to change in a balanced manner thus preserving circuit balance and common mode rejection . the circuit had a common mode rejection of over 50 db over the frequency range of 5hz to 1 mhz . the gain of the circuit was about 1 when operated single ended ( that is taking one output with respect to ground ) and about 2 when operated in the differential mode ( that is taking one output with respect to the other output ). the common mode input could be driven between the limits of about + 9 to about - 13 volts while maintaining the excellent common mode rejection . the amplifier input impedance approximated a resistance in excess of 1 . 5k ohms shunted by a capacitance of less than 30 pfarads . thus the amplifier is easily driven over great bandwidths by terminated transmission lines in the 75 - ohm impedance range . the foregoing has disclosed a high performance differential amplifier and an example given showing its excellent performance . clearly equivalents and alternatives will occur to a person skilled in the art . for example while the circuit is shown in discrete device form , it is clear that the circuit would be quite suitable for integrated microcircuits either hybrid or monolithic type . accordingly it is intended that my invention be limited only by the following claims . | 7 |
hereinbelow , the preferred embodiments of the present disclosure will be detailed with reference to the drawings to make advantages and features of the present disclosure more apparent to those skilled in the art so that the protection scope of the present disclosure can be defined more explicitly . referring to fig1 to fig6 , embodiments of the present disclosure will be described as follows . a music earphone comprises an auricle - shaped shell , a cover , and a cavity formed by the auricle - shaped shell and the cover . one or more receivers are disposed in the cavity , a sound aperture is disposed at an upper end of the shell , an edge of the sound aperture extends towards the interior of the cavity to form a cylindrical hearing tube , a lower end of the hearing tube is fixedly connected with the receiver ( s ), a lower end of each of the receiver ( s ) is connected with a conductor , an upper end surface of the shell and the cover are formed with a first vent hole and a second vent hole communicating with the first vent hole via a vent tube respectively , a noise filtering core is disposed inside the vent tube , the first vent hole on the upper end surface of the shell is provided with a guard screen , and a door is disposed or not disposed on the cover at a position corresponding to the second vent hole , and the door is of a flip - over type or a sliding type . ( i ) the shell of the present disclosure is a customized soft shell . there are the following four methods to make the customized earphone soft cover , and the four methods may also be used in combination to make the cover of the earphone into a soft cover of a general type , which may be one of the ite - half shell type , the itc type , and the cic type , and may be of a large size , a medium size , a small size or other different sizes . 1 . there is no need to extract an ear print , and a soft polymer material ( the soft polymer material is one or more of a silicone rubber , polyurethane , a tpu rubber , a tpe or polymers of silicone and polyurethane ) is directly injected into the ear canal of the user for instant molding so that a soft cover can be fabricated on site . 2 . an ear print is extracted firstly , and then a soft polymer material is used to fabricate a soft cover according to the ear print . the soft polymer material is one or more of a silicone rubber , polyurethane , a tpu rubber , a tpe or polymers of silicone and polyurethane . 3 . an ear print is extracted firstly , and then a hard polymer material is used to fabricate a hard cover according to the ear print and a soft material coating is further coated on the outer surface of the hard cover . the hard polymer material may be one or more of acrylonitrile butadiene styrene ( abs ), polypropylene ( pp ), polyethylene ( pe ), polycarbonate ( pc ) or polymers of pc / abs . the soft material is one or more of a silicone rubber , polyurethane , a tpu rubber , a tpe or polymers of silicone and polyurethane . 4 . alternatively , an earphone cover is fabricated according to principles of fabricating the shell of a flexible cic - type audiphone , and a soft ear mold is disposed at an end portion of the cover . the hard cover of the earphone may also be fabricated into a size slightly smaller than that of the auricle according to the cic method for fabricating a customized hard cover ; and then , one or more elastic rubber rings for sealingly contacting the wall of the ear canal are disposed around the cover . the material of the elastic rings is one or more of a silicone rubber , polyurethane , a tpu rubber , a tpe or polymers of silicone and polyurethane . ( ii ) a noise filtering core of a multi - sectional structure is disposed inside a breather tube . 1 . in order to improve the breathability , more than one communicating mini breather tubes or vent tubes are disposed inside the earphone to filter out the ambient noise while allowing the air to circulate between the interior and the exterior of the ear . the breather tube may be one or more kinds of tubes that extend through the shell , through a wall of the shell , or along the outer wall of the shell . the vent tube may be of a linear form , or of a regular or irregular curved or helical form . the breather tube may be in a circular shape , an oval shape , a triangular shape , a quadrangular shape , or a polygonal shape . the maximum radial dimension is 0 . 3 mm to 0 . 5 mm , and the minimum radial dimension is no less than 0 . 1 mm . the vent tube may be hollow , or may be filled with a noise filtering core . in a special case where the diameter of the vent tube is less than 1 . 0 mm , the ambient noise can be effectively filtered out even when no filtering core is filled inside the vent tube . 2 . no less than one vent tube is disposed to connect the openings at two ends of the cover respectively , and the wall of the tube ( s ) and the vent tube ( s ) are bonded sealingly together by means of an adhesive to prevent air leakage . the material of the vent tube ( s ) is one or more of the aforesaid soft or hard materials . the cross - sectional shape of the vent tube ( s ) may be any one of the aforesaid vent hole shapes , and may be the same as or different from the vent hole shapes , and the maximum inner diameter thereof is 0 . 5 mm to 4 . 5 mm and the thickness of the wall thereof is 0 . 1 mm to 2 . 0 mm . 3 . in an alternative method of filtering out the noise , one or more noise filtering core sections are filled inside the vent tube to keep certain degrees of breathability while filtering out the ambient noise . the noise filtering core is made of a special porous polymer ( the maximum radial dimension of pores is less than 0 . 5 mm ) selected from an ultrahigh molecular weight polyethylene ( uhmw - pe ), a high - density polyethylene ( hdpe ), polytetrafluoroethylene ( ptfe ), polypropylene ( pp ), polyvinylidene fluoride ( pvdf ), nylon 6 , polyethersulfone ( pes ), or a mixture thereof . the cross - sectional shape of the noise filtering core may be circular , oval , triangular , quadrangular , or polygonal . the breathability of the core ( i . e ., the damping factor to the sound wave transmission , or the frequency and loudness of the external noise to be filtered ) depends on the size , the shape and the distribution density of the pores of the filtering core , the diameter and length of the core , the matching degree between the shape and size of the core and the shape and size of the vent tube , and so on . the multi - sectional filtering core comprises a plurality of cores having different pores , different diameters and different lengths , and the plurality of cores are arranged into one line ( i . e ., in series ) or a plurality of lines ( i . e ., in parallel ) in sequence according to their effective filtering frequency values or not in sequence . in this way , the ambient noise of various frequencies ( 50 hz to 20000 hz ) and loudness ( 10 db to 200 db ) can be filtered out . one testing method to determine the effective noise filtering range of the filtering core is to , by using an audiphone analyzer or an analyzer related to the acoustics , perform experimental calibration directly or indirectly on frequencies and loudness of given ambient noises according to the core material , the size and density of the pores as well as the diameter and length of the core . ( iii ) a door is disposed or not disposed on the cover at a position corresponding to the second vent hole . 1 . as an option for the user , a door that can be opened or closed may be installed on the cover at a position corresponding to the vent hole . 3 . the opening and closing of an electric door may be driven by a micro piezo - electric element . for example , a fixed baffle is disposed to the exterior of the opening , and a plurality of pores are formed on the fixed baffle ; and an movable baffle is disposed in the opening and in close proximity to the exterior baffle , and a plurality of pores similar to those of the fixed baffle are also formed on the movable baffle . the movable baffle can move linearly or rotate in a certain preset direction along the baffle surface so that the pores on the two baffles are offset from each other with a result that the pores of the fixed baffle are blocked by solid portions of the movable baffle . a piezo - electric element is connected to the movable baffle to directly drive motion of the movable baffle . 4 . the weak direct - current power supply required by the piezo - electric element is provided by the power supply of a music player . one end of a power line is connected with the piezo - electric element and the other end of the power line is connected with the earphone plug , and the plug can be plugged into the player to connect with the power supply . a power switch that is controlled manually or wirelessly is disposed on the power line . according to the above descriptions , a micro receiver of a cic - type earphone can extend deep into the second curve of the ear canal and keep a close distance from the ear drum , and a soft ear mold is disposed at an end portion of the cover like the flexible cic - type audiphone . the soft ear mold can fix the earphone inside the ear canal while providing breathability inside the ear canal . alternatively , if the user does not like the earphone wire in case of the wired connection , he or she can adopt the wireless bluetooth technology to connect the earphone with the music player wirelessly . for this purpose , a bluetooth module is added into the earphone so that communication between the bluetooth module and a bluetooth component in the music player can be achieved through wireless connection , and a fully automatic operation can be achieved wirelessly . as a low - impedance conductor and plug technology , thin metal wires ( with a diameter of 0 . 001 mm to 2 . 0 mm ) that are made of materials having low impedance , good toughness , and corrosion resistance such as silver , platinum , mp35n , mp - dft - ag , titanium alloys , nitinol and the like are used to make the earphone conductor or earphone cable ; and the plug may also be made of the same material as the conductor . what described above are only the embodiments of the present disclosure , but are not intended to limit the scope of the present disclosure . any equivalent structures or equivalent process flow modifications that are made according to the specification and the attached drawings of the present disclosure , or any direct or indirect applications of the present disclosure in other related technical fields shall all be covered within the scope of the present disclosure . | 7 |
the car seat transformable into a bed disclosed herein has been conceived to solve the above described problem by a simple mechanism , as it is formed by a minimal number of parts that allow folding the backrest backwards while simultaneously raising slightly the seat cushion to form a horizontal surface and , by means of a simple latch formed by a swivelling part , allow locking the backrest in both the folded and vertical positions , keeping them in this position unless the said locking part is intentionally actuated . more specifically , the mechanism applicable to the car seat object of the invention is characterised in that the backrest is joined to the seat structure by a shaft with respect to which the backrest can revolve , while the backrest is connected to the cushion by another rotation shaft that allows the free folding or rotation of one with respect to the other about this hinge point for the two elements ( the backrest and the cushion ). the structure of the backrest comprises a part in which is established the hinge shaft with the cushion , which in the resting position of the backrest is located under the rear part of the cushion , so that when the backrest is folded backwards the cushion is pushed and raised . in turn , the front part of the cushion is connected by a hinged rod to the fixed seat structure . this seat structure supports all loads and is provided with support elements that act as stops when reaching one of the two final positions corresponding to the seat function as such and the bed function in the seat transformation . these final positions are stabilised by a swivelling part that acts as a latch , mounted by a swivelling shaft to the seat structure so that in one position this part locks a pin provided for such purpose in the backrest structure , fixing its position , while when the backrest is folded the same part , after being released from the aforementioned locking position , again latches onto another pin in the backrest structure to stabilise the new position until the latch part is actuated . according to the description provided so far , it can be seen that the means that allow transforming a car seat into a bed consist of a minimum number of parts with a simple operation while securing the stable positions that the assembly can assume when the backrest is vertical acting as a seat , or when it is horizontal with the cushion raised , acting as a bed . it should be remarked that the aforementioned characteristics , as relates to the configuration of the structure of the backrest in relation to the seat cushion , as well as to the arrangement and assembly of the various parts constituting the mechanism as a whole , make it impossible to move the backrest without moving the cushion , as they are permanently connected through the swivelling shaft common to both and about which they can revolve freely , as mentioned before . to complete the description being made and in order to aid a better understanding of the characteristics of the invention , according to an example of a preferred embodiment of it , a set of drawings is accompanied forming an integral part of the description where , for purposes of illustration only and in a non - limiting sense , the following is shown : fig1 .— shows a lateral cross section view of the car seat assembly in its resting position . fig2 .— shows another lateral cross section view , in this case of the car seat assembly transformed into a bed by folding back the backrest and slightly raising the seat cushion . in view of the aforementioned drawings , it can be seen that the car seat of the invention , transformable into a bed and which conventionally includes a backrest ( 1 ) and a seat cushion ( 2 ), has the specific characteristic that the structure ( 3 ) of the backrest ( 1 ) is hinged to the fixed structure of the seat assembly through a swivelling shaft ( 4 ). the structure ( 5 ) of the cushion ( 2 ) is connected to the fixed structure ( 6 ) by a connecting rod ( 7 ) that is hinged on one end through the swivelling shaft ( 8 ) to the structure ( 5 ) of the cushion ( 2 ). the other end of the connecting rod ( 7 ) is hinged by the shaft ( 9 ) to the general fixed structure ( 6 ) of the seat assembly . the connecting rod ( 7 ) is placed near the front part of the cushion ( 2 ) and under it , as shown clearly in the figures . the structure ( 3 ) of the backrest ( 1 ) and the structure ( 5 ) of the cushion ( 2 ) are related to each other by a swivelling shaft ( 10 ) with respect to which both structures can revolve , this shaft ( 10 ) constituting the hinged coupling means between the seat and the cushion . the structure ( 3 ) of the backrest ( 1 ), in addition to the swivelling shaft ( 4 ) for said backrest and the swivelling or hinge shaft ( 10 ) with respect to the cushion , comprises two pins ( 11 ) and ( 12 ) in which a swivelling part ( 13 ) can lock in the form of a latch . the part ( 13 ) is hinged to the general structure of the seat through a swivelling shaft ( 14 ), so that this part acting as a latch ( 13 ) is provided with a pair of notches ( 15 ) and ( 16 ) that according to the position of the backrest ( 1 ) will form positioning means for the pin ( 11 ) or the pin ( 12 ) respectively , determining the locking and immobilization means for the backrest in either position , that is , the resting position shown in fig1 or its position when transformed into a bed as shown in fig2 . the structure ( 3 ) of the backrest ( 1 ) extends under and behind the seat cushion ( 2 ), determining an end portion ( 17 ) in which are precisely provided the pin ( 11 ) for locking the backrest ( 1 ) in the resting position and the hinging and swivelling shaft ( 10 ) between said structure ( 3 ) of the backrest ( 1 ) and the structure ( 5 ) of the cushion ( 2 ). according to these characteristics , in the resting position shown in fig1 the seat acts as such , the backrest ( 1 ) maintained stable and locked in this position by the latch part ( 13 ) that locks in the pin ( 11 ) of the structure ( 3 ) of the backrest ( 1 ), preventing the latter from folding backwards . however , if the latch ( 13 ) is released from the pin ( 11 ) the backrest ( 1 ), this is its structure ( 3 ), can be folded backwards . this action makes the backrest push on the structure ( 5 ) of the cushion ( 2 ), moving the latter and slightly raising its rear part , while the connecting rod ( 7 ) coupled to the structure ( 5 ) of the cushion ( 2 ) and to the fixed structure ( 6 ) of the seat will swivel to lift the front part of the cushion ( 2 ), providing a continuous surface between the cushion ( 2 ) and the backrest ( 1 ) as shown in fig2 . in this position the pin ( 12 ) of the structure ( 3 ) of the backrest ( 1 ) is locked in the notch ( 16 ) of the latch ( 13 ), remaining stable in his position until the latch ( 13 ) is intentionally released from the pin ( 12 ). as may be seen , the transformation of the car seat into a bed in order to lie on it is achieved in a simple manner , with a minimal number of parts and with full efficiency both functionally and safely between the final positions as a seat and as a bed . | 1 |
fig1 shows an example search system 114 . the search system 114 is an example of an information retrieval system implemented on one or more computers in one or more locations , in which the systems , components , and techniques described below can be implemented . a user 102 can interact with the search system 114 through a user device 104 . for example , the user device 104 can be a computer coupled to the search system 114 through a local area network ( lan ) or wide area network ( wan ), e . g ., the internet . in some implementations , the search system 114 and the user device 104 can be one machine . for example , a user can install an application that facilitates searches on the user device 104 . the user device 104 will generally include a random access memory ( ram ) 106 and a processor 108 . a user 102 can submit a query 110 to a search system 114 . a search engine 130 within the search system 114 performs the search to identify resources matching the query . when the user 102 submits a query 110 , the query 110 may be transmitted through a network 112 to the search system 114 . the search system 114 can be implemented as , for example , computer programs installed on one or more computers in one or more locations that are coupled to each other through a network . the search system 114 includes an index database 122 and the search engine 130 . the search system 114 responds to the query 110 by generating search results 128 , which are transmitted through the network to the user device 104 for presentation to the user 102 , e . g ., as a search results web page to be displayed in a web browser running on the user device 104 . when the query 110 is received by the search engine 130 , the search engine 130 identifies resources that match the query 110 . the search engine 130 will generally include an indexing engine 120 that indexes resources , e . g ., web pages , images , or news articles on the internet , an index database 122 that stores the index information , and a ranking engine 152 or other software that ranks the resources that match the query 110 . the indexing and ranking of the resources can be performed using conventional techniques . the search engine 130 can transmit the search results 128 through the network to the user device 104 for presentation to the user 102 . the search system 114 also includes or can communicate with a spelling suggestion engine 140 that can generate multiple spelling suggestions , i . e ., multiple correctly - spelled words that the user may have been attempting to spell , for each of one or more terms in the query 110 . the generated spelling suggestions are then transmitted with the search results 128 to the user device 104 for presentation to the user 102 . when the user device 104 receives a user input selecting one of the spelling suggestions , the user device can transmit data identifying the selected suggestion to the search system to obtain search results for a query that includes the spelling suggestion from search engine 130 and present the search results to the user 102 . the spelling suggestion engine 140 can be triggered to generate spelling suggestions when certain criteria are met , e . g ., when the number or quality or both of search results included in the search results 128 is below a threshold value or when an estimate generated by a probabilistic language model of a likelihood that the user 102 intended to type the query 110 is below a different threshold value . in some implementations , once the spelling suggestions have been generated by the spelling suggestion engine 140 , the search system 114 determines whether the difference between the number or quality or both of search results for queries including the generated spelling suggestions and the search results 128 exceeds a threshold value . if the difference exceeds the threshold value , the search system 110 transmits the spelling suggestions with the search results 128 to the user device . if the difference does not exceed the threshold value , the search system 110 discards the generated spelling suggestions . in some circumstances , the spelling suggestions generated by the spelling suggestion engine 140 for a particular search query can include at least one aggressive spelling suggestion . a spelling suggestion for a particular term in the query is an aggressive spelling suggestion if it is sufficiently different from the particular term . that is , a spelling suggestion can be an aggressive spelling suggestion if the suggestion and the original term do not share a common phonetic representation in , for example , an alphabetic system of phonetic notation , e . g . the international phonetic alphabet ( ipa ). alternatively , a spelling suggestion can be an aggressive spelling suggestion if the edit distance , e . g ., a damerau - levenshtein distance , between the spelling suggestion and the particular query term is greater than a specified threshold value . the edit distance is defined by the minimum number of operations , e . g ., inserting , removing , or substituting a character or transposing two adjacent characters , required to transform the spelling suggestion into the particular query term . for example , a spelling suggestion can be considered aggressive if it takes more than two operations to transform the correction into the query term . for instance , in order to transform the word “ ammunition ” into an example received query “ amoniction ,” a minimum of three operations are required . one such set of operations is as follows : an “ m ” is removed to generate “ amunition ,” an “ o ” is substituted for the “ u ” to generate “ amonition ,” and a “ c ” is inserted to generate “ amoniction .” a spelling suggestion for a query term can also be considered an aggressive spelling suggestion if the edit distance is greater than a specified proportion of the length of the query term and of the suggestion . for example , the spelling suggestion can be an aggressive spelling suggestion if the edit distance between the suggestion and the query term is more than one - third of the number of characters in each of the query term and the suggestion . a query that includes a badly misspelled word may trigger the spelling suggestion engine 140 to generate aggressive spelling suggestions for the query . in the case of a badly misspelled word , the user intent may be highly uncertain , e . g ., it would be reasonable to conclude that the user was attempting to spell any one of two or more distinct words . in one example , when the received user query is “ amoniction ,” the user may have been attempting to type any one of the words “ ammunition ,” “ admonition ,” or even “ ammonization .” thus , these aggressive spelling suggestions may be included in the spelling suggestions provided by the spelling suggestion engine 140 in response to receiving a query “ amoniction .” fig2 illustrates an example user interface 200 that includes search results 204 and spelling suggestions 206 . the user interface can be presented to a user by a user device , e . g ., a personal computer or a smart phone . the user interface can be implemented as a markup language document , e . g ., an html ( hypertext markup language ) or xml ( extensible markup language ) document , and can have been sent to the user device by a search system , e . g ., the search system 114 of fig1 . the user interface 200 includes the original query 202 , “ credation ” in this example , and a set of search results 204 returned from a search engine , e . g ., search engine 130 of fig1 , in response to the original query 202 . a search result referencing a particular resource can include a selectable link to the resource 220 and a snippet 230 of content about the resource . the user interface 200 also includes spelling suggestions 206 based on the original query 202 displayed in a “ did you mean ” portion of the user interface 200 . a selectable control , e . g ., a link , is displayed for each spelling suggestion . in the illustrated example , the spelling suggestions 206 are spelling suggestions for the original query 202 “ credation .” each spelling suggestion , e . g ., “ creation ,” “ crenation ,” or “ predation ,” is a different word that the user may have been intending to spell when submitting “ credation .” in some implementations , the user interface 200 includes executable instructions that cause the user device , in response to a user input selecting one of the spelling suggestions 206 , to modify the appearance of the user interface 200 to include , in part , search results responsive to the selected spelling suggestion . these executable instructions can be part of a client - side script , e . g ., javascript or vbscript code . alternatively , the executable instructions can be instructions executable on the user device , e . g ., user device - executable java instructions or native device instructions executable on a native user device platform . once the user selects one of the spelling suggestions 206 , the executable instructions can cause the user device to obtain search results for a query including the selected spelling suggestion , and to modify the user interface to remove the spelling suggestions and display search results for a query including the selected spelling suggestion in place of the search results 204 . the instructions can also cause the user device to replace the original query 202 with a query that includes the selected spelling suggestion . in other implementations , in response to the user input selecting one of the spelling suggestions 206 , the user device can obtain , e . g ., from the search system 114 of fig1 , and display a modified user interface that includes search results responsive to a query including the selected spelling suggestion but does not include the spelling suggestions . fig3 illustrates another example user interface 300 that includes search results 304 and spelling suggestions 306 . the user interface 300 includes the original query 302 , “ kolgerne ” in this example , and a set of search results 304 returned from a search engine , e . g ., search engine 130 of fig1 , in response to the original query 302 . the user interface 300 also includes spelling suggestions 306 based on the original query 302 . a selectable link is displayed for each spelling suggestion . in the illustrated example , the spelling suggestions 306 are spelling suggestions for the original query 302 “ kolgerne .” each spelling suggestion , e . g ., “ kolburne ,” “ kalgene ,” or “ kolene ,” is a different word that the user may have been intending to spell when submitting “ kolgerne .” in some implementations , the user interface 300 includes executable instructions that cause the user device , in response to a user input selecting one of the spelling suggestions 306 , to modify the appearance of the user interface 300 to include search results responsive to a query including the selected spelling suggestion while still displaying the spelling suggestions 306 . in other implementations , in response to the user input selecting one of the spelling suggestions 206 , the user device can obtain , e . g ., from the search system 114 of fig1 , and display a modified user interface that includes search results responsive to a query including the selected spelling suggestion and the spelling suggestions 306 . fig4 illustrates an example modified user interface 400 that includes search results 404 that are each responsive to a selected spelling suggestion 402 . in the illustrated example , a user has selected a spelling suggestion 402 (“ kalgene ”), which is one of the spelling suggestions 306 generated for an original query 410 (“ kolgerne ”). in some implementations , in response to user input selecting the spelling suggestion 402 , executable instructions included in the user interface cause the user device to modify the user interface 300 of fig3 to generate the modified user interface 400 . alternatively , the modified user interface 400 can have been obtained from a search system by the user device by activating a link associated with the selected spelling suggestion 402 . in particular , the modified user interface 400 displays search results 406 responsive to the query “ kolgerne ” in place of search results previously displayed in response to the original query 410 . although the search results are different , each of the spelling suggestions 306 is still displayed . this gives the user an opportunity to select another of the spelling suggestions 306 if the search results for the selected spelling suggestion 402 are not satisfactory . additionally , the displayed original query 410 is associated with a link so that , in response to a user input selecting the displayed original query , the user device obtains , either from a local store or from the search system , and displays search results responsive to the original query . furthermore , the appearance of the selected spelling suggestion 402 in the modified user interface 400 has been modified to indicate that it has been selected . in this example , it has been modified by bolding the text of the displayed suggestion and changing the appearance of the suggestion to indicate that it is no longer associated with a link to other search results . the modified user interface 400 also displays the selected spelling suggestion in the input field 404 in place of the original query . this indicates that the displayed search results 406 are responsive to the selected spelling suggestion rather than to the original query . fig5 is a flow chart of an example process 500 for generating a user interface document for displaying spelling suggestions . the process 500 can be performed by a system of one or more computers located in one or more locations . for example , a search system , e . g ., search system 114 of fig1 , can be used to perform the process 500 . the system receives a search query from a user device ( step 502 ). the system obtains search results responsive to the search query and spelling suggestions at least one term in the search query ( step 504 ). the system generates a user interface document that includes the search results , the spelling suggestions , and executable instructions ( step 506 ). when rendered by the user device , the user interface document presents a user interface that displays the search results and the spelling suggestions . the executable instructions , when executed by the user device , cause the user device to modify the presented user interface in response to a user input selecting a displayed spelling suggestion . in some implementations , the instructions cause the user device to modify the user interface to display search results responsive to a query including the selected spelling suggestion in place of the search results responsive to the search query while continuing to display the spelling suggestions . in other implementations , the instructions cause the user device to modify the user interface to no longer display the spelling suggestions in response to the user input . the system transmits the generated user interface document to the user device ( step 508 ). other implementations for modifying a user interface in response to a user selection of a spelling suggestion are possible . for example , instead of the user interface document including executable instructions that cause the user device to modify the user interface , the system can generate a new user interface document and transmit the new user interface document to the user device in response to receiving data identifying the selected spelling suggestion . the new user interface document , when rendered by the user device , can present the modified user interface as described above . in some implementations , the user device receives and displays spelling suggestions for a search query before a user has explicitly submitted the search query to a search system . fig6 illustrates an example user interface 600 that includes spelling suggestions 606 for a search query 602 obtained before the search query has been submitted by a user . the user interface 600 includes executable instructions that cause the user device to detect user input in the input field 608 defining the original search query 602 (“ credation ”) and to transmit data identifying the user input , i . e ., query 602 , to a search system to obtain search results for the query 602 . if spelling suggestions are triggered for a query , the search system may transmit spelling suggestions for at least one term in the query to the user device along with the search results responsive to the query . the instructions can cause the user device to obtain search results , for example , at predetermined intervals , after the user has entered a specified number of characters , or after the user device has detected that no user input has been received for over a threshold period of time . in the illustrated example , the instructions cause the user device to obtain and display the obtained search results 604 and the spelling suggestions 606 before the user has explicitly submitted the original search query 602 , i . e ., without receiving a user input selecting the displayed search button 610 or any other user input submitting the search query . once the spelling suggestions 606 are obtained , they are displayed in a drop - down box below the search query 602 . if a user input selecting one of the spelling suggestions is received , the instructions can cause the client device to obtain search results for a query including the spelling suggestion and to modify the user interface to present the search results for the query including the selected spelling suggestion in place of search results 604 . embodiments of the subject matter and the operations described in this specification can be implemented in digital electronic circuitry , or in computer software , firmware , or hardware , including the structures disclosed in this specification and their structural equivalents , or in combinations of one or more of them . embodiments of the subject matter described in this specification can be implemented as one or more computer programs , i . e ., one or more modules of computer program instructions , encoded on a tangible non - transitory computer storage medium for execution by , or to control the operation of , data processing apparatus . alternatively or in addition , the program instructions can be encoded on an artificially - generated propagated signal , e . g ., a machine - generated electrical , optical , or electromagnetic signal , that is generated to encode information for transmission to suitable receiver apparatus for execution by a data processing apparatus . a computer storage medium can be , or be included in , a computer - readable storage device , a computer - readable storage substrate , a random or serial access memory array or device , or a combination of one or more of them . moreover , while a computer storage medium is not a propagated signal , a computer storage medium can be a source or destination of computer program instructions encoded in an artificially - generated propagated signal . the computer storage medium can also be , or be included in , one or more separate physical components or media ( e . g ., multiple cds , disks , or other storage devices ). the operations described in this specification can be implemented as operations performed by a data processing apparatus on data stored on one or more computer - readable storage devices or received from other sources . the term “ data processing apparatus ” encompasses all kinds of apparatus , devices , and machines for processing data , including by way of example a programmable processor , a computer , a system on a chip , or multiple ones , or combinations , of the foregoing the apparatus can include special purpose logic circuitry , e . g ., an fpga ( field programmable gate array ) or an asic ( application - specific integrated circuit ). the apparatus can also include , in addition to hardware , code that creates an execution environment for the computer program in question , e . g ., code that constitutes processor firmware , a protocol stack , a database management system , an operating system , a cross - platform runtime environment , a virtual machine , or a combination of one or more of them . the apparatus and execution environment can realize various different computing model infrastructures , such as web services , distributed computing and grid computing infrastructures . a computer program ( also known as a program , software , software application , script , or code ) can be written in any form of programming language , including compiled or interpreted languages , declarative or procedural languages , and it can be deployed in any form , including as a stand - alone program or as a module , component , subroutine , object , or other unit suitable for use in a computing environment . a computer program may , but need not , correspond to a file in a file system . a program can be stored in a portion of a file that holds other programs or data ( e . g ., one or more scripts stored in a markup language document ), in a single file dedicated to the program in question , or in multiple coordinated files ( e . g ., files that store one or more modules , sub - programs , or portions of code ). a computer program can be deployed to be executed on one computer or on multiple computers that are located at one site or distributed across multiple sites and interconnected by a communication network . the processes and logic flows described in this specification can be performed by one or more programmable processors executing one or more computer programs to perform actions by operating on input data and generating output . the processes and logic flows can also be performed by , and apparatus can also be implemented as , special purpose logic circuitry , e . g ., an fpga ( field programmable gate array ) or an asic ( application - specific integrated circuit ). processors suitable for the execution of a computer program include , by way of example , both general and special purpose microprocessors , and any one or more processors of any kind of digital computer . generally , a processor will receive instructions and data from a read - only memory or a random access memory or both . the essential elements of a computer are a processor for performing actions in accordance with instructions and one or more memory devices for storing instructions and data . generally , a computer will also include , or be operatively coupled to receive data from or transfer data to , or both , one or more mass storage devices for storing data , e . g ., magnetic , magneto - optical disks , or optical disks . however , a computer need not have such devices . moreover , a computer can be embedded in another device , e . g ., a mobile telephone , a personal digital assistant ( pda ), a mobile audio or video player , a game console , a global positioning system ( gps ) receiver , or a portable storage device ( e . g ., a universal serial bus ( usb ) flash drive ), to name just a few . devices suitable for storing computer program instructions and data include all forms of non - volatile memory , media and memory devices , including by way of example semiconductor memory devices , e . g ., eprom , eeprom , and flash memory devices ; magnetic disks , e . g ., internal hard disks or removable disks ; magneto - optical disks ; and cd - rom and dvd - rom disks . the processor and the memory can be supplemented by , or incorporated in , special purpose logic circuitry . to provide for interaction with a user , embodiments of the subject matter described in this specification can be implemented on a computer having a display device , e . g ., a crt ( cathode ray tube ) or lcd ( liquid crystal display ) monitor , for displaying information to the user and a keyboard and a pointing device , e . g ., a mouse or a trackball , by which the user can provide input to the computer . other kinds of devices can be used to provide for interaction with a user as well ; for example , feedback provided to the user can be any form of sensory feedback , e . g ., visual feedback , auditory feedback , or tactile feedback ; and input from the user can be received in any form , including acoustic , speech , or tactile input . in addition , a computer can interact with a user by sending documents to and receiving documents from a device that is used by the user ; for example , by sending web pages to a web browser on a user &# 39 ; s user device in response to requests received from the web browser . embodiments of the subject matter described in this specification can be implemented in a computing system that includes a back - end component , e . g ., as a data server , or that includes a middleware component , e . g ., an application server , or that includes a front - end component , e . g ., a user computer having a graphical user interface or a web browser through which a user can interact with an implementation of the subject matter described in this specification , or any combination of one or more such back - end , middleware , or front - end components . the components of the system can be interconnected by any form or medium of digital data communication , e . g ., a communication network . examples of communication networks include a local area network (“ lan ”) and a wide area network (“ wan ”), an inter - network ( e . g ., the internet ), and peer - to - peer networks ( e . g ., ad hoc peer - to - peer networks ). the computing system can include users and servers . a user and server are generally remote from each other and typically interact through a communication network . the relationship of user and server arises by virtue of computer programs running on the respective computers and having a user - server relationship to each other . in some embodiments , a server transmits data ( e . g ., an html page ) to a user device ( e . g ., for purposes of displaying data to and receiving user input from a user interacting with the user device ). data generated at the user device ( e . g ., a result of the user interaction ) can be received from the user device at the server . while this specification contains many specific implementation details , these should not be construed as limitations on the scope of any inventions or of what may be claimed , but rather as descriptions of features specific to particular embodiments of particular inventions . certain features that are described in this specification in the context of separate embodiments can also be implemented in combination in a single embodiment . conversely , various features that are described in the context of a single embodiment can also be implemented in multiple embodiments separately or in any suitable subcombination . moreover , although features may be described above as acting in certain combinations and even initially claimed as such , one or more features from a claimed combination can in some cases be excised from the combination , and the claimed combination may be directed to a subcombination or variation of a subcombination . similarly , while operations are depicted in the drawings in a particular order , this should not be understood as requiring that such operations be performed in the particular order shown or in sequential order , or that all illustrated operations be performed , to achieve desirable results . in certain circumstances , multitasking and parallel processing may be advantageous . moreover , the separation of various system components in the embodiments described above should not be understood as requiring such separation in all embodiments , and it should be understood that the described program components and systems can generally be integrated together in a single software product or packaged into multiple software products . thus , particular embodiments of the subject matter have been described . other embodiments are within the scope of the following claims . in some cases , the actions recited in the claims can be performed in a different order and still achieve desirable results . in addition , the processes depicted in the accompanying figures do not necessarily require the particular order shown , or sequential order , to achieve desirable results . in certain implementations , multitasking and parallel processing may be advantageous . | 6 |
the following examples illustrate methods of planning the computation of specifications for burners in implementation of the method , designed for operation at the two levels in question . tubular burner for an appliance operating with natural circulation of combusted air and gas , and with any given rate of aeration : a1 ) section of burner body with aspect ratio ( height to width ) advantageously greater than 1 . 5 , to give mean velocity of the mixture no greater than 2 m / s through the annular section between venturi tube and diffuser . b1 ) venturi tube allowing mean velocity of mixture through the throat equal to or less than 4 m / s ; length of venturi tube exceeding the pierced surface of the diffuser at least by a quantity equal to 50 . . . 150 % of outlet section ; distance between outlet section of venturi and end wall of diffuser such that velocity of the mixture at inversion is on average greater than 2 m / s . c1 ) groups of slots distributed at least over the topmost surface of a diffuser with horizontal axis , and occupying a total area such as to determine a specific loading on the diffuser of less than 0 . 7 kw / cm 2 ; the single slots arranged around and extending transversely or tangential to a central zone , intercalated with smaller complementary holes or otherwise , and circular , rectangular , triangular , trapezoidal in shape or of other non geometrical shape ; the central zone pierced with holes or otherwise , all according to the invention . d1 ) distribution of the groups of slots in ranks ( transverse to the diffuser axis ) set apart one from the next by a distance at least equal to 65 % of the maximum transverse dimension of the group , with an axial distance between the groups of two successive files equal at least to nd / 2 , where d is the axial dimension of one group and n is the number of groups in one rank , or in two successive ranks in a chequered pattern ; e1 ) fuel feed nozzles of variable outlet section , according to the invention . tubular burner for an appliance operating with forced circulation of combusted air and gas , and with a rate of aeration greater than 1 . 1 : a2 ) section of burner body with diffuser of tubular , circular , polygonal or any other profile . d2 ) arrangement of the groups of slots in ranks with groups separated one from the next by a distance at least equal to 65 % of the maximum dimension of the group as measured along the direction of separation . e2 ) nozzle outlet pressures between 100 and 450 mbar at maximum output , according to the pressure rise overcome in effecting the circulation of post - combustion gases ( given , surprisingly , that the value of the aeration rate remains constant with the diminishing pressure value ), maintained advantageously through the use of a variable speed centrifugal compressor of which the outlet is branched to recirculate part of the delivery flow and the inlet is connected to on - off valves by which the gas and air supplies are controlled and alternated to ensure a smooth transition from ignition to steady burn by flooding the combustion chamber initially with air . burner embodied in matching halves for installation preferably in banked elements , in appliances with natural or forced circulation of post - combustion gases and with any given rate of aeration . a3 ) essentially tall mixing and distribution element of elongated rectangular cross section , inserted between the outlet section of a curvilinear axis venturi tube and the diffuser . b3 ) groups of slots according to the invention , aligned longitudinally along the topmost surface of the diffuser , and set apart one from the next at a distance calculable simply as less than half the longitudinal dimension of the group . burner with horizontal axis tubular diffuser , and coaxially disposed internal venturi tube . ______________________________________length of diffuser 394 . 6 mmlength of venturi tube 339 mmdiameter of venturi throat section 26 mmdiameter of venturi outlet section 35 mmdistance between diffuser inlet 324 mmand farthest group of slots______________________________________ cross section of profile appearing as a pair of opposed and upwardly convergent curvilinear lines interconnected uppermost by an arc and connected at bottom through further arcs to a curvilinear base ( see fig1 ): ______________________________________height of diffuser 61 . 3 mmwidth of diffuser 51 . 5 mmradius of curvature of each of 76 mmthe two opposite sidesradius of curvature of base 45 . 5 mmradius of top interconnecting arc 23 mmradius of arcs connecting 13 mmsides and basecentres to the base and top arc coinciding with thevertical axis of symmetry of the diffuser ; centres to the opposite sides coinciding with thehorizontal axis on either side of the vertical axis ofsymmetry . ______________________________________ ______________________________________width of single slot 0 . 5 mmdistance between centres of slots 1 . 25 mmnumber of slots 14slots disposed with axes mutually parallel and within aperipheral zone bordering internally on a rhombus withgreater and lesser diagonals 6 . 1 mm and 5 . 5 mmrespectively and encompassed by a regular octagon withapothem 5 . 75 mm approx . ______________________________________ the groups are distributed along the top surface of the diffuser in four longitudinal files staggered one from the next by a distance of 13 mm , or a distance discernibly half the distance separating groups of the same file , and set apart transversely by a distance ( pitch p2 in fig4 ) of 13 mm , the distance separating groups of the same file ( p1 ) being 26 mm . burner with horizontal axis tubular diffuser and coaxially disposed internal venturi tube . ______________________________________length of diffuser 325 . 6 mmlength of venturi tube 290 mmdiameter of venturi throat section 26 mmdiameter of venturi outlet section 33 mmdistance between diffuser inlet 290 . 6 mmand farthest group of slots______________________________________ cross section of profile appearing as a pair of opposed and downwardly convergent curvilinear lines interconnected at bottom by an arc and connected through further arcs to a curvilinear top stretch ( fig1 ), of dimensions corresponding to those of example 4 and obtained by rotation of the relative axis of symmetry through 180 °. the groups are distributed along the top surface of the diffuser in four longitudinal files staggered one from the next by a distance of 14 . 8 mm , or a distance discernibly half the distance separating groups of the same file , set apart at transverse pitch ( p2 ) of 13 mm , and longitudinal pitch ( p1 ) of 29 . 5 mm . burner with horizontal axis tubular diffuser and coaxially disposed internal venturi tube . ______________________________________length of diffuser 336 . 3 mmlength of venturi tube 302 mmdiameter of venturi throat section 30 mmdiameter of venturi outlet section 42 mmdistance between diffuser inlet 294 . 5 mmand farthest group of slots______________________________________ cross section of profile appearing as a pair of opposed and downwardly convergent curvilinear lines interconnected at bottom by an arc and connected through further arcs to a curvilinear top stretch ( fig1 ): ______________________________________height of diffuser 82 . 9 mmwidth of diffuser 54 . 5 mmradius of curvature of each of 156 mmthe two opposite sidesradius of bottom interconnecting arc 23 . 7 mmradius of curvature of top stretch 44 . 2 mmradius of arcs connecting sides and top 13 mmcentres to the top stretch and interconnecting bottom arecoinciding with the vertical axis of symmetry of thediffuser ; centres to the opposite sides situated at 13 . 5 mm from thehorizontal axis on either side of the vertical axis ofsymmetry . ______________________________________ the groups are distributed along the top surface of the diffuser in four longitudinal files staggered one from the next by a distance of 13 mm , or by a distance discernibly half of that separating groups of the same file , set apart at a transverse pitch ( p2 ) of 14 mm between the first and the second file and between the third and the fourth , and of 13 mm between the second and third , and at a longitudinal pitch ( p1 ) of 26 mm . burner consisting in a bank of discrete slimline diffuser elements exhibiting elongated rectangular section , each liberating 2 km approx , installed in an appliance with natural circulation of combusted air and gas : diameter of central flame stabilizing holes approx 0 . 6 mm to approx 1 mm ; distance between centres of stabilizing holes approx 1 . 3 mm to approx 1 . 7 mm ; transverse pitch of slimline elements approx 18 mm to approx 25 mm ; greater radius of outer oval profile approx 5 mm to approx 15 mm ; lesser radius of outer oval profile approx 2 . 5 mm to approx 7 . 5 mm ; distance between the top surface of the diffuser and the bottom surface of the heat exchanger approx 80 mm to approx 160 mm ; height of distribution chamber between a few mm and 50 mm . burner consisting in a bank of discrete slimline diffuser elements exhibiting elongated rectangular section , for installation in an appliance with natural circulation of combusted air and gas : ______________________________________type of diffuser : sheet metal , marginally convex ; width of diffuser 8 mmheight of distribution chamber 50 mmnumber of slots per group on each of 5two sidesnumber of endmost slots per group 2length of single slot 2 . 5 mmwidth of single slot 0 . 65 mmwidth of each group 7 . 75 mmlength of each group ( between 7 . 8 mmaxes of endmost slots ) pitch of slots 1 . 3 mmpitch of groups 12 . 25 mm______________________________________ burner consisting in a bank of discrete slimline diffuser elements exhibiting elongated rectangular section , for installation in an appliance with natural circulation of combusted air and gas : ______________________________________type of diffuser : sheet metal , marginally convex ; width of diffuser 8 mmheight of distribution chamber 50 mmnumber of slots per group on each 5of two sidesnumber of endmost slots per group 2length of single slot 2 . 5 mmwidth of single slot 0 . 65 mmwidth of each group 7 . 75 mmlength of each group ( between 7 . 8 mmaxes of endmost slots ) pitch of slots 1 . 3 mmpitch of groups 12 . 25 mmdiameter of central hole 0 . 8 mm______________________________________ burner consisting in a bank of discrete slimline diffuser elements exhibiting elongated rectangular section , for installation in an appliance with natural circulation of combusted air and gas : ______________________________________type of diffuser : sheet metal , marginally convex ; width of diffuser 8 mmheight of distribution chamber 50 mmnumber of slots per group on each 5of two sidesnumber of endmost slots per group 2length of single slot 2 . 5 mmwidth of single slot 0 . 65 mmwidth of each group 7 . 75 mmlength of each group ( between 7 . 8 mmaxes of endmost slots ) pitch of slots 1 . 3 mmpitch of groups 12 . 25 mmdiameter of 2 × central hole 0 . 8 mmdistance between centres of central holes 1 . 4 mm______________________________________ when carried into effect , the materials utilized , the dimensions and the constructional details of the invention might be other than disclosed whilst remaining equivalent in terms of the art and by no means straying from within the bounds of protection afforded by the appended claims . for example , the topographics of the holes and slots described and illustrated are applicable not only to conventional tubular and / or slimline diffusers and their derivatives , but also to diffusers of newly conceived geometry . | 5 |
properties of excited luminescence can be fully described by two two - dimensional function , lifetime excitation emission matrix ( l - eem ) τ ( k ex , k em ) and intensity excitation matrix ( i - eem ) eem ( k ex , k em ). the emission spectrum of a fluorophore under an illumination source is the projection of i - eem on the emission axis s m ( σ 2 )=∫ s 0 ( σ 1 ) ieem ( σ 1 , σ 2 ) dσ 2 ( 1 ) where s 0 ( σ 1 ) is the illumination source spectrum . the excitation spectrum of the fluorophore is the projection of i - eem on the excitation axis s x ( )=∫ q ( σ 2 ) ieem ( σ 1 , σ 2 ) dσ 2 ( 2 ) where q ( σ 2 ) is the spectral response of the detector , which could contain a spectrometer or narrowband filter . properties of a fluorophore can be visualized as an object in a multi - dimensional space , whose dimensions are lifetime , spectral intensity , excitation wave vector and emission wave vector . anisotropy may be incorporated as one or more additional dimensions . measurement results can be represented as a projection of the object on the measured axis . fluorophores are distinguishable as long as their projections do not overlap . fig1 depicts an example of prior art of emission multiplexing . as a rule of thumb , emission spectra of multiple fluorophore are distinguishable if half - width of their emission spectra is smaller than emission peak separations . 100 , 105 and 110 are emission spectra of three different fluorophores . 100 and 105 can be distinguished by emission spectra because their emission peak separation 120 is lager than the average of their peak half width 115 and 125 . 105 and 110 cannot be distinguished because peak separation 135 is smaller than the average of peak width 125 and 130 . fig2 depicts multidimensional multiplexing by measuring l - eem ( or i - eem ). l - eem or i - eem of two fluorophores 200 and 205 ( grey scale map in the figure ) are clearly separated in the excitation - emission two - dimensional space , although projections of l - eem ( or i - eem ) on the emission axis overlap . fig3 depicts multiplexing by measuring l - eem and i - eem . two fluorophores 300 and 305 ( visualized as gray spheres ) are clearly separated although they have overlap i - eem ( circular projection on k ex - k em plane ), however different lifetime ( τ axis ). fig4 is an experimental result on measuring i - eem of a mixture of two fluorophores , rhodamine 6g and tris ( 2 , 2 ′- bipyridyl ) ruthenium ( ii ). despite their overlapping emission and excitation spectra , these two fluorophores can be clearly distinguished by the i - eem . intensities peak at excitation 460 mm emission 610 nm are from tris ( 2 , 2 ′- bipyridyl ) ruthenium ( ii ). intensities peak at excitation 525 nm emission 560 nm are from rhodamine 6g . to achieve multidimensional luminescence multiplexing , exemplary devices that can simultaneously measurement lifetime , excitation , emission , and anisotropy of fluorophores ( see , e . g ., u . s . patent application no . 60 / 760 , 085 filed jan . 19 , 2006 ) can be used . for example , fig5 shows an exemplary embodiment of multidimensional multiplexing device . the exemplary instrument may contain a light source ( 500 ), an optical instrument that performs multidimensional measurement ( 505 ). the instrument first performs spectral encoding on the light from 500 ( 501 ). light 501 is sent into optical instrument 505 . spectrally and / or frequency encoded light 510 is focused onto the sample ( 515 ) by an objective ( 520 ). 520 collects the fluorescence emission ( 525 ) and send it back to 505 for detection . imaging can be accomplished by either moving the sample with a translation stage ( 530 ), by scanning the focus of the objective lens , or by scanning the illuminating beam . in another embodiment , the detector may an imaging device such as a ccd or cmos or iccd camera coupled . the detector may be coupled to a spectrometer device or alternatively an interferometer for fourier transform spectral detection . an exemplary embodiment of the slee instrument according to the present invention is capable of determining and / or detecting , e . g ., lifetime , excitation , emission , and anisotropy data of samples . based on the data , various concentrations of multiple fluorescent targets in the samples can be recovered by the exemplary nonlinear unmixing method / procedure with prior knowledge regarding fluorescence characteristics of fluorescent targets . an exemplary multiplexing fluorescent image can be mathematically provided as : where c i ( x , y , z ) can be the concentration distribution of the n th targets , ieem i may be its steady state i - eem of an unit concentration , and τ i may be its lifetime ( assuming lifetime is a constant for a pure fluorophore ). ieem i and τ i can be obtained by measuring pure fluorophores . using such prior knowledge , a recovery of c i ( x , y , z ) can be considered as a non - linear unmixing problem , where the mixing function may follow the multi - exponential decay model . equation ( 4 ) herein above includes four terms . for example , the first term is the total steady state emission power ; the second term is the one - dimensional excitation spectrum s x ( σ 1 ); the third term is the one - dimensional emission spectrum s m ( σ 2 ), and the last term is the raw eem data , which can contain information about both the steady state i - eem and the l - eem eem raw = m ieem ( σ 1 , σ 2 ) s 0 ( σ 1 ) exp ( iφ ) ( 6 ) in which , e . g ., only an exemplary quantity c i ( x , y , z ), highlighted in the equation above , may be unknown . for example , c i ( x , y , z ) can be independent of excitation emission wavenumbers ( σ 1 , σ 2 ). thus , the concentration recovery can be considered as a global analysis problem with respect to the concentrations . an exemplary expression of each targets can be determined simultaneously by , e . g ., least square fitting on c i ( x , y , z ) with equation 6 provided herein . exemplary maps of locations and concentrations of each of the targets can be formed by repeating the least square fitting one each image point . alternative additional linear combinations of data or statistical exemplary methods and / or procedures including partial least squares , principle component analysis , neural nets , or genetic procedures may be utilized to parse the multidimensional luminescence characteristic space to discriminate different targets . alternatively or in addition , a clustering statistical systems and procedures including but not limited to euclidean , normalized , or malahanobis distance , and classification methods , pattern recognition , and / or supervised learning may be utilized to discriminate different targets in the multidimensional luminescence characteristic space . in addition , the association between multiple targets can be measured by , e . g ., a fluorescence energy transfer effect , which can occur when two fluorescent targets ( donor and acceptor ) can have a distance within tens of nanometers . the ieem of fret signals may be provided as follows : ieem fret ( σ 1 , σ 2 )= s x - donor ( σ 1 ) s m - acceptor ( σ 2 ) ( 9 ) where s x - donor ( σ 1 ) can be the excitation spectrum of the donor , and s m - acceptor ( σ 2 ) may be the emission spectrum of the acceptor . a fluorophore “ palette ” with tens to hundreds of unique l - eem and i - eem can be built for densely multiplexed imaging . every fluorophore in the palette may be assigned to individual markers . for example , eem &# 39 ; s of labeled probes of uniform concentration can be measured with sflee prior to the exemplary imaging application . such eem &# 39 ; s can be used in concentration recoveries in the exemplary imaging reconstruction . a list of roughly tens of fluorophores have been widely used in fluorescence imaging procedures . such list provides enough information and materials for imaging biochemical markers in most biomedical applications , but likely not enough for certain applications where a long list of markers have been identified , such as , e . g ., gene profiling . further labeling strategies can be provided for these applications . one exemplary strategy that has been used generally utilizes combinations of fluorophores with fret effects . in such exemplary procedures , probes labeled with a fret pair may have a new i - eem that is not the linear combination of the donor and the acceptor i - eem . lifetime changes caused by fret are also known . for example , exemplary probes labeled with a fret pair can have unique l - eem and i - eem , which can be generated by controlling the fret efficiency , for example by site - selective labeling during oligonucleotide synthesis . with one exemplary fret pair combination , tens of genetic probes with distinguishable eems can be produced . another exemplary strategy / procedure can include the implementation of silicon quantum dots . both theory calculation and experiment have demonstrated that silicon nanocrystals smaller that 5 nm in diameter generally emit luminescence under uv or blue illumination . theory calculations and experimental observations also indicate that while the luminescence is generated by the quantum confinement effect in the nanocrystal structure , surface electron states also likely have an effect . silicon nanocrystals generally have rich variations in both lifetime and spectral intensities that can be maneuverable by different core size / surface coating combinations . one exemplary prediction of quantum confinement theory can be , when the size of the nanocrystal decreases , excitation and emission spectra shift towards shorter wavelength , and emission lifetime decreases . fig6 is the experiment result of the lifetime of porous silicon as a function of excitation wavelength , measured by the sflee device . porous silicon is a material that contains numerous silicon nanocrystals at different sizes . under the prediction of quantum confinement theory , shorter excitation wavelengths probe nanocrystals with smaller sizes , and therefore lifetimes corresponding to shorter excitation wavelengths should be smaller . the results shown fig6 validate this prediction . the purpose of coating is first preventing silicon nanocrystals from oxidization , second , providing function groups that can be further link to specific targets . fig7 depicts a prior art of the structure of a functionized silicon nanocrystal . the crystal has a silicon core ( 700 ). a layer of organic coating ( 705 ) covalently bonds to the surface silicon atoms in the core via c — si or si — o — si bonds . the organic coating molecule consists of a carbon chain ( 710 ) and a reactive group ( 715 ) on the outside . the reactive group ( 715 ) is linked with a biological molecule ( 720 ), for example , an antibody . the biological molecule ( 720 ) has specific binding to the target that the nanocrystal is designed to detect . silicon nanocrystals with different l - eem and i - eem are engineered by changing the core size and the organic coating combination . the foregoing merely illustrates the principles of the invention . various modifications and alterations to the described embodiments will be apparent to those skilled in the art in view of the teachings herein . indeed , the arrangements , systems and methods according to the exemplary embodiments of the present invention can be used with any oct system , ofdi system , spectral domain oct ( sd - oct ) system or other imaging systems , and for example with those described in international patent application pct / us2004 / 029148 , filed sep . 8 , 2004 , u . s . patent application ser . no . 11 / 266 , 779 , filed nov . 2 , 2005 , and u . s . patent application ser . no . 10 / 501 , 276 , filed jul . 9 , 2004 , the disclosures of which are incorporated by reference herein in their entireties . it will thus be appreciated that those skilled in the art will be able to devise numerous systems , arrangements and methods which , although not explicitly shown or described herein , embody the principles of the invention and are thus within the spirit and scope of the present invention . in addition , to the extent that the prior art knowledge has not been explicitly incorporated by reference herein above , it is explicitly being incorporated herein in its entirety . all publications referenced herein above are incorporated herein by reference in their entireties . | 6 |
hereinafter reference will now be made in detail to various embodiments of the present invention , examples of which are illustrated in the accompanying drawings and described below . fig1 is a side view showing a state in which a button of a liquid instrument according to the present invention is closed , fig2 is a perspective view showing a state in which a button of a liquid instrument according to the present invention is closed , fig3 is a perspective view showing a button of a liquid instrument being up - downed to be pumped in a state in which a button of a liquid instrument according to the present invention is opened , fig4 to 7 are a plain view , a side view and a perspective view , respectively , showing the button of the liquid instrument according to the present invention , fig8 to 11 are a plain view , a side view and a perspective view , respectively , showing a button body of the liquid instrument according to the present invention , fig1 to 15 are a plain view , a side view and a perspective view , respectively , showing a shoulder of the liquid instrument according to the present invention , and fig1 and 17 are cross - sectional views showing an opening state and a closing state of the button , respectively , of the liquid instrument according to the present invention . as shown in the drawings , a liquid instrument of the present invention comprising a container 10 for receiving the contents in a liquid state or a gel phase , and a discharging pump 50 which is connected to the upper inside of the container 10 and discharges the contents through an external pressure , may include a shoulder 20 connected to an upper part of the container 10 , a button body 30 inserted into the shoulder 20 and movable vertically , and a button 40 which is connected to an upper surface of the button body 30 and allows the button body 30 not to be operated while opening and closing the contents pumping hole 31 of the button body 30 . the button body 30 is configured such that its lower surface is opened and its upper surface is concaved , and further a sliding hole 32 formed symmetrically on both sides so that a plurality of leg portions of the button 40 are inserted and slid therein . further , a side wall 32 a is formed on the respective side of the sliding hole 32 so that the side wall is stumbled - connected to a stumbling protrusion 42 formed on a lower end of the leg portion of the button 40 and a contents pumping hole 31 is formed on a middle of the upper surface . here , a guide cap 33 is formed forward on the upper surface of the button body 30 for guiding the sliding of the button 40 . a sliding limitation groove 34 is formed on a peripheral region of the contents pumping hole 31 of the button body 30 so that a lower hole 44 is inserted to a lower part of the button 40 for limiting the button not to slide excessively . the upper surface of the button 40 is shaped as the same concave surface as the upper surface of the button body 30 and the leg portions are formed on the lower surface of the button to be inserted , respectively into the sliding hole 32 of the button body 30 . the leg portions includes a guide protrusion 42 which is guided along the sliding hole 32 , a leg 43 protruding downward on a rear end of the guide protrusion 42 , and a stumbling protrusion 41 to be hung over the side wall lower end of the sliding hole 31 at the distal end of the leg 43 . a lower hole 44 protruding downward is formed on a center line in a sliding direction on a lower surface of the button 40 so that when the button 40 is slid forward totally , that is , the button is biased rearward , the lower hole corresponds to the contents pumping hole 31 of the button body 30 . further , a front lower surface discharging hole 45 for discharging the contents is formed on a front side lower surface of the button 40 to be communicated with the lower hole 44 . the shoulder 20 includes a screw connection portion to be screw - connected to the upper outer peripheral surface of the container 10 on its lower part , a cylindrical protrusion 23 protruding upward and having a smaller inner diameter than that of the screw connection portion 22 , an inner protrusion 24 protruding as a cylinder form and forming a groove 24 a spaced at a predetermined distance from the inner peripheral surface of the cylinder protrusion 23 , and a stepped surface 25 at a lower level , forming a hollow space 25 a on an inner peripheral surface of the inner protrusion 24 on a center . here , the leg 43 of the button 40 is placed on the stepped surface 25 when the button is locked , and when the button is slid forward , the leg 43 is placed on the hollow space 25 a at a center of the stepped surface 25 for the button body 30 to be compressed . with respect to an operation of the open and close apparatus of a button sliding type of a contents instrument according to the present invention as configured in the forgoing , firstly , when the button 40 is placed at a center of the container 10 , as shown in fig1 , the button body 30 , together with the button 40 , is not compressed , as shown in fig1 . in order to open the contents instrument for discharging the contents through the discharging hole 45 , firstly , an upper surface of the button is slid by using a finger , the guide protrusion 42 of the button 40 is moved forward within the sliding hole 32 of the button body 30 and the discharging hole 45 is protruded toward a front lower end . at this time , the lower hole 44 corresponds to the contents pumping hole 31 of the button body 30 and at the same time the leg 43 of the button 40 is placed on the hollow space 25 a of the stepped surface 25 of the shoulder 20 at a center , thereby compressing the button body 30 . in this state , the button 40 is compressed downward , the button body 30 descends to operate the discharging pump 50 , thereby pumping the contents . after pumping the contents , when the button 40 is slid back rearward to be placed on a center ( a state in which the button is not further slid by the sliding limitation groove 34 on the upper surface of the button body 30 ), the leg 43 of the button 40 is placed on the stepped surface 25 of the shoulder 20 and at the same time the lower hole 44 of the button 40 is departed from the contents pumping hole 31 of the button body 30 . in this state , even in case of the button 40 being pushed downward , the button is not to be compressed due to the stepped surface 25 of the shoulder 20 . according to the open and close apparatus of a button sliding type for a liquid instrument as configured in the foregoing , the lid is opened and closed by sliding a pump button provided on the liquid instrument without separating a lid when using the liquid instrument so that a separate lid is not prepared to configured simply and save manufacturing cost , and further its appearance is beautiful due to a simple structure and functionality is improved . while the invention will be described in conjunction with exemplary embodiments , it will be understood that present description is not intended to limit the invention to those exemplary embodiments . on the contrary , the invention is intended to cover not only the exemplary embodiments , but also various alternatives , modifications , equivalents and other embodiments , which may be included within the spirit and scope of the invention as defined by the appended claims . | 1 |
the compounds of the present invention are generally named according to the iupac or cas nomenclature system . abbreviations which are well known to one of ordinary skill in the art may be used ( e . g . “ ph ” for phenyl , “ me ” for methyl , “ et ” for ethyl , “ h ” for hour or hours , “ rt ” for room temperature , and etc .). the carbon atom content of various hydrocarbon - containing moieties is indicated by a prefix designating the minimum and maximum number of carbon atoms in the moiety , i . e ., the prefix c i - j indicates a moiety of the integer “ i ” to the integer “ j ” carbon atoms , inclusive . thus , for example , c 1 - 7 alkyl refers to alkyl of one to seven carbon atoms , inclusive . specific and preferred values listed below for radicals , groups , moieties , substituents , or ranges , are for illustration only ; they do not exclude other defined values or other values within defined ranges . alkyl denotes both straight and branched groups ; but reference to an individual group or moiety such as “ propyl ” embraces only the straight chain group or moiety , a branched chain isomer such as “ isopropyl ” being specifically referred to . aryl denotes a phenyl radical or an ortho - fused bicyclic carbocyclic group or moiety having about nine to ten ring atoms in which at least one ring is aromatic . it is to be understood that the present invention encompasses any racemic , optically - active , polymorphic , tautomeric , or stereoisomeric form , or mixture thereof , of a compound of the invention , which possesses the useful properties described herein . in cases where compounds are sufficiently basic or acidic to form stable nontoxic acid or base salts , administration of the compounds as salts may be appropriate . examples of pharmaceutically acceptable salts are organic acid addition salts formed with acids which form a physiological acceptable anion , for example , tosylate , methanesulfonate , acetate , citrate , malonate , tartarate , succinate , benzoate , ascorbate , ( α - ketoglutarate , maleate , fumarate , benzenesulfonate and ( α - glycerophosphate . suitable inorganic salts may also be formed , including hydrobromide , hydrochloride , sulfate , nitrate , bicarbonate , and carbonate salts . pharmaceutically acceptable salts may be obtained using standard procedures well known in the art , for example by reacting a sufficiently basic compound such as an amine with a suitable acid affording a physiologically acceptable anion . alkali metal ( for example , sodium , potassium or lithium ) or alkaline earth metal ( for example calcium ) salts of carboxylic acids can also be made . in one embodiment , r 1 is h or c 1 - 4 alkyl . in another embodiment , each r 2 is independently h or c 1 - 6 alkyl . in one embodiment , each r 3 is independently h , fluoro or c 1 - 4 alkyl . in one embodiment , each r 3 is fluoro , n is one or two . in one embodiment , each r 5 is h independently or c 1 - 4 alkyl . in one embodiment , each r 5 is independently h , or c (═ o ) r 1 . in one embodiment , each r 5 is independently h , or c (═ o ) rch 3 . in one embodiment , each r 5 is independently h , s ( o ) 2 r 1 , c ( o ) nr 1 r 1 , co 2 r 1 , or csr 1 . in one embodiment , r 6 is h , methyl or ethyl . in one embodiment , r 8 is h or fluoro , or methyl . specific example of the present invention is n -[ 5 -( 1 , 4 - diazepan - 1 - yl )- 2 -[( 3 - fluorophenyl ) sulfonyl ] phenyl ] acetamide , or its pharmaceutically acceptable salt thereof . specific example of the present invention is 5 -( 1 , 4 - diazepan - 1 - yl )- 2 -( phenylsulfonyl ) phenylamine , or its pharmaceutically acceptable salt thereof . specific example of the present invention is n -[ 5 -( 1 , 4 - diazepan - 1 - yl )- 2 -( phenylsulfonyl ) phenyl ] acetamide , or its pharmaceutically acceptable salt thereof . chart i and chart ii describe the preparation of compounds of the present invention . all of the starting materials are prepared by procedures described herein or by procedures that would be well known to one of ordinary skill in organic chemistry . as shown in chart i , treatment of commercially available substituted or unsubstituted 2 , 5 - difluoronitro - benzene 1 with the desired arylthiol gave thioether 2 . this reaction is usually carried out in the presence of a suitable base such as potassium carbonate and a suitable solvent such as acetonitrile . the oxidation of 2 to sulfone 3 is usually carried out using m - cpba ( in ch 2 cl 2 ) or h 2 o 2 ( in hot acetic acid ) as the oxidizing agents . when using m - cpba , the reaction is done at ambient temperature in a solvent such as ch 2 cl 2 . the desired arylpiperazine moiety 4 is formed by a second nucleophilic substitution reaction , using the appropriate amine . again , this displacement is done using potassium carbonate as the base and a solvent such as acetonitrile . depending on the r 1 - substituent , reduction of nitrobenzene 4 to the aniline 5 is accomplished using raney nickel and hydrazine . the solvent system most typically utilized is etoh / thf . if further purification of 5 is desired , piperazine 4 is protected as the tert - butyl carbamate using di - tert - butyl dicarbonate ( thf , h 2 o ) to give carbamate 6 . this compound is reduced as described above using raney nickel , to give aniline 7 . in contrast to compound 5 , carbamate 7 can be readily purified by chromatography . deprotection using tfa in ch 2 cl 2 provided bis - sulfone 5 . if desired , carbamate 7 can be alkylated to give compound of structure 8 . in this case , treatment of 7 with methyltriflate in the presence of potassium hydride gives the methylamine 8 . deprotection , as described above , using tfa in ch 2 cl 2 provides a compound of structure 5 . alternatively , n - alkylated compound of structure 5 can be prepared according to chart ii as shown here . reaction of a compound of structure 2 with a desired piperazine , as described in chart i ( potassium carbonate / acetonitrile ; at ambient to elevated temperatures ), provided piperazine 9 . protection of 9 using di - tert - butyl dicarbonate provided carbamate 10 . reduction of nitro 10 using raney nickel and hydrazine gives aniline 11 , which can be readily reacted with acetyl chloride to give 12 . this reaction is carried out quite effectively using acetyl chloride ( or other acyl chlorides or ethyl formate ), in the presence of dmap , and hunigs base , in a suitable solvent such as ch 2 cl 2 . oxidation of 12 to the sulfone is accomplished with m - cpba ( ch 2 cl 2 , − 78 ° c .- rt ) to give 13 . reduction of amide 13 utilizing borane - methylsulfide complex gives the desired alkylamine 14 . the piperazine is the deprotected and alkylated to provide a compound of structure 5 . if desired , a dialkylated compound can also be prepared according to the methods well - known in the art . if desired , amides such as 13 in chart ii may be simply deprotected using either tfa , hcl in ethoh , or tsoh to give acetamide 5 ( r5 ═ coch 3 ). sulfonamides can be prepared in a similar fashion . the inventive compounds may be used in their native form or as salts . in cases where compounds are sufficiently basic or acidic to form stable nontoxic acid or base salts , administration of the compounds as salts may be appropriate . examples of pharmaceutically acceptable salts are organic acid addition salts formed with acids which form a physiological acceptable anion , for example , tosylate , methanesulfonate , acetate , citrate , malonate , tartarate , succinate , benzoate , ascorbate , etoglutarate , and glycerophosphate . suitable inorganic salts may also be formed , including hydrochloride , sulfate , nitrate , bicarbonate , and carbonate salts . pharmaceutically acceptable salts may be obtained using standard procedures well known in the art , for example by reacting a sufficiently basic compound such as an amine with a suitable acid affording a physiologically acceptable anion . alkali metal ( for example , sodium , potassium or lithium ) or alkaline earth metal ( for example calcium ) salts of carboxylic acids can also be made . compounds of the present invention can conveniently be administered in a pharmaceutical composition containing the compound in combination with a suitable excipient , the composition being useful in combating cns diseases . pharmaceutical compositions containing a compound appropriate for cns diseases &# 39 ; use are prepared by methods and contain excipients which are well known in the art . a generally recognized compendium of such methods and ingredients is remington &# 39 ; s pharmaceutical sciences by e . w . martin ( mark publ . co ., 15th ed ., 1975 ). the compounds and compositions of the present invention can be administered parenterally ( for example , by intravenous , intraperitoneal or intramuscular injection ), topically ( including but not limited to surface treatment , transdermal application , and nasal application ), intravaginally , orally , or rectally , depending on whether the preparation is used to treat a specific disease . for oral therapeutic administration , the active compound may be combined with one or more excipients and used in the form of ingestible tablets , buccal tablets , troches , capsules , elixirs , suspensions , syrups , wafers , and the like . such compositions and preparations should contain at least 0 . 1 % of active compound . the percentage of the compositions and preparations may , of course , be varied and may conveniently be between about 2 to about 60 % of the weight of a given unit dosage form . the amount of active compound in such therapeutically useful compositions is such that an effective dosage level will be obtained . the tablets , troches , pills , capsules , and the like may also contain the following : binders such as gum tragacanth , acacia , corn starch or gelatin ; excipients such as dicalcium phosphate ; a disintegrating agent such as corn starch , potato starch , alginic acid and the like ; a lubricant such as magnesium stearate ; and a sweetening agent such as sucrose , fructose , lactose or aspartame or a flavoring agent such as peppermint , oil of wintergreen , or cherry flavoring may be added . when the unit dosage form is a capsule , it may contain , in addition to materials of the above type , a liquid carrier , such as a vegetable oil or a polyethylene glycol . various other materials may be present as coatings or to otherwise modify the physical form of the solid unit dosage form . for instance , tablets , pills , or capsules may be coated with gelatin , wax , shellac or sugar and the like . a syrup or elixir may contain the active compound , sucrose or fructose as a sweetening agent , methyl and propylparabens as preservatives , a dye and flavoring such as cherry or orange flavor . of course , any material used in preparing any unit dosage form should be pharmaceutically acceptable and substantially non - toxic in the amounts employed . in addition , the active compound may be incorporated into sustained - release preparations and devices such as the osmotic release type devices developed by the alza corporation under the oros trademark . the compounds or compositions can also be administered intravenously or intraperitoneally by infusion or injection . solutions of the active compound or its salts can be prepared in water , optionally mixed with a nontoxic surfactant . dispersions can also be prepared in glycerol , liquid polyethylene glycols , triacetin , and mixtures thereof and in oils . under ordinary conditions of storage and use , these preparations contain a preservative to prevent the growth of microorganisms . pharmaceutical dosage forms suitable for injection or infusion can include sterile aqueous solutions or dispersions or sterile powders comprising the active ingredient which are adapted for the extemporaneous preparation of sterile injectable or infusible solutions or dispersions , optionally encapsulated in liposomes . in all cases , the ultimate dosage form should be sterile , fluid and stable under the conditions of manufacture and storage . the liquid carrier or vehicle can be a solvent or liquid dispersion medium comprising , for example , water , ethanol , a polyol ( for example , glycerol , propylene glycol , liquid polyethylene glycols , and the like ), vegetable oils , nontoxic glyceryl esters , and suitable mixtures thereof . the proper fluidity can be maintained , for example , by the formation of liposomes , by the maintenance of the required particle size in the case of dispersions or by the use of surfactants . the prevention of the action of microorganisms can be brought about by various antibacterial and antifungal agents , for example , parabens , chlorobutanol , phenol , sorbic acid , thimerosal , and the like . in many cases , it will be preferable to include isotonic agents , for example , sugars , buffers or sodium chloride . prolonged absorption of the injectable compositions can be brought about by the use in the compositions of agents delaying absorption , for example , aluminum monostearate and gelatin . sterile injectable solutions can be prepared by incorporating the active compound in the required amount in the appropriate solvent with various of the other ingredients enumerated above , as required , followed by filter sterilization . in the case of sterile powders for the preparation of sterile injectable solutions , the preferred methods of preparation are vacuum drying and the freeze drying techniques , which yield a powder of the active ingredient plus any additional desired ingredient present in the previously sterile - filtered solutions . for topical administration , the present compounds may be applied in pure form , i . e ., when they are liquids . however , it will generally be desirable to administer them to the skin as compositions or formulations , in combination with a dermatologically acceptable carrier , which may be a solid or a liquid . useful solid carriers include finely divided solids such as talc , clay , microcrystalline cellulose , silica , alumina and the like . useful liquid carriers include water , alcohols or glycols or water - alcohol / glycol blends , in which the present compounds can be dissolved or dispersed at effective levels , optionally with the aid of non - toxic surfactants . adjuvants such as fragrances and additional antimicrobial agents can be added to optimize the properties for a given use . the resultant liquid compositions can be applied from absorbent pads , used to impregnate bandages and other dressings , or sprayed onto the affected area using pump - type or aerosol sprayers . thickeners such as synthetic polymers , fatty acids , fatty acid salts and esters , fatty alcohols , modified celluloses or modified mineral materials can also be employed with liquid carriers to form spreadable pastes , gels , ointments , soaps , and the like , for application directly to the skin of the user . examples of useful dermatological compositions which can be used to deliver the compounds of formula i to the skin are known to the art ; for example , see jacquet et al . ( u . s . pat . no . 4 , 608 , 392 ), geria ( u . s . pat . no . 4 , 992 , 478 ), smith et al . ( u . s . pat . no . 4 , 559 , 157 ) and wortzman ( u . s . pat . no . 4 , 820 , 508 ). useful dosages of the compounds of formula i can be determined by comparing their in vitro activity , and in vivo activity in animal models . methods for the extrapolation of effective dosages in mice , and other animals , to humans are known to the art ; for example , see u . s . pat . no . 4 , 938 , 949 . the compound is conveniently administered in unit dosage form ; for example , containing 1 to 1000 mg , conveniently 5 to 750 mg , most conveniently , 5 to 400 mg of active ingredient per unit dosage form . the desired dose may conveniently be presented in a single dose or as divided doses administered at appropriate intervals , for example , as two , three , four or more sub - doses per day . the sub - dose itself may be further divided , e . g ., into a number of discrete loosely spaced administrations ; such as multiple inhalations from an insufflator or by application of a plurality of drops into the eye . the compositions can be administered orally or parenterally at dose levels , calculated as the free base , of about 0 . 01 to 300 mg / kg mammal body weight , preferably 0 . 1 to 50 mg / kg of mammal body weight , more preferably 1 . 0 to 30 mg / kg of mammal body weight , and can be used in man in a unit dosage form , administered one to four times daily in the amount of 1 to 1000 mg per unit dose . generally , the concentration of the compound ( s ) of formula i in a liquid composition , such as a lotion , will be from about 0 . 1 - 25 wt -%, preferably from about 0 . 5 - 10 wt -%. the concentration in a semi - solid or solid composition such as a gel or a powder will be about 0 . 1 - 5 wt -%, preferably about 0 . 5 - 2 . 5 wt -%. the exact regimen for administration of the compounds and compositions disclosed herein will necessarily be dependent upon the needs of the individual subject being treated , the type of treatment and , of course , the judgment of the attending practitioner . the compounds of the present invention can be administered to an animal in need of treatment . in most instances , this will be a human being , but the treatment of livestock and companion animals is also specifically contemplated as falling within the scope of the instant invention . generally , compounds of the invention are 5 - ht ligands . the ability of a compound of the invention to bind or act at a 5 - ht receptor , or to bind or act selectively at a specific 5 - ht receptor subtype can be determined using in vitro and in vivo assays that are known in the art . as used herein , the term “ bind selectively ” means a compound binds at least 2 times , preferably at least 10 times , and more preferably at least 50 times more readily to a given 5 - ht subtype than to one or more other subtypes . preferred compounds of the invention bind selectively to one or more 5 - ht receptor subtypes . the ability of a compound of the invention to act as a 5 - ht receptor agonist or antagonist can also be determined using in vitro and in vivo assays that are known in the art . all of the example compounds provided above are 5 - ht ligands , with the ability to displace & gt ; 50 % of a radiolabeled test ligand from one or more 5 - ht receptor subtypes at a concentration of 1 μm . the procedures used for testing such displacement are well known and illustrated below . hela cells containing the cloned human 5 - ht 6 receptor are acquired from dr . david r . sibley &# 39 ; s laboratory in national institute of health ( see sibley , d . r ., j . neurochemistry , 66 , 47 - 56 , 1996 ). cells are grown in high glucose dulbecco &# 39 ; s modified eagle &# 39 ; s medium , supplemented with l - glutamine , 0 . 5 % sodium pyruvate , 0 . 3 % penicillin - streptomycin , 0 . 025 % g - 418 and 5 % gibco fetal bovine serum and then are harvested , when confluent , in cold phosphate buffered saline . harvested intact cells are washed once in cold phosphate - buffered saline . the cells are pelleted and resuspended in 100 ml of cold 50 mm tris , 5 mm edta and 5 mm egta , ph 7 . 4 . homogenization is with a vir tishear generator , 4 cycles for 30 seconds each at setting 50 . the homogenized cells are centrifuged at 700 rpm ( 1000 × g ) for 10 minutes and the supernatant is removed . the pellet is resuspended in 100 ml of the above buffer and rehomogenized for 2 cycles . the rehomogenized cells are then centrifuged at 700 rpm ( 1000 × g ) for 10 minutes and the supernatant is removed . the combined supernatant ( 200 ml ) is centrifuged at 23 , 000 rpm ( 80 , 000 × g ) for 1 hour in a beckman rotor ( 42 . 1 ti ). the membrane pellet is resupended in 50 - 8 - ml of assay buffer containing hepes 20 mm , mgcl2 10 mm , nacl 150 mm , edta 1 mm , ph 7 . 4 and stored frozen in aliqouts at − 70 ° c . the radioligand binding assay used [ 3 h ]- lysergic acid diethylamnide ( lsd ). the assay is carried out in wallac 96 - well sample plates by the addition of 11 μl of the test sample at the appropriate dilution ( the assay employed 11 serial concentrations of samples run in duplicate ), 11 μl of radioligand , and 178 μl of a washed mixture of wga - coated spa beads and membranes in binding buffer . the plates are shaken for about 5 minutes and then incubated at room temperature for 1 hour . the plates are then loaded into counting cassettes and counted in a wallac microbeta trilux scintillation counter . eleven serial dilutions of test compounds are distributed to assay plates using the pe / cetus pro / pette pipetter . these dilutions were , followed by radioligand and the bead - membrane mixture prepared as described above . the specifically bound cpm obtained are fit to a one - site binding model using graphpad prism ver . 2 . 0 . estimated ic 50 values are converted to ki values using the cheng - prusoff equation ( cheng , y . c . et al ., biochem . pharmacol ., 22 , 3099 - 108 , 1973 ). the ki values obtained from the assay are shown in 1 . the compounds and their preparations of the present invention will be better understood in connection with the following examples , which are intended as an illustration of and no a limitation upon the scope of the invention . to a mixture of thiophenol ( 0 . 96 ml , 9 . 3 mmol ) and potassium carbonate ( 1 . 4 g , 10 . 1 mmol ) in 16 ml of dry acetonitrile is added 2 , 5 - difluoronitrobenzene ( 1 . 0 ml , 9 . 2 mmol ). the mixture is allowed to stir overnight at rt . water ( 30 ml ) and ch 2 cl 2 are added and the layers seperated . the aqueous layer is extracted with ch 2 cl 2 ( 3 × 25 ml ). the combined organics are dried over mgso 4 , filtered , and concentrated . recrystallization from etoac / heptane gives 2 . 3 g ( 99 %) of the title compound as a solid , mp 66 - 67 ° c . ir ( drift ) 1576 , 1526 , 1468 , 1344 , 1286 , 1269 , 1209 , 946 , 866 , 819 , 806 , 756 , 749 , 693 , 645 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 95 , 7 . 54 - 7 . 60 , 7 . 46 - 7 . 52 , 7 . 07 - 7 . 15 , 6 . 85 ; ms ( ei ) m / z 249 ( m + ), 203 , 202 , 186 , 185 , 184 , 78 , 77 . a solution of 3 - chloroperoxybenzoic acid ( 15 g , 87 mmol ) in 110 ml of ch 2 cl 2 is slowly added to a mixture of 4 - fluoro - 2 - nitro - 1 -( phenylsulfanyl ) benzene ( 8 . 7 g , 35 mmol ) and sodium bicarbonate ( 7 . 3 g , 87 mmol ) in 260 ml of ch 2 cl 2 , at − 78 ° c . the solution is stirred at − 78 ° c . for 1 h , then warmed to rt and allowed to stir overnight . the mixture is partitioned between nahco 3 ( 200 ml ) and ch 2 cl 2 ( 3 × 100 ml ). the combined organics are dried over mgso 4 , filtered and concentrated to a white solid . recrystallization from etoac / heptane gives 9 . 7 g ( 99 %) of the title compound as a solid , mp 127 - 129 ° c . ; ir ( drift ) 1602 , 1590 , 1551 , 1371 , 1329 , 1318 , 1274 , 1227 , 1161 , 1083 , 881 , 811 , 752 , 728 , 685 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 37 - 8 . 43 , 7 . 92 - 8 . 00 , 7 . 43 - 7 . 70 ; ms ( ei ) m / z 281 ( m + ), 200 , 188 , 186 , 170 , 97 , 93 , 77 . a solution of 4 - fluoro - 2 - nitro - 1 -( phenylsulfonyl ) benzene ( 1 . 0 g , 3 . 6 mmol ), piperazine ( 0 . 37 g , 4 . 3 mmol ), and potassium carbonate ( 0 . 79 g , 5 . 7 mmol ) is stirred in 35 ml of acetonitrile overnight at reflux . the mixture is cooled to rt and 35 ml of water and ch 2 cl 2 are added . the layers are separated and the aqueous layer extracted with ch 2 cl 2 ( 3 × 35 ml ). the combined organics are dried over mgso 4 , filtered , and concentrated . purification via flash column chromatography ( 15 % meoh / ch 2 cl 2 ) gives 1 . 1 g ( 92 %) of title compound as a solid , mp 180 - 182 ° c . ir ( drift ) 1601 , 1536 , 1448 , 1367 , 1358 , 1303 , 1254 , 1153 , 1138 , 1085 , 1022 , 774 , 750 , 724 , 688 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 10 , 7 . 89 - 7 . 95 , 7 . 47 - 7 . 55 , 6 . 95 - 7 . 05 , 3 . 31 - 3 . 45 , 2 . 96 - 3 . 08 , 2 . 51 ; ms ( el ) m / z 347 ( m + ), 305 , 275 , 258 , 152 , 118 , 77 . to a solution of 1 -[ 3 - nitro - 4 -( phenylsulfonyl ) phenyl ] piperazine ( 1 . 5 g , 4 . 3 mmol ) and naoh ( 0 . 38 g , 9 . 5 mmol ) in 64 ml of a 1 : 1 thf : h 2 o solvent system is added a solution of di - tert - butyl dicarbonate ( 1 . 0 g , 4 . 7 mmol ) in 5 ml of thf . the solution is stirred at rt for 16 h . the mixture is neutralized with 6 n hcl and 25 ml of etoac is added . the layers are separated and the aqueous layer is extracted with etoac ( 3 × 25 ml ). the combined organics are dried over mgso 4 , filtered , and concentrated . recrystallization from etoac / hexane gives 1 . 7 g ( 87 %) of the title compound as solid , mp 190 - 191 ° c . ir ( drift ) 1690 , 1607 , 1544 , 1415 , 1362 , 1350 , 1322 , 1306 , 1290 , 1243 , 1177 , 1151 , 1138 , 748 , 688 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 13 , 7 . 89 - 7 . 97 , 7 . 47 - 7 . 62 , 6 . 96 - 7 . 05 , 3 . 53 - 3 . 64 , 3 . 34 - 3 . 45 , 1 . 48 ; ms ( ei ) m / z 447 ( m + ), 305 , 275 , 258 , 152 , 91 , 77 . to a solution of tert - butyl 4 -[ 3 - nitro - 4 -( phenylsulfonyl ) phenyl ]- 1 - piperazinecarboxylate ( 0 . 85 g , 1 . 8 mmol ) in 20 ml of a 4 : 1 etoh : thf solvent system is added raney nickel ( 130 mg suspension in etoh ) followed by hydrazine monohydrate ( 0 . 44 ml , 9 . 1 mmol ). the mixture is stired vigorously for 2 h and then filtered through celite that is pretreated with water . the filtrate is concentrated , and the residue crystallized from meoh / etoac / hexane to give 0 . 76 g ( 99 %) of the aniline as a white solid , mp 135 - 137 ° c . ir ( drift ) 1693 , 1602 , 1552 , 1448 , 1420 , 1390 , 1366 , 1306 , 1288 , 1249 , 1224 , 1168 , 1142 , 1097 , 736 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 85 - 7 . 93 , 7 . 68 , 7 . 41 - 7 . 56 , 6 . 32 , 5 . 98 , 5 . 09 , 3 . 48 - 3 . 58 , 3 . 18 - 3 . 28 , 1 . 47 ; ms ( ei ) m / z 417 ( m + ), 361 , 317 , 275 , 167 , 91 , 77 to a solution of tert - butyl 4 -[ 3 - amino - 4 -( phenylsulfonyl ) phenyl ]- 1 - piperazinecarboxylate ( 0 . 68 g , 1 . 6 mmol ) in 18 ml of ch 2 cl 2 at 0 ° c ., is added trifluoroacetic acid ( 18 ml ). the solution is stirred at 0 ° c for 2 h and then concentrated . methylene chloride ( 30 ml ) and 1 n naoh ( 30 ml ) are added and the layers seperated . the aqueous layer is extracted with ch 2 cl 2 ( 3 × 25 ml ) and the combined organic layers dried over mgso 4 , filtered , and concentrated to give 0 . 46 g ( 89 %) of a white solid . the solid is dissolved in 50 ml of meoh and hcl / meoh ( 5 ml ) is added slowly and stirred under n 2 for 2 min . the solvent is removed under vacuum to give a white solid . recrystallization from meoh / etoac / hexane gives the pure title compound as the hydrogen chloride salt , mp 165 - 166 ° c . ir ( drift ) 3371 , 2831 , 1600 , 1550 , 1447 , 1304 , 1284 , 1260 , 1225 , 1140 , 1092 , 1034 , 736 , 688 , 602 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 86 - 7 . 94 , 7 . 66 , 7 . 40 - 7 . 55 , 6 . 33 , 5 . 98 , 5 . 03 , 3 . 16 - 3 . 30 , 2 . 91 - 3 . 04 , 2 . 31 ; ms ( ei ) m / z 317 ( m + ), 276 , 275 , 91 , 77 . a solution of 1 -[ 4 -[( 3 - fluorophenyl ) sulfonyl ]- 3 - nitrophenyl ]- 1 , 4 - diazepane ( using the similar procedure as described in example 1 , step 3 , 0 . 382 g , 1 . 10 mmol ) and pd / c ( 0 . 0573 g , 15 % by wt . of iv ) in 35 ml of a 4 : 1 etoh : thf solvent is exposed to hydrogen gas ( 25 psi ) in a parr bottle . the pressure of hydrogen is constantly monitored and kept near 25 psi . after 2 h , the mixture is filtered , the solids rinsed with meoh and ch 2 cl 2 , and the filtrate concentrated to give 0 . 349 g ( 99 %) of a while solid . the hcl salt is prepared by standard methods to give an off - white solid . recrystallization from hot meoh / etoac / hexane gives a nearly quantitative yield of the title compound as hydrochloride salt , mp 106 - 108 ° c . ir ( drift ) 1600 , 1550 , 1506 , 1474 , 1458 , 1313 , 1290 , 1270 , 1222 , 1135 , 1085 , 727 , 691 , 678 , 651 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 67 - 7 . 71 , 7 . 56 - 7 . 63 , 7 . 35 - 7 . 47 , 7 . 10 - 7 . 23 , 6 . 17 , 5 . 80 , 4 . 95 , 3 . 48 - 3 . 59 , 3 . 00 , 2 . 83 , 2 . 11 , 1 . 81 - 1 . 92 ; ms ( ei ) m / z 349 ( m + ), 307 , 293 , 281 , 148 . following the general procedure of example 2 and making non critical variations , 2 , 5 - difluoronitrobenzene is converted to the title compound , mp144 - 146 ° c . ir ( drift ) 2924 , 2919 , 2685 , 2676 , 2589 , 1599 , 1552 , 1492 , 1451 , 1286 , 1265 , 1236 , 1141 , 1092 , 601 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 83 - 7 . 91 , 7 . 64 , 7 . 03 - 7 . 12 , 6 . 69 - 6 . 74 , 6 . 23 - 6 . 30 , 3 . 46 , 3 . 06 - 3 . 15 , 2 . 81 - 2 . 89 ; ms ( el ) m / z 335 ( m + ), 293 , 96 , 95 , 93 , 91 , 83 following the general procedure of example 2 and making non critical variations , the title compound is obtained , mp 85 - 89 ° c . ir ( drift ) 2957 , 2926 , 2850 , 2828 , 2793 , 2714 , 1592 , 1552 , 1492 , 1450 , 1287 , 1238 , 1139 , 1090 , 837 cm − 1 ; 1 h nmr ( 300 mhz , meoh - d 4 ) δ 8 . 30 , 7 . 64 - 7 . 75 , 7 . 37 , 7 . 04 - 7 . 12 , 3 . 36 - 3 . 44 , 2 . 54 - 2 . 62 , 2 . 36 , 1 . 67 ; ms ( ei ) m / z 349 ( m + ), 334 , 279 , 213 , 120 , 96 , 91 . following the general procedure of example 1 ( steps 1 - 6 ) and making non critical variations , the title compound is obtained , mp 102 - 106 ° c . ir ( drift ) 1599 , 1551 , 1448 , 1302 , 1282 , 1262 , 1139 , 1092 , 812 , 728 , 705 , 680 , 671 , 667 , 657 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 77 , 7 . 66 , 7 . 20 - 7 . 30 , 6 . 31 , 5 . 97 , 5 . 09 , 3 . 17 - 3 . 30 , 2 . 93 - 3 . 03 , 2 . 37 ; ms ( ei ) m / z 331 ( m + ), 290 , 289 , 119 , 93 , 92 , 91 , 65 , 57 , 56 . following the general procedure of example 1 ( steps 1 - 6 ) and making non critical variations , the title compound is obtained , mp 148 - 151 ° c . ir ( drift ) 3334 , 2954 , 2857 , 1598 , 1552 , 1453 , 1296 , 1288 , 1255 , 1140 , 1095 , 833 , 759 , 708 , 654 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 42 - 8 . 60 , 7 . 72 - 7 . 81 , 7 . 62 - 7 . 72 , 7 . 20 - 7 . 33 , 6 . 58 , 6 . 20 - 6 . 30 , 6 . 00 , 5 . 12 , 3 . 35 - 3 . 50 , 2 . 83 , 2 . 60 , 2 . 38 ; ms ( ei ) m / z 345 ( m + ), 330 , 120 , 92 , 91 , 71 , 65 , 58 , 57 , 56 . following the general procedure of example 2 and making non critical variations , the title compound is obtained , mp 90 - 93 ° c . ir ( drift ) 3458 , 3370 , 2843 , 1601 , 1552 , 1448 , 1289 , 1264 , 1230 , 1140 , 1095 , 737 , 689 , 644 , 610 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 87 - 7 . 92 , 7 . 71 , 7 . 66 , 7 . 42 - 7 . 51 , 6 . 75 , 6 . 33 , 5 . 98 , 5 . 03 , 3 . 27 - 3 . 33 , 3 . 25 - 3 . 29 , 2 . 56 - 2 . 59 , 2 . 48 - 2 . 52 , 2 . 36 , 2 . 33 ; ms ( ei ) m / z 331 ( m + ), 316 , 261 , 92 , 78 . following the general procedure of example 2 and making non critical variations , the title compound is obtained , mp 89 - 92 ° c . ir ( drift ) 2670 , 2580 , 2467 , 2446 , 1601 , 1552 , 1474 , 1451 , 1293 , 1267 , 1222 , 1135 , 1087 , 697 , 616 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 30 , 7 . 11 - 7 . 19 , 6 . 82 - 6 . 86 , 6 . 68 - 6 . 78 , 6 . 38 , 6 . 31 , 4 . 24 , 3 . 20 - 3 . 28 , 2 . 55 - 2 . 59 , 2 . 36 ; ms ( ei ) m / z 349 ( m + ), 334 , 279 , 91 , 86 . following the general procedure of example 2 and making non - critical variations , the title compound is obtained . ms ( ei ) m / z 367 ( m +), 311 , 299 , 134 , 122 , 119 , 91 , 70 , 65 , 63 , 57 . following the general procedure of example 2 and making non critical variations but using 1 -[ 4 -[( phenyl ) sulfonyl ]- 3 - nitrophenyl ]- 1 , 4 - diazepane as a starting material , the title compound is obtained . ms ( fab ) m / z 332 ( mh +), 486 , 408 , 348 , 334 , 333 , 332 , 331 , 330 , 191 , 44 . following the general procedure of example 2 and making non critical variations , the title compound is obtained . ms ( ei ) m / z 367 ( m +), 325 , 311 , 299 , 146 , 119 , 113 , 91 , 84 , 69 , 57 . tert - butyl 4 -[ 3 - amino - 4 -( phenylsulfonyl ) phenyl ]- 5 -( 1 , 4 - diazepan - 1 - yl )- 1 - carboxylate ( prepared as described in example 1 , step 5 ; 2 . 3 g , 5 . 1 mmol ) and methyl trifluoromethane sulfonate ( 0 . 58 ml , 5 . 1 mmol ) in 54 nil of dry thf is added sodium hydride ( 0 . 21 g , 5 . 1 mmol ) in small portions . upon complete addition , the mixture is stirred overnight under a blanket of n 2 . the solution is quenched by the addition of 55 ml of nh 4 cl and the layers are separated . the aqueous layer is extracted with etoac ( 3 × 50 ml ). the combined organic layers are dried over mgso 4 , filtered , and concentrated . purification via column chromatography ( 30 % etoac / hexane ) gives the desired methylaniline . the carbamate is deprotected following the synthetic route for example 1 ( step 6 ) to give 0 . 11 g ( 6 . 0 % overall ) of the title compound as a solid . recrystallization from meoh / etoac / hexane gives the pure product as the hcl salt , mp 153 - 154 ° c . ir ( drift ) 2944 , 2811 , 2734 , 2685 , 1596 , 1560 , 1468 , 1290 , 1270 , 1220 , 1133 , 795 , 732 , 691 , 677 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 45 - 7 . 65 , 7 . 34 - 7 . 45 , 7 . 12 - 7 . 21 , 6 . 15 - 6 . 30 , 6 . 10 , 5 . 72 , 3 . 51 - 3 . 60 , 3 . 30 - 3 . 44 , 3 . 01 , 2 . 81 , 2 . 27 , 1 . 80 - 1 . 91 ; ms ( ei ) m / z 363 ( m + ), 307 , 295 , 234 , 216 , 146 , 81 , 77 . to a mixture of piperazine ( 1 . 0 g , 12 mmol ) and potassium carbonate ( 2 . 0 g , 14 mmol ) in 80 ml of dry acetonitrile is added 4 - fluoro - 2 - nitro - 1 -( phenylsulfanyl ) benzene ( 2 , example 1 , step 1 , 2 . 7 g , 9 . 5 mmol ). the mixture is allowed to stir overnight at rt . water and ch 2 cl 2 ( 80 ml each ) are added and the layers separated . the aqueous layer is extracted with ch 2 cl 2 ( 3 × 50 ml ). the combined organic layers are dried over mgso 4 , filtered , and concentrated . purification via column chromatography ( 50 % etoac / hexane ) gives 1 . 6 g ( 47 %) of the title compound as a red oil . ir ( drift ) 3683 , 3020 , 2400 , 1547 , 1521 , 1441 , 1338 , 1295 , 1215 , 851 , 758 , 754 , 707 , 692 , 669 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 63 , 7 . 35 - 7 . 60 , 6 . 90 - 7 . 00 , 6 . 81 - 6 . 96 , 3 . 16 - 3 . 23 , 3 . 02 - 3 . 08 ; ms ( ei ) m / z 315 ( m + ), 273 , 243 , 226 , 184 , 139 , 84 , 77 . to a solution of 1 -[ 3 - nitro - 4 -( phenylsulfanyl ) phenyl ] piperazine ( 1 . 6 g , 4 . 5 mmol ) and naoh ( 0 . 39 g , 9 . 8 mmol ) in 64 ml of a 1 : 1 thf : h 2 o solvent system is added a solution of di - tert - butyl dicarbonate ( 1 . 1 g , 4 . 9 mmol ) in 5 ml of thf . the solution is stirred at rt for 16 h . the mixture is made neutral with 6 n hcl and 25 ml of etoac is added . the layers are separated and the aqueous layer is extracted with etoac ( 3 × 25 ml ). the combined organic layers are dried over mgso 4 , filtered , and concentrated . purification by column chromatography ( 15 % etoac / hexane ) gives 1 . 7 g ( 85 %) of the title compound as a oil . ir ( drift ) 3437 , 3344 , 2976 , 1682 , 1613 , 1595 , 1501 , 1429 , 1365 , 1290 , 1258 , 1221 , 1165 , 1128 , 733 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 66 , 7 . 49 - 7 . 57 , 7 . 39 - 7 . 47 , 6 . 98 , 6 . 85 , 3 . 56 - 3 . 64 , 3 . 13 - 3 . 23 , 1 . 50 ; ms ( ei ) m / z 415 ( m + ), 385 , 329 , 285 , 244 , 243 , 227 , 151 . to a solution of tert - butyl 4 -[ 3 - nitro - 4 -( phenylsulfanyl ) phenyl ]- 1 - piperazinecarboxylate ( 1 . 7 g , 3 . 8 mmol ) in 42 ml of a 4 : 1 etoh : thf solvent system is added raney nickel ( 260 mg suspension in etoh ) followed by hydrazine monohydrate ( 0 . 92 ml , 19 mmol ). the mixture is stirred vigorously for 2 h and then filtered through celite that is pretreated with water . the filtrate is concentrated , the residue crystallized from meoh / etoac / hexane to give 1 . 5 g ( 92 %) of the aniline as a white foam . ir ( drift ) 3344 , 2976 , 1682 , 1613 , 1595 , 1501 , 1430 , 1365 , 1290 , 1259 , 1221 , 1166 , 766 , 733 , 687 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 34 , 7 . 16 - 7 . 24 , 7 . 02 - 7 . 11 , 6 . 30 - 6 . 41 , 4 . 34 , 3 . 54 - 3 . 64 , 3 . 15 - 3 . 24 , 1 . 49 ; ms ( ei ) m / z 385 ( mh + ), 285 , 244 , 243 , 229 , 227 , 151 , 104 . a solution of tert - butyl 4 -[ 3 - amino - 4 -( phenylsulfanyl ) phenyl ]- 1 - piperazinecarboxylate ( 0 . 69 g , 1 . 6 mmol ) in 7 ml of dry ch 2 cl 2 is cooled to 0 ° c . acetyl chloride ( 0 . 13 ml , 1 . 8 mmol ), diisopropylethylamine ( 0 . 32 ml , 1 . 8 mmol ), and dmap ( 0 . 020 g , 0 . 16 mmol ) are added and the solution allowed to warm to rt overnight with stirring . water and ch 2 cl 2 ( 10 ml each ) are added and the layers separated . the aqueous layer is extracted with ch 2 cl 2 ( 3 × 10 ml ) and the combined organic layers are washed with 1 n hcl , h 2 o , and brine . after drying over mgso 4 , the mixture is filtered and concentrated to give the crude product . purification by column chromatography ( 25 % etoac / hexane ) gives 0 . 70 g ( 99 %) of the titel compound as a oil . ir ( mull ) 1694 , 1596 , 1582 , 1557 , 1518 , 1440 , 1430 , 1395 , 1294 , 1271 , 1238 , 1179 , 1120 , 744 , 739 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 22 - 8 . 26 , 8 . 20 , 7 . 46 , 7 . 19 - 7 . 26 , 7 . 10 - 7 . 15 , 7 . 01 - 7 . 03 , 6 . 68 , 3 . 56 - 3 . 61 , 3 . 25 - 3 . 29 , 2 . 05 , 1 . 48 ; ms ( ei ) m / z 427 ( m + ), 371 , 327 , 285 , 227 , 218 , 161 , 147 , 134 . a mixture of 3 - chloroperoxybenzoic acid ( 1 . 3 g , 7 . 7 mmol ) in 17 ml of ch 2 cl 2 is added to a mixture of tert - butyl 4 -[ 3 -( acetylamino )- 4 -( phenylsulfanyl ) phenyl ]- 1 - piperazinecarboxylate ( 1 . 3 g , 3 . 1 mmol ) and nahco 3 ( 0 . 65 g , 7 . 7 mmol ) in 36 ml of ch 2 cl 2 , cooled to − 78 ° c . the solution is stirred at − 78 ° c . for 1 h and then warmed to rt and stirred for 6 additional hours . the mixture is partitioned between nahco 3 ( 50 ml ) and ch 2 cl 2 ( 3 × 50 ml ), dried over mgso 4 , filtered , and concentrated . purification by column chromatography ( 10 % meoh / ch 2 cl 2 ) gives 0 . 51 g ( 36 %) of the pure title compound as a solid , mp 129 - 130 ° c . ir ( drift ) 1697 , 1592 , 1461 , 1442 , 1418 , 1393 , 1366 , 1287 , 1264 , 1252 , 1174 , 1149 , 1036 , 752 , 690 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 10 . 48 , 8 . 70 - 8 . 75 , 8 . 26 , 7 . 70 , 7 . 44 - 7 . 56 , 3 . 84 - 4 . 24 , 3 . 60 - 3 . 83 , 3 . 41 , 3 . 08 - 3 . 18 , 2 . 11 ; ms ( ei ) m / z 459 ( m + ), 310 , 261 , 218 , 185 , 161 , 150 , 128 , 85 , 77 . to a mixture of tert - butyl 4 -[ 3 -( acetylamino )- 4 -( phenylsulfonyl ) phenyl ]- 1 - piperazinecarboxylate ( 0 . 44 g , 0 . 96 mmol ) in 7 ml of dry thf is added borane - methyl sulfide complex ( 0 . 28 ml , 2 . 8 mmol , 10 . 0 m ). the mixture is stirred at rt overnight . the reaction is quenched upon dropwise addition of 10 % hcl . water ( 3 . 0 ml ) and koh ( 2 . 0 g ) are added , the mixture heated at reflux for 6 h . at that time methanol ( 2 ml ) is added and the mixture stirred at reflux overnight . after cooling to rt , the organics are removed under reduced pressure , the aqueous layer is saturated with nacl , and extracted with ch 2 cl 2 ( 3 × 10 ml ). the combined organic layers are dried over mgso 4 , filtratered , and concentrated to give the crude product . purification by column chromatography ( 15 % etoac / hexane ) gave 0 . 18 g ( 43 %) of the pure title compound as an oil . ir ( drift ) 2970 , 1690 , 1592 , 1561 , 1476 , 1457 , 1430 , 1363 , 1288 , 1243 , 1215 , 1173 , 1128 , 993 , 743 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 48 - 7 . 55 , 7 . 36 - 7 . 46 , 7 . 32 , 6 . 20 , 5 . 96 , 5 . 90 , 3 . 49 - 3 . 59 , 3 . 17 - 3 . 25 , 2 . 82 - 3 . 06 , 1 . 47 , 1 . 05 ; ms ( ei ) m / z 445 ( m +), 414 , 357 , 324 , 280 , 271 , 147 , 136 , 104 , 58 , 57 . to a solution of tert - butyl 4 -[ 3 -( ethylamino )- 4 -( phenylsulfonyl ) phenyl ]- 1 - piperazinecarboxylate ( 0 . 18 g , 0 . 40 mmol ) in 4 . 6 ml of ch 2 cl 2 at 0 ° c . is added trifluoroacetic acid ( 4 . 6 ml ). the solution is stirred at 0 ° c . for 2 h and then concentrated . methylene chloride ( 10 ml ) and 1 n naoh ( 10 ml ) are added and the layers seperated . the aqueous layer is extracted with ch 2 cl 2 ( 3 × 15 ml ) and the combined organic layers are dried over mgso 4 , filtered , and concentrated to give 0 . 13 g ( 86 %) of a white solid . the solid is dissolved in 25 ml of meoh and hcl / meoh ( 5 ml ) is added slowly . the solvent is removed under vacuum to give a white solid . recrystallization from meoh / etoac / hexane gives the pure title compound as the hydrogen chloride salt , mp 121 - 123 ° c . ir ( drift ) 2957 , 2932 , 2822 , 2778 , 2747 , 2720 , 2692 , 1599 , 1588 , 1566 , 1512 , 1449 , 1440 , 1220 , 739 cm − 1 ; 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 36 , 7 . 17 - 7 . 25 , 7 . 03 - 7 . 12 , 6 . 30 , 6 . 20 , 4 . 77 - 4 . 85 , 3 . 22 - 3 . 29 , 3 . 11 - 3 . 22 , 3 . 03 - 3 . 10 , 2 . 00 , 1 . 18 ; ms ( ei ) m / z 345 ( m + ), 313 , 271 , 147 , 136 , 133 , 117 , 91 , 77 . following the general procedure of example 13 ( steps 1 - 7 ) and making non critical variations , 1 -[ 4 - fluoro - 2 - nitro - 1 -( phenylsulfanyl )]- 3 - fluorobenzene ( prepared as described in example 1 , step i ) is converted to the title compound , ms ( ei ) m / z 377 ( m +), 321 , 310 , 309 , 135 , 131 , 119 , 117 , 83 , 77 , 69 . to a mixture of 3 - fluorothiophenol ( 8 . 36 g , 65 . 2 mmol ) and potassium carbonate ( 9 . 81 g , 71 . 0 mmol ) in 115 ml of dry acetonitrile is added 2 , 5 - difluoronitrobenzene ( 7 . 00 ml , 64 . 55 mmol ). the mixture is allowed to stir at room temperature for 2 hours . water and ch 2 cl 2 ( 120 ml each ) are added and the layers separated . the aqueous layer is extracted with ch 2 cl 2 ( 3 × 50 ml ). the combined organics are dried over mgso 4 , filtered , and concentrated to give a bright yellow solid . the solid is triturated with hexane to give 17 . 1 g ( 99 %) of the title compound as a bright yellow solid . [ 0195 ] 1 h nmr ( 300 mhz , cdcl 3 ) δ 7 . 95 , 7 . 41 - 7 . 51 , 7 . 33 - 7 . 38 , 7 . 26 - 7 . 31 , 7 . 12 - 7 . 24 , 6 . 91 . a mixture of 4 - fluoro - 2 - nitrophenyl 3 - fluorophenyl sulfide ( 17 . 1 g , 64 . 1 mmol ) in 430 ml of glacial acetic acid is heated to 100 ° c . and treated with 7 . 4 ml of a 30 % h 2 o 2 solution . after stirring for 20 min at 100 ° c ., another 7 . 4 ml of the h 2 o 2 solution is added and the mixture stirred at 100 ° c . for an additional 30 min . after cooling to room temperature , the mixture is diluted with 450 ml of water and the resulting white solid is filtered . the solids are rinsed with 1 n naoh , and water until neutral to litmus , triturated with hexane , and dried under vacuum to give 18 . 5 g ( 96 %) of the title compound as a white solid . [ 0198 ] 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 38 - 8 . 43 , 7 . 74 - 7 . 77 , 7 . 62 - 7 . 66 , 7 . 47 - 7 . 60 , 7 . 31 - 7 . 48 . a mixture of 4 - fluoro - 2 - nitrophenyl 3 - fluorophenyl sulfone ( 5 . 00 g , 16 . 7 mmol ), homopiperazine ( 2 . 09 g , 20 . 9 mmol ), and potassium carbonate ( 3 . 46 g , 25 . 1 mmol ) in 140 ml of dry acetonitrile is stirred vigorously for 4 h at 60 ° c . after cooling to room temperature , water and ch 2 cl 2 ( 140 ml each ) are added and the layers separated . the aqueous layer extracted with ch 2 cl 2 ( 3 × 50 ml ). the combined organics are dried over mgso 4 , filtered , and concentrated to give an orange solid . the crude product is triturated with a hot et 2 o : ch 2 cl 2 mixture ( 4 : 1 ) until solid . further trituration with hot etoac / hexane gave 6 . 31 g ( 99 %) of the title compound as bright yellow solid . [ 0201 ] 1 h nmr ( 300 mhz , cdcl 3 ) δ 8 . 05 , 7 . 71 - 7 . 76 , 7 . 59 - 7 . 64 , 7 . 46 - 7 . 54 , 7 . 22 - 7 . 30 , 6 . 90 , 6 . 83 , 3 . 54 - 3 . 70 , 3 . 00 - 3 . 07 , 2 . 80 - 2 . 88 , 1 . 82 - 1 . 94 . to a mixture of 4 -( 1 , 4 - diazepan - 1 - yl )- 2 - nitrophenyl 3 - fluorophenyl sulfone ( 49 . 1 g , 129 mmol ) and sodium hydroxide ( 11 . 4 g , 286 mmol ) in 650 ml of a 1 : 1 thf : h 2 o solvent is slowly added a mixture of di - tert - butyl dicarbonate ( 32 . 4 g , 148 mmol ) in 5 ml of thf . the solution is stirred at rt for 16 h . the mixture is neutralized with 6 n hcl and 200 ml of ch 2 cl 2 is added . the layers are separated and the aqueous layer extracted with ch 2 cl 2 ( 3 × 100 ml ). the combined organics are dried over mgso 4 , filtered , and concentrated to give an orange solid . the crude product is triturated with etoac and hexane to give 60 . 35 g ( 99 %) of the title compound as a bright yellow solid . [ 0204 ] 1 h nmr ( 400 mhz , cdcl 3 ) δ 8 . 12 , 7 . 76 - 7 . 80 , 7 . 63 - 7 . 67 , 7 . 52 - 7 . 58 , 7 . 31 - 7 . 34 , 6 . 94 - 6 . 97 , 6 . 87 - 6 . 92 , 3 . 62 - 3 . 75 , 3 . 39 - 3 . 45 , 3 . 30 - 3 . 35 , 1 . 94 - 2 . 03 , 1 . 42 , 1 . 34 . a mixture of tert - butyl 4 -{ 4 -[( 3 - fluorophenyl ) sulfonyl ]- 3 - nitrophenyl }- 1 , 4 - diazepane - 1 - carboxylate ( 58 . 0 g , 121 mmol ) and pd / c ( 8 . 70 g , 15 % by wt .) in 1 . 5 l of a 2 : 2 : 1 thf : meoh : etoh solvent is exposed to hydrogen gas ( 25 psi ) in a parr bottle . the pressure of hydrogen is constantly monitored and kept near 25 psi . after 16 h , the mixture is filtered , solids rinsed with meoh and ch 2 cl 2 , and filtrate concentrated to give a brown solid . the solid is triturated with etoac and hexane to give 53 . 4 g ( 98 %) of the title compound as an off white solid . [ 0207 ] 1 h nmr ( 400 mhz , cdcl 3 ) δ 7 . 72 - 7 . 76 , 7 . 64 , 7 . 44 - 7 . 51 , 7 . 21 - 7 . 27 , 6 . 22 - 7 . 26 , 5 . 84 - 5 . 87 , 5 . 03 - 5 . 09 , 3 . 52 - 3 . 63 , 3 . 33 - 3 . 38 , 3 . 23 - 3 . 29 , 1 . 91 - 1 . 99 , 1 . 45 , 1 . 34 . a mixture of tert - butyl 4 -[ 3 - amino - 4 -[( 3 - fluorophenyl ) sulfonyl ] phenyl ]- 1 , 4 - diazepane - 1 - carboxylate ( 0 . 29 g , 0 . 66 mmol ) and anhydrous acetic anhydride ( 1 . 0 ml ) is stirred at 60 ° c . for 1 h under a nitrogen atmosphere . after cooling to rt , 5 ml of toluene is added and the mixture concentrated . the crude product is triturated with more toluene then with etoac and et 2 o to give 0 . 31 g ( 97 %) of the title compound as a white solid . [ 0210 ] 1 h nmr ( 400 mhz , cdcl 3 ) δ 9 . 50 - 9 . 66 , 7 . 78 - 7 . 85 , 7 . 67 , 7 . 51 - 7 . 54 , 7 . 37 - 7 . 45 , 7 . 14 - 7 . 19 , 6 . 35 - 6 . 44 , 3 . 50 - 3 . 58 , 3 . 21 - 3 . 27 , 3 . 12 - 3 . 17 , 2 . 15 , 1 . 86 - 1 . 94 , 1 . 33 , 1 . 28 . to a mixture of tert - butyl 4 -[ 3 -( acetylamino )- 4 -[( 3 - fluorophenyl ) sulfonyl ] phenyl ]- 1 , 4 - diazepane - 1 - carboxylate ( 0 . 508 g , 1 . 03 mmol ) in 20 ml of a 1 : 1 et 2 o : ch 2 cl 2 solvent is added anhydrous methanesulfonic acid ( 0 . 109 g , 1 . 14 mmol ) and the mixture is stirred at rt for 2 . 5 h . hot et 2 o ( 10 ml ) is added and the white solid is filtered , rinsed with et 2 o and dried under vacuum to give 0 . 497 g ( 99 %) of the title compound as a white solid . [ 0213 ] 1 h nmr ( 400 mhz , dmso - d 6 ) δ 9 . 42 , 8 . 62 - 8 . 64 , 7 . 84 , 7 . 64 - 7 . 69 , 7 . 50 - 7 . 56 , 7 . 18 - 7 . 22 , 6 . 77 , 3 . 69 - 3 . 74 , 3 . 49 - 3 . 55 , 3 . 22 - 3 . 28 , 3 . 11 - 3 . 18 , 2 . 29 , 2 . 04 - 2 . 08 , 1 . 98 - 2 . 03 . following the general procedure of example 2 and making non critical variations , the title compound is obtained . ms ( ci ) m / z 406 ( mh + ), 408 , 406 , 249 , 247 , 245 , 219 , 69 , 58 , 56 , 52 . following the general procedure of example 15 and making non critical variations but using fluorothiophenol as a starting material , the title compound is obtained . hrms ( fab ) calcd for c 19 h 23 n 3 o 3 s + h 1 374 . 1538 , found 374 . 1515 . following the general procedure of example 15 and making non critical variations , the title compound is obtained . hrms ( fab ) calcd for c 20 h 24 fn 3 o 3 s + h 1 406 . 1600 , found 406 . 1602 . following the general procedure of example 15 and making non critical variations , the title compound is obtained . hrms ( fab ) calcd for c 21 h 26 fn 3 o 3 s + h 1 420 . 1757 , found 420 . 1760 . following the general procedure of examples 1 - 19 and making non critical variations , the following compounds can be obtained . examples of these compounds are : | 2 |
referring initially to fig1 , a system is shown , generally designated 10 , which includes receivers 12 and transmitters 14 exchanging information with each other . it is to be understood that fig1 is illustrative only and is non - limiting . for instance , fig1 shows an exemplary non - limiting protocol stack that in practice may include greater or fewer layers than shown . also , fig1 assumes that the protocol portion used to ensure correct data delivery is user datagram protocol ( udp ) and that the data being exchanged is telephony data , but other data delivery correctness protocols may be used such as reliable udp ( r - udp ) and transmission control protocol ( tcp ) to ensure correct delivery of either or both telephony data and computer data . thus , without limitation the receiver 12 and transmitter 14 may be nodes in a wired or wireless communication system , and may communicate over a local area network ( lan ) in which variations in packet delivery times do not greatly vary , although communication can be over wide area networks ( wan ) such as the internet . in a non - limiting implementation the receiver 12 and transmitter 14 may be mobile telephones or computers or one or both might be a fixed asset such as a wireless communication system base station , fixed computer , or other communication device . with the above in mind , the exemplary receiver 12 includes a processor 16 that can access a program storage device 18 to execute the logic shown below in fig2 . it is to be understood that the program storage device 18 is any suitable electronic storage medium including solid state storage , disk storage , removable storage , etc . it is to be further understood that the logic can be implemented in hardware if desired . whether implemented in hardware or software , the present logic set forth below can be executed to establish the size of a retransmit buffer 20 . by “ size ” of buffer is meant the length , in data elements , of the buffer , which can be directly correlated to and / or represented by the time data is delayed in the buffer . fig1 schematically shows that the receiver 12 processes data in a so - called protocol stack that includes several layers of protocols through which data is passed , up to the highest level where the data is used . in the exemplary non - limiting embodiment shown , the protocol stack of the receiver 12 can include a physical layer 22 which receives the transmitted signal from the transmitter 14 . data from the physical layer 22 , including voice over internet protocol ( voip ) data , may be packetized into internet protocol ( ip )- formatted data in an ip layer 24 . data from the ip layer 24 is then passed to a udp layer 26 and thence to a data verification layer 28 to verify that all packets have been received . in the exemplary embodiment shown , the layer 26 uses udp , it being understood that it may use other protocols including , without limitation , reliable udp ( r - udp ) and transmission control protocol ( tcp ). at the top of the protocol stack is an application layer 32 , which represents the data in a format that is appropriate for the intended end use , e . g ., audible display of a voice or data transformation and processing using an end - use software application . now referring to fig2 , a diagram of the logic for establishing a buffer length is shown , with fig2 being executed by the receiver 12 preferably at the start of each packetized stream transmission and , if desired , every time a retransmission is requested for , e . g ., missing packets . first , at state 60 the data stream is initiated . proceeding to block 62 , the first packet in the stream is received and queued in , e . g ., the buffer 20 shown in fig1 for eventual passing to the upper layers of the protocol stack . after the first ( or substantially the first ) packet is received , at block 64 retransmission of the first packet , which may be thought of as a test packet , is requested of the transmitter to acquire a real - time measurement of retransmission delay and therefore to be able to dynamically establish the buffer size to accommodate the measured delay , as discussed further below . as indicated at block 64 , the current time and packet id of the test packet are also noted in order to acquire real time data . proceeding to decision diamond 66 , it is determined whether the retransmit action has failed as indicated by an excessive period elapsing without receiving the retransmitted packet from the transmitter . if it has , the logic reverts back to block 62 and starts over again . if the action has not failed , a packet has been received and the logic proceeds to block 68 . still referring to fig2 , once the packet is received at block 68 , at decision diamond 70 it is determined whether the packet fits into the next slot in the total packet sequence ( indicating that the packet received at block 68 was not out of sequence and hence was not the test packet ). if it is the next packet in the sequence , the logic then moves to block 72 where the packet is placed in the queue ( e . g ., in the buffer 20 shown in fig1 ) for eventual passing on to the upper layers of the protocol stack . should it be determined at decision diamond 70 that the packet received at block 68 is not the next one in sequence , the logic flows from decision diamond 70 to decision diamond 74 , wherein it is determined , by means of comparing the id of the packet received at block 68 with the packet id recorded at block 64 , whether the packet received was the test packet . if the logic determines that it was the test packet , the logic proceeds to block 76 wherein the time period between the time recorded at block 64 and the time the test packet was received at block 68 is determined . because this period can be correlated to a buffer length by , e . g ., multiplying the data rate by the measured retransmission delay period to find a total number of data elements that must be buffered during the retransmission delay period determined at block 76 , the length of the buffer 20 shown in fig1 can be calculated . once this calculation has been completed , the logic concludes at state 78 . returning to decision diamond 74 , if the packet received at block 68 is not the test packet , the logic proceeds to decision diamond 80 , wherein it is determined whether the packet is a retransmitted packet from a slot in the packet stream at which a packet was missed . if it was , the logic then flows to block 82 where the packet is inserted into its correct slot in the queue for subsequent passing on to the upper levels of the protocol stack . in contrast , if , at decision diamond 80 , the logic determines that the packet received is not a retransmitted packet but rather some other packet out of sequence , indicating that some packet or packets have been missed , the logic moves to block 84 where a request for the retransmission is made of the missed packet ( s ) ( i . e ., those preceding the packet received at block 68 that should have followed the latest packet before that in the buffer ). after the request has been made , a space in the data stream for the missed packet is reserved at block 86 , and then the logic moves to block 72 to function as set forth above . now referring to fig3 , a system is shown , generally designated 110 , which illustrates details of a transmitter 112 that can execute the logic described below in reference to fig4 . it is to be understood that both the receiver 12 shown in fig1 may execute the logic shown in fig2 , and / or the transmitter 112 shown in fig3 may execute the logic shown in fig4 . the transmitter 112 shown in fig3 thus may communicate with a receiver 114 that in all essential respects may be identical to the receiver 12 shown in fig1 . the transmitter 112 thus may be a mirror image of the previously described receiver . with more specificity , the transmitter 112 may include a processor 116 that can access a program storage device 118 to execute the logic shown in fig4 . it is to be understood that the program storage device 118 is any suitable electronic storage medium including solid state storage , disk storage , removable storage , etc . it is to be further understood that the logic can be implemented in hardware if desired . whether implemented in hardware or software , the present logic set forth below can be executed to establish the size of a retransmit buffer 120 . by “ size ” of buffer is meant the length , in data elements , of the buffer , which can be directly correlated to and / or represented by the time data is delayed in the buffer before discarding . fig3 schematically shows that the transmitter 112 processes data in a so - called protocol stack that includes several layers of protocols through which data is passed , up to the highest level where the data is used . in the exemplary non - limiting embodiment shown , the protocol stack of the transmitter 112 can include a physical layer 122 which sends the data to be transmitted to the receiver 114 . the physical layer 122 receives data , including voice over internet protocol ( voip ) data that may be packetized in internet protocol ( ip )- formatted data from an ip layer 124 . data from the ip layer 124 in turn is received from a udp layer 126 , which accepts data from a data verification layer 128 . in the exemplary embodiment shown , the layer 126 uses udp , it being understood that it may use other protocols including , without limitation , reliable udp ( r - udp ) and transmission control protocol ( tcp ). at the top of the protocol stack , from which data originates , is an application layer 130 , which represents the data in a format that is appropriate for the intended end use at the receiver 114 , e . g ., audible display of a voice or data transformation and processing using an end - use software application . now referring to fig4 , a diagram of the logic for establishing a buffer length at the transmitter 112 is shown , with fig4 being executed by the transmitter 112 preferably at the start of each packetized stream transmission and , if desired , every time a retransmission is requested for , e . g ., missing packets . the logic starts at state 132 . proceeding to block 134 , the next packet from the stack is accepted for transmission . initially , the first packet in a stream to be transmitted is the “ next ” packet . at block 136 the packet is transmitted and the time of its transmission is recorded . the packet is then placed in a discard queue in the buffer 120 for subsequent discarding after the elapse of the transmitter buffer expiration period determined herein . moving to decision diamond 140 , the transmitter 112 determines whether it has received a request from the receiver 114 to retransmit a packet . if not , the logic proceeds to decision diamond 142 to determine whether any packets in the discard queue have expired by , e . g ., comparing their times of transmission with the below - established expiration period . in the first iteration ( i . e ., for the first packet ) the test at decision diamond 142 should be negative , in which case the logic loops back to block 134 as shown to retrieve the next packet in the stream for transmission . in the event that expired packets exists in the discard queue at decision diamond 142 , the packet ( s ) are discarded , e . g ., flushed from the buffer 120 , at block 144 . in the event that a retransmission request is received by the transmitter 112 at decision diamond 140 , fig4 shows that the logic moves to block 146 to retransmit the requested packet ( s ). at block 148 , the actual retransmission latency is calculated . in one implementation this is done by obtaining the difference in time , i . e ., the period between , the time the dropped packet ( identified by its packet id ) was first transmitted , and the time the requested packet of the same packet id is retransmitted . or , the expiration period may be calculated by obtaining the difference in time between the time the dropped packet was first transmitted , and the time the retransmission request is received . block 150 indicates that the transmitter buffer length , i . e ., the packet expiration period used at decision diamond 142 , may be adjusted using the calculation at block 150 . the adjustment may include simply resetting the expiration period to the period most recently obtained at block 150 , or it may include averaging the period obtained at block 150 with previous periods such that the expiration period used at decision diamond 142 represents an average of measured retransmission periods . if desired , the steps at blocks 148 and 150 may be performed only once , e . g ., for the first packet transmitted in a stream , or they may be performed for each retransmitted packet as shown , or for only some packets on a periodic basis . in any case , the amount of data kept in the buffer 120 is dynamically established for each stream transmitted . while the particular system and method for dynamically determining retransmit buffer time as herein shown and described in detail is fully capable of attaining the above - described objects of the invention , it is to be understood that it is the presently preferred embodiment of the present invention and is thus representative of the subject matter which is broadly contemplated by the present invention , that the scope of the present invention fully encompasses other embodiments which may become obvious to those skilled in the art , and that the scope of the present invention is accordingly to be limited by nothing other than the appended claims , in which reference to an element in the singular is not intended to mean “ one and only one ” unless explicitly so stated , but rather “ one or more ”. it is not necessary for a device or method to address each and every problem sought to be solved by the present invention , for it to be encompassed by the present claims . furthermore , no element , component , or method step in the present disclosure is intended to be dedicated to the public regardless of whether the element , component , or method step is explicitly recited in the claims . absent express definitions herein , claim terms are to be given all ordinary and accustomed meanings that are not irreconcilable with the present specification and file history . | 7 |
[ 0046 ] fig1 is a perspective view of an electro - dynamic loudspeaker 100 of the invention . as shown in fig1 the electro - dynamic loudspeaker is a generally planar loudspeaker having a frame 102 with a diaphragm 104 attached in tension to the frame 102 . a conductor 106 is positioned on the diaphragm 104 . the conductor 106 is shaped in serpentine fashion having a plurality of substantially linear sections ( or traces ) 108 longitudinally extending along the diaphragm interconnected by radii 110 to form a single current path . permanent magnets 202 ( shown in fig2 ) are positioned on the frame 102 underneath the diaphragm 104 , creating a magnetic field . linear sections 108 are positioned within the flux fields generated by permanent magnets 202 . the linear sections 108 carry current in a first direction 112 and are positioned within magnetic flux fields having similar directional polarization . linear sections 108 of conductor 106 having current flowing in a second direction 114 , that is opposite the first direction 112 , are placed within magnetic flux fields having an opposite directional polarization . positioning the linear sections 108 in this manner assures that a driving force is generated by the interaction between the magnetic fields developed by magnets 202 and the magnetic fields developed by current flowing in conductor 106 . as such , an electrical input signal traveling through the conductor 106 causes the diaphragm 104 to move , thereby producing an acoustical output . [ 0048 ] fig2 is an exploded perspective view of the electro - dynamic loudspeaker 100 shown in fig1 . as illustrated in fig2 the flat panel loudspeaker 100 includes a frame 102 , a plurality of high energy magnets 202 , a diaphragm 104 , an acoustical dampener 236 and a grille 228 . frame 102 provides a structure for fixing magnets 202 in a predetermined relationship to one another . in the depicted embodiment , magnets 202 are positioned to define five rows of magnets 202 with three magnets 202 in each row . the rows are arranged with alternating polarity such that fields of magnetic flux are created between each row . once the flux fields have been defined , diaphragm 104 is fixed to frame 102 along its periphery . a conductor 106 is coupled to the diaphragm 104 . the conductor 106 is generally formed as an aluminum foil bonded to the diaphragm 104 . the conductor 106 can , however , be formed from other conductive materials . the conductor 106 has a first end 204 and a second end 206 positioned adjacent to one another at one end of the diaphragm 104 . as shown in fig2 frame 102 is a generally dish - shaped member preferably constructed from a substantially planar contiguous steel sheet . the frame 102 includes a base plate 208 surrounded by a wall 210 . the wall 210 terminates at a radially extending flange 212 . the frame 102 further includes apertures 214 and 216 extending through flange 212 to provide clearance and mounting provisions for a conductor assembly 230 . conductor assembly 230 includes a terminal board 218 , a first terminal 220 and a second terminal 222 . terminal board 218 includes a mounting aperture 224 and is preferably constructed from an electrically insulating material such as plastic , fiberglass or other insulating material . a pair of rivets or other connectors ( not shown ) pass through apertures 214 to electrically couple first terminal 220 to first end 204 and second terminal 222 to second end 206 of conductor 106 . a fastener such as a rivet 226 extends through apertures 224 and 216 to couple conductor assembly 230 to frame 102 . a grille 228 functions to protect diaphragm 104 from contact with objects inside the listening environment while also providing a method for mounting loudspeaker 100 . the grille 228 has a substantially planar body 238 having a plurality of apertures 232 extending through the central portion of the planar body 238 . a rim 234 extends downward , substantially orthogonally from body 238 , along its perimeter and is designed to engage the frame 102 to couple the grille 228 to the frame 102 . an acoustical dampener 236 is mounted on the underside of the base plate 208 of the frame 102 . dampener 236 serves to dissipate acoustical energy generated by diaphragm 104 thereby minimizing undesirable amplitude peaks during operation . the dampener 236 may be made of felt , or a similar gas permeable material . [ 0054 ] fig3 is a cross - sectional view of the electro - dynamic loudspeaker taken along line 3 - 3 of fig1 . fig3 shows the frame 102 having the diaphragm 104 attached in tension to the frame 102 and the permanent magnets 202 positioned on the frame 102 underneath the diaphragm 104 . linear sections 108 of the conductor 106 are also shown positioned on top of the diaphragm 104 . [ 0055 ] fig4 is an enlarged cross - sectional view of the encircled area of fig3 . as illustrated by fig4 the diaphragm 104 is comprised of a thin film 400 having a first side 402 and a second side 404 . first side 402 is coupled to frame 102 . generally , the diaphragm 104 is secured to the frame 102 by an adhesive 406 that is curable by exposure to radiation . however , the diaphragm 104 may secured to the frame 102 by other mechanism , such as those known in the art . to provide a movable membrane capable of producing sound , the diaphragm 104 is mounted to the frame 102 in a state of tension and spaced apart a predetermined distance from magnets 202 . the magnitude of tension of the diaphragm 104 depends on the speaker &# 39 ; s physical dimensions , materials used to construct the diaphragm 104 and the strength of the magnetic field generated by magnets 202 . magnets 202 are generally constructed from a highly energizable material such as neodymium iron boron ( ndfeb ), but may be made of other magnetic materials . the thin diaphragm film 400 is generally a polyethylenenaphthalate sheet having a thickness of approximately 0 . 001 inches ; however , the diaphragm film 400 may be formed from materials such as polyester ( e . g ., known by the tradename “ mylar ”), polyamide ( e . g ., known by the tradename “ kapton ”) and polycarbonate ( e . g ., known by the tradename “ lexan ”), and other materials known by those skilled in the art for forming diaphragms 104 . the conductor 106 is coupled to the second side 404 of the diaphragm film 400 . the conductor 106 is generally formed as an aluminum foil bonded to diaphragm film 400 , but may be formed of other conductive material known by those skilled in the art . the frame 102 includes a base plate 208 surrounded by a wall 210 extending generally orthogonally upward from the plate 208 . the wall 210 terminates at a radially extending flange 212 that defines a substantially planar mounting surface 414 . a lip 416 extends downwardly from flange 212 in a direction substantially parallel to wall 210 . base plate 208 includes a first surface 418 , a second surface 420 and a plurality of apertures 422 extending through the base plate 208 . the apertures 422 are positioned and sized to provide air passageways between the first side 402 of diaphragm 104 and first surface 418 of frame 102 . an acoustical dampener 236 is mounted to second surface 420 of frame base plate 208 . conductor 106 , as shown in fig1 may be formed by bonding an aluminum foil to the film 400 and chemically etching away portions of the aluminum foil in order to define the linear sections 108 and radii 110 of the conductor 106 . accordingly , it is desirable to provide additional methods of forming the conductor on a diaphragm of an electro - dynamic loudspeaker that is capable of carrying current , preferably has a low mass , and is permanently attached to the film even at high power and high temperature implementations . fig6 - 10 show the forming of a conductor 600 by attaching magnet wire 602 to the film 604 . the conductor 600 , which is comprised of magnet wire , may be arranged in a serpentine fashion and applied to the film 604 by an adhesive . as is the case with the electro - dynamic loudspeaker described above with reference to fig1 - 5 , the electro - dynamic loudspeaker 606 includes a frame 608 having a plurality of magnets 610 mounted therein as is described above . the film 604 is attached to the frame 608 by an adhesive 612 . in fig8 - 10 , a method for forming the magnet wire 602 in a serpentine configuration is shown , including a fixture 800 having a plurality of retractable spindles 802 around which the magnet wire 602 is wound in a serpentine pattern as illustrated in fig8 and 9 . the fixture 800 includes an upper plate 900 and a retractable plate 902 to which the spindles 802 are fixedly connected . the spindles 802 pass through apertures provided in the upper plate 900 . after the magnet wire 602 is wound around the spindles 802 , the fixture 800 is disposed adjacent to a film material and the retractable plate 902 is moved away from the upper plate 900 so as to cause the spindles 802 to retract . once the spindles 802 are retracted to the point that their extension is less than a diameter of the magnet wire 602 , the magnet wire 602 comes in contact with the film material . according to a preferred embodiment , the magnet wire 602 is coated with an adhesive which fixes the magnet wire 602 in the serpentine configuration to the film material . optionally , a light can be shown through the film material in order to speed up the curing process of the adhesive that is applied to the magnet wire in order to more rapidly cure the adhesive . once the adhesive is given appropriate time to cure , the spindles 802 are completely retracted so as to free the spindles from the magnet wire 602 . the spindles 802 can be formed of a self - lubricating material or can be highly polished , or both , in order to reduce the friction between the spindles 802 and the magnet wire 602 . in addition , the spindles 802 can be chemically treated to resist bonding with the adhesive applied to the magnet wire 602 . the conductor 600 can be applied to the film 400 either prior to or after the film has been mounted to the frame 102 of the electro - dynamic loudspeaker . in fig1 and 12 , an electro - dynamic loudspeaker 1100 is provided with a conductor 1102 that is formed by ribbon - shaped wire 1104 which is provided with two narrow side edges 1200 , 1202 and a pair of relatively wide faces 1204 , 1206 . the ribbon - shaped conductor preferably extends below an upper attachment surface 1208 of the frame 1210 . by suspending the ribbon - shaped conductor below the upper attachment surface 1208 of the frame 1210 , the conductor 1102 extends towards the magnets 1212 so as to be closer to the magnetic field lines generated by the magnets 1212 . the ribbon - shaped conductor 1102 is attached to the film 1106 by an adhesive 1214 and can be formed in the same manner as the wire conductor 600 described above . in other words , the ribbon - shaped wire 1104 can be wrapped around a fixture such as that disclosed in fig8 - 10 ( fig1 shows the ribbon - shaped wire 1104 ) and applied to the film 1106 in the same manner as described above . by placing the ribbon - shaped conductor 1102 closer to the magnetic field , the intensity of the magnetic field lines are increased to allow a reduced strength magnet 1212 to be utilized which results in a cost savings for the manufacture of the electro - dynamic loudspeaker 1100 . alternatively , the performance can be enhanced by taking advantage of the stronger magnetic flux density with the ribbon - shaped conductor being closer to the magnetic field . in fig1 , cap members 1700 can optionally be applied to the upper surface of the magnets 1212 in order to focus the magnetic field lines in a preferred direction relative to the conductor 1102 . although the cap members are shown in combination with a ribbon - shaped conductor 1102 , the shape and configuration of the cap members 1700 can be varied in order to provide a desired magnetic field . as shown in fig1 , smaller caps 1800 permit a different shaped magnetic field for use with different configurations of conductors . the cap members 1700 , 1800 are preferably made from a ferrous material and can be glued or otherwise held in place on the upper surface of the magnets 1212 . [ 0064 ] fig1 illustrates an electro - dynamic loudspeaker 1300 having a diaphragm 1302 that has channels 1304 formed in the diaphragm 1302 and has electrical traces 1306 of a conductor 1308 disposed on opposite angularly disposed faces 1310 , 1312 of the channels 1304 . the channels 1304 allow the traces 1306 to be suspended below an upper attachment surface 1314 of the frame 1316 so that the traces 1306 can be placed within the higher intensity magnetic field lines generated by the magnets 1318 . the film 1302 preferably has a thickness of between 2 - 5 mills in order to provide an appropriate rigidity for forming the channels 1304 . the channels 1304 are formed by placing the film 1302 in a heated mold provided with upper and lower die members provided with a channel - shaped protrusion in one die member and a channel - shaped recess in the other die member so as to permanently deform the film member 1302 into the configuration shown in fig1 . the film 1302 can be deformed prior to or after the conductor 1308 is applied thereto . the ability to place the conductor traces 1306 within the higher intensity magnetic field lines facilitates the use of weaker magnets than are typically required for an electro - dynamic loudspeaker . the reduced strength magnets 1318 therefore contribute to a lesser expensive electro - dynamic loudspeaker 1300 . [ 0065 ] fig1 illustrates a flowchart of an alternative method for forming the conductor on the film of an electro - dynamic loudspeaker . at step 1400 , an aluminum foil layer is applied to a film using an adhesive . at step 1401 , a laser is utilized to etch away aluminum from the surface of the film in order to define the traces of the conductor . during the laser etching process , coolant fluid can be sprayed at the film material in order to cool the film material to prevent damage thereto due to the heat generated by the laser etching process . lasers of this type are currently used to cut vias in printed circuit boards but have not been utilized for removing a conductive material from a laminate . [ 0066 ] fig1 and 16 illustrate an alternative method of forming the conductor where the conductor is laser cut from an aluminum foil in order to form flat traces 1600 . at step 1501 , the conductor traces 1600 are applied to a film 1602 . adhesive is applied to a surface of the aluminum foil prior to laser cutting and the adhesive is cured by passing selective bands of light through the film material 1602 in order to more rapidly cure the adhesive . [ 0067 ] fig1 illustrates a method of forming an electrical conductor on a film is illustrated using an electron discharge machining ( edm ) process . the film 1900 is provided with a layer of foil and an electrode plate 1902 having a face configuration with a void 1904 ( shown in phantom in fig1 on the underside of the plate 1902 ) in the desired shape of the electrical conductor . the electrode plate 1902 is brought in close proximity to the foil layer on the film 1900 and through a known “ burning ” process , an arc is formed from the electrode plate and “ burns away ” or otherwise removes the foil material so that the remaining foil is in the shape of the void 1904 , which is in the desired shape of the electrical conductor 1906 , as shown in fig1 . the electron discharge machining process is carried out with the electrode and workpiece immersed in a machining fluid which is a dielectric ; i . e ., an insulating medium . to generate a spark between the two parts , a voltage higher than the breakdown voltage of the gap is applied . this breakdown voltage depends on the distance between the two electrodes at their closest point , the insulating characteristic of the dielectric fluid , and the level of pollution in the gap . at the point in the gap where the electric field is strongest a discharge commences which then develops as follows : ( a ) under the effect of the electric field , the free positive ions and electrons are accelerated , acquiring a high velocity and , very rapidly , they form an electrically - conductive ionized channel . ( b ) at this stage , current can pass through the channel . a spark is initiated between the electrodes and a plasma is formed . this rapidly attains a very high temperature , expanding under the effect of numerous impacts of charged particles and causing instantaneous local melting of material at the surface of both conductors . at the same time , due to vaporization of the electrodes and of the dielectric fluid , a gas bubble expands , and its pressure increases . at the moment the current is cut off , the gas bubble implodes due to the sudden fall of temperature , generating dynamic forces that results in melted material being ejected from the crater . this melted material is re - solidified in the dielectric fluid as small spheres and flushed away . [ 0072 ] fig2 illustrates a method of forming an electrical conductor on a film is illustrated . in the process , a foil , such as aluminum , is applied to a film 2000 . a mask 2002 in the desired shape of a conductor is applied to the foil . an abrasive removing process is then employed to remove the foil in the unmasked areas . preferably , a water jet device 2004 can be used with an abrasive slurry for abrading away the unmasked foil surface in order to leave the masked conductor shaped foil on the film 2000 . other known abrasive and polishing type processes can also be employed for abrasively removing the foil from the unmasked areas . while various embodiments of the invention have been described , it will be apparent to those of ordinary skill in the art that other embodiments and implementations are possible that are within the scope of this invention . accordingly , the invention is not restricted except in light of the attached claims and their equivalents . | 7 |
with respect first to fig1 an electrical interconnection is shown as comprised of a plug connector 2 and a receptacle connector 4 . the plug connector 2 is adapted to be connected to a shielded cable 6 which preferably contains a plurality of twisted pair conductors , whereas receptacle 4 is adapted to be connected to a printed circuit board ( not shown ). both electrical connectors are fully shielded where the plug connector 2 includes a shielded enclosure 8 which is preferably a die - cast housing of two similar halves , whereas receptacle 4 includes a shield 10 which in the preferred embodiment is a stamped metallic housing . each electrical connector also includes a mating interface comprised of a shielding shroud , plug connector 2 having a shielding shroud shown generally at 12 which is profiled to receive in shielding engagement , the shielding shroud 14 of receptacle 4 . finally , plug connector 2 includes elongate jackscrews 16 and 18 which are profiled for threaded engagement with complementary threaded posts 20 and 22 , respectively , of the receptacle 4 . it should be appreciated that , when the jackscrews 16 , 18 are fully threaded into their respective threaded posts 20 , 22 , the two electrical connectors 2 , 4 are in a fully mated condition where electrical terminals within plug connector 2 are fully electrically engaged with electrical terminals in receptacle 4 , as will be described in greater detail herein . the interface configuration is more described in co - pending patent application filed on even date as serial no . 60 / 264 , 761 ( attorney &# 39 ; s docket number 17628 ) incorporated herein by reference . the plug connector is described more fully in co - pending patent application filed on even date as serial no . 60 / 264 , 763 ( attorney &# 39 ; s docket number 17629 ), incorporated herein by reference . with respect now to fig2 the receptacle 4 is generally comprised of the outer shield member 10 , the front shielding shroud 14 , an inner housing 30 , boardlock members 32 , and a terminal lead frame assembly shown best at 40 . with respect now to fig3 and 4 , the housing 30 will be described in greater detail . housing 30 generally includes side walls 44 and 46 with an intermediate top wall 48 . the side walls 44 , 46 and top wall 48 together form a contact receiving area 50 intermediate side surfaces 52 , 54 , and rearward of rear face 56 . as shown in fig3 the housing 30 further includes a front face 58 having an integrally molded shroud portion 60 extending forwardly therefrom having a front face 62 . the shroud member 60 includes two rectangular recesses shown at 64 and 66 ( fig3 and 6 ) which extend rearwardly to rear face 56 ( fig4 ). as shown in fig6 the openings 64 and 66 form therein upper and lower surfaces , for example , upper surface 68 and surface 70 of opening 64 , and upper surface 72 and lower surface 74 of opening 66 . also , side - by - side terminal receiving slots 80 extend through the rear wall 56 and partially into surfaces 68 , 70 , 72 , and 74 as best shown in fig3 - 6 . while the terminal receiving slots are shown generally at 80 , it should be appreciated from fig5 and 6 that a plurality of positions exist , extending in horizontal rows and vertical columns . as shown best in fig5 in the preferred embodiment of the invention , there are four rows of terminal receiving slots 80 , and fourteen vertical columns . more specifically , the terminal receiving slots are , from left to right as viewed in fig5 positions 82 a , 82 b ; 84 a , 84 b ; 86 a , 86 b ; 88 a , 88 b ; 90 a , 90 b ; 92 a , 92 b ; and 94 a , 94 b . housing 30 further includes latching projections 100 extending from top wall 48 ( fig3 ) as well as latching projection 102 extending from lower wall 104 ( fig4 ). housing member 30 also includes apertures 110 and 112 , which open up into respective square cavities 114 , 116 ( fig4 ), as further described herein . the housing 30 also includes recessed wall portions 120 , 122 having elongate projections 124 and 126 . recessed wall portion 120 further includes cut - out portions at 130 and a lower standoff wall 132 forming locking edges 134 . likewise , recessed wall portion 122 includes cut - out portions 135 , a standoff wall at 136 having locking edges at 138 . as shown best in fig7 and 8 , shroud 14 generally includes a front wall portion 150 having apertures 152 and 154 extending therethrough . latching ears 156 extend from top and lower edges of the wall 150 and include latching apertures 160 . a drawn shroud portion 170 extends integrally from the wall portion 150 and is complementary to the shielding shroud 12 of the plug connector which was described in fig1 . shroud portion 170 includes top and bottom wall portions 172 and 174 and side wall portions 176 and 178 . side wall portion 176 is angled upwardly and outwardly so as to define an obtuse angle relative to lower wall 174 and an acute angle relative to top wall 172 . side wall 178 includes a portion 180 extending generally vertical relative to lower wall 174 and a concave radiused portion 182 which extends between side wall portion 180 and upper wall portion 172 . it should be appreciated that the shroud portion 170 is profiled to interferingly fit within shroud portion 12 . with reference now to fig1 , the boardlock member 32 generally includes a plate section 190 having an elongate opening at 192 , and folded - over lower tab portions 194 . tabs 196 extend from opposite ends of the plate portion , while compliant boardlock portions 198 extend from a lower edge of the plate portion 190 . with reference now to fig9 the outer shield 10 will be described in greater detail . outer shield member 10 includes a front face 200 having side walls 202 , 204 extending integrally therefrom . also , a top wall 206 , rear wall 208 , and lower wall 210 extend therefrom . openings 212 , 214 are provided to overlap with openings 152 , 154 in shielding shroud 14 ( fig8 ). furthermore , integral shielding contacts 220 extend from the marginal side edges of front face 200 and extend into side walls 202 , 204 , top wall 206 , and lower wall 210 . furthermore , printed circuit board tines 222 extend downwardly from side walls 202 , 204 , and from rear wall 208 . an opening 224 through front face 200 is like profiled as the shroud portion 170 , so as to fit thereover . with reference now to fig1 - 21 , the terminal assembly 40 will be described which includes a plurality of overmolded terminal lead frames , shown in fig1 - 21 . with reference first to fig1 , a lead frame is shown generally at 250 which is a stamped and formed lead frame including a plurality of contacts 252 , 254 , 256 , and 258 . in the embodiment of fig1 , the terminals 252 - 258 are still retained by the integral carrier strip at 260 . however , it should be understood that the carrier strip 260 will be removed for final assembly . with respect still to fig1 , the terminals generally include contact arms 252 a , 254 a , 256 a , and 258 a . contact portions 252 b , 254 b , 256 b , and 258 b extend integrally forwardly therefrom . furthermore , leg portions 252 c - 258 c extend from the arm portions 252 a - 258 a , respectively , and include printed circuit board tine portions 252 d - 258 d . with reference now to fig1 - 21 , a plurality of overmolded subassemblies are shown at 302 - 312 . it should be understood that all of the subassemblies 302 - 312 begin with the identical lead frame 250 , but that the lead frame 250 is overmolded in a different manner depending upon which terminal subassembly is required . more specifically , with reference to fig1 - 15 , the inserts are defined by two different overmolded webs , that is , webs 320 and 322 . overmolded web 320 includes a side surface 324 and an opposite side 326 . meanwhile , overmolded web 322 includes a side surface 328 and an opposite side 330 . it should be understood by comparing fig1 and 14 with those of fig1 and 19 , that subassembly 306 is depicted in fig1 , whereas subassembly 308 is depicted in fig1 . the terminal subassemblies are designed , such that the substantially solid side wall , for example , 324 , 328 , always has the smallest distance to the centerline of the lead frame 250 . furthermore , the lead frames 250 are positioned in the overmolded webs so as to be asymmetric , whereby distance d 1 in fig1 and 15 is smaller than distance d 2 in fig1 and 15 . furthermore , in the preferred embodiment of the invention , d 3 is equal to 1 . 2 mm , whereas distance d 1 equals 0 . 475 mm and distance d 2 equals 0 . 725 mm . furthermore , and still with reference to fig1 through 21 , each of the subassemblies 302 - 312 includes respective webs , for example , 302 a - 312 a ; first air pocket 302 b - 312 b ; second air pocket 302 c - 312 c ; third air pocket 302 d - 312 d ; and fourth air pocket 302 e - 312 e . it should also be appreciated that the air pockets are provided on the thick side of the respective webs 302 a - 312 a , that is , through the side where the thickness of the web is equal to d 2 . it should also be appreciated from reviewing fig1 - 21 , that some of the contact portions have been severed , for example , by comparing fig1 with fig1 and 17 , that inserts 302 and 304 have front contact portions 256 b and 258 b removed , and that by comparing fig1 with fig2 and 21 , that inserts 310 and 312 have contact portions 252 b and 254 b removed . finally , it should be understood that the terminal subassemblies are defined in pairs , such that subassemblies 302 , 304 ; 306 , 308 ; and 310 , 312 are pairs of inserts as described herein . with respect now to fig1 - 21 , together with fig5 it should be understood that terminal subassembly 302 is first inserted such that the contact portions 252 b and 254 b are positioned in terminal receiving slots 82 a . this positions the air pockets 302 b - 302 e towards the left side as viewed in fig5 or toward the outside . this also positions the thin web material , that is , distance d 1 , towards the right side or towards the center of the connector housing 30 . terminal subassembly 304 is next inserted in terminal receiving slots 82 b which positions the thin web of material of subassemblies 302 and 304 in abutting relation so that the centerline spacing between the lead frames in adjacent slots 82 a , 82 b is one millimeter . it should be appreciated that the next ten vertical columns , that is , columns 84 a , 84 b , 86 a , 86 b , 88 a , 88 b , 90 a , 90 b , and 92 a , 92 b are next assembled in a similar manner where once again subassemblies 306 and 308 are positioned in side - by - side relation with the terminal portions 252 b - 258 b in respective slot 84 a , etc . it should be appreciated that , as assembled , for example , air gap 306 b is positioned adjacent to and adjoining air gap 304 b in the adjacent contact assembly 304 . it should also be appreciated that terminal subassemblies 306 and 304 , while adjacent contact assemblies , are not in the same pair of terminals . said differently , the terminals are paired such that a pair of terminals are adjacent and in the same row , for example , slots 82 a , 82 b ; 84 a , 84 b ; and the like . it should also be appreciated that five pairs of subassemblies 306 and 308 are positioned in their respective slots 84 a - 92 b as these are like vertical columns of terminal receiving slots . finally , subassemblies 310 and 312 are positioned in respective slots 94 a and 94 b , once again with their thin webs of material being intermediate the lead frames 250 . as positioned in the housing , the terminals of a pair , for example , terminals 252 b of subassembly 302 and terminal 252 b of subassembly 304 are positioned with the centerline spacing of one millimeter . likewise , the adjacent terminals in different pairs of terminals , for example , terminal 252 b of subassembly 304 , and terminal 252 b of subassembly 306 , have a centerline spacing between them of 1 . 5 millimeters . thus , as positioned in the housing , the one - millimeter spacing between pairs of terminals maximizes the coupling between the pairs , whereas the 1 . 5 mm spacing between adjacent contacts of different pairs , together with the air gap defined by their abutting air gaps maximizes the impedance between them to minimize cross - talk . with the terminal subassemblies as described above , the remainder of the receptacle 4 will be described in greater detail . the shielding shroud 14 is connectable to the housing 30 by snapping the openings 160 ( fig7 ) over the latch projections 100 ( fig3 ) on the housing . the boardlock members 32 are then attached to the housing 30 , with the tabs 196 ( fig1 ) positioned in slots 130 , with tabs 194 positioned behind edges 138 and with elongate slot 192 positioned over elongate projection 124 . with the shielding shroud 14 , terminal subassemblies , and boardlock 32 assembled to the housing 30 , the assembly is completed by assembly of the shield 10 over the housing 150 . a square threaded insert 300 is positioned in respective square openings 114 , 116 and the shielding member 10 is thereafter positioned over the housing 30 such that shield extension 170 extends through opening 224 of the shield 10 . the threaded posts 20 and 22 can thereafter be positioned through openings 212 , 214 , through openings 152 , 154 ( fig8 ), and thereafter through openings 110 , 112 to be threadably connected with the square inserts 300 . this retains the threaded posts 20 , 22 to the front face of the receptacle for connection with the plug 2 . to connect the two connectors together , it should be appreciated that the shroud portion 170 is inserted within the shielding shroud 12 . this positions of respective shroud portions 12 , 14 in contact therewith . this also interconnects pairs of terminals in the receptacle 4 , for example , terminals 252 b of subassembly 302 , and terminal 252 b of subassembly 304 , with one of the twisted pairs of wire in cable 6 . this also provides for an excellent electrically compensated assembly . as mentioned above , the thin web of material between adjacent contacts of a pair , maximizes the coupling between the pair . furthermore , the alignment of the air gaps between adjacent pairs minimizes the cross - talk between them . | 7 |
for further illustrating the invention , experiments detailing use of 1 -( alkylsulfinyl )- 2 - isothiocyanatoalkyl - 1 - alkene for treating or preventing human or mammalian cancers and tumors are described below . it should be noted that the following examples are intended to describe and not to limit the invention . preparation of sulforaphene : glucosinolates in pre - ground radish seeds were hydrolyzed by an endogenous myrosinase in a phosphate buffer solution ( pbs ) having a ph value of 7 at the room temperature . in order to remove proteins and other impurities , the ph value was regulated to be 2 . 0 , and a resulting solution was filtered , extracted , and dried to obtain a natural crude extract , and sulforaphene having a purity of larger than 98 wt . % was yielded by a high - speed counter - current chromatography ( hsccc ). general operations : human cancer cells are cultured in a rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of a fetal bovine serum ( fbs ), and the culture medium is then placed in an incubator ( 37 ° c ., 5 % co 2 ) for 24 hrs . a 0 . 25 % trypsin solution and 0 . 02 % edta solution are utilized after cell proliferation for common digestion and subculture . the edta solution is a traditional digestion mean . trypsin is a serine protease possessing substrate specificity and used to digest adherent cells . however , divalent cations , such as calcium ions and magnesium ions , exist in the cells and are able to inhibit the digestion . edta is used to chelate these divalent cations so as to enhance the digestion effect of the trypsin . mtt assay is commonly used to measure the cell proliferation , the percentage of viable cells , and the cytotoxicity . mtt ( 3 -( 4 , 5 - dimethylthiazol - 2 - yl )- 2 , 5 - diphenyltetrazolium bromide ) ( also called thiazolyl blue tetrazolium bromide ) is a kind of yellow dye . the principle of the mtt assay is that the succinate dehydrogenase in mitochondria of living cells is capable of reducing the exogenous mtt into water - insoluble blue - purple crystalline formazan , which forms a precipitate in the cells , while dead cells do not have such function . dimethyl sulfoxide ( dmso ) dissolves formazan in cells . the absorbance measured at a 490 nm wavelength using an enzyme - linked immunosorbent assay indirectly represents the number of viable cells . in a certain range of the cell numbers , the amount of the formed mtt crystals is in positive proportion to the cell number . thus , the mtt assay is used to evaluate and determine the survival rate or the inhibition rate of the cells . such method has been widely applied in activity detection of some bioactive factors , large scale screen of antitumor drugs , cytotoxicity test , and determination of tumor radiosensitity and features high sensibility . specific embodiments of the invention are described hereinbelow for further explaining the advantages of the invention , however , the following embodiments should not be considered as limitations of the protection scope of any or all of the claims . 1 . experimental cell lines and related chemical reagents : human lung adenocarcinoma cell line a549 purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of a549 cells in vitro by sulforaphene and sulforaphane : a549 cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the a549 cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and a 50 % inhibitory concentration ( ic 50 ) on the cell growth was calculated . the experiment results were listed in fig1 . it was indicated from fig1 that sulforaphene has significant inhibition effect on the growth and proliferation of the human lung adenocarcinoma cells a549 . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the a549 cells was 10 . 5 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human lung adenocarcinoma cells a549 . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the a549 cells was 14 . 7 μm . 1 . experimental cell lines and related chemical reagents : human lung squamous carcinoma cell line h460 purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of h460 cells in vitro by sulforaphene and sulforaphane : h460 cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the h460 cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and the ic 50 on the cell growth was calculated . the experiment results were listed in fig2 . it was indicated from fig2 that sulforaphene has significant inhibition effect on the growth and proliferation of the human lung squamous carcinoma cells h460 . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the h460 cells was 25 . 7 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human lung squamous carcinoma cells h460 . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the h460 cells was 34 . 62 μm . 1 . experimental cell lines and related chemical reagents : human pancreatic carcinoma cell line panc - i purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of panc - i cells in vitro by sulforaphene and sulforaphane : panc - i cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the panc - i cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and the ic 50 on the cell growth was calculated . the experiment results were listed in fig3 . it was indicated from fig3 that sulforaphene has significant inhibition effect on the growth and proliferation of the human pancreatic carcinoma cells panc - i . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the panc - i cells was 5 . 18 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human pancreatic carcinoma cells panc - i . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the panc - i cells was 6 . 73 μm . 1 . experimental cell lines and related chemical reagents : human breast carcinoma cell line mcf - 7 purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of mcf - 7 cells in vitro by sulforaphene and sulforaphane : mcf - 7 cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the mcf - 7 cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and the ic 50 on the cell growth was calculated . the experiment results were listed in fig4 . it was indicated from fig4 that sulforaphene has significant inhibition effect on the growth and proliferation of the human breast carcinoma cells mcf - 7 . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the mcf - 7 cells was 14 . 3 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human breast carcinoma cells mcf - 7 . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the mcf - 7 cells was 19 . 46 μm . 1 . experimental cell lines and related chemical reagents : human hepatocarcinoma cell line hepg2 purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of hepg2 cells in vitro by sulforaphene and sulforaphane : hepg2 cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the hepg2 cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and the ic 50 on the cell growth was calculated . the experiment results were listed in fig5 . it was indicated from fig5 that sulforaphene has significant inhibition effect on the growth and proliferation of the human hepatocarcinoma cells hepg2 . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the hepg2 cells was 59 . 0 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human hepatocarcinoma cells hepg2 . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the hepg2 cells was 47 . 33 μm . 1 . experimental cell lines and related chemical reagents : human cervical carcinoma cell line hela purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of hela cells in vitro by sulforaphene and sulforaphane : hela cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the hela cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and the ic 50 on the cell growth was calculated . the experiment results were listed in fig6 . it was indicated from fig6 that sulforaphene has significant inhibition effect on the growth and proliferation of the human cervical carcinoma cells hela . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the hela cells was 24 . 1 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human cervical carcinoma cells hela . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the hela cells was 25 . 8 μm . 1 . experimental cell lines and related chemical reagents : human malignant melanoma cell line a375 purchased from us atcc cell bank was cultured in the rpmi - 1640 ( hyclone ) culture medium comprising 10 v . % of the fbs , digested by the 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . all related chemical reagents in this experiment were purchased from sigma . 2 . inhibition of a375 cells in vitro by sulforaphene and sulforaphane : a375 cells at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator ( 37 ° c ., 5 % co 2 ) for culture . sulforaphene and sulforaphane were respectively dissolved by sterile deionized water , resulting solutions were then allowed to pass through 0 . 22 μm filters for removing bacteria . filtrates were then diluted by a serum - containing medium to enable final concentrations of the sulforaphene or sulforaphane to be 10 μm , 20 μm , 30 μm , 40 μm , and 50 μm , respectively . after 24 hrs of cultivation , the a375 cells were then cultured by the culture solutions comprising the sulforaphene or sulforaphane of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 48 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm . the number of viable cells in the negative control group at 0 hr was taken as a basis , and the ic 50 on the cell growth was calculated . the experiment results were listed in fig7 . it was indicated from fig7 that sulforaphene has significant inhibition effect on the growth and proliferation of the human malignant melanoma cells a375 . after 48 hrs of treatment , the ic50 of sulforaphene on the growth of the a375 cells was 7 . 8 μm . sulforaphane has significant inhibition effect on the growth and proliferation of the human malignant melanoma cells a375 . after 48 hrs of treatment , the ic50 of sulforaphane on the growth of the a375 cells was 9 . 11 μm . erlotinib , gemcitabine , paclitaxel , and 5 - fu are four effective drugs for treating lung cancer and mammary cancer . as a drug for target therapy , the erlotinib is applicable to a third - line treatment of locally advanced or metastatic non - small cell lung cancer when two or more than two chemotherapies are failed . currently , the gemcitabine is clinically utilized as the drug of the first - line therapy in treating advanced non - small cell lung cancer and the metastatic breast cancer . the paclitaxel is primarily applied in the mammary cancer and has a certain efficacy in treating the lung cancer as well . the 5 - fu has relatively good efficacy in treating the mammary cancer and the digestive system cancer ( esophageal cancer , stomach cancer , colon cancer , pancreatic cancer , and liver cancer ). thus , the above four drugs are selected as the chemotherapeutic drugs in the control groups to study the differences antitumor effects compared with the sulforaphene . 1 . experimental cell lines and related chemical reagents : sources and cultivation of the human lung adenocarcinoma cells a549 , the human lung squamous carcinoma cell line h460 , the human breast carcinoma cell line mcf - 7 are described in the above . the related chemical reagents in the experiment are all purchased from sigma . 2 . inhibition of cells a549 , h460 , and mcf - 7 in vitro by the sulforaphene and other chemotherapeutic drugs : cells a549 , h460 , and mcf - 7 at exponential growth phase were collected , digested into single cells , and inoculated to 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into the incubator ( 37 ° c ., 5 % co 2 ) for culture . the cells were respectively treated by 10 μm of the sulforaphene and 10 μm of other chemotherapeutic drugs ( erlotinib , gemcitabine , paclitaxel , and 5 - fu ), cells in culture media of negative control groups were cultured by equal volume of sterile deionized water . the anti - tumor effects of the above drugs were measured by the mtt assay . the number of viable cells in the negative control groups at 0 hr was taken as a basis to calculate the anti - tumor effects . the inhibition rates of the drugs against the tumor cells were specifically listed in table 1 . it is known from the experiment results in table 1 that compared with the erlotinib , the gemcitabine , and the paclitaxel , the sulforaphene has much significant inhibition effect against the growth and proliferation of cells a549 and h460 . in cells mcf - 7 , the anti - tumor effect of the sulforaphene is not comparable with the paclitaxel of the same concentration but is significantly higher than the gemcitabine and the 5 - fu . thus , the sulforaphene has comparable or much superior inhibition effect against most tumor cells compared with the sulforaphane and other third - line chemotherapeutic or targeting drugs , which include but are not limited to the erlotinib , the gemcitabine , and the paclitaxel . thus , sulforaphene possesses significant inhibition effect on the growth of the following tumor cells , which include but are not limited to human lung adenocarcinoma , human lung squamous carcinoma , human pancreatic cancer , human liver cancer , human breast cancer , human cervical cancer , and human malignant melanoma . 1 . 1 preparation of experimental animals : 30 nude mice with equal numbers of females and males were fed in normal conditions in the laboratory for between 3 and 5 days . 1 . 2 . preparation of h460 cells : h460 tumor cells were normally cultured , and diluted using the pbs so as to prepare a suspension of tumor cells having a concentration of 7 . 5 × 10 6 tumor cells per milliliter . 1 . 3 inoculation of tumor cells : the suspension of the tumor cells was fully shaken and 0 . 2 ml of the suspension was then sucked by a sterile syringe having a capacity of 1 ml . the tumor cells were then inoculated into armpits of the nude mice via subcutaneous injection . the inoculated mice were then fed for between 2 and 3 days in normal conditions . when the tumor tissue grew to a size with a long axis of approximately 3 mm and a short axis of approximately 2 mm , all the nude mice having the tumor tissues were randomly divided into three groups , which were utilized in subsequent administration experiments . 2 . design of the experimental groups : an aqueous solution of an orally administrated drug had a concentration of 35 . 37 × 10 − 3 mol - l − 1 ; 2 . 1 control group : five male mice and five female mice having tumor tissues were orally administered with ultrapure water for three times each week ( respectively at monday , wednesday , and friday afternoons ), and the administered volume was 0 . 3 ml for each time . 2 . 2 experimental group 1 : five male mice and five female mice having tumor tissues were orally administered with sulforaphene with a dosage of 75 mg of the sulforaphene per kg of weight for three times each week ( respectively at monday , wednesday , and friday afternoons ), and the administered volume was 0 . 3 ml for each time . 2 . 3 experimental group 2 : five male mice and five female mice having tumor tissues were orally administered with sulforaphane with a dosage of 75 mg of the sulforaphane per kg of weight for three times each week ( respectively at monday , wednesday , and friday afternoons ), and the administered volume was 0 . 3 ml for each time . 3 . 1 acquisition of weight data of nude mice : weight data of the nude mice were collected three times per week ( respectively at monday , wednesday , and friday afternoons ). an electronic balance was utilized to record the weight data , and an accuracy of the weight data was 0 . 01 g . 3 . 2 . acquisition of sizes of tumor tissues in the nude mice : the sizes of the tumor tissues in the nude mice were measured three times per week ( respectively at monday , wednesday , and friday afternoons ). an electronic vernier caliper was utilized to measure the long axis and the short axis of the tumor tissues , and an accuracy of the data was 0 . 01 mm . 3 . 3 . observations of other data and phenomenon : the survival conditions of the nude mice were closely observed . in case of death , the time of death , the number of the nude mouse , and the corresponding group were timely recorded . and in case of abnormal conditions of the nude mice , the time of the occurrence and the symptoms were timely recorded . 3 . 4 finish time of the experiments : when the tumor tissues in the nude mice of the control group reach an average size of 1000 mm3 ( volume = long axis × short axis 2 × 0 . 5236 ), the weights and the sizes of the tumor tissues of the nude mice were recorded , and then the experiments were stopped and the nude mice were treated . 3 . 5 treatment of nude mice when finishing the experiments : the nude mice were killed , arranged according to different groups , and photographed . six representative mice were selected from each group and photographed . then the tumor tissues were respectively isolated , weighed , placed at corresponding positions , and photographed . experiment results were listed in table 2 : each group of the nude mice was orally administered with the sulforaphene or drugs of the control groups ( with 75 mg / kg each time ). it is known from the above results that the sulforaphene has significant inhibition effect on the growth of the tumor cells in vivo ( as shown in fig8 ), and the inhibition effect of the sulforaphene is superior to that of the sulforaphane ( as shown in fig9 ). general operations : normal peripheral blood cells were isolated by ficoll to obtain mononuclear cells . the mononuclear cells were rinsed by the pbs for three times , and added with imdm + 10 % fbs to prepare suspensions . 10 μm , 30 μm , and 50 μm of sulforaphene or sulforaphane and other four chemotherapeutic drugs were added to the suspensions for treatment , respectively . the suspensions were then inoculated into 96 - well plates , with each hole containing 25 thousands cells per 100 μl of the culture medium , and cultured overnight at 37 ° c . treatment : because the proliferation of the pbmcs is very limited and the pbmcs quickly enter a decline phase . thus , the cell viability was measured by the mtt assay after 24 hrs of culture . four drugs with different mechanisms were employed to treat leukocytes , which were cis - platinum , 5 - fluorouracil ( 5 - fu ), paclitaxel , and adriamycin , respectively , and a drug concentration of thereof was 10 μm . a total of eleven experiment groups were divided : sulforaphene treated groups with concentrations of 10 μm , 30 μm , and 50 μm , sulforaphane treated groups with concentrations of 10 μm , 30 μm , and 50 μm , a cis - platinum treated group , a paclitaxel treated group , an adriamycin treated group , a 5 - fu treated group , and a negative control group , specific data of which are listed in table 3 . the group where pbmcs were treated by the sterile deionized water was selected as the negative control group . 1 . experimental cells : normal peripheral blood cells were isolated by ficoll to obtain mononuclear cells . the mononuclear cells were rinsed by the pbs for three times , added with imdm + 10 % fbs to prepare suspensions , commonly digested by 0 . 25 % trypsin solution and 0 . 02 % edta solution , and then subcultured . 2 . inhibition of pbmcs in vitro by sulforaphene and the contrast chemotherapeutic drugs : signal cells of the digested pbmcs were inoculated to the 96 - well plates with each hole containing 3000 cells . then the 96 - well plates were transferred into an incubator at 37 ° c . for culture . the sulforaphene was dissolved by the sterile deionized water , and a resulting solution was then allowed to pass through a 0 . 22 μm filter for removing bacteria . a filtrate was thereafter diluted by a serum - containing medium to enable final concentrations of the sulforaphene to be 10 μm , 30 μm , and 50 μm , respectively . the sulforaphane was prepared in the same way . concentrations of the contrast chemotherapeutic drugs were as follows : 50 μm of the cis - platinum , 60 μm of the 5 - fu , 20 μm of the paclitaxel , 5 μm of the adriamycin . after 12 hrs of cultivation , the pbmcs were then cultured by culture solutions comprising the sulforaphene of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 24 hrs of cultivation , 20 μl of mtt was added to each hole , and the plates were incubated for 3 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed and replaced by 150 μl of dmso . thereafter , the plates were cultured in a shaking table for 10 min , and the absorbance of each hole was measured at the wavelength of 490 nm experiment results were listed in table 3 . it is indicated from table 3 that the toxicity of the sulforaphene on the pbmcs is significantly lower than the sulforaphane and the other selected chemotherapeutic drug treated groups . the contrast chemotherapeutic drugs have significant inhibition effect on the growth and proliferation of the pbmcs . the sulforaphane has certain effect on the proliferation of the cells , while the effect of the sulforaphene on the proliferation of the cells is not significant . general operations : 1 - 2 day old neonatal sd rats ( female or male ) were selected and cardiomyocytes were isolated in sterile condition . cardiomyocytes were cultured for 3 days and then treated with sulforaphene or sulforaphane of concentrations of 10 μm , 30 μm , and 50 μm , or adriamycin of the concentration of 10 μm for 24 hrs . the cardiotoxicity of the above drugs were represented by a ratio of atp / total protein . the experiment was performed in 8 groups : sulforaphene treated groups with concentrations of 10 μm , 30 μm , and 50 μm , sulforaphane treated groups with concentrations of 10 μm , 30 μm , and 50 μm , an adriamycin treated group , and a negative control group , specific data were listed in table 3 . the group where pbmcs were treated by the sterile deionized water was selected as the negative control group . 1 . experimental cells : 1 - 2 day old neonatal sd rats ( female or male ) were selected and sterilized . then ventricular muscles were collected and digested by trypsin to prepare cardiomyocyte suspensions . the suspensions were cultured in the incubator ( 37 ° c ., 5 % co 2 ), and primary cardiomyocytes were cultured by differential adhesion . an average viability of the cardiomyocytes evaluated by trypan blue staining was 98 . 2 %, and a purity of the cardiomyocytes evaluated by immunofluorescence method is 98 . 7 %. 2 . inhibition of the rat primary cardiomyocytes in vitro by sulforaphene and the contrast chemotherapeutic drugs : single cells of the digested rat primary cardiomyocytes were inoculated to 24 - well plates and incubated in the incubator ( 37 ° c ., 5 % co 2 ). the sulforaphene , the sulforaphane , and the adriamycin were prepared by the same methods as described in the above . after 12 hrs of cultivation , the rat primary cardiomyocytes were then cultured by culture solutions comprising the sulforaphene , the sulforaphane , or the adriamycin of corresponding concentrations , and to the culture media of the negative control group an equal volume of sterile deionized water was added for cell culture . after another 6 hrs of cultivation , the culture solution in each hole was replaced by the normal culture solution not containing any drugs , and incubated for 42 hrs in the incubator ( 37 ° c ., 5 % co 2 ). solution in each hole was then removed , and cells therein were rinsed by the pbs for three times , digested by the trypsin , and gathered into two parts . one part of the cells was utilized to measure the atp level by the reporter gene assay , and the other part of the cells was utilized to measure the cellular protein concentration by bac assay . the ratio of atp ( ng ) to the protein concentration ( ng ) was calculated , and the ratio of each experimental group is divided by the ratio of the contrast group to obtain the relative ratio of atp / total protein , experimental results were listed in table 4 . it is known in table 4 that the toxicity of the sulforaphene on the cardiomyocytes is significantly lower than that of the sulforaphane , and the adriamycin has obvious toxicity on the cardiomyocytes . conclusion : it is indicated from the systematic study of the invention that sulforaphene is superior to conventional antitumor drugs including sulforaphane , erlotinib , gemcitabine , and paclitaxel in inhibiting the growth of many kinds of cancer cells , and has higher security than sulforaphane , cis - platinum , 5 - fluorouracil , paclitaxel , and adriamycin . so , sulforaphene has potential antitumor activities against lung cancer , lung squamous cell carcinoma , pancreas cancer , liver cancer , mammary cancer , cervical carcinoma , malignant melanoma , and so on . unless otherwise indicated , the numerical ranges involved in the invention include the end values . while particular embodiments of the invention have been shown and described , it will be obvious to those skilled in the art that changes and modifications may be made without departing from the invention in its broader aspects , and therefore , the aim in the appended claims is to cover all such changes and modifications as fall within the true spirit and scope of the invention . | 0 |
now referring to fig1 - 3 , the leather decorative laminate of the present invention is generally represented by reference numeral 10 . the leather decorative laminate 10 includes a core layer 12 and a decorative layer 14 . the core layer 12 is of known construction , consisting of paper , woven fabrics , mats , felts , or the like . the core layer 12 preferably consists of one or more cellulosic sheets , preferably kraft paper , impregnated with a laminating resin . the basis weight of the cellulosic sheets can be varied to suit the application at hand . any of the conventional laminating resins commonly used for the core layer , such as a phenolic , melamine , amino , epoxy , polyester , silicone , and diallyl phthalate resins , to name a few , may be used . the preferred laminating resin for the core layer sheets is a phenolic resin made from reaction of phenols with formaldehyde . the resin content of the impregnated sheets can be varied to suit the application at hand , but in most cases is between about 25 % to about 35 %. resins of this type can be purchased commercially or prepared according to conventional procedures . alternatively , the core layer 12 may include a pigmented core paper such as that used in melcor ® brand laminates produced by the assignee of the present application . the melcor ® core paper provides the option of colored edges . the decorative layer 14 includes a leather material . the “ leather ” referred to herein is an animal hide and is not limited to any particular type of animal . preferably , the leather material of the present invention is a “ bonded leather ”. the term “ bonded leather ” as used herein refers to a leather product that comprises leather shavings made from scrap and / or recycled leather . the shavings are processed into a sheet product using bonding agents . bonded leather is commercially available and will not , therefore , be further described herein . a leather sheet thickness in the range of about 0 . 2 mm to about 4 . 0 mm is acceptable for most applications . a sheet thickness of about 0 . 2 mm to about 0 . 8 mm has particular utility . although leather with an embossed finished surface can be used , it is preferable to use leather that initially has a smooth surface . textures and other design features can be imparted to the laminate during the manufacturing process as will be explained in greater detail below . referring to fig2 , in some embodiments the present leather decorative laminate 10 further includes an overlay 16 disposed on the side of the leather decorative layer 14 opposite the core layer 12 . the overlay 16 may , for example , consist of one or more sheets of high - quality alpha cellulose paper impregnated with a melamine formaldehyde resin . the alpha - cellulose paper acts as a translucent carrier for the resin , imparts strength to the resin , facilitates maintaining a uniform resin thickness , and provides additional abrasion resistance to the leather layer 14 . in some embodiments of the present invention , the leather decorative laminate 10 further includes a backer layer 20 disposed on the side of the core layer 12 opposite the first decorative layer 14 . the backer layer 20 is of known construction , consisting of paper , woven fabrics , mats , felts , or the like . the backer layer 20 preferably consists of one or more cellulosic sheets impregnated with a laminating resin such as a melamine formaldehyde type resin . backing sheets of this type can be purchased commercially or prepared according to conventional procedures . referring to fig3 , in some embodiments of the present invention the leather decorative laminate 10 further includes a second leather decorative layer 18 disposed on the side of the core layer 12 opposite the first decorative layer 14 . depending on the application , the core layer 12 can be increased in thickness to provide structural integrity . a first process for manufacturing the present leather decorative laminate 10 involves stacking the core layer 12 sheets and the leather decorative layer 14 ( and may include one or more of an overlay sheet 16 , a backing sheet 20 , and a second decorative layer 18 ) in a superimposed relationship ( also referred to as a “ build - up ”) between steel plates . a release sheet is placed between the press and the core layer 12 , and between the decorative sheet 14 , 18 and the steel plate . the physical properties of each release sheet is chosen to ensure the release sheet does not bond with the decorative layer 14 or otherwise negatively affect the laminate materials . the release sheet contiguous with the leather decorative layer 14 , 18 is typically textured to impart an embossed texture or pattern to the laminate 10 . the build - up is then subjected to a predetermined pressure and temperature for a time sufficient to cure the laminating resins impregnating the respective layers . in production environment , a multiple opening press can be used to process multiple build - ups at the same time . in this process , a book of build - ups is created by stacking the respective layers of a first build - up in the aforementioned order ( e . g ., core layer sheets , decorative sheet ). a release sheet is placed on top of the decorative sheet 14 ( or overlay 16 if used ), and a double - sided steel plate is placed on top of the release sheet . the next build - up is then stacked in opposite order on top of the double - sided steel plate ( e . g ., release paper , decorative sheet 14 , core layer 12 sheets ), and so on until the book is produced . once the appropriate book size is created , the book is stored on the loading rack and the process is repeated until a plurality of books are stacked on the loading rack . the loading rack is then used to insert the books between the platens in the press . pressure is applied to the press . after full pressure is reached , heat is applied until the predetermined temperature is reached . the press is held at the predetermined pressure and temperature for a period of time referred to as the “ heating cycle ”, typically in the range of 2 to 20 minutes . the heat is subsequently removed , but the pressure maintained , for another predetermined period of time referred to as the “ cooling cycle ”, typically in the range of 7 to 15 minutes . the pressure is then released and the build - ups , which are now leather decorative laminates 10 , are removed . the heating cycle time range provided reflects the amount of time typically necessary for all of the laminates 10 in the press to reach and stay at the desired predetermined temperature . the actual temperature and pressure ranges may vary for different applications and process equipment . the cooling cycle is dictated by the amount of time necessary before the laminates 10 can be removed from the press and practically handled . a second process for manufacturing the present leather decorative laminate 10 involves dispensing the core layer 12 sheets and the leather decorative layer 14 ( and one or more of an overlay sheet 16 , a backing sheet 20 , and a second decorative layer 18 , if used ) in the aforesaid superimposed relationship upstream of a continuous press . the press is set up to create the temperature and pressure environment required to bond the layers into the finished laminate product . the line speed of the continuous press is chosen to create a dwell time within the press for the laminate 10 that is adequate to ensure sufficient bonding . a release sheet is disposed on each side of the build - up prior to entering the press . as stated above , the release sheet contiguous with the leather decorative layer 14 is typically textured to impart an embossed texture to the laminate . the release sheets are typically drawn off after the laminate exits the press , and rolled for further handling . the leather decorative laminate 10 continues onto downstream handling equipment ; e . g ., equipment that cuts the continuous laminate product into sheets , and handling equipment for the sheets . the continuous press is advantageous because it decreases the processing time of the laminate 10 . in both manufacturing processes , the elevated temperature and pressure environment causes the impregnated resins within the sheets to flow , which consolidates the constituents within each build - up into the integral leather decorative laminate 10 . the present leather decorative laminate 10 is typically processed at a temperature in the range from about 120 ° c . to about 250 ° c ., and at a pressure within the range of about 400 psi to about 1600 psi . the following examples are illustrative of the present leather decorative laminate and do not constitute any limitation with regard to the subject matter of the invention : a single leather decorative laminate 10 is manufactured using a non - continuous press . a build - up consisting of a release sheet , a plurality of core layer 12 sheets , a leather decorative layer 14 , and a textured release sheet is made in a superimposed relationship and placed between steel plates . the build - up is then subjected to a pressure of about 1100 psi . once the predetermined pressure is reached , the press is heated to a predetermined temperature of about 125 ° c . the press is held at the predetermined pressure and temperature for a heating cycle of about 14 minutes . after the heating cycle is completed , the heat is subsequently removed , but the pressure is maintained for a cooling cycle of about 11 minutes . the pressure is then released and the build - up , which is now a leather decorative laminate 10 , is removed . the release sheets are removed and the leather decorative laminate 10 is complete . a leather decorative laminate 10 can be manufactured in a continuous process using a grecon ® continuous high - pressure laminating press , which includes an inlet section , a heating section and a cooling section . the temperature of each section is controlled independently . the total amount of heat imparted to the layers of the build - up is controlled by the temperature of the different sections and the dwell time , which is dependent on the line speed . this continuous process requires that all of the various layers used to manufacture the laminate be fed into the press as continuous webs . in the present example , the build - up consists of , from top to bottom , a textured release paper , a pre - dried leather decorative layer 14 and the core layer 12 . all layers are fed in a continuous manner into the press at 5 feet / min . the temperature settings of the different press sections are as follows : the inlet section is set at 90 ° c ., the heating section is 135 ° c ., and the cooling section is 115 ° c . the pressure is set at approximately 400 psi . it will be obvious to those skilled in the art that various changes may be made without departing from the scope of the present invention and that the invention is not to be considered limited to what is described and exemplified in the specification . | 1 |
fig1 illustrates an embodiment of a fractal structure which in addition to the offset fractal characteristic of this invention also includes merging and contact channels , a fractal collector and a heat exchange enclosure . this embodiment is useful as a processing ( mixing and / or reaction element in pipe configurations . flow input channels 1 and 2 are for the separate fluids which will be mixed . additional inputs can be added if more than two fluids are to be mixed . input 1 provides flow to offset fractal distributor 7 while input 2 provides flow to offset fractal distributor 6 . the fluid flows are scaled and distributed through these offset fractals . after independent fractal scaling of the fluids , the two input lows contact one merging channels 8 and proceed in a mixed condition through channels 9 . in the channels 9 , hereinafter denominated “ contact channels ,” the fluids are finally brought into contact one with another . the flows in contact channels 9 are re - scaled to a single flow through fractal collector 10 and exit channel 3 . the enclosure 11 is used if temperature control is required for mixing or reaction or if an enclosure is needed for flanging or other attachment . in the case of temperature control , a heat exchange fluid is typically passed from conduit 4 to the inside volume of the mixer for heat exchange with the internal conduit and out conduit 5 . in the case of using the enclosure as an attachment structure , enclosure 11 can be a solid material surrounding the internal channels . for example , enclosure 11 can be used as a simple flange for attachment to a pipe flange . fig2 illustrates the offset of fractal distributors 6 and 7 . the fractal distributors not intersect because they are set on different planes , as shown in fig3 . note that the flows through fractals 6 and 7 are independent and cannot contact one another until after they exit fractals 6 and 7 . if more than two fluids are mixed , additional independent offset fractals can be used . if more than two fluids are mixed or reacted by these devices , all can be merged simultaneously or they can be progressively mixed . this can easily be accomplished by placing merging channels at different positions along the length of the device . an example of such a use would be when two fluids must first be mixed or reacted before mixing or reacting with a third fluid . the third fluid would merge at an appropriate distance downstream from the merging of the first two fluids . for purposes of illustration , each input conduit is shown scaled to 64 smaller conduits . however it is a basic characteristic of this device that the fractal conduits can be progressively bifurcated to smaller and more numerous paths until restrictions on manufacturing are reached . it is recognized that increasing the number of bifurcations will provide a progressively improved homogeneity of mixing and reaction . because each independent distribution fractal ( 6 and 7 ) in these figures bifurcates to 64 flow paths , there are 128 total distribution channels prior to merging and these merge to form 64 contact channels ( 9 ). fig3 illustrates the approximate location of fractal collector 10 . because this invention uses fractals for the offset structures , those skilled in the art will recognize that this provides an inherent geometric variability which adds to the practical value of this invention . one reason variable geometry may be desired for the fractals is that the device may require a geometry constrained by the corresponding geometry of an enclosure it is contained in or a receiving device it exits into . another reason for variable geometry is to provide the artisan with control over hydraulic characteristics such as pressure drop . fractals are constructed using an initiator structure , or parent structure , with self similar structure added at smaller and smaller scales . the initiator in the illustrated embodiment is in the form of an “ h ” and as a result , four new child structures are added to each “ h ” as smaller scale structure is added . it is well known in the art that fractals can be constructed using variations in the initiator geometry , number of branches , branch angles and in the amount of initiator symmetry ( fig1 ). just as an example , the initiator could be a symmetric “ y ” having one leg longer that than the other two . another way to vary the device geometry is by altering the child structures . the child structures need not exhibit scaled - down geometry identical to the initiator . this type of variation can include the geometry or symmetry of the child structures at each iteration , for example by using variable scaling factors for determining child structure dimensions and channel diameters . we note that the number of generations of child structure can be varied as desired ( the number of fractal iterations ) to obtain a desired level of scaling prior to mixing / reaction or to meet practical requirements such as the avoidance of device plugging . ( fig1 ) the offset fractals need not be identical . ( fig1 ) as an example , if three offset fractals are used to mix or react three materials , two of the fractals could of an identical geometry while a third is not , or all three could be of different geometry . the reason for this is that the materials to be treated may have variable characteristics which would suggest to a person skilled in the art to use different geometries . for example , the flow rate through one fractal may be very high compared with a second so that pressure drop may be best controlled by using differing channel cross sectional area or number of fractal iterations through each individual fractal . fig4 is a top view and fig5 is an isometric view of the pipe element embodiment . while this embodiment is useful when the flow from the mixing or reactor process should be re - collected into a single flow , the device can be used to advantage without the collector . this can be useful , for example , when mixing air and gas for a combustion application or for injecting the mixture into the side of a tank or other vessel . fig6 illustrates an embodiment without re - collection . in this case the fluids from inputs 1 and 2 are scaled and distributed in the same manner as described earlier but the flows are not re - collected into one flow , i . e ., output channel 3 and fractal collector 10 have been removed . in this embodiment the large number of contact channels 9 exit the device independently at contact channel exits 12 . because the rest of the device is the same as described earlier , in this example there will be 64 such exits . it is also possible to eliminate the merging channels 8 and mixing channels 9 so that the scaled and intermingled flows exit the device prior to contact with one another . fig7 illustrates this minimal configuration for the invention and consists of the flow inputs 1 and 2 , and the offset fractals 6 and 7 . fractal 7 exits through outlets 13 and fractal 6 exits through outlets 14 . for these last two embodiments , the enclosure ( 11 ) is again optional but can be useful for either heat exchange or for attaching or flanging the device to a vessel . we note that the area 17 ( fig7 ) that the offset fractals exit into need not be a plane . the fractals can exit to a curved ( fig9 ) or irregular surface ( fig1 ). this can be useful , for example , if the target vessel has a curved or irregular shape . in such a case , it can be useful to match the curved surface of the vessel with a complementary curve on the exit surface of the mixing device . the figures show the offset fractals bifurcated perpendicular to the large scale inlet and outlet flow direction . it is possible to bifurcate the fractals at any angle from perpendicular to nearly parallel to these flow directions . configuring at angles which are not perpendicular to the large scale flow can have advantages as well as disadvantages . one advantage of using fractal bifurcations more in - line with the flow direction is that it may be possible to operate the device with less pressure drop since flow momentum will not be forced to make as drastic a change in direction as the bifurcations are - carried out . a disadvantage can be that the device will become longer in the direction of the flow and perhaps less compact . it is therefore a user decision which advantages are most important for a given process and from these considerations chose the appropriate bifurcation angles . this invention uses two or more offset fractals which independently scale fluids before they contact one another . the method of offset scaling can be different than in the figures . for example , the separate fractals can be contained within one another . ( fig1 and 13 ) a smaller conduit carrying one fluid can be placed inside a second larger conduit . a second fluid can therefore flow between the inner surface of the larger conduit and the outer surface of the smaller inner conduit . the two conduits can progressively be bifurcated to smaller and smaller scale until a desired exit size is reached . as with the above embodiments , the flows can be merged , in this case by simply ending the inner conduit so that the inner flow contacts the outer flow . the merged flows can also be collected and further merged into a single flow , if desired , as described earlier . note that we are defining “ offset ” to include smaller conduit inside of larger conduit since the flows are properly kept offset from one another by this optional method . this method of offsetting fractal conduits within one another can be extended to any number of separate fluids by adding a separate enclosed conduit for each fluid . we note that in the event of operation with fluctuating pressures between the independent flows or in the event that a particular flow is temporally shut off it can be useful to have check valves on channels to avoid backflow of one fluid through the distribution fractal of a different fluid . this invention can be applied over the entire range of fluid processing scales from very small scale applications to very large scale industrial use . the reason for this is that the fractal structures used in this invention provide a continuing scaling function as application scale changes . this wide range of applicability is one of the inherent advantages of this mixer design . because this device is used for mixing and / or reaction of fluids , the resulting products can be used as desired in subsequent processing equipment . it is noted that a particular manufacturing technique is not required to realize this invention . computer aided machining , stereolithography , photochemical etching , laser cutting , molding , micro - machining , nanotechnology , ion deposition and conduit construction techniques are a few appropriate methods for building these devices . it is recognized that future manufacturing techniques which may improve the ability to construct small scale structure will also be useful for construction of these devices . | 1 |
ordinarily a diode rectifier in a rectenna would not require different operating voltages for different frequencies . however , quantum rectification ( i . e ., photon - assisted tunneling ) that takes place for visible and near - infrared photons requires photon - energy - dependent ( or similarly wavelength - dependent ) operating voltages . in order to take advantage of the photon - energy - dependent voltage , the present invention passively or actively splits the solar spectrum into different spectral bands , each of which is absorbed by rectennas having an operating voltage that optimizes the power conversion efficiency for that band . as shown in fig1 , a radiation source ( e . g ., the sun , or any source of thermal radiation like a hot body ) provides radiation 10 ( visible / infrared ) that is split by a spectral splitting device 12 into previously defined spectral frequency bands 20 . the previously defined spectral frequency bands 20 are directed by the spectral splitting device 12 to rectennas 30 having customized operating voltages . the operating voltage is determined by selecting the resistance of the load for a given input power . the given input power is determined by the received spectral band . each rectenna 30 is designed to absorb radiation over a well defined spectral band corresponding to the operating voltage for that rectenna . in one embodiment as shown in fig2 , splitting of the spectrum 10 is accomplished optically , using a wavelength - selective device 40 . a prism or a grating will suitably spatially split the spectrum into spectral components . the wavelength - selective device 40 sends spectral bands 21 to a group of frequency - insensitive rectennas 31 located on a substrate 34 ( e . g ., printed circuit board ). the rectennas 31 are coplanar , with different spectral bands 21 being processed by spatially separated rectennas . in one embodiment , the antennas used in the rectennas 31 include broadband bowtie antennas . as shown in fig3 , a substrate 50 includes frequency - sensitive rectennas 52 that absorb only a predefined band of wavelengths . thus , the spectral splitting is done passively . the frequency - sensitive rectennas 52 include wavelength - selective dipole antennas 54 . the spectrum is incident on the surface of the substrate 50 . the frequency - sensitive rectennas 52 include a diode 51 and a load resistor 60 . the diodes 51 and the load resistor 60 are configured to operate at a particular operating voltage . an example diode 51 includes a metal insulator metal ( mim ) diode . because the dipole antennas 54 can absorb radiation over an area that is larger than their physical size , the dipole antennas 54 that are sensitive to different spectral bands are arrayed over the substrate surface 50 . different spectral portions of the total radiation ( incident over the large area ) are absorbed by the selective antennas occupying no more footprint than the area occupied by the incident radiation . as a result , spectral splitting is achieved by spatially separated rectennas on the same plane and does not require a grating . as shown in fig4 , a rectenna system 70 includes stacks of semi - permeable substrates 72 that include one or more frequency - sensitive rectenna 74 . each level of the stack of rectennas absorbs different frequency bands . thus , non - absorbed frequency bands penetrate to the next substrate layer 72 . the material chosen depends on the incident spectrum ( visible , nir , long wavelength ir ). examples include quartz , fused silica , transparent polymers / plastics , calcium fluoride and potassium bromide ir transparent substrates . in another embodiment , a single broadband antenna absorbs the entire spectrum of interest , or a substantial fraction of it . the electric current coming from the antenna is split into frequency bands , and each frequency band of current is directed to a separate diode whose operating voltage is tuned for that band . one way to accomplish the splitting is with the use of passive inductor - capacitor ( lc ) filters , as is conventionally used to filter ac signals . fig5 shows an exemplary rectenna circuit 90 . the rectenna circuit 90 includes an adjustable load resistor 92 , an antenna ( frequency sensitive or insensitive ) 98 , a diode 94 and a dc output filter 96 . the dc output filter 96 blocks ac power dissipation in the load resistor 92 . the adjustable load resistor 92 is adjusted to provide a desired voltage across the diode 94 . fig6 shows current - voltage [ i ( v )] characteristics for a rectenna diode ( such as the diode 94 ). the solid curve 100 is the i ( v ) for an exemplary rectenna in the dark ( i . e ., not exposed to the spectral source ), and the dashed curve 102 shows the i ( v ) under illumination from a specific spectral band . the voltage at which the dashed curve 102 crosses the voltage axis is equal to the photon energy divided by the electron charge . the location where the curve 102 crosses the v - axis indicates the maximum voltage that the rectenna can extract from the incident spectrum . beyond this voltage , the current is negative and the rectenna cannot generate any energy . for an ideal rectenna diode illuminated by a monochromatic source , the rectenna efficiency approaches 100 % when the bias voltage is equal to the photon energy divided by the electron charge . therefore , for a high - photon - energy slice ( band ) of the spectrum the dashed line 102 extends farther to the left on the voltage axis than for a low - photon - energy slice . a load - line 106 intersects the rectenna illuminated i ( v ) ( the dashed curve 102 ) at the operating voltage v o . rectenna output power is the area under the dashed curve 102 at the load - line 106 intersection . the slope of the load - line 106 and hence the operating voltage can be chosen for high rectenna efficiency by tuning the load impedance . the illuminated i ( v ) curve ( dashed curve in fig6 ) is a function of the power and the energies of the different photons in the incident spectral band . all the different spectral bands ( i . e ., frequencies ) can be absorbed using rectennas composed of the same materials . the spectral sensitivity is determined by the operating voltage , and can also be affected by the antenna design and size . this provides a great reduction in the cost of making a wide spectral band rectenna system . this is particularly advantageous over spectrum splitting in conventional solar cells , where different materials are required for each spectral region . for optimum efficiency , the diode i ( v ) characteristic has to be such that the diode impedance presented to a slice of the spectrum is matched to the antenna impedance . this results in maximum power transfer from the antenna to the diode . also , the diode must have a fast response time so that its rc time constant is less than the inverse of ( 2 times π times the maximum frequency in the incident band ). the present invention applies to solar radiation and to any broad optical or infrared spectrum ( e . g ., near , mid , and long - wave ir spectrum ). for example , power conversion from a hot object or source that produces blackbody radiation in the infrared would also benefit from the spectrum - splitting approach that is taught in detail herein . other examples and implementations are within the scope and spirit of the disclosure and appended claims . for example , features implementing functions can also be physically located at various positions , including being distributed such that portions of functions are implemented at different physical locations . also , as used herein , including in the claims , “ or ” as used in a list of items prefaced by “ at least one of ” indicates a disjunctive list such that , for example , a list of “ at least one of a , b , or c ” means a or b or c or ab or ac or bc or abc ( i . e ., a and b and c ). further , the term “ exemplary ” does not mean that the described example is preferred or better than other examples . various changes , substitutions , and alterations to the techniques described herein can be made without departing from the technology of the teachings as defined by the appended claims . moreover , the scope of the disclosure and claims is not limited to the particular aspects of the process , machine , manufacture , composition of matter , means , methods , and actions described above . processes , machines , manufacture , compositions of matter , means , methods , or actions , presently existing or later to be developed , that perform substantially the same function or achieve substantially the same result as the corresponding aspects described herein can be utilized . accordingly , the appended claims include within their scope such processes , machines , manufacture , compositions of matter , means , methods , or actions . | 6 |
the following description of the preferred embodiment ( s ) is merely exemplary in nature and is in no way intended to limit the invention , its application , or uses . some embodiments of the present invention provide a dissolvable film ( film 1 ) comprising a cellulose ether , a plasticizer , a non - ionic surfactant and a pigment , wherein the film is in the form of a particle . for the purposes of the invention , the term particle refers to smaller sizes or fragments of the film , e . g . the film is cut or ground into smaller sizes or fragments . various embodiments of the film include , but are not limited to : 1 . 1 . film 1 wherein the film comprises cellulose ethers , e . g ., selected from ( i ) alkylcellulose , e . g ., methylcellulose ; ( ii ) hydroxyalkyl cellulose , e . g ., selected from hydroxypropyl methyl cellulose , hydroxyethylpropyl cellulose , hydroxybutyl methyl cellulose , hydroxy propyl methyl cellulose , carboxymethyl cellulose and mixtures thereof ; and ( iii ) mixtures thereof ; 1 . 2 . any of the foregoing films comprising a starch , e . g . a pregelatinized starch ; 1 . 3 . any of the foregoing films comprising a plasticizer , e . g , a polyalcohol , e . g ., sorbitol , propylene glycol , glycerol , or low molecular weight polyethylene glycol , e . g ., peg 200 ; 1 . 4 . any of the foregoing films comprising propylene glycol , e . g ., in an amount effective to provide plasticity to the film , e . g ., about 20 - 30 % by dry weight of the film ; 1 . 5 . any of the foregoing films comprising a non - ionic surfactant or emulsifier , e . g ., a polysorbate , e . g ., polysorbate 80 ( also known as polyoxyethylene ( 20 ) sorbitan monooleate , available commercially e . g ., as tween ® 80 ), e . g ., in an amount of about 1 - 5 % by dry weight of the film ; 1 . 6 . any of the foregoing films comprising a pigment , which can include , but is not limited to pigment blue 15 [ 147 - 14 - 8 ], pigment blue 15 : 2 , pigment green 7 [ 1328 - 53 - 6 ], pigment orange 5 [ 3468 - 63 - 1 ], pigment red 4 [ 2814 - 77 - 9 ], pigment red 5 [ 6410 - 41 - 9 ], pigment red 48 : 4 [ 5280 - 66 - 0 ], pigment red 53 : 1 [ 5160 - 02 - 1 ], pigment red 57 [ 5858 - 81 - 1 ]. pigment red 57 : 1 [ 5281 - 04 - 9 ]; pigment red 57 : 2 barium lake [ 17852 - 98 - 1 ], pigment red 63 : 1 [ 6417 - 83 - 0 ], pigment red 64 : 1 [ 6371 - 76 - 2 ], pigment red 68 [ 5850 - 80 - 6 ], pigment red 83 , pigment red 90 : 1 aluminum lake [ 16508 - 80 - 8 ], pigment red 112 [ 6535 - 46 - 2 ], pigment red 172 aluminum lake [ 12227 - 78 - 0 ], pigment red 173 aluminum lake , pigment violet 19 [ 1047 - 16 - 1 ], pigment yellow 1 [ 2512 - 29 - 0 ], pigment yellow 3 [ 6486 - 23 - 3 ], pigment yellow 12 [ 6358 - 85 - 6 ], pigment yellow 13 [ 5102 - 83 - 0 ], pigment yellow 73 [ 13515 - 40 - 7 ] or a combination of any of these pigments . 1 . 7 . any of the foregoing films comprising which is substantially dissolved after a period of greater than 30 seconds and less than 180 seconds of brushing , scrubbing or agitation in the oral cavity or on the skin in the presence of water ; 1 . 8 . any of the foregoing films wherein the particle size is within a range selected from the group consisting of 10 - 100 mesh ( 0 . 0059 - 0 . 0787 inch ), 20 - 80 mesh ( 0 . 0070 - 0 . 0331 inch ); 25 - 60 mesh ( 0 . 0098 - 0 . 0278 inch ) and 30 - 50 mesh ( 0 . 0117 - 0 . 0234 inch )— note : 1 mil = 0 . 001 inch ; 1 . 9 . any of the foregoing films , wherein the pigment of the film particle is released upon dissolution of the film particle thereby changing the color of the toothpaste after brushing for a period of 30 - 180 seconds , e . g ., about 45 - 60 seconds in a toothpaste for use by a child or about 90 - 120 seconds in a toothpaste for use by an adult , thereby releasing the pigment and providing a color signal to the user of adequate brushing ; 1 . 10 . any of the foregoing films comprising , by dry weight of the film , 20 - 60 % cellulose ethers ; 10 - 30 % plasticizer ; 1 - 5 % non - ionic surfactant ; and 15 - 55 % pigment ; 1 . 11 . any of the foregoing films comprising , by dry weight of the film , 20 - 60 % cellulose ethers selected from methyl cellulose , hydroxypropylmethyl cellulose , and mixtures thereof ; 10 - 30 % propylene glycol ; 1 - 5 % polysorbate 80 ; and 15 - 55 % pigment ; 1 . 12 . any of the foregoing films wherein film further comprises an active is selected from flavors , fragrances , antibacterial agents , aesthetic agents or combinations thereof ; 1 . 13 . any of the foregoing films which are topically acceptable ; 1 . 14 . any of the foregoing films which are orally acceptable ; 1 . 15 . any of the foregoing films comprising an antibacterial agent ; in one embodiment of the invention , the antibacterial agent is selected from triclosan and essential oils from plant extracts , e . g ., menthol . the films of the invention are able to achieve sufficient release of the pigment in the oral cavity , but are surprisingly removed quickly when the film is disposed of onto a surface area and rinsed away . the invention also provides a product ( product 1 ) which comprises a dissolvable film ( film 1 ) comprising a cellulose ether , a plasticizer , a non - ionic surfactant and a pigment , wherein the film is in the form of a particle as described above . 1 . 16 . product 1 wherein the product is a an oral care product , an oral care product , e . g ., a dentifrice , for example a toothpaste , e . g ., a clear gel or opaque toothpaste , comprising film 1 described above ; 1 . 17 . product 1 of 1 . 16 wherein the product is a clear gel or opaque toothpaste and the pigment of the film particle is released upon dissolution of the film particle thereby changing the color of the toothpaste after brushing for a period of 30 - 180 seconds , e . g ., about 45 - 60 seconds in a toothpaste for use by a child or about 90 - 120 seconds in a toothpaste for use by an adult , thereby releasing the pigment and providing a color signal to the user of adequate brushing ; 1 . 18 . any of the foregoing products wherein the product further contains an active agent , which includes , but is not limited to a flavoring , an aesthetic , an antibacterial agent , an amino acid , a fluoride source , a whitening agent , a zinc compound and mixtures thereof . 1 . 19 . any of the foregoing products wherein the product is a hand or body soap ; 1 . 20 . any of the foregoing products wherein the product is a chewing gum ; 1 . 21 . any of the foregoing products which is a chewing gum wherein the different actives are different flavorings , such that the chewing gum changes flavor over time . 1 . 22 . any of the foregoing products wherein the product further comprises an anionic surfactant , which includes but is not limited to water - soluble salts of c 8 - 20 alkyl sulfates , sulfonated monoglycerides of c 8 - 20 fatty acids such as the sodium salt of the monsulfated monoglyceride of hydrogenated coconut oil fatty acids , sarcosinates , taurates and mixtures thereof . illustrative examples of these and other surfactants are higher alkyl sulfates such as sodium lauryl sulfate , sodium coconut monoglyceride sulfonate , sodium lauryl sarcosinate , sodium lauryl isoethionate , sodium laureth carboxylate , alkyl aryl sulfonates such as sodium dodecyl benzenesulfonate , higher alkyl sulfoacetates , sodium lauryl sulfoacetate , higher fatty acid esters of 1 , 2 - dihydroxy propane sulfonate , and the substantially saturated higher aliphatic acyl amides of lower aliphatic amino carboxylic acid compounds , such as those having 12 to 16 carbons in the fatty acid , alkyl or acyl radicals , amides are n - lauroyl sarcosine , and the sodium , potassium , and ethanolamine salts of n - lauroyl , n - myristoyl , or n - palmitoyl sarcosine , and the like and mixtures thereof . in one embodiment of the invention , the anionic surfactant is sodium lauryl sulfate ( sls ). 1 . 23 . any of the foregoing products wherein the amount of anionic surfactant is in a range selected from the group consisting of in an amount from 1 . 5 wt . % to 5 . 0 wt . %. and 1 . 5 wt . % to 2 . 0 wt . %. 1 . 24 . any of the foregoing products wherein the product further comprises an abrasive abrasives such as silica , calcined alumina , sodium bicarbonate , calcium carbonate , dicalcium phosphate and calcium pyrophosphate may be included in the base dentifrice compositions used in the practice of the present invention . other abrasives may also be suitable for use in the compositions described herein . visually clear dentifrice compositions may be obtained by using an abrasive such as collodial silica , e . g ., those sold under the trade designation zeodent ® available from the huber corporation or alkali metal aluminosilicate complexes ( that is , silica containing alumina combined in its matrix ) which have refractive indices close to the refractive indices of gelling agent - liquid ( including water and / or humectant ) systems used in dentifrice compositions . 1 . 25 . any of the foregoing products wherein the antibacterial agent includes , but is not limited to triclosan ( 5 - chloro - 2 -( 2 , 4 - dichlorophenoxy ) phenol ); 8 - hydroxyquinoline and salts thereof , zinc and stannous ion sources such as zinc citrate , zinc sulphate , zinc glycinate , sodium zinc citrate and stannous pyrophosphate ; copper ( ii ) compounds such as copper ( ii ) chloride , fluoride , sulfate and hydroxide ; phthalic acid and salts thereof such as magnesium monopotassium phthalate ; sanguinarine ; quaternary ammonium compounds , such as alkylpyridinium chlorides ( e . g ., cetylpyridinium chloride ( cpc ), combinations of cpc with zinc and / or enzymes , tetradecylpyridinium chloride , and n - tetradecyl - 4 - ethylpyridinium chloride ); bisguanides , such as chlorhexidine digluconate , hexetidine , octenidine , alexidine ; halogenated bisphenolic compounds , such as 2 , 2 ′ methylenebis -( 4 - chloro - 6 - bromophenol ); benzalkonium chloride ; salicylanilide , domiphen bromide ; iodine ; sulfonamides ; bisbiguanides ; phenolics ; piperidino derivatives such as delmopinol and octapinol ; magnolia extract ; grapeseed extract ; thymol ; eugenol ; menthol ; geraniol ; carvacrol ; citral ; eucalyptol ; catechol ; 4 - allylcatechol ; hexyl resorcinol ; methyl salicylate ; antibiotics such as augmentin , amoxicillin , tetracycline , doxycycline , minocycline , metronidazole , neomycin , kanamycin and clindamycin ; and mixtures thereof . 1 . 26 . any of the foregoing products wherein the product further comprises an amino acid ( unless otherwise specified , include free amine and salt forms ). in one embodiment of the invention , the amino acid is selected from the group consisting of arginine , cysteine , leucine , isoleucine , lysine , alanine , asparagine , aspartate , phenylalanine , glutamate , glutamic acid , threonine , glutamine , tryptophan , glycine , valine , praline , serine , tyrosine , and histidine , and a combination of two or more thereof . in another embodiment of the invention , the 1 . 27 . any of the foregoing products wherein the product further comprises a fluoride source . in one embodiment , the fluoride source selected from stannous fluoride , sodium fluoride , potassium fluoride , sodium monofluorophosphate , sodium fluorosilicate , ammonium fluorosilicate , amine fluoride , ammonium fluoride , and mixtures thereof . 1 . 28 . any of the foregoing products wherein the product further comprises a whitening agent . in one embodiment , the whitening agent is a peroxide ( which includes , but is not limited to hydrogen peroxide or urea peroxide ), peroxy acids , or a non - peroxide compound ( which includes , but is not limited to high cleaning silicas , chlorine dioxide , chlorites , hypochlorites and colorants ( such as titanium dioxide and hydroxyapatite )). 1 . 29 . any of the foregoing products wherein the product further comprises a zinc compound . in one embodiment , the zinc compound is selected from the group consisting of zinc acetate , zinc borate , zinc butyrate , zinc carbonate , zinc citrate , zinc formate , zinc gluconate , zinc glycerate , zinc glycolate , zinc lactate , zinc oxide , zinc phosphate , zinc picolinate , zinc proprionate , zinc salicylate , zinc silicate , zinc stearate , zinc tartrate , zinc undecylenate and mixtures thereof the invention provides , in another embodiment , a method of improving post - use disposal of an oral care composition containing a pigment to be released during use which comprises adding a film as described above during the process of making the oral care composition wherein post - use disposal of the oral care composition does not stain the surface of the disposal area . in another embodiment of the method , the process of making the oral care composition further comprises adding an anionic surfactant in an amount from 1 . 5 wt . % to 5 . 0 wt . %. and 1 . 5 wt . % to 2 . 0 wt . %. in another embodiment of this aspect of the invention , the anionic surfactant is sodium lauryl sulfate . in some embodiments , substantially all of the pigment is released at one time . as used herein , the term “ substantially all ” refers to greater than 90 % of the total amount of pigment contained in the film . in some embodiments , the first film releases at least 90 % of the total amount of pigment contained therein , at a particular point in time . in some embodiments , the first film releases greater than 90 % of the total amount of pigment contained therein , at a designated point in time . in some embodiments , the first film releases at least 91 % of the total amount of pigment contained therein , at the designated point in time . in some embodiments , the first film releases at least 95 % of the total amount of pigment contained therein , at the designated point in time . in some embodiments , the first film releases at least 96 % of the total amount of pigment contained therein , at the designated point in time . in some embodiments , the first film releases at least 97 % of the total amount of pigment contained therein , at the designated point in time . in some embodiments , the first film releases at least 98 % of the total amount of pigment contained therein , at the designated point in time . in some embodiments , the first film releases at least 99 % of the total amount of pigment contained therein , at the designated point in time . orally acceptable or topically acceptable : the compositions of the invention are intended for topical use in the mouth or on the skin , thus components for use in the present invention should be orally acceptable , that is , safe for topical use in the mouth , in the amounts and concentrations provided . as used throughout , ranges are used as shorthand for describing each and every value that is within the range . any value within the range can be selected as the terminus of the range . in addition , all references cited herein are hereby incorporated by referenced in their entireties . in the event of a conflict in a definition in the present disclosure and that of a cited reference , the present disclosure controls . unless otherwise specified , all percentages and amounts expressed herein and elsewhere in the specification should be understood to refer to percentages by weight . the amounts given are based on the active weight of the material . embodiments of the present invention are further described in the following examples . the examples are merely illustrative and do not in any way limit the scope of the invention as described and claimed . the films of the invention can be prepared as follows . approximately fifty percent of the required film formula water is weighed out and heated as necessary depending on the polymer type . polymers ( hpmc , mc , etc ) are slowly added to the water under mixing conditions and the polymers are allowed to disperse and hydrate for 10 - 15 minutes . additional water up to the full amount is added until the slurry has the consistency of honey . plasticizers and surfactants should then be added while mixing and allowed to mix for 5 minutes . other particles such as dyes , pigments , etc . should then be added to the mixture and allowed to mix for 10 additional minutes . the slurry should then be de - aerated . films can then be cast and dried from the slurry to the desired thickness typically 1 - 10 mils . these procedures resulted in 30 - 50 mesh film particles which comprised of : 10 - 50 g of liquid toothpaste from example 2 are placed into a scintillation vial . a sufficient quantity of film particles described in example 1 is added to the liquid toothpaste and visually evaluated ( typically 0 . 2 % or less ). the liquid toothpaste and film is shaken vigorously by hand for 15 seconds and placed on a benchtop . the initial distribution and quantity on bottom of vial is noted before starting the timer . the liquid toothpaste and film is visually inspected and the percentage of film deprecating over time is recorded . at completion , the contents of the scintillation vial is emptied into a sink . the scintillation vial is place under the tap and water is permitted to flow for 10 seconds from the tap . the scintillation vial is drained and and then inverted . the difference in the amount of film residue left behind is recorded . the amount of film settling was compared for a toothpaste of the invention which has a ground film particles of 30 - 50 mesh with a comparative toothpaste with film of 1 . 6 mm ( approx . 12 mesh ) thick squares ( toothpaste of pct / us2011 / 065308 ). as can be seen from the data in table 3 below , the amount of film setting after 10 minutes was drastically reduced . fig1 depicts a glass surface after 20 minutes of settling and subsequent rinsing . surface ( a ) was exposed to the toothpaste slurry with 1 . 6 mm square film whereas surface ( b ) was exposed to the toothpaste slurry with ground film 30 - 50 mesh . as can be seen from the figure , surface ( a ) shows significant staining compared to surface ( b ). while not wishing to be bound by theory , it is believed that the residual films which have smaller size film particles have increased buoyancy and are therefore easier to rinse away with water before residual staining is observed , i . e . the release of pigment from the discarded film particles onto a surface . the film particles described in example 1 were incorporated into a toothpaste composition with the formula described in table 4 below . one of the embodiments of the invention was the further addition of an anionic surfactant to the film particle composition . fig2 shows the effect of adding differing amounts of an anionic surfactant , e . g . sodium lauryl sulfate ( sls ), to the oral care composition described by example 5 . increasing the amount of sls to about 1 . 75 % resulted in significantly less residual staining by the pigment . as those skilled in the art will appreciate , numerous changes and modifications may be made to the embodiments described herein without departing from the spirit of the invention . it is intended that all such variations fall within the scope of the appended claims . | 0 |
the invention will be further illustrated in more detail with reference to accompanying drawings . it is noted that , the following embodiments are intended for purposes of illustration only and are not intended to limit the scope of the invention . the present invention provides a g method for improving glcnac production in engineered b . subtilis . specifically , the method comprises the steps of deletion of phosphoenolpyruvate carboxykinase encoding gene pcka , deletion of pyruvate kinase encoding gene pyk and overexpression of pyruvate carboxylase encoding gene pyca in a recombinant bacillus subtilis . in a preferable embodiment , the starting strain is bsgnk - pxyla - glms - p43 - gna1 ( bsgnk ), and the finally obtained strain with improved glcnac production and yield is bpts3 . deletion of phosphoenolpyruvate carboxykinase encoding gene pcka of the strain bsgnk to block the anaplerosis from pep to oxaloacetate , to obtain the recombinant strain bpts1 , wherein bsgnk is obtained by the method disclosed in china patent application ser . no . 201510394205 . 7 . deletion of phosphoenolpyruvate carboxykinase pcka was first performed to block the anaplerosis from pep to oxaloacetate . specifically , a primer pcka - f ( acggacttcacttaggcggc )/ pcka - r ( gacggatttttatatttgcgcg ) was used to amplify a pcka disrupt cassette , which included a pcka upstream homology sequence ( 1 kb ), a zeocin resistant gene expression cassette , and a pcka downstream homology sequence ( 1 kb ), from b . subtilis 168 . dna sequence of the pcka disrupt cassette is as shown in seq id no . 1 . the amplified pcka disrupt cassette was transformed into the strain bsgnk , and transformants were selected on lb plate with 30 μg / ml zeocin . positive transformants with pcka gene deletion were further verified by colony pcr with primers pcka - f / pcka - r . the vector ptsc was introduced into the positive transformants to promote the recombination between lox71 and lox66 , thereby deleting the resistance marker cassette . plasmid ptsc was then evicted by incubating at 50 ° c . for 12 h to obtain the strain without the selected marker and plasmid , naming bpts1 . deletion of pyruvate kinase encoding gene pyk in the strain bpts1 to block the synthesis from pep to pyruvate by glycolysis pathway . deletion of pyruvate kinase pyk was performed to block the synthesis from pep to pyruvate by glycolysis pathway . specifically , the primer pyk - f ( acgaataggggtattaacgagcg )/ pyk - r ( cagctaacagcaaagcaatcagc ) was used to amplify a pyk disrupt cassette , which included a pyk upstream homology sequence ( 1 kb ), a zeocin resistant gene expression cassette , and a pyk downstream homology sequence ( 1 kb ), from b . subtilis 168 . dna sequence of the pyk disrupt cassette is as shown in seq id no . 2 . the amplified pyk disrupt cassette was transformed into the strain bpts1 , and transformants were selected for on lb plate with 30 μg / ml zeocin . positive transformants with pyk gene deletion were further verified by colony pcr with primers pyk - f / pyk - r . the vector ptsc was introduced into the positive transformants to promote the recombination between lox71 and lox66 , thereby deleting the resistance marker cassette . plasmid ptsc was then evicted by incubating at 50 ° c . for 12 h to obtain the strain without the selected marker and plasmid , naming bpts2 . overexpression of pyruvate carboxylase encoding gene pyca of the strain bpts2 to facilitate cell growth . overexpression of pyruvate carboxylase encoding gene pyca was performed to facilitate cell growth . specifically , a primer pyca - f ( gcagagctggtttaaaatcgg )/ pyca - r ( cccaagttgaaagcttaacgaga ) was used to amplify a pyca overexpressed cassette , which included a pyca upstream homology sequence ( 1 kb ), a zeocin resistant gene expression cassette , a p43 strong promoter , a pyca sequence with replacing the start codon gtg with atg , from b . subtilis 168 . dna sequence of pyca overexpressed cassette is as shown in seq id no . 3 . the amplified pyca overexpressed cassette was transformed into the strain bpts2 , and transformants were selected on lb plate with 30 μg / ml zeocin . positive transformants with pyca gene overexpression were further verified by colony pcr with primers pyca - f / pyca - r . the vector ptsc was introduced into the positive transformants to promote the recombination between lox71 and lox66 , thereby deleting the resistance marker cassette . plasmid ptsc was then evicted by incubating at 50 ° c . for 12 h to obtain the strain without the selected marker and plasmid , naming bpts3 . the seed medium was luria - bertani broth or agar plates containing ( g / l ): tryptone 10 , yeast extract 5 , and nacl 10 . the fermentation medium contained ( g / l ): tryptone 6 , yeast extract 12 , ( nh 4 ) so 4 6 , k 2 hpo 4 . 3h 2 o 12 . 5 , kh 2 po 4 2 . 5 , mgso 4 . 7h2o 3 , caco 3 5 , glucose 60 , and 15 ml of trace metal solution . the trace metal solution contained ( per liter of 5m hcl ) ( g / l ): fsso 4 . 7h 2 o 4 . 0 , cacl 2 4 . 0 , mnso 4 . 5h 2 o 1 . 0 , cocl 2 . 6h 2 o 0 . 4 , namno 4 . 2h 2 o 0 . 2 , znso 4 . 7h 2 o 0 . 2 , alcl 3 . 6h 2 o 0 . 1 , cucl 2 . h2o 0 . 1 , and h 3 bo 4 0 . 05 . seed culture was carried out in 250 - ml shake flasks each containing 20 ml of seed medium with shaking at 200 rpm and 37 ° c . for 12 h . the seed culture ( 5 ml ) was inoculated into 500 - ml shake flasks containing 95 ml of fermentation medium . and then , fermentation was carried out at 220 rpm and 37 ° c . for 48 h on rotary shakers . when the optical density at 600 nm ( od600 ) reached 0 . 4 , xylose was added to the medium to a final concentration of 5 g / l to induce gene expression under the control of the xylose - inducible p xyla promoter . effects of deletion of phosphoenolpyruvate carboxykinase encoding gene pcka on cell growth and glcnac production to determine the effects of deletion of phosphoenolpyruvate carboxykinase encoding gene pcka on cell growth and glcnac production , the strain bpts1 and bsgnk were inoculated with an inoculum size of 5 % ( v / v ) into 500 - ml shake flasks each containing 95 ml of fermentation medium . and then , fermentation was carried out at 220 rpm and 37 ° c . for 48 h on rotary shakers . it can be seen from fig1 - 2 that the strain bpts1 produced glcnac to a higher concentration than bsgnk by 7 . 14 g / l in the flask cultivation , which was 1 . 16 - fold of that of bsgnk , and deletion of phosphoenolpyruvate carboxykinase encoding gene pcka had little influence on cell growth . the results indicate that deletion of phosphoenolpyruvate carboxykinase encoding gene pcka is benefit for the glcnac synthesis . effects of deletion of pyruvate kinase encoding gene pyk on cell growth and glcnac production to determine the effects of deletion of pyruvate kinase encoding gene pyk on cell growth and glcnac production , the strains bpts2 and bpts1 were inoculated with an inoculum size of 5 % ( v / v ) into 500 - ml shake flasks each containing 95 ml of fermentation medium . and then , fermentation was carried out at 220 rpm and 37 ° c . for 48 h on rotary shakers . it can be seen from fig2 that the strain bspt2 produced glcnac to a higher concentration than bpts1 by 8 . 5 g / l in the flask cultivation , which was 1 . 18 - fold of that of bpts1 . however , deletion of pyruvate kinase encoding gene pyk leaded to the low glucose consumption rate and decreased dcw . fig3 shows the time profile of glucose consumption of bsgnk , bpts1 , bpts2 , bpts3 in shake flask . the residual glucose concentration of bpts2 was 12 . 2 g / l . this was thought to be the non - optimal tca flux and reduced glycolytic flux . overexpression of pyruvate carboxylase encoding gene pyca to facilitate cell growth it is possible that the overexpression of pyca can lead more pyruvate to synthesize oaa and facilitates the glutamine synthesis . finally , we tested the effects of overexpression of pyruvate carboxylase to cell growth and glcnac production . it can be seen from fig1 - 2 that the overexpression of pyca can facilitate cell growth , and the glucose consumption rate of bpts3 was improved than that of bpts2 . finally , the glcnac production of bpts3 reached 11 . 3 g / l , which was 32 . 8 % higher than that of bpts2 and 1 . 84 - fold of that of bsgnk . fig1 - 3 show the effects of deletion of phosphoenolpyruvate carboxykinase encoding gene pcka and pyruvate kinase encoding gene pyk and overexpression of pyruvate carboxylase encoding gene pyca on cell growth , glcnac production and glucose consumption . table 1 shows the comparison of the maximum glcnac titer , the maximum dcw and the glcnac productivity of bsgnk , bpts1 , bpts2 , bpts3 in shake flask fermentation system . the above preferred embodiments are described for illustration only , and are not intended to limit the scope of the invention . it should be understood , for a person skilled in the art , that various improvements or variations can be made therein without departing from the spirit and scope of the invention , and these improvements or variations should be covered within the protecting scope of the invention . | 2 |
a method of stacking a flexible substrate and a method of fabricating a flexible display according to the present invention will now be described more fully hereinafter with reference to the accompanying drawings , in which exemplary embodiments of the present invention are shown . fig1 a to 1d are cross - sectional views illustrating a method of stacking a flexible substrate according to an exemplary embodiment of the present invention . referring to fig1 a , a carrier substrate 110 is prepared . the carrier substrate 110 may be formed of various kinds of materials , for example , glass , silicon , etc . referring to fig1 b , an adhesive layer 120 is stacked on the carrier substrate 110 . the adhesive layer 120 is composed of a support 121 and bonding materials 122 and 123 respectively formed on and under the support 121 . the support 121 may be formed of polyethylene terephthalate , polybutylenes terephthalate , polyimide , polyester , or polyolefine . as illustrated in fig1 b , the adhesive layer 120 is disposed by a laminator method using rollers 140 a and 140 b . rollers rolling in the same direction are prepared under the carrier substrate 110 and over the adhesive layer 120 , and upper and lower rollers 140 a and 140 b formed over and under the carrier substrate 110 roll over and under the carrier substrate 110 so as to dispose the adhesive layer 120 thereon . in the next step , as illustrated in fig1 c , a flexible substrate 130 on which an image display device will be formed is stacked on the adhesive layer 120 using the roller 140 a . the flexible substrate 130 may be a metal thin film ( stainless foil and aluminum thin film ), a thin glass substrate ( e . g ., thinner than 0 . 3 mm ) or a plastic substrate . to stack the flexible substrate 130 , the upper roller 140 a is prepared on the flexible substrate 130 , and the lower support 150 is prepared under the carrier substrate 110 . by such a structure , the lower support 150 fixes and supports the carrier substrate 110 , and the upper roller 140 a rolls on the flexible substrate 130 so as to stack the flexible substrate 130 . meanwhile , the rollers 140 a and 140 b illustrated in fig1 b and 1c are composed of a roller main body 142 and a protective body 141 surrounding the roller main body 142 and formed of rubber or soft fabric . to minimize damage to the stacked structures ( e . g ., the adhesive layer , the flexible substrate , the carrier substrate , etc . ), the protective body 141 surrounds or coats the roller main body 142 . the lower support 150 formed under the carrier substrate 110 is composed of a support main body 152 and a support protective body 151 . like the protective body 141 , the support protective body 151 is also formed of rubber or soft fabric . referring to fig1 b and 1c , in fig1 b , the rollers 140 a and 140 b are disposed on and under the adhesive layer 120 and a different number of rollers are disposed thereon , respectively . in fig1 c , the upper roller 140 a is disposed over the flexible substrate 130 , and the lower support 150 is disposed under the carrier substrate 110 . that is , to stack the adhesive layer 120 and the flexible substrate 130 , without regard to the number of the rollers 140 a and 140 b , a support supporting the carrier substrate may be used instead of the roller . when using the rollers , one to five rollers may be used over and under the carrier substrate , respectively . a gap between the rollers may be controlled to ensure close adhesion between the carrier substrate 110 and the adhesive layer 120 , and between the adhesive layer 120 and the flexible substrate 130 . here , the gap between the rollers 140 a and 140 b may be controlled mechanically and by air pressure . when the gap between the rollers is controlled by air pressure , the air pressure may depend on the size and use of the adhesive layer 120 or the flexible substrate 130 , but preferably be 0 . 1 to 10 kg / cm 2 . also , a preferable temperature of the rollers 140 a and 140 b is in the range of 0 to 160 ° c . to enhance the close adhesion between the carrier substrate 110 and the adhesive layer 120 . in the embodiments described above , the adhesive layer 120 utilizes the upper and lower rollers 140 a and 140 b , and the flexible substrate 130 utilizes the upper roller 140 a and the lower support 150 , but these may be freely changed . fig1 d illustrates a stacking structure of a flexible substrate fabricated by the stacking method of the flexible substrate shown in fig1 a to 1c . as illustrated in fig1 d , the stacking structure of the flexible substrate is composed of the carrier substrate 110 , the adhesive layer 120 and the flexible substrate 130 . fig2 a to 2c are cross - sectional views schematically illustrating a method of stacking a flexible substrate according to another exemplary embodiment of the present invention . referring to fig2 a to 2c , a carrier substrate 110 is prepared , and an adhesive layer 120 is stacked on the carrier substrate 110 . the adhesive layer 120 is stacked using a presser p , and the presser p is composed of an upper presser 240 disposed over the adhesive layer 120 , and a lower presser 250 or a fixed presser 260 . the upper and lower pressers 240 and 250 and the fixed presser 260 are composed of presser main bodies 242 , 252 and 262 , and protective bodies 241 , 251 and 261 corresponding to the adhesive layer 120 formed under the presser main bodies 242 , 252 and 262 and protecting structures which will be stacked later . the protective bodies 241 , 251 and 261 are made of rubber or soft fabric , and coated or stacked on the presser main bodies 242 , 252 and 262 , respectively . referring to fig2 b , the upper and lower pressers 240 and 250 move vertically and press the structures . and , referring to fig2 c , the upper presser 240 which can move vertically and the fixed presser 260 press the structures . the presser p may operate at a temperature ranging from 0 to 160 ° c ., and be controlled mechanically or by air pressure for close adhesion to the adhesive layer 120 or the flexible substrate 130 . when the presser p is controlled by air pressure , the air pressure may be in a range of 0 . 1 to 100 kg / cm 2 . when the presser is controlled mechanically , pressure may be controlled by a screw , etc . also , the presser p may ensure the close adhesion of the adhesive layer 120 by operating under atmospheric pressure , inert atmosphere or vacuum . then , a flexible substrate 130 is stacked on the adhesive layer 120 using the presser p as described above . in the above - described embodiment , the adhesive layer 120 utilizes the upper and lower pressers 240 and 250 which can move vertically , and the flexible substrate 130 utilizes the upper presser 240 which can move vertically , and the fixed presser 260 disposed under the substrate . however , the present invention may not be limited to the embodiment , and freely make other choices . fig3 a to 3c are cross - sectional views schematically illustrating a method of fabricating a display having a flexible substrate using a method of stacking the flexible substrate according to the present invention . in the exemplary embodiment , first , a carrier substrate 110 , an adhesive layer 120 , and a flexible substrate 130 are sequentially stacked . when the flexible substrate 130 is stacked on the carrier substrate 110 , an image display device including a light - emitting device 330 and a transistor 310 , i . e . a driving device is formed on the flexible substrate 130 . to form the light - emitting device 330 and the transistor 310 , a buffer layer 301 and a semiconductor layer 315 are sequentially formed on the flexible substrate 130 , and a gate insulating layer 302 , a gate electrode 311 , an interlayer insulating layer 303 , source and drain electrodes 312 and a passivation layer 304 are formed on the semiconductor layer 315 . then , the light - emitting device 330 electrically connected to the transistor 310 through a contact hole ( not illustrated ) formed in the passivation layer is formed on the transistor 310 including the gate electrode 311 and the source and drain electrodes 312 . the light - emitting device 330 includes an anode 331 , an emission layer 333 and a cathode 335 . a pixel defining layer 305 is formed on the anode 331 of the light - emitting device 330 and the passivation layer 304 . as described above , when a display having the image display device including the light - emitting device 330 and the transistor 310 is formed on the flexible substrate 130 , the carrier substrate 110 disposed under the flexible substrate 130 is removed . here , the adhesive layer 120 may be removed with the carrier substrate 110 . in this case , the carrier substrate 110 may be removed by heat or pressure . consequently , an adhesive layer for a flexible display can offset stress generated by a difference in coefficients of thermal expansion between a flexible substrate and a carrier substrate in a process of forming an image display device on a flexible substrate such as a plastic substrate , thereby effectively reducing bending of the flexible substrate . also , a method of stacking a flexible substrate using a laminator or presser with rollers enables mass - production of flexible displays using flexible substrates without an additional investment in manufacturing equipment , because a conventional manufacturing line for semiconductors and displays can be applied to the present invention without equipment modification . while the present invention has been shown and described with reference to certain exemplary embodiments thereof , it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the appended claims . | 8 |
the club cleaner is sized such that it can be easily carried in one hand . in particular , the portable golf club cleaner provides an efficient cleaning device that can be attached to a golf bag , pull cart , an electric golf cart , or similar golfing equipment . it will also be cherished , because the portable golf club cleaner is electrically powered ; therefore , the golfer is not required to exert himself operating it during a given round of play . the club cleaner module ( 1 ) all references to the following figures ! is the encompassing unit for the inner housing ( 18 ), which is comprised of the micro - motor ( 19 ), the cylinders ( 8 ) lined with positioned bristles ( 10 ), and area for club insertion ( 15 ). the module ( 1 ) facilitates operation via triggering the power button ( 3 ) which is located on the contour molding ( 5 ) at the brim of respective golfer &# 39 ; s index finger . upon depression of the on / off button ( 3 ) an electrical impulse is sent to the micro - motor ( 19 ). the micro - motor ( 19 ) is powered by rechargeable batteries ( 22 ) through the use of multiple battery tabs ( 23 ) and tab connectors ( 24 ). the micro - motor ( 19 ) houses a power shaft ( 13 ) which initiates the operation of the struts ( 9 ). the struts ( 9 ) provide the rotation through multiple gears ( 12 ) to the three sets of three cylinders ( 8 ). the cylinders ( 8 ) are covered with specialized bristles ( 10 ) which rotate in simultaneous fashion creating a large cleaning area which can negotiate the entire club head ( 6 ) and respective club head grooves ( 7 ). the actual operation or use of the club cleaner module is as follows . a golfer will hold the module ( 1 ) with the bottom facing the ground and the insertion hole ( 15 ) pointing to the left . ( depiction for right hand golfers , all of the following will be performed in reverse for left handed golfers ) this leaves the exit hole to the right of the little finger and pointing to the right . the golfer &# 39 ; s hand grips the module on the top , and sides , of the module utilizing the contour molding ( 5 ) as a reference . the golfer will place his / her index finger within the contour molding with the tip of the index finger on the on / off button ( 3 ). the golfer will then grip his / her club by the end of the club so that the club head affixed on the shaft is positioned inward from the left hand . the golfer will then insert the entire club head ( 6 ) into the insertion area ( 15 ), between the opening flaps , and into the cleaning area . the golfer will hold the club face up , the module down and depress the operation button . fig1 -- the module ( 1 ) is shown in the standard side view depicting the core external components . these components are the contour molding ( 5 ), which allows the golfer to grip the module , the front opening ( 2 ), and exit hole ( 4 ). the module is comprised of an upper and lower molding which can be constructed of either plastic , wood , or equivalent material . this molding houses the functional components detailed in fig3 , 6 , 7 , 8 . fig2 -- this top view is the operation view . by placing your right hand , thumb pointing toward your body , and hand reaching out in front of the body , is how the contour molding ( 15 ) allows easy gripping of the module ( 1 ). your left hand grips the bottom of the club shaft with the toe and club head pointing to the right , parallel with the club cleaner module . this is the standard operating position . once held , the golfer inserts the club head ( 6 ) straight into the module ( 1 ) through the front opening ( 2 ) into the insertion area . once inserted , the golfer will depress the on / off button ( 3 ) which begins the cleaning process . the debris on the club head ( 6 ) and related club head grooves ( 7 ) will be channeled through the module ( 1 ) out through the exit hole ( 4 ). this process completes the cleaning within a few seconds . fig3 -- this cross - sectional view of the module ( 1 ) details the cylinders ( 8 ) configuration . in greater detail , there are three horizontal upper cylinders ( 8 ) connected by struts ( 9 ) and rotated by the gearing configurations ( 12 ). these three upper horizontal cylinders ( 8 ) are mounted to the inner housing of the module ( 1 ) and are held together by six supports ( 11 ). also depicted are the six vertical cylinders ( 8 ) which line the two sides of the module ( 1 ). all of these cylinders ( 8 ) are lined with cleaning bristles ( 10 ) which , when in operation , rotate in simultaneous fashion further detailed in fig6 . the gearing of these components is detailed in fig7 . the configuration gives the cleaning area 180 degrees of accessibility to the club head , detailed as the insertion area ( 15 ). the composition and make of the cylinders can be various with positioned bristles being stiff in nature but not abrasive enough to scratch club head alloys . the power shaft ( 13 ) is extended from the micro - motor ( 19 ) and is powered by two nickel cadmium rechargeable batteries ( 22 ), via battery tabs ( 23 ) and tab connectors ( 24 ) which is all positioned efficiently beside the micro - motor ( 19 ). fig4 -- this frontal view shows the front opening ( 2 ) of the module ( 1 ), and details the process in which the golfer inserts the dirty club head through the flaps ( 16 ) via the flap slit ( 17 ). the rotating cylinders ( 8 ) and the insertion area ( 15 ) define a front opening ( 2 ) which receives the golf club head to be brushed . this allows the cylinder bristles ( 10 ) to access and clean the club head grooves in 180 - degree fashion . the bottom figure details the same view with a cross - sectional outlook of the module ( 1 ), whose housing ( 18 ) houses the cylinders ( 8 ) and bristles ( 10 ) surrounding the insertion area ( 15 ). one can also see the area of cleanability ( 38 ) the cylinder configurations create . this view also details the removable bottom ( 25 ) so the golfer may clean larger driving clubs as well . fig5 -- this figure splits the module ( 1 ) depicted in operational view in the center of the three figures , by butterflying the top and bottom at the center of the module ( 1 ). the top figure details the cylinder configuration of the three upper horizontal brushes ( 8 & amp ; 10 ). the bottom half depicts the two sets of vertical cylinders ( 8 ) lined with bristles ( 10 ) and powered struts ( 9 ) on either side of the module housing ( 18 ). this bottom figure also details the rotation ( 26 ) of the cylinders ( 8 ) and their creation of the debris flowpath ( 27 ) which flows from the entry hole ( 2 ) through the cleaning area ( 38 ) and out through the exit hole ( 4 ). fig6 -- this figure details the club cleaner module with the side cover removed , revealing the housing ( 18 ) which supports the operational components . the compartment has a front wall , sidewalls and a section facilitating the micro - motor ( 19 ). the sidewalls support each end of the cylinders ( 8 ). the micro - motor ( 19 ) is affixed to the rear of the module ( 1 ) and is mounted by a water tight adhesive or other water resistant sealer . the powershaft ( 13 ) connects the micro - motor ( 19 ) to the cylinders ( 8 ). the cylinders ( 8 ) have a respective strut ( 9 ) facilitating the rotation motion so that the bristles ( 10 ) affixed to the cylinders ( 8 ) may perform the cleaning operation . in a manner known to those skilled in the art , the cylinders are contained within the module ( 1 ) housing ( 18 ). in detail , the cylinders have cylindrical housing ( 18 ) supports ( 11 ) which are mounted on cylindrical housing struts ( 9 ). those skilled in the art will appreciate that the cylindrical housing strut ( 9 ) is secured at both ends to the module ( 1 ) housing ( 18 ). this diagram also simulates the debris flowpath ( 27 ) from the club head ( 6 ) and related club head grooves ( 7 ) through the module ( 1 ) and out the exit hole . this flow path ( 27 ) is channel - like in nature . this channel is formed from the rotation of the nine respective cylinders ( 8 ). six cylinders ( 8 ) rotate from the outside to inside as caused by the rotation generated by the gearing configuration detailed in fig7 and depicted earlier in fig5 . the flowpath ( 27 ) is further enhanced by the rotation motion ( 26 ) from the three horizontally mounted cylinders ( 8 ) which are held up by six supports ( 11 ). these upper cylinders ( 8 ) rotated from top to bottom and from front to back ( 26 ). this figure also details the button ( 36 ) and the hinge ( 37 ) which allow the removable bottom ( 25 ) to be opened , thus allowing the golfer to clean his / her drivers . fig7 -- this figure details a top view of the operational components only . power is delivered within the housing ( 18 ) to the micro - motor ( 19 ) from the nickel cadmium batteries ( 22 ) through the use of positive and negative battery tabs ( 23 ) and tab connectors ( 24 ). the micro - motor ( 19 ) rotates the power shaft ( 13 ) through the clutch ( 14 ) to the gearing configurations ( 12 ). the upper horizontal bristles ( 10 ) are rotated through the use of the respective worm wheels and the related horizontal struts ( 9 ) which the cylinders ( 8 ) are attached to . this figure summarizes that all nine cylinders ( 8 ) are rotated by one power shaft ( 13 ) through the use of the gearing configuration ( 12 ). fig8 details how power is transferred to the vertical cylinders . briefly , the left verticals are linked directly to the power shaft ( 13 ) through the use of worm gears , while the right set receives power through the horizontal struts ( 9 ) via miter gears ( 20 ) which is further portrayed in fig8 . the figure also details the insertion area ( 15 ) for reference purposes for operation . fig8 -- this figure details a frontal view of only the housing ( 18 ) and gearing operational components as detailed from the top view in fig7 . this figure depicts how rotational power is given to the vertical cylinders ( 8 ). the power shaft detailed in fig7 drives the gears ( 12 ), worm wheels ( 21 ), and worm gears ( 39 ), which in turn power the respective struts ( 9 ). the left set of vertical cylinders ( 8 ) are powered solely through the worm gears ( 39 ). the right set of vertical cylinders ( 8 ) are powered through the horizontal strut ( 9 ) which is anchored to the housing ( 18 ) by supports ( 11 ) and end with three miter gears ( 20 ) one for each strut ! which rotate the respective right struts ( 9 ). this figure also details the cylinders ( 8 ) lined with bristles ( 10 ) as well as where the insertion area ( 15 ) is . this figure further details , from a new angle , the removable bottom ( 25 ) for direct access to bristles . fig9 -- another aspect of the present invention is that the power supply is a rechargeable set of nickel cadmium batteries . this diagram details how the batteries , in aforementioned figures , would receive charge through the utilization of the wall module ( 28 ). the module &# 39 ; s ( 1 ) housing has positive and negative battery tabs whose operation is outlined below . the wall module ( 28 ) is plugged into any standard ac unit ( 32 ). the back of the module ( 1 ) has a module charge adapter ( 33 ) with twin access channels ( 34 ) allowing the tab connector plate ( 35 ) and associated charge tabs - module to be connected to the wall module ( 29 ) recharge area . the wall module ( 28 ) has contour molding ( 29 ) which allows the module ( 1 ) to be affixed for recharging . the charge tabs ( 35 ) on the module ( 1 ) slide into the access channel - adapter ( 30 ) allowing the connection to the charge tabs - adapter ( 31 ) which initiates the recharging process . thus , it can be seen that the objects of the club cleaner invention have been satisfied by the module described in the aforementioned figures and descriptions . it should be apparent to those skilled in the art that the components of the present invention can be operated with an electrical power supply and will easily remove debris from any existing golf club efficiently and with effective results . the invention here - in creates a cleaning field of 180 degrees through multiple positioned brushes . these brushes cylindrical rotational force , create a channeling of coverage area , larger than a golf club head , for which debris is forced off the club head and out through the exit hole . | 0 |
the exemplary illustrations provided herein are generally based on techno - physical realization that frictional effects within the interior of a spray jet generate a negative pressure which contributes to a concentration of the spray jet so that the spray jet is stable over relatively great distances . in addition , the friction on the outer lateral surface of the spray jet is generally too small to create any substantial widening of the spray jet . as a result , the spray jet discharged by the rotary atomizer can have a great spatial length while keeping up the inner flow velocity , so that particles of the coating agent applied can still cause soiling at a great distance from the rotary atomizer . the present disclosure therefore includes the general technical teaching of generating turbulences within the shaping air jet in a targeted manner and thus in the spray jet as well , in order to limit the undisturbed range of the spray jet , and thus the spatial soiling potential , to a predetermined distance . it should be taken in to consideration here that turbulences in the spray jet are on principle undesirable , and , within the context of the exemplary illustrations , should therefore be restricted to a remote region . in a close region , e . g ., within the predetermined distance described above , the spray jet and the surrounding shaping air jet respectively should , however , preferably be of low turbulence and directed so that the coating quality is not affected by turbulences . an exemplary spray jet therefore has a substantially greater degree of turbulence in the remote region than it does in the close region . to generate the turbulences in the shaping air jet , the exemplary illustrations provide for additional irregularities in comparison to a conventional shaping air ring with a rotationally symmetrical arrangement of shaping air nozzles , which irregularities retain the original shaping function of the spray jet on the one hand , but , through a targeted variation of flow velocity and / or direction of flow , also disturb the laminarity or homogeneity in the shaping air jet to the extent that turbulences are generated in the remote region , which destroy flow energy , reduce flow velocity and widen the shaping air jet and thus also the spray jet . in addition , effects thus actively induced or generated in the lateral surface of the flow cylinder enable inflow of ambient air into the inner negative - pressure region of the spray jet , thereby reducing the above - mentioned concentrating forces subsequently . in one example , the shaping air jet has a length of decay from the shaping air ring to the turbulent remote region that is shorter than 1 m , 75 cm , 50 cm , 40 cm , 30 cm or 20 cm . the spatial soiling potential of the atomizer is thereby limited to the close region of the atomizer , i . e ., within the predetermined distance of 1 m , 75 cm , 50 cm , 40 cm , 30 cm or 20 cm , so that soiling of distant surfaces beyond the predetermined distance is prevented . in addition , the length of decay of the shaping air jet is preferably greater than the component distance between the shaping air ring and the component to be coated , so that the component to be coated is located within the directed and low turbulence close region of the spray jet . this is advantageous as the component to be coated is then located within the close region so that the quality of coating is not affected by the relatively strong turbulences in the remote region . in an exemplary shaping air ring , the irregularities for generating the turbulences include shaping air nozzles that are arranged asymmetrically with respect to the spray axis or the axis of rotation of the atomizer , i . e . are not rotationally symmetrical . for example , the nozzle cross - section and / or the jet direction of the individual shaping air jets can be varied along the circumference of the shaping air ring for generating the turbulences . in varying the flow velocity along the circumference of the shaping air ring , faster and slower flows are then flowing next to one another within the shaping air jet , which leads to velocity gradients , and thus flow friction within the spray jet , whereby turbulences are then generated in the course of the spray jet . in one exemplary illustration with shaping air nozzles in a ring - shaped arrangement , a part of the shaping air nozzles have a jet direction that is substantially aligned parallel to the spray axis of the atomizer , while another part of the shaping air nozzles have a jet direction that , compared to the spray axis , are inclined radially inward . for instance , the shaping air ring can have six groups of five shaping air nozzles each , three groups having shaping air nozzles that are substantially aligned parallel to the spray axis , while the other three groups comprise shaping air nozzles that have a spray direction which , compared to the spray axis , is inclined radially inward . in another example of a shaping air ring with a ring - shaped arrangement of the shaping air nozzles , a part of the shaping air nozzles have a jet direction that is inclined radially inward compared to the spray axis of the atomizer , while another part of the shaping air nozzles has a jet direction that , compared to the spray axis , is inclined radially outward . thus , the individual shaping air nozzles are inclined either radially inward or radially outward . preferably , the individual shaping air nozzles are also subdivided into groups with a uniform jet direction here , wherein the different groups of shaping air nozzles are arranged alternately in a circumferential direction . another exemplary shaping air ring with a ring - shaped arrangement of the shaping air nozzles may include a portion of the shaping air nozzles arranged along an inner ring , while another portion of the shaping air nozzles is arranged on an outer ring . here , the shaping air nozzles on the inner ring may have a jet direction that is inclined radially outward compared to the spray axis , while the shaping air nozzles on the outer ring preferably have a jet direction that is inclined radially inward compared to the spray axis . here also , the shaping air nozzles may be arranged in groups with a uniform jet direction , the different groups being arranged alternately in a circumferential direction . by contrast , in another exemplary illustration , the shaping air jet has the form of a planar jet . for this purpose , two groups of shaping air nozzles placed opposite one another each have a jet direction that is inclined radially inward compared to the spray axis , while two other groups of shaping air nozzles , also placed opposite one another , have a jet direction that is aligned substantially parallel to the spray axis or is inclined radially outward compared to the spray axis . thus , the shaping air nozzles inclining radially inward compress the resulting shaping air jet together into a planar jet . in a further exemplary illustration of a shaping air ring with a ring - shaped arrangement of the shaping air nozzles , the individual shaping air nozzles have a jet direction that is inclined radially inward compared to the spray axis , which leads to a crossing shaping air flow and causes a constriction of the spray jet downstream behind the bell cup . behind the constriction , however , the shaping air jet or the spray jet have in this example a widening with the soil - producing range of the spray jet being reduced . in the examples described above , the irregularities for generating the turbulences substantially consist of variations in the jet direction of the shaping air nozzles . the irregularities for generating the desired turbulences can , however , also consist of variations in the nozzle cross - sections of the individual shaping air nozzles , which lead to corresponding variations in flow velocity . in a ring - shaped arrangement of the shaping air nozzles , for example , the nozzle cross - section can be varied along the circumference of the shaping air ring and the shaping air nozzles can again be divided into different groups with uniform cross - sections . in addition , the irregularities for generating the turbulences can consist in that the nozzle cross - section of the shaping air nozzles is conically widened or tapered in the direction of flow . furthermore , it is possible to alter the nozzle cross - section in the direction of flow with one or more steps , with a tapering or widening of the nozzle cross - section being possible again . beyond that , within the context of the present disclosure , there is the possibility that the irregularities for generating turbulences consist of slits that are adjacent to the shaping air nozzles and substantially run parallel to the direction of flow . in a ring - shaped arrangement of the individual shaping air nozzles , the slit can likewise be arranged in a ring shape along the shaping air nozzle ring and intersecting all of the shaping air nozzles . alternatively , there is also the possibility to arrange the slits in a cross shape and concentrically with the individual shaping air nozzles . furthermore , the irregularities for generating turbulences can consist in the flow profile of the shaping air nozzles being distorted in a targeted manner . within the context of the exemplary illustrations , the nozzle mouth of an individual shaping air nozzle can be inclined in opposition to the preceding shaping air bore . in addition , the irregularities for generating turbulences can also be formed by notches into each of which one or more ( for example , 2 or 3 ) shaping air bores open , wherein the notches are preferably triangular in cross - section and form the shaping air nozzles . it should furthermore be mentioned that the exemplary illustrations encompass not only the shaping air ring according as described above , but also an atomizer with such a shaping air ring as well as a coating machine , in particular a painting robot with such a rotary atomizer . finally , the present disclosure and exemplary illustrations also encompass a corresponding coating process , which arises from the above description . the side - view in fig1 shows in highly simplified form a rotary atomizer 1 with a shaping air ring 2 and a bell cup 3 which in operation rotates on a rotational axis 4 and discharges a spray jet 5 in a conventional manner . the shaping air ring 2 has on its front side numerous shaping air nozzles , which are arranged in a ring shape and direct a shaping air jet 6 from behind onto the lateral surface of the bell cup 3 so that the spray jet 5 has a constriction behind the bell cup 3 and subsequently widens in jet direction . using the arrangement of the shaping air nozzles according to the exemplary illustrations in the fig2 to 6 , the spray jet 5 is subdivided into a low turbulence directed close region and a turbulent remote region , the spray jet 5 falling apart after a predetermined distance , e . g ., decay length l decay , at the transition from the close region to the remote region . here , the rotary atomizer 1 is guided such that the component to be coated 7 is located within the directed close region , such that the coating of the component 7 is not disturbed by turbulences . in the turbulent remote region , however , turbulences 8 are generated that destroy the flow energy of the spray jet 5 and reduce its velocity , thus contributing to a widening of the spray jet 5 . in addition , defects are generated in the lateral surface of the spray jet 5 , which enable the inflow 9 of ambient air into the inner negative - pressure region of the spray jet 5 , so that the concentrating forces of the spray jet 5 are reduced . here , the turbulences 8 are generated in a targeted manner with the shaping air nozzles in the shaping air ring 2 having irregularities compared to a rotationally symmetric arrangement , for instance variations in jet direction and / or nozzle cross - section . fig2 shows a simplified perspective view of a modification of the shaping air ring 2 from fig1 , this modification being largely in accordance with the example shown in fig1 , such that , for avoiding repetitions , reference is made to the above description and the same reference numerals are subsequently used for corresponding details . one distinctive feature of this exemplary illustration consists in that different shaping air nozzles 10 , 11 are distributed along the circumference of the shaping air ring 2 , wherein the shaping air nozzles 11 have a smaller nozzle cross - section than the shaping air nozzles 10 , which leads to correspondingly different flow velocities . here , the shaping air nozzles 10 or 11 , respectively , are subdivided into six groups of five shaping air nozzles 10 and 11 , respectively , each , wherein the shaping air nozzles 10 and 11 , respectively , within the individual groups each have a uniform nozzle cross - section . along the circumference of the shaping air ring 2 , therefore , slower and faster shaping air flows emerge next to one another , so that the flow friction resulting from this velocity difference generates turbulences in the further course of the shaping air jet . the exemplary illustration according to fig3 largely corresponds to that mentioned above and illustrated in fig2 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are subsequently used for corresponding details . one distinctive feature of this example consists in that the shaping air nozzles 10 , 11 do not differ by the nozzle cross - section , but rather by the jet direction . the shaping air nozzles 10 thus have a jet direction that is substantially aligned parallel to the rotational axis 4 of the bell cup 3 . the shaping air nozzles 11 , however , have a jet direction that is inclined radially inward compared to the rotational axis 4 , the angle of inclination being preferably in a region between 5 ° and 30 °. fig4 shows a further exemplary illustration of the shaping air ring 2 that largely corresponds to the example described above and illustrated in fig2 , such that , for avoiding repetitions , reference is made to the above description and the same reference numerals are subsequently used for corresponding details . one distinctive feature of this example consists in that the shaping air nozzles 10 have a jet direction that is directed radially outward compared to the rotational axis 4 of the bell cup 3 , whereas the shaping air nozzles 11 have a jet direction that is directed radially inward compared to the rotational axis 4 of the bell cup 3 . fig5 shows a further exemplary illustration of the shaping air ring 2 , this example largely corresponding to that described above and illustrated in fig2 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one distinctive feature of this example consists in that the shaping air nozzles 10 are arranged on an inner ring 12 , while the shaping air nozzles 11 are arranged on an outer ring 13 , both rings 12 , 13 being concentrically arranged . the shaping air nozzles 11 on the outer ring 13 here have a jet direction that is radially inclined inward compared to the rotational axis 4 of the bell cup 3 . in this example , the shaping air nozzles 10 on the inner ring 12 have , however , a jet direction that is directed radially outward compared to the rotational axis 4 of the bell cup 3 . fig6 shows a further exemplary illustration of the shaping air ring 2 , wherein this example also largely corresponds to that described above and illustrated in fig2 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one distinctive feature of this example consists in that the shaping air nozzles 10 have a jet direction that is inclined radially inward compared to the rotational axis 4 of the bell cup 3 , whereas the other shaping air nozzles 11 have a jet direction that is substantially parallel to the axis of the jet direction . thus , the shaping air nozzles 10 constrict the shaping air jet , such that the shaping air flow assumes the form of a planar jet . fig7 largely corresponds to the representation in fig1 , so that , for avoiding repetitions , reference is made to the above description of fig1 . an additional outcome of this representation is that , due to the jet direction being inclined inward , the shaping air ring 2 discharges an intersecting shaping air jet 6 . fig8 also shows an exemplary shaping air ring 1 , wherein this example largely corresponds to the example described above and illustrated in fig1 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one distinctive feature of this example consists in that the shaping air ring 2 has three concentric shaping air nozzle rings that discharge shaping air jets 6 . 1 , 6 . 2 and 6 . 3 . the outer shaping air jet 6 . 1 here has a jet direction that is inclined radially inward compared to the rotational axis 4 . the middle shaping air jet 6 . 2 , however , has a jet substantially parallel with the jet direction . finally , the inner shaping air jet 6 . 3 has a jet direction that is inclined radially outward compared to the rotational axis 4 of the bell cup 3 . fig9 shows a simplified cross - sectional view of a shaping air nozzle 14 according to an exemplary illustration that is fed with shaping air from a shaping air bore 15 . in so doing , the shaping air nozzle 14 widens step - wise here at the transition from the shaping air bore 15 to the shaping air nozzle 14 , turbulences being generated in the shaping air nozzle 14 . fig1 shows a simplified cross - sectional view of a further example of a shaping air nozzle 14 , which in part corresponds to fig9 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one distinctive feature of this example consists in that the shaping air nozzle at the transition of the shaping air bore 15 not widens step - wise , but rather conically . fig1 shows a further exemplary illustration of a shaping air nozzle 14 , which in part corresponds to fig9 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one principal distinctive feature of this example consists in that the shaping air nozzle 14 does not widen in the jet direction , but rather is tapered in the jet direction . on the other hand , the shaping air nozzle 14 has three consecutive stepped nozzle sections 17 , 18 and 19 , the cross - sections of which diminish in the direction of flow . in addition , the example shown in fig1 partly corresponds to the above - described examples , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one distinctive feature consists in that the shaping air nozzle 14 is tapered in the direction of flow . a further distinctive feature of this example consists in that the shaping air nozzle 14 has a conical inner contour . fig1 shows a detail from a shaping air ring according to the exemplary illustrations with shaping air nozzles arranged in a ring shape , wherein only two shaping air nozzles 20 , 21 are illustrated in the drawing . in this case , a ring - shaped slit 22 , the diameter of which matches the diameter of the shaping air ring , runs through both shaping air nozzles 20 , 21 . fig1 shows a schematic representation of a shaping air nozzle 23 according to an exemplary illustration with a cross - shaped , concentric slit arrangement 24 . the example according to fig1 provides for a distortion of the flow profile in order to generate turbulences . here , a shaping air bore 25 opens into a shaping air nozzle 26 , the nozzle cross - section of the shaping air nozzle 26 being inclined compared to the cross - section of the shaping air bore 25 . the shaping air flow in the shaping air bore 25 therefore has a conventional parabolic profile 27 , while the shaping air jet emerging from the shaping air nozzle 26 has a distorted flow profile 28 . fig1 furthermore shows two shaping air nozzles that are formed by notches 29 , 30 , with a shaping air bore 31 , 32 opening into both notches 29 , 30 . here , both notches 29 , 30 each are triangular in cross - section . the example shown in fig1 again largely corresponds to that shown in fig1 , so that , for avoiding repetitions , reference is made to the above description and the same reference numerals are used for corresponding details . one distinctive feature of this exemplary illustration consists in that both shaping air bores 31 , 32 open into a common notch 33 that forms a shaping air nozzle and is likewise triangular in cross - section . reference in the specification to “ one example ,” “ an example ,” “ one embodiment ,” or “ an embodiment ” means that a particular feature , structure , or characteristic described in connection with the example is included in at least one example . the phrase “ in one example ” in various places in the specification does not necessarily refer to the same example each time it appears . with regard to the processes , systems , methods , heuristics , etc . described herein , it should be understood that , although the steps of such processes , etc . have been described as occurring according to a certain ordered sequence , such processes could be practiced with the described steps performed in an order other than the order described herein . it further should be understood that certain steps could be performed simultaneously , that other steps could be added , or that certain steps described herein could be omitted . in other words , the descriptions of processes herein are provided for the purpose of illustrating certain embodiments , and should in no way be construed so as to limit the claimed invention . accordingly , it is to be understood that the above description is intended to be illustrative and not restrictive . many embodiments and applications other than the examples provided would be evident upon reading the above description . the scope of the invention should be determined , not with reference to the above description , but should instead be determined with reference to the appended claims , along with the full scope of equivalents to which such claims are entitled . it is anticipated and intended that future developments will occur in the arts discussed herein , and that the disclosed systems and methods will be incorporated into such future embodiments . in sum , it should be understood that the invention is capable of modification and variation and is limited only by the following claims . all terms used in the claims are intended to be given their broadest reasonable constructions and their ordinary meanings as understood by those skilled in the art unless an explicit indication to the contrary in made herein . in particular , use of the singular articles such as “ a ,” “ the ,” “ the ,” etc . should be read to recite one or more of the indicated elements unless a claim recites an explicit limitation to the contrary . | 1 |
referring now to the drawings , wherein the showings are for the purpose of illustrating certain exemplary embodiments only and not for the purpose of limiting the same , fig1 illustrates a series of work pieces with spot welds in different locations in accordance with the present disclosure . as mentioned above , manufacturing process variability can lead to weld location variability , affecting resulting joint strength . each sample or coupon includes two flat work pieces situated to create an overlap . a spot weld is positioned on each overlap in order to create a joint between the work pieces . coupon a describes case 1 , in which the spot weld is located in the center of the overlap . coupons b through e illustrate cases 2 through 5 , displaying edge welds or welds which contact the edge of the overlap . the percentages indicated denote the percentage of weld area of the intended circular weld effected on the samples in the overlap . the migration of welds as illustrated all moved toward the left , but it will be appreciated that a weld would just as equally be considered an edge weld if it existed tangential to or overlapping with the dotted line representing the edge of the lower work piece to the right of center . the production of effective resistance welds is a well known art . welding engineering includes known methods , procedures , and best practices known to produce welds of appropriate strength and quality . engineering mechanics includes known principles regarding the study of forces acting upon a workpiece , the resulting internal stresses upon the workpiece , and the associated strain or deformation experienced by the workpiece . materials engineering includes known principles regarding strength of materials , strength of metallic objects resulting from molten metals cooling at certain rates and in certain environments , and the compatibility of materials to be welded together . principles and techniques involved in creating proper welds are well known , and will not be explored in detail herein . for the purposes of this disclosure , it is assumed that proper welding practices have been employed , and that the welds applied in all exemplary embodiments have been created through known methods . fig2 illustrates test results displaying joint strength data for a series of coupons with different weld locations , in accordance with the present disclosure . experimental data is displayed against data predicted by computer analysis of models of the work pieces . a comparison of the data shows strong correlation of a trend indicating that a spot weld located in the center of the overlap has the highest strength , with consistently or approximately linearly decreasing weld strength as first the weld is moved tangentially next to the edge and then is steadily reduced over the edge as described in the coupons of fig1 . fig3 illustrates a sectional view of two work pieces being resistance welded together in the center of an overlap in accordance with the present disclosure . work pieces 10 a and 10 b in this exemplary embodiment are flat pieces with main sections projecting off in opposite directions . it should be appreciated that the welding techniques described herein and the work pieces described can take many embodiments and are not intended to be limited to the specific examples illustrated herein . for example , the two edges could be lined up , and the main bodies of work pieces 10 a and 10 b could extend off in the same direction . the resistance welding technique used in the method can take many forms , including spot welding , weld - bonding , resistance seam welding , and projection welding . many forms of resistance welding are known , and specific details of each will not be described herein . the methods utilized herein can be used in any welding process wherein two pieces are affixed together by melting together portions of work pieces resulting in a deformation or indentation of the work pieces in a predictable manner . the disclosure is not intended to be limited to the particular welding processes described herein . additionally , two work pieces are illustrated . however , it will be appreciated that multiple work pieces could be located and joined together similarly according to methods described herein . electrodes 20 a and 20 b describe exemplary tools which would be used to pass a current through the work pieces to create a weld . weld 30 represents the combination of material originally from work pieces 10 a and 10 b which is melted into a single mass , which when cooled becomes the weld joint between work pieces 10 a and 10 b . as electrodes 20 a and 20 b come into contact with work pieces 10 a and 10 b , the current flowing through the work pieces softens the material , and a clamping force applied to the electrodes in combination with the softened material in the work pieces causes an indentation to form on each of the work pieces . the flat planes of material surrounding the electrodes and the resulting weld provide stability and maintain the orientation of the molten and softened material to the surrounding work pieces . fig4 illustrates a sectional view of two work pieces being resistance welded together close to an edge of an overlap in accordance with the present disclosure . as shown in fig3 , electrodes 20 a and 20 b come into contact with work pieces 10 a and 10 b . as current passes through the work pieces , the material softens , weld 30 is created , and the soft material in combination with a clamping force applied to the electrodes causes an indentation to form on each of the work pieces . however , where in the exemplary embodiment of fig3 , the flat planes of material surrounding the electrodes and the resulting weld provided stability for the molten material of the weld to stay in place , the proximity to the electrodes and of the weld to the edge of work piece 10 a creates instability where softened or molten material from the work pieces can deform outwards past the edge . results of this deformation can be seen in fig5 , where a top view of work piece 10 a after the welding process is illustrated in accordance with the present disclosure . as mentioned above , the effects of the current applied and the clamping force of the electrodes , in combination with the proximity to the edge of the work piece , causes instability in the material of the work piece . fig5 shows how weld 30 and a softened material area 40 react to being open to the edge of work piece 10 a , where as the material of the work piece changes from a solid to some degree closer to a liquid , the material is pushed out of its normal position past the edge of the work piece . returning to fig4 , the instability in the material of the work pieces caused by the weld in close proximity to the edge allows material to move away from the electrodes that would in the center of an overlap be kept in place . this movement of material leads to less material remaining between the electrodes and around the resulting weld , causing increased indentation thickness and deformation in the resulting alignment of the work pieces . the resulting weld 30 is weaker and leads to the experimental and calculated results described in fig2 . the exemplary embodiment of work pieces 10 a and 10 b described in fig4 and 5 were in close proximity or tangential to the edge , as in coupon b illustrated in fig1 . as the electrodes 20 a and 20 b and the resulting weld 30 move past the edge of a work piece , as described in coupons c , d , and e of fig1 , instability in the softened material and the molten material of the weld increases . fig6 illustrates an exemplary embodiment of a spot weld resulting from electrodes lined up partially off the edge of work piece 10 a in accordance with the present disclosure . as in the exemplary embodiment described in fig4 and 5 , material from work piece 10 a , placed between a pair of electrodes and welded together through application of a current , has deformed and extended past the original edge of work piece 10 a . material from work pieces 10 a and 10 b has melted together to form weld 30 . however , in this exemplary embodiment , some of the material originally part of workpiece 10 a , has escaped from the weld area and has either been left as non - functional weld residue 50 or has been expelled in the welding process . those having ordinary skill in the art will appreciate that the reduction in area of weld 30 and the large amount of material lost to the non - functional weld residue 50 or expelled reduces the strength of the resulting weld joint in comparison to the welds illustrated in fig3 and 4 . as the alignment of the electrodes goes further off the edge of the work pieces , the weld strength will continue to decrease as the resulting quality of weld 30 decreases . fig7 illustrates exemplary test results showing a relationship of distance from the edge of a work piece to both weld indentation and resulting weld strength in accordance with the present disclosure . distance from the edge of the work piece in this particular exemplary test is measured from the center of the electrode to the edge . so long as the distance from the edge of the work piece maintains a minimum distance where the softened and molten material remains contained in a stable plane of material , the weld indentation and resulting weld strength remain relatively stable . however , a point can be seen in the exemplary data around 8 mm and lower from the edge , where the weld indentation sharply rises and the weld strength decreases precipitously . it should be noted that 8 mm is a threshold distance for the sample pieces tested , but this value will change as a function of the particular work pieces and weld process employed . such a value can be determined through testing of samples or predicted through any method sufficient to comprehend the strength of the resulting weld joint . as described above , the proximity of the electrodes and the resulting weld to the edge of the workpiece creates instability and decreases the quality of the resulting weld . this graph demonstrates a strong correlation between distance from the edge , weld indentation , and resulting weld strength . while there exists evidence of strong correlation between distance from the edge of the workpiece and resulting weld strength , parts created in the welding process can be complicated , large , and unwieldy . the size and orientation of the parts may inhibit taking measurements from the weld location to the closest edge . also , as described above , the weld can move close to different edges of the work pieces . the exemplary embodiments described above were simple planes with straight edges , however , work pieces in practical applications are frequently complex , employ curved or complex shapes , and variability in the manufacturing process can move in many directions . however , the effect of moving close to an edge of a work piece upon the thickness of the weld indentation will remain steady . a method is disclosed to detect and repair edge welds based upon weld indentation thickness . while the exemplary processes illustrated above were spot welds , the methods described below may work equally well in resistance welds of different shapes and configurations , and are not intended to be limited merely to spot welds . welds of non - circular or larger geometry might require multiple measures of indentation thickness to apply the methodology described herein . referring back to fig7 , as described above , too great of a weld indentation thickness value indicates that the weld occurred too close to an edge . however , it can also be seen from the information in the chart that the weld indentation thickness does not go below a particular level regardless of distance from the edge . the application of current and the clamping force on the electrodes necessary to produce a proper resistance weld will produce weld indentation thicknesses of at least a certain value . by comparing measured weld indentation thicknesses to a minimum weld indentation thickness , a determination can be performed whether some anomaly in the welding process prevented a proper weld from taking place . once estimated , weld integrity can be used to adjust welding operations on the work pieces to compensate for disparate weld readings . weld thickness readings or estimations can be made in real - time , allowing for the particular welding work station to adjust and contain any actions within that work station or minimize effects upon other work stations downstream in the manufacturing process . for example , a weld thickness sensor can be constructed integrally with the machinery deploying the electrodes to the work pieces in order to get a weld thickness measurement immediately after the weld is created . the weld thickness sensor would be signally connected to a weld work station . alternatively , weld thickness may be estimated by tracking movement of the electrodes and inferring weld thickness based on electrode movement . alternatively , real - time tracking of weld thickness allows calculation of a first derivative of weld thickness , denoted by i , with respect to time , denoted by t ; the derivative yielding di / dt or instantaneous weld thickness change . this measured instantaneous weld thickness change can be compared with expected results , and if the electrodes are creating an indentation too quickly or too slowly , steps can be taken during the weld including changing welder parameters or aborting the weld for a repair step . one having skill in the art will appreciate that any similarly available measure of indentation or movement of the electrodes , for example , integration of di / dt as a measure of indentation through a time or alternatively a second derivative of weld thickness with respect to time , can be used to evaluate the weld . in this way , an indication of the weld thickness or a weld indentation characteristic can be tracked and used to diagnose weld integrity . in order to monitor and process weld thickness data collected by the methods described above , an exemplary weld work station can comprise a data processing computer , a graphical user interface , and a non - volatile memory storage area capable of storing threshold weld indentation characteristic values for a plurality of work pieces . the weld work station is operably and signally connected to a resistance welding control station in order to receive weld thickness data from a sensor , encoder , or any other weld thickness detection device , and can be capable to direct weld gun motion through weld gun electrode deployment machinery . the weld work station processor would have software executable to interpret and manipulate weld thickness data from the weld thickness detection device , and compare monitored weld thickness values with stored threshold weld thickness values . fig8 illustrates process 100 wherein an exemplary method to detect and repair edge welds based upon weld indentation thickness is utilized in accordance with the present disclosure . in step 102 , a set of work pieces are aligned in a manufacturing process , and a resistance weld is performed upon the work pieces . in step 104 , a measurement is then taken of weld indentation thickness , and in step 106 , the measured weld indentation thickness is compared to a threshold weld indentation thickness . if the measured weld indentation thickness is not greater than the threshold weld indentation thickness , then the relationship of weld indentation thickness to distance from the edge of the work pieces and resulting weld strength described above indicate that the weld was not performed too close to an edge , and the process moved on to step 108 . if the measured weld indentation thickness is greater than the threshold weld indentation thickness , then the relationship described above indicates that manufacturing variability has caused the weld to be performed too close to the edge of the workpiece , that a low quality weld has been performed , and that the process must go to step 110 to determine a containment or repair action . step 110 adjusts the welding gun containing the necessary electrodes and instrumentation used to measure workpiece thickness to a new location and workpiece thickness is measured . the detection of workpiece and electrode location and control of movement may be generically set , may involve a recalibration to a coordinate system based on tooling or the workpiece , may be directed by the movement of deployment machinery controlled with an encoder of electric servomotor ( i . e ., servo gun ) or other location sensing methods ( lvdt and laser ), or may employ other means to select the direction of movement . at step 112 , information regarding the movement of the gun and the measured workpiece thickness at step 110 is used to determine or estimate current gun location . at step 114 , a determination is made as to whether the gun is currently in a location to perform a repair weld . if the gun is determined to be in a proper location , then the process is reinitiated to step 102 . if the gun is determined to be in an improper location , then step 116 undertakes some procedure to find a proper location to perform a repair weld or the weld location is skipped , and containment actions are taken to ensure the quality of the next weld . actions in 116 may involve moving the gun by logic similar to the previous movement as described in step 110 or an overall algorithm can be applied to determine the proper containment action . for example , a factor of safety could be employed in programming welds in a workpiece , wherein if a single weld malfunction occurs during manufacture , the workpiece is still deemed acceptable and no repair function is needed . alternatively , a workpiece with a failed weld can be flagged and put through a separate repair loop in the process , flagged and identified for individual inspection and repair off line , or otherwise contained . upon passing the weld indentation thickness comparison in step 106 , the workpiece can be presumed to pass , or as is illustrated in process 100 , at step 108 a presumption may be applied that the weld location has to have at least a minimum weld indentation thickness to indicate that a healthy weld was performed at that location . as described above , the measured weld indentation thickness can be compared to a minimum weld indentation thickness to determine whether something interfered with the creation of a proper weld . if the measured weld indentation thickness is smaller than the minimum weld indentation thickness then the weld is considered improper , and at step 118 , the weld process variables such as weld time and current applied are adjusted and the process is reinitiated at step 102 . in alternative to step 118 , a failure in the comparison at step 108 could initiate other containment actions as described above in step 116 or other containment means could be applied . if the measured weld indentation thickness at step 108 is greater than the minimum weld indentation thickness , then the weld is deemed acceptable , and the process is reinitiated at step 102 for the next weld point . the threshold weld indentation thickness and minimum weld indentation thickness are values that will change from application to application and can be determined experimentally , empirically , predictively , through modeling or other techniques adequate to accurately predict resulting strength in the weld joint . the disclosure has described certain preferred embodiments and modifications thereto . further modifications and alterations may occur to others upon reading and understanding the specification . therefore , it is intended that the disclosure not be limited to the particular embodiment ( s ) disclosed as the best mode contemplated for carrying out this disclosure , but that the disclosure will include all embodiments falling within the scope of the appended claims . | 1 |
as shown in the drawings for purposes of illustration , the present invention pertains to a technique for reshaping or reformatting an output beam from a laser diode bar array of the type that may be used in high power applications , such as for pumping a fiber laser . a well known difficulty associated with laser diode bar arrays of wide stripe emitters is that the resultant output beam is elliptical in cross section and diverges differently in the transverse and lateral directions . the output beam is said to exhibit anamorphism , as often defined by the beam invariant , which is the product of the near field diameter ( in millimeters ) and the far field diameter ( in milliradians ). ideally , the beam invariant in the transverse and lateral directions should be roughly the same , meaning that the beam exhibits low astigmatism and a high degree of circularity of cross section . in this context , the “ lateral ” direction extends across the emitter array , parallel to the linear array of emitter bars , and the “ transverse ” direction is perpendicular to the transverse direction , and perpendicular to the optical axis along which the beam is propagated . unfortunately , a typical laser diode bar having , for example 19 100 - μm stripes has a transverse beam invariant of about 1 mm - mr and a lateral beam invariant of about 450 mm - mr . the principal object of the invention is provide a composite output beam that is more nearly circular in cross section and has more nearly equal invariants in the lateral and transverse directions . a typical optical fiber has beam acceptance criterion of about 44 mm - mr invariant , and it is , therefore , also an object of the invention to provide a composite output beam having transverse and lateral invariants both less than 44 mm - mr . in accordance with the present invention , an array 10 of right - angle roof prisms 12 is positioned to intercept light from a diode bar 14 , as indicated diagrammatically in fig1 and 2 a - 2 c . each sub - beam emitted from the diode bar 14 impinges on its own prism 12 , which receives the sub - beam through and approximately normal to the hypotenuse face of the prism . the sub - beam is reflected from one angled face of the prism 12 to the other , and follows a return path out of the prism in a direction parallel to , but oppositely directed and offset from the original path of sub - beam from the diode bar 14 . a critical aspect of the invention is that the roof prisms 12 are each rotated such that the roof lines of the prisms lie at 45 ° to the direction of orientation of the laser diode bar 14 ( the lateral direction ). therefore , to align the prisms 12 with the sub - beams from the diode bar 14 , each prism is offset from its nearest neighbors by a uniform offset distance in the lateral direction . the prisms are preferably stacked in contact with each other , as best shown in fig2 a and 2b , to form a unitary array structure , although it is not a requirement that they be in contact with each other . by way of further clarification of the geometry of the array 10 of prisms 12 , the hypotenuse faces of the prisms are disposed in a single plane , as best seen in fig2 b , but because the prisms are oriented at 45 ° to the lateral direction on which the diode bar emitters are arrayed , each prism is offset with respect to its nearest neighbor in a direction that is parallel to the plane of the hypotenuse faces and parallel to the triangular faces of the prisms . the effect on each sub - beam as it is internally reflected from two angled surfaces of the corresponding roof prism 12 , is to rotate the cross - sectional shape of the beam by 90 °. as the sub - beams enter the array 10 , their cross sections 16 ( fig3 a ) are highly elongated in the lateral direction , but as the beams leave the array their cross sections 16 ′ ( fig3 b ) are elongated in the transverse direction , which is to say that the sub - beam cross sections have their longer dimensions rendered parallel in the transverse direction , instead of being arranged “ end - to - end ” in the lateral direction . the originally very narrow dimension of the output array in the transverse direction is effectively increased by passage through the prism array 10 , by a factor of approximately three to four , or more , depending on the width - to - height ratio of the original sub - beam cross section 16 . this beam rotation has the effect of more nearly circularizing the composite beam cross section , after appropriate collimation , and greatly reduces the disparity between the invariant values in the lateral and transverse directions . for the illustrative 19 - emitter array , the reformatted beam has a transverse beam invariant of 19 mm - mr and a lateral beam invariant of 25 mm - mr , values that are more nearly equal and permit launching of the beam into an optical fiber without significant losses . as described to this point , the invention accomplishes the principal object of the invention and provides an output beam that is oppositely directed and slightly offset from the output beam from the laser diode bar 14 . unfortunately , this beam path may be inconveniently close to cooling and electrical connections to the laser diode bar 14 . in accordance with another aspect of the invention , the reshaped output beam from the array 10 of prisms 12 is directed into a single roof prism 20 having its roof line generally parallel to lateral direction of the beam cross section . all of the sub - beams reflected from the prism array 10 enter the prism 20 through , and generally normal to , the hypotenuse face of the prism . the sub - beams are reflected from each of the two angled faces of the prism 20 in turn , and emerge in a direction parallel to the original direction of propagation from the laser diode bar 14 , but offset a short distance from the original beam because of the offsets inherent in the prism array 10 and the prism 20 . thus , the prism 20 operates as a retro prism , reversing the direction of the composite output beam , but otherwise retaining its desirably improved symmetry . use of the retro prism 20 , therefore , avoids passing the output beam close to the laser diode bar 14 and its required cooling and electrical connections . since the output of the diode bar 14 is polarized , and since the total internal reflections in the prism array 10 lie in planes which have both components of polarization present , a relative phase shift between the polarization components will be induced in the array . it can be shown that if the index of refraction of the prism array 10 and the retro prism 20 are chosen properly , the output polarization will be linear and in a direction 45 ° from the line of the diode bar 14 . this state of polarization is a convenient one for using for subsequent beam combining of bars through a polarization beam combiner ( not shown ). the surfaces of the prisms 12 and the retro prism 20 are either anti - reflection ( ar ) coated ( the hypotenuse faces , through which light is to be transmitted ), or provide for total internal reflection ( the internal angled faces of the prisms ). losses for this type of device are typically lower than for other types of optical components , such as cylindrical lenses or mirrored surfaces . prisms are also relatively easy and less costly to manufacture than the other types of optical components . it will be appreciated from the foregoing that the present invention represents a significant advance in the field of high power lasers . in particular , the invention provides a relatively symmetrical composite output beam from a linear laser diode array , permitting the output beam to be easily launched into an optical fiber or coupled to some other optical component . it will also be appreciated that , although a specific embodiment of the invention has been illustrated and described by way of example , various modifications may be made without departing from the spirit and scope of the invention . accordingly , the invention should not be limited except as by the appended claims . | 6 |
one or more embodiments of the present disclosure relate to controlling and deploying intravascular devices . an intravascular device may be controlled and deployed by a controller operated by a medical profession outside the patient &# 39 ; s vasculature . the controller may allow for the actuation of various components of the intravascular device and may allow the placement of the intravascular device . the placement of the device may include rotational and longitudinal placement in a vessel . rotational placement may be effected by the translational of torque from the controller to the intravascular device . an elongate mandrel may connect the controller to the intravascular device and transmit longitudinal force and torque therebetween . the controller may include a rotatable actuator knob that may disconnect the intravascular device from the elongate mandrel . the actuator knob may disconnect the intravascular device from the elongate mandrel when the actuator knob , and hence the elongate mandrel , is rotated in a counter clockwise direction . however , when rotated in the clockwise direction , the actuator knob , and hence the elongate mandrel , may damage the connection between the elongate mandrel and the intravascular device . a one - way bearing located between a body of the controller and a rotating assembly inside the controller may substantially limit the ability of the actuator knob to rotate in the clockwise direction and damage the connection between the elongate mandrel and the intravascular device . the one - way bearing may allow the rotation of the elongate mandrel without any perceivable interference to a user in a first direction . the one - way bearing may transmit torque from the actuator knob to the body of the controller , and hence the user &# 39 ; s grip on the controller , when rotated in an opposite second direction . an incorrectly assembled controller may substantially inhibit counter clockwise rotation of the actuator knob and , hence , a medical professional &# 39 ; s ability to disconnect and deploy an intravascular device . a method of manufacture is also presented herein to ensure correct directional assembly of a controller . fig1 depicts an intravascular device delivery system 100 including a controller 102 , an elongate mandrel 104 , and an intravascular device 106 . the controller 102 may be connected to a proximal end of the elongate mandrel 104 and the intravascular device 106 may be connected to a distal end of the elongate mandrel 104 . the intravascular device 106 may include a variety of devices and is depicted schematically . in some embodiments , the intravascular device 106 may include a mitral valve repair device , such as a mitraclip available from abbott vascular . in other embodiments , the intravascular device 106 may include other vascular repair devices . in yet other embodiments , the intravascular device 106 may include filtration devices . in further embodiments , the intravascular device 106 may include pharmaceutical eluting devices . in some embodiments , the elongate mandrel 104 may connect to the intravascular device 106 by an internal threaded connection , an external threaded connection , a bayonet connection , other suitable rotational connection , or combinations thereof . the elongate mandrel 104 may include a catheter , guidewire , other vascular sleeve , or combinations thereof . in some embodiments , the elongate mandrel 104 may have a working length less than about 1000 mm in length , greater than about 1000 mm in length , greater than about 1200 mm in length , or about 1220 mm in length . as used herein , “ working length ” should be understood to be the effective , usable length of a component or device during a medical procedure . for example , total length of the elongate mandrel 104 may be greater than the working length of the elongate mandrel 104 as portions of the elongate mandrel may be contained within other components , such as the intravascular device 106 or the controller 102 . the controller 102 is located at a distal end of the elongate mandrel 104 . the controller 102 may include a variety of buttons 108 in order to control various functions or conditions of the intravascular device 106 , pressure system ( e . g . a bleedback valve ) and / or a delivery mechanism . in the depicted embodiment , the controller 102 may include an arm positioner knob 110 for manipulating the arm positions of a mitral valve repair device . actuator knob 112 is located at the proximal end of the controller 102 . the rotation of the actuation knob 112 may be restricted by an actuator clip 114 . the actuator clip 114 rotationally fixes a position of the actuator knob 112 relative to a controller body 116 . the actuator clip 114 may be removed when rotation of the actuator knob 112 , hence deployment of the intravascular device 106 is intended . fig2 illustrates a detail view of the controller 102 and actuator knob 112 with the actuator clip 114 removed . the actuator knob 112 may be fixed to a threaded rod 118 that is inserted and threaded into a crimping cam 120 ( visible in fig3 ). the actuator knob 112 may thereby rotate the crimping cam 120 via torque transmitted by the threaded rod 118 . the crimping cam 120 may rotate relative to the controller body 116 when the actuator clip 114 is removed from the crimping cam 120 . fig3 shows a cross - sectional view of the controller 102 depicted in fig2 . as described , the actuator knob 112 may be fixed to a threaded rod 118 , which is threaded into the crimping cam 120 . the crimping cam 120 may include within it a collet 122 . in some embodiments , the crimping cam 120 may be generally cylindrical , for example , having a circular transverse cross - section . in other embodiments , the interior surface 124 of the crimping cam 120 may have a polygonal transverse cross - section such a square , a pentagon , a hexagon , and similar or an irregular polygon . similarly , in some embodiments , the collet 122 may be generally cylindrical and have a circular transverse cross - section . in other embodiments , the collet 122 may have a polygonal transverse cross - section such a square , a pentagon , a hexagon , and similar or an irregular polygon . in some embodiments , the collet 122 may mate complimentarily with an interior surface 124 of the crimping cam 120 . the actuator knob 112 , threaded rod 118 , crimping cam 120 , collet 122 may share a longitudinal axis 126 about which they may all rotate . as such , the shared longitudinal axis 126 may also be a shared rotational axis . the threaded rod 118 may apply a longitudinal compression force upon the collet 122 as the threaded rod 118 is rotated against the complimentarily threaded crimping cam 120 . the compression force on the collet 122 may cause the collet to move longitudinally and strike one or more tapers 128 on the crimping cam 120 . the tapers 128 may apply a lateral compression force upon the collet 122 . the lateral compression force may , in turn , cause the collet 122 to impinge upon a proximal end 130 of the elongate mandrel 104 . the collet 122 may thereby hold the proximal end 130 of the elongate mandrel 104 in within the rotating assembly 132 . the rotating assembly 132 may include the actuator knob 112 , threaded rod 118 , collet 122 , and crimping cam 120 . the rotating assembly 132 may rotate relative to the controller body 116 . in some embodiments , the rotating assembly 132 may rotate upon a one - way bearing 134 located between the rotating assembly 132 and an actuator slider 136 . the actuator slider 136 may be rotationally fixed relative to the controller body 116 . in other embodiments , the rotating assembly 132 may rotate upon a one - way bearing 134 located between the rotating assembly 132 and the controller body 116 . in some embodiments , the one - way bearing 134 may be a rotational clutch bearing . in other embodiments , the one - way bearing 134 may be a ratcheting bearing . in an embodiment , the one - way bearing 134 may be an annular or cylindrical rotational bearing . the rotating assembly 132 may be rotationally fixed relative an inner surface of the one - way bearing . in various embodiments , the rotating assembly 132 and one - way bearing 134 are fixed using a friction fit , a press fit , an adhesive , a weld , other suitable attachment mechanism , or combinations thereof . a clutch bearing may freely enable rotation of the rotating assembly 132 in a first direction while allowing for nearly instant resistance to be applied when rotated in a second direction . similarly , a ratcheting bearing may allow freely enable rotation in the first direction , but may allow some degree of backlash in the second direction . as used herein , “ rotating direction ” should be understood to refer to the rotational direction in which the one - way bearing 134 rotates with relatively little friction . “ locking direction ” should be understood to refer to the rotational direction in which the one - way bearing 134 may resist rotation and transfer torque . the ratcheting bearing may result in a tactile “ clicking ” sensation during operation . in some environments , such a sensation may be undesirable due to medical professional &# 39 ; s experience and training with other rotation systems . when changing from a rotation system such as a bi - direction actuator having a rotating inner component and stationary outer component separated only by a simple bearing surface , the change from a simple bearing surface with near constant friction to a ratcheting system may result in a foreign tactile sensation . in at least some embodiments therefore , it may be desirable to retain as much familiar tactile performance as possible to encourage adoption of embodiments incorporating a one - way bearing 134 . the one - way bearing 134 may rotate freely in the “ rotating direction ” and “ lock ” when torque is applied in the “ locking direction .” to help ensure the one - way bearing 134 is installed in the controller 102 in the proper orientation , a number of indicators and design structures may be employed . in an embodiment , the one - way bearing may have a visual indicator imprinted , embossed , and / or applied to a surface indicating the rotating direction . in another embodiment , the locking direction may be leveraged during the assembly process . fig4 depicts a controller 102 expanded along the longitudinal axis 126 . in some embodiments , the one - way bearing 134 is connected to the interior of a threaded insert 138 . in other embodiments , the one - way bearing 134 may have threads integrated into the one - way bearing 134 , itself . the one - way bearing 134 may be connected to the interior of a threaded insert 138 by a friction fit , a press fit , an adhesive , a weld , other suitable attachment mechanism , or combinations thereof . the threaded insert 138 may use the locking direction of the affixed one - way bearing 134 to drive the threaded insert 138 into the actuator slider 136 . the threaded insert 138 may include left - hand threads 140 ( opposite of the common threading direction ) on a lateral surface thereof , which may mate with complimentary threads 142 on the actuator slider 136 . the locking direction of the one - way bearing 134 may therefore transfer torque to the threaded insert 138 when the one - way bearing 134 is aligned such that the locking direction is oriented in the direction of the left - hand threads 140 . the rotating direction of the one - way bearing 134 may also substantially prevent the transfer of torque to the threaded insert 138 when the one - way bearing 134 is aligned such that the rotating direction is oriented in the direction of the left - hand threads 140 . the threaded insert 138 may be driven into the actuator slider 136 therefore when the locking direction of the one - way bearing 134 is oriented counter - clockwise when viewed from a distal end 144 of the controller 102 . when viewed from a proximal end 146 of the controller 102 , the locking direction of the one - way bearing 134 may be the clockwise direction . accordingly , the rotating direction of the one - way bearing 134 may permit rotation in the counter - clockwise direction when viewed from the proximal end 146 of the controller 102 . as an operator will view the controller 102 from the proximal end 146 , the one - way bearing 134 may allow rotation of the actuator knob 112 , and hence rotating assembly 132 and elongate mandrel 104 in a counter - clockwise direction . the counter - clockwise rotation of the elongate mandrel 104 may disconnect and / or deploy the intravascular device 106 at the distal end of the elongate mandrel 104 . as shown in fig5 , applying torque to the actuator knob 112 may apply a torque to the rotating assembly 132 . when the torque vector is in the distal direction ( according to the right - hand rule ) toward the distal end 144 of the controller 102 , the one - way bearing 134 may transmit the torque to act upon the actuator slider 136 . the actuator slider 136 may be rotationally fixed to the controller body 116 . the controller body 116 may be held by a user during operation of the actuator knob 112 . the actuator knob 112 may have a smaller radius than the controller body 116 . therefore , the user may use comparatively little force to hold the controller body 116 still during the transmission of torque from the actuator knob 112 to the controller body 116 . this may effectively prevent substantial movement of the controller 102 during application of torque to the actuator knob 112 in the locking direction . as shown in fig6 , applying torque to the actuator knob 112 toward the proximal end 146 ( according to the right - hand rule ) may apply torque to the rotating assembly 132 . the one - way bearing 134 may transmit little to no torque to the controller body 116 through the threaded insert 138 , thereby allowing rotation of the rotating assembly 132 about the longitudinal axis 126 . the rotation of the rotating assembly 132 about the longitudinal axis may rotate the elongate mandrel 104 . the rotating assembly 132 may be connected via the one - way bearing to the controller body 116 directly or via the actuator slider 136 . the rotating assembly 132 may be “ held ” in place when the one - way bearing 134 transfers torque to the actuator slider 136 , which may be , in turn , held in place by the body 116 . an operator may then resist the rotation of the body manually . the rotating assembly 132 may also be connected to the controller body 116 directly via the one - way bearing 134 , such that the one - way bearing 134 transfers torque directly from the rotating assembly 132 to the controller body 116 . as described in relation to fig3 , the intravascular device delivery system 100 of the present disclosure may use the mechanical characteristics of some components during a manufacturing process . as shown in fig7 , the assembly of an intravascular device delivery system 100 may include the assembly of a controller 102 . the elongate mandrel 104 may be inserted into the collet 122 . the elongate mandrel 104 may extend from a tapered end 148 of the collet 122 and the proximal end 130 of the elongate mandrel 104 may be within the collet 122 . the collet 122 may be inserted into the crimping cam 120 . in an embodiment , the crimping cam 120 may include one or more tapers 128 that compliment tapers 150 on the collet 122 . in other embodiments , the crimping cam 120 may include one or more tapers 128 that do not compliment tapers 150 on the collet 122 . the crimping cam 120 may have a decreasing inner radius that applies a compressive force to the collet 122 as the collet 122 moves proximally within the crimping cam 120 . while fig7 depicts an embodiment of a crimping cam 120 having tapers 150 , the depicted profile should be understood to be a non - limiting example of a crimping cam design . the collet 122 may be retained within the crimping cam 120 by the threaded rod 118 . when threaded through the complimentary threads on the crimping cam 120 , the threaded rod 118 may apply a longitudinal compressive force on the collet 122 . the crimping cam 120 , collet 122 , actuator knob 112 , and threaded rod 118 form the rotating assembly 132 and define the rotational component within the actuator slider 136 and the controller body 116 . fig8 depicts the assembly of the controller body 116 , actuator slider 136 , threaded insert 138 , and one - way bearing 134 . in an embodiment , the assembly process may include attaching the one - way bearing 134 to the interior of the threaded insert 138 . the one - way bearing 134 may include indicia ( not shown ) that indicate the rotating direction and locking direction . in some embodiments , the threaded insert 138 may include a slight taper on the interior diameter 158 such that the one - way bearing 134 may be inserted into the threaded insert from the proximal end of the threaded insert 160 ( the end opposing the flange 154 ) such that the one - way bearing 134 can only be inserted into the threaded insert 138 before the threaded insert 138 is inserted into the actuator slider 136 . the threaded insert 138 may include left - hand threads 140 and a flange 154 that complimentarily mate with the complimentary threads 142 and a notch 156 on the actuator slider 136 . the threaded insert 138 may , therefore , fit in the actuator slider 136 in one direction . the threaded insert 138 may then be driven into the actuator slider 136 along the left - hand threads 140 and complimentary threads 142 by applying torque to the one - way bearing 134 and rotating the one - way bearing 134 in the locking direction . if the one - way bearing 134 is oriented correctly in the threaded insert 138 , and the threaded insert 138 is aligned correctly with the actuator slider 136 , the threaded insert 138 will drive into the actuator slider 136 and affix the one - way bearing 134 to the actuator slider 136 in the desired orientation . if the one - way bearing 134 is oriented incorrectly in the threaded insert 138 , the application of torque to the one - way bearing 134 will result in the one - way bearing 134 rotating in the rotating direction and fail to transfer any torque to drive the threaded insert 138 into the actuator slider 136 . the actuator slider 136 may have a bore 152 extending therethrough , into which the rotating assembly 132 may fit . fig9 shows a schematic representation of the rotating assembly 132 being inserted into the one - way bearing 134 that has been affixed to the actuator slider 136 according to the method described in relation to fig8 . the rotating assembly 132 may be connected to the interior of the one - way bearing 134 using a friction fit , a press fit , an adhesive , a weld , other suitable attachment mechanism , or combinations thereof , as described in relation to fig3 . the rotating assembly 132 may be contained within a bore 152 that extends through the actuator slider 136 . the rotating assembly 132 may contact the wall of the bore 152 . in an embodiment , the controller 102 may include a layer of boundary material 162 between the rotating assembly 132 and the wall of the bore 152 . in some embodiments , the boundary material 162 may be made of or include a low - friction and / or lubricious material . for example , the the boundary material 162 may be made of or include polyoxymethylene , polytetraflouroethylene , or similar materials . in other embodiments , the boundary material 162 may be a low - wear , high durability coating . in some embodiments , the boundary material 162 may include a coating on the rotating assembly 132 , a coating on the wall of the bore 152 , integral to the rotating assembly 132 , integral to the wall of the bore 152 , or combinations thereof . additionally , the boundary material 162 may be a discrete component providing a substantially circumferential boundary around the rotating assembly 132 . in an embodiment , the boundary material 162 may be a continuous layer . for example , the boundary material 162 may cover the entirety of the surface , longitudinally and / or circumferentially around the rotating assembly 132 . in another embodiment , the boundary material 162 may include a non - continuous and / or intermittent distribution that provides a set space between the rotating assembly 132 and the wall of the bore 152 . for example , the boundary material 162 may include a plurality of circumferential strips that are spaced along the longitudinal length of the rotating assembly 132 . in another example , the boundary material 162 may include a plurality of longitudinal strips that are spaced along the circumference of the rotating assembly 132 . the terms “ approximately ,” “ about ,” and “ substantially ” as used herein represent an amount close to the stated amount that still performs a desired function or achieves a desired result . for example , the terms “ approximately ,” “ about ,” and “ substantially ” may refer to an amount that is within less than 10 % of , within less than 5 % of , within less than 1 % of , within less than 0 . 1 % of , and within less than 0 . 01 % of a stated amount . in the description herein , various relational terms are provided to facilitate an understanding of various aspects of some embodiments of the present disclosure . relational terms such as “ bottom ,” “ below ,” “ top ,” “ above ,” “ back ,” “ front ,” “ left ,” “ right ,” “ rear ,” “ forward ,” “ up ,” “ down ,” “ horizontal ,” “ vertical ,” “ clockwise ,” “ counterclockwise ,” “ upper ,” “ lower ,” and the like , may be used to describe various components , including their operation and / or illustrated position relative to one or more other components . for example , “ proximal ” and “ distal ” may indicate position and direction relative to the operator during use of the intravascular delivery system . relational terms do not indicate a particular orientation for each embodiment within the scope of the description or claims . accordingly , relational descriptions are intended solely for convenience in facilitating reference to various components , but such relational aspects may be reversed , flipped , rotated , moved in space , placed in a diagonal orientation or position , placed horizontally or vertically , or similarly modified unless otherwise specified . certain descriptions or designations of components as “ first ,” “ second ,” “ third ,” and the like may also be used to differentiate between identical components or between components which are similar in use , structure , or operation . such language is not intended to limit a component to a singular designation . as such , a component referenced in the specification as the “ first ” component may be the same or different than a component that is referenced in the claims as a “ first ” component . furthermore , while the description or claims may refer to “ an additional ” or “ other ” element , feature , aspect , component , or the like , it does not preclude there being a single element , or more than one , of the additional element . where the claims or description refer to “ a ” or “ an ” element , such reference is not be construed that there is just one of that element , but is instead to be inclusive of other components and understood as “ at least one ” of the element . it is to be understood that where the specification states that a component , feature , structure , function , or characteristic “ may ,” “ might ,” “ can ,” or “ could ” be included , that particular component , feature , structure , or characteristic is provided in some embodiments , but is optional for other embodiments of the present disclosure . the terms “ couple ,” “ coupled ,” “ connect ,” “ connection ,” “ connected ,” “ in connection with ,” and “ connecting ” refer to “ in direct connection with ,” or “ in connection with via one or more intermediate elements or members .” components that are “ integral ” or “ integrally ” formed include components made from the same piece of material , or sets of materials , such as by being commonly molded or cast from the same material , or commonly machined from the same piece of material stock . components that are “ integral ” should also be understood to be “ coupled ” together . although various example embodiments have been described in detail herein , those skilled in the art will readily appreciate in view of the present disclosure that many modifications are possible in the example embodiments without materially departing from the present disclosure . accordingly , any such modifications are intended to be included in the scope of this disclosure . likewise , while the disclosure herein contains many specifics , these specifics should not be construed as limiting the scope of the disclosure or of any of the appended claims , but merely as providing information pertinent to one or more specific embodiments that may fall within the scope of the disclosure and the appended claims . any described features or elements from the various embodiments disclosed may be employed in combination with any other features or elements disclosed herein . a person having ordinary skill in the art should realize in view of the present disclosure that equivalent constructions do not depart from the spirit and scope of the present disclosure , and that various changes , substitutions , and alterations may be made to embodiments disclosed herein without departing from the spirit and scope of the present disclosure . equivalent constructions , including functional “ means - plus - function ” clauses are intended to cover the structures described herein as performing the recited function , including both structural equivalents that operate in the same manner , and equivalent structures that provide the same function . it is the express intention of the applicant not to invoke means - plus - function or other functional claiming for any claim except for those in which the words ‘ means for ’ appear together with an associated function . each addition , deletion , and modification to the embodiments that falls within the meaning and scope of the claims is to be embraced by the claims . | 0 |
the background of conventional systems has been discussed in connection with the discussion of fig1 - 4 . it will be noted particularly from fig4 a and fig4 b that there is a significant drop in engine rpm ( ne ) shortly after the application of the electric load ( after this load goes from off to on ). as the quantity of electric power generated by the generator 3 increases initially , the engine rpm decreases . there is a response time in generating the needed power and , thus , there is a time period before the engine speed rises . the concept of the present invention , and the embodiments thereof shown and described herein , functions to force the field current of the generator to be switched off for a predetermined time in a manner so as to stretch out the generator recovery time to reduce the immediate transient load on the engine , to thereby keep from reducing the rpm of the engine as much as would normally be the case . an example is a prolongation of approximately one second longer than in conventional systems , and it has been found that this can prevent the substantial drop in engine rpm . note the ton period in the &# 34 ; sw &# 34 ; waveform in prior art fig3 a as compared to the similar ton period in fig6 a which includes a forced off time t c in accordance with the concepts of the present invention . note also the waveform comparison in fig1 b of prior art ( dashed lines ) and an embodiment of the present invention ( solid lines ) for the curves of quantity of electric power and engine rpm ( ne ). these graphs and curves provide a graphic indication of what is accomplished according to the present invention as compared to the prior art , and which results in a significant decrease in the drop in rpm ( ne ) upon application of the electric load as illustrated , for example , in the ne curve ( solid line vs . dashed line ) in fig1 b . turning now to exemplary embodiments of circuits , systems , methods and procedures according to the present invention , and first to fig5 this figure shows a combined circuit and block diagram of a first embodiment of the present invention . the circuit of fig5 shows a comparator ( cmp ) for comparing a terminal voltage v b of the battery 1 with a predetermined generating voltage v s , and a controller cnt for receiving the output signal from the comparator cmp and , in turn , controlling an on / off switching device sw for switching a field coil of the generator 3 to an enhanced state . considering first a typical prior art operation of this type system , the reference voltage v s is set to a given voltage , for example 14 . 5 v , by a voltage divider comprising resistors r1 and r2 , and also is set to be a second lower voltage , for example 12 . 5 v , by division into the resulting resistance divider of r1 and resistors r2 and r3 . the resistor r3 can be connected in parallel with the divider resistor r 2 by the transistor t r when the associated load is off ( making vs 12 . 5 v ). the transistor switch tr receives its control signal from a logic circuit 5 which receives signal s1 representing an air conditioner , signal s2 representing a headlight signal , and signal s3 indicating deceleration . the transistor switch is caused to turn on and off in response to the electrical load signal and engine operating condition . when the reference voltage v s is changed upon switching of the electric load ( e . g . the air conditioner is turned on ) from off to on as shown in fig3 a , the switch sw is conventionally turned on and off as shown in fig3 a so that the battery voltage v b is attempted to be held to the reference voltage in response to the output signal from the comparator cmp . in this case , if v b is less than v s , the output signal from the comparator cmp becomes high to cause the switching device sw to turn on . if v b is greater than or equal to v s the output signal from the comparator cmp becomes a low level signal to switch off the switching device sw . this action is shown in the bottom waveform of fig3 a . however , in this simple on / off switching scheme of the switch sw according to the output signal from the comparator cmp , when the electric load 4 , such as an air conditioner , is turned on at t1 as shown in fig3 a , the switch sw goes on by switching of the reference voltage v s but a long time ton is required until the voltage recovers to the reference voltage v s at time t2 . further , as shown in fig4 a , the quantity of electric power generated by the generator 3 also is rapidly increased to compensate for the rush of current upon turning on of the electric load 4 . as a result , the engine operational speed ne ( rpm ) is rapidly decreased , and the engine load is increased before a response time until the engine rotational speed ne rises to a predetermined value irrespective of the idle - up control ( idle increase ) of the engine . therefore , with conventional systems it is difficult to prevent a reduction in the engine speed under these conditions . according to the present invention and the embodiment of fig5 the controller cnt is provided with means for measuring and holding the on - time of the switching device sw by an internal counter , means for detecting whether or not a present on - time becomes longer than a previous on - time by a predetermined time , and means for temporarily forcing the switching device sw to turn off upon detection of the present on - time this forced off - time is shown as tc in fig6 a . in the case that the forced off - time tc is provided after an on - time comprising a previous on - time t ( n - 1 ) and an excess time td as shown in fig6 a for example ( these time periods equal tn which can be considered to be one type of a &# 34 ; control period &# 34 ;), a forced off switching is conducted several times during the period t &# 39 ; on , while the battery voltage v b lowers to the reference voltage vs or less , at a time t1 is recovered to the reference voltage vs again , and the on - time is variably controlled such that the on - time is increased every time the forcible on - switching is repeated ( where the forced off - time is constant ) or an off - time is variably controlled such that the forced off - time is increased every time the forced off - time is repeated , providing that each initial value of td and tc is preliminarily set . in this case , the following various techniques will provide a variable on - time or a variable off - time . fig7 is a flow chart and fig8 - 14 are subroutines used in this flow chart ( all to be described later ) for implementing the several methods described below . in the case where the on - time is to be variably controlled , a first method ( fig7 and subroutine of fig8 ) can define the present on time td as a function of the previous time td ( n - 1 ), that is , td = f [ td ( n - 1 )], and the present time td ( b in fig8 ) is set to the sum of the previous time td ( n - 1 ) ( a in fig8 ), and a constant time k1 , so that the time td may be additively increased every constant time k1 . as a second method ( fig9 ), the relation , td = f [ td ( n - 1 )] is defined , and the present time td is set to be the product of the previous time td ( n - 1 ) and a constant coefficient k1 , so that the time td may be proportionally increased at a constant rate . as a third method ( fig1 ), the present time td is defined as a function of a frequency ( n ) ( d in fig1 ) of the forced off - switching as has been conducted ; that is , td = f ( n ), and the time td is set to be the sum of the previous time td ( n - 1 ) and the product of the frequency ( n ) of the forced off - switching and a constant coefficient k2 , so that the time td may be increased at a constant rate according to the frequency ( n ) of the forced off - switching . as a fourth method ( fig1 ), the present time td is defined as a function of the previous time td ( n - 1 ) and the frequency ( n ) of the forced off - switching , that is , td = f [ td ( n - 1 )], n ], and the present time td is set to be the sum of the product of the previous time td ( n - 1 ) and the constant coefficient k1 and the product of the frequency ( n ) and the constant coefficient k2 , so that the time td may be increased at a constant rate according to ( i ) the previous time td ( n - 1 ) and ( ii ) the frequency of the forcible off - switching . in the case that the off - time is variably controlled ( instead of the on - time as described above ), a first method ( fig1 ) can define the present time tc ( e in fig1 ) as a function of the previous time tc ( n - 1 ) ( c in fig1 ), that is tc = f [ tc ( n - 1 )], and the present time tc is set to be the difference of the previous time tc ( n - 1 ) and a constant time k2 , so that the time tc may be decreased every constant time k2 . in this case , the first method is accompanied by the aforementioned method where the on - time td is additively increased every constant time k1 . as a second off - time method ( fig1 ), the present time tc is defined as a function of the frequency ( n ) of the forced off - switching as has been conducted , that is , tc = f ( n ), and the present time tc is set to the quotient of a constant coefficient k3 divided by the frequency ( n ) of the forced off - switching , so that the time tc may be decreased at a constant rate according to the frequency ( n ) of the forcible off - switching . in this case , the second method is also accompanied by the aforementione method where the on - time td is additively increased every constant time k1 . as a third off - time method ( fig1 ), the present time tc is defined as a function of the previous time tc ( n - 1 ) and the frequency ( n ) of the forced off - switching , that is , tc = f [ tc ( n - 1 ), n ] and the present time tc is set to be the difference of the product of the previous time tc ( n - 1 ) and a constant coefficient k4 and the product of the frequency ( n ) and the constant coefficient k2 , so that the present time tc may vary at a constant rate according to : ( i ) the previous time tc ( n - 1 ) and ( ii ) the frequency ( n ) of the forcible off - switching . in this case , this third method is also accompanied by the aforementioned method where the on - time td is additively increased every constant time k1 . as is discussed above , in on / off control of switching to the higher power generating level of the generator 3 , when a relatively large electric load 4 is turned on and switched to the larger generating level under a high output torque operational condition of the engine 2 , the engine 2 is little influenced by the generator load such that a rotational speed of the engine is reduced . therefore , according to one embodiment of the invention , the controller cnt has means for detecting a high output torque operational condition of the engine 2 by an operational condition signal ds , along with means for releasing the forced off - switching of the switching device sw upon detection of the high output torque . stated differently , if the output torque is high , this routine is not followed since it is not necessary . the high output torque operational condition of the engine 2 from the operational condition signal ds can be derived as follows . an operational speed ne of the engine 2 or the generator 3 is employed as the operational condition signal ds , and the actual detected rotational speed ne of the engine 2 is compared with a predetermined reference rotational speed ns ( 1000 rpm for example ). then , if ne is greater than or equal to ns , it is considered that the output torque of the engine 2 is not lower than a predetermined value . in another way , a throttle opening degree θ t ( or an accelerator opening degree ) is employed as the operational condition signal ds , and the detected throttle opening degree θ t is compared with a reference opening degree θ s ( 10 degrees for example ). then if θ t is greater than or equal to θ s , it is determined that the output torque of the engine 2 is not lower than a predetermined value . in a further way , an intake manifold pressure of the engine 2 is employed as the operational condition signal ds , and the detected engine vacuum p b is compared with a predetermined reference pressure p s ( 400 mmhg , for example ). then , if p b is greater than or equal to p s , it is determined that the output torque of the engine 2 is not lower than a predetermined value . turning now to fig7 this figure is a flow chart showing processing in the controller cnt in one embodiment . the flow chart , and subsequent subroutines , can be implemented in a microprocessor in the controller cnt in a conventional manner as will be readily apparent to those skilled in the art . in the flow chart of fig7 it is first determined whether or not an output signal from the comparator cmp is a high level h , that is , an on - command for the switching device sw . then , if the output signal is the high level h , it is determined whether or not an output torque t of the engine 2 is not lower than a fixed torque t s . if the torque t is greater than or equal to t s , the switching device sw is held in the on - condition if t is less than t s , a count value a of a td on - time counter for measuring the time td ( the td counter is in the controller cnt ) is compared with a set value b for the time td . it should be noted that this torque step ( t greater than or equal to t s ) preferably is used but is not necessary ; that is , the method can progress from h = yes to the a & gt ; b step . if a is less than or equal to b , the count value a is incremented , and it is determined whether or not a flag fa for setting the times td and tc is set . if the flag fa is set , an on - signal is fed to the switching device sw to switch the field coil fc of the generator 3 to an enhanced state . if the flag fa is not set , the flag fa is set and program goes to an operation subroutine ( discussed below ), where the times td and tc are reset . then , the on - signal is fed to the switching device sw . if a is greater than b , a content in a tc counter for measuring the time tc ( the tc counter is in the controller cnt ) is incremented to give a count value c , and the count value c is compared with a set value e for the time tc . then , if c is greater than e , a content in an n - counter for counting the frequency ( n ) of the forced off - switching ( the n - counter in th controller cnt ) is incremented , and it is determined whether or not the flag fa is set . thereafter , the same processing as described above is conducted . if c is less than or equal to e , the flag fa is reset to 0 , and an off - signal is fed to the switching device sw to hold field system of the generator 3 in an off or broken condition . on the other hand , if the output signal from the comparator cmp is a low level l , the content in the n - counter is set to zero , and the flag fa is reset to 0 . then , the off - signal is fed to the switching device sw . in the above - mentioned processing , the td counter and tc counter function as a soft timer ( flow chart cycle ) for effecting soft ( gradual ) generation of the generator 3 . further , each of a , b , and fa is initially set to zero . fig8 to 11 show the content of each operation subroutine ( the &# 34 ; subroutine &# 34 ; in fig7 ) in using the first to fourth methods in the case of variable control of the on - time as described above . fig1 to 14 show the content of each operation subroutine in using the first to third methods in the case of variable control of the off - time as described above . according to the preceding embodiment of the invention , when the battery voltage is reduced , and a switching time from the low generating level to the high generating level in the generated energy of the generator 3 is made long , the generated energy of the generator is temporarily forcibly switched to the low generating level so that the switching time to the high generating level may be gradually increased , and in association with this , a gradual increase in generation of the generator occurs . accordingly , as shown in fig1 a , even when a large electric load 4 is turned on , the generated energy of the generator 3 is prevented from being rapidly increased as conventionally occurs . as a result , the load on the engine 2 is lightened to prevent the engine rotational speed ne from being rapidly decreased . fig1 b , which was discussed earlier , is a more detailed graph of the curves of fig1 a . further , in controlling idle - up of the engine 2 , a response time t up &# 39 ;; when the engine rotational speed ne rises to a predetermined value , may be shortened thereby to attain highly responsive idle - up of the engine 2 . furthermore , especially under the high output torque operational condition of the engine 2 , the generator 3 is temporarily forcibly switched to the off level during the on - state of the field current of the generator 3 to release the gradual generation of the generator . therefore , the battery 1 may be efficiently charged without injuring the responsiveness of the engine . thus , in accordance with the invention and the foregoing embodiment , when the field current of the charging generator is controlled to be switched on and off so as to try to maintain the battery voltage equal to the reference voltage , and the generator is switched to its high generating level upon closing of a large electric load , it is possible to effectively prevent rapid application of load to the engine . turning now to the second embodiment of the concepts of the present invention , fig1 shows a generalized block diagram , and fig1 a shows a more detailed block diagram , of a hard wired system according to the present invention . in this system , the controller includes means for counting and retaining the on - period of the field coil , means for detecting that the on - period of this time is longer than that of the last time by a predetermined length of time , and means for forcibly switching the field coil current off temporarily . the system is similar to that of the previously described fig5 but the controller cnt ( shown in fig1 ) is hard wired to perform its various functions rather than program controlled . in the present embodiment , the controller cnt as shown in fig1 ( and also shown in greater detail in fig1 a ) functions to count the on - period of time of the switching element sw , detects whether the on - period of this time is longer than the on - period last time by a predetermined length of time , and forcibly turns off the switching element sw when this decision is made . thus , if the present on - time is longer than the last on - time , the switch sw is turned off . the cnt circuit of fig1 includes an on - delay timer 6 to be triggered by an on / off signal output b for the switching element sw which is supplied from output of the circuit , a one - shot timer 7 ( set time tc ) to be triggered by the timer output c of the timer 6 , and an and circuit 8 to generate a logical product of an inverted signal of the timer output d of the timer 7 , and the output a of the comparator cmp which is supplied to the input terminal of the circuit the time chart of these signals is shown in fig1 wherein l means low and h means high . with the above described structure , if , as shown in fig6 a , for example , an electrical load pulling in a large rush current is turned on at time t1 and the battery voltage v b is thereby caused to sharply drop and it takes a relatively long time t &# 39 ; on until its voltage is restored to the reference voltage v s at the time t2 , then the on - period of the switching element sw will become longer than the set time ta of the timer 6 . thus , when the time ta has elapsed after the time t1 ( e . g ., tn ), the switch sw will be forced off through operations of the timers 6 and 7 . a detailed example of a circuit for the comparator cmp , controller cnt , switching element sw , and the field coil portion fc is shown in fig1 a . fig1 b shows various waveforms and signals at different points in the circuit of fig1 a . referring again to fig6 a , various methods and systems can be used to produce forced turnin - off of switch sw within the period t &# 39 ; on from the time t1 when the battery v b drops below the reference voltage v s to the time t 2 when the voltage is restored to the reference voltage v s by the turning on of the switch sw as described below . a first method makes the times ta and tc always constant even if several forced off - times occur during the period t &# 39 ; on . this is attained simply by connecting the potential of the dividing point in the resistance type voltage divider circuit of fig1 c to each of the comparators cmp1 and cmp2 in the circuit arrangement of fig1 a as the reference voltage ( b and d ) for each comparator . a second method , while keeping the time tc constant , makes the time ta a function of the actual time t , i . e ., ta = lapse of time as long as the on command of high - level h is kept on at the output ( a ) of the comparator cmp . this is attained by employing an rc timer circuit as shown in fig1 a in which a capacitor c p is adapted to be charged at a predetermined rc time constant when the output signal of the comparator cmp is at high level h and the capacitor c p is adapted to discharge when the output signal of cmp is a low level l and by taking out the potential of the capacitor c p via an operational amplifier 10 to be supplied ( as reference b ) to the comparator cmp1 of the circuit arrangement of fig1 a as its reference voltage . in this case the reference ( d ) of the comparator cmp2 in the circuit arrangement of fig1 a is the voltage derived from the voltage dividing point in the circuit of fig1 c . when the second method is employed , it is preferable that a zener diode zd be inserted in the circuit as shown in fig1 b , thereby to provide the capacitor c p with an initial value . alternatively , in carrying out the second method , it is also possible to keep the time ta constant , not prolonged with the lapse of time and , instead , to make the time tc a function of the time t , i . e ., tc = f ( t ), whereby the time tc is allowed to be decreased as time goes by as long as the on command on high level h is provided from the output of the comparator cmp . in this case , the circuit arrangement as shown in fig1 c can be used and its output voltage ( d ) may be supplied to the comparator cmp2 in the circuit arrangement of fig1 a as its reference voltage value ( d ). also it is preferable to use the circuit arrangement of fig1 d in which a zener diode zd &# 39 ; is inserted for providing the capacitor c &# 39 ; p with an initial value . in a third method both the times ta and tc are made to become functions of the battery voltage v b , i . e . ta = tc = f ( v b ), and thus , the times ta and tc vary as the battery voltage v b varies in such a way that times ta and tc are shortened as the battery voltage v b drops . in this case , a comparator cmp 3 as shown in fig2 is used which makes the reference voltage ( b or d ) variable in response to the comparison output between the battery voltage v b and the reference voltage . its output may be supplied to either of the comparators cpm1 and cpm2 in the circuit arrangement of fig1 a as its reference voltage . in practicing the third method , it is also possible , while keeping the time ta constant , to make only the time tc variable according to the voltage v b or , it is also possible , while keeping the time tc constant , to make only the time ta variable according to the battery voltage v b . a fourth method is such that , while the time ta is kept constant , the time tc is made variable as a function of the number of times the forced turning off of switch sw occurs , i . e ., i . e . tc = f ( n ), and the time tc is adapted to be uniformly prolonged with an increase of the number of repetitions of the on / off switching . in this case , a circuit as shown in fig2 a can be employed which forms a charging circuit to charge the capacitor ct as long as the output ( a ) from the comparator cpm remains on at the high level h and forms a discharging circuit for the capacitor ct having a predetermined time constant when the switching element sw is turned off while the output signal from the comparator cpm is held at the high h level . the potential of the capacitor ct may be taken out through an operational amplifier 10 and supplied ( at d ) to the comparator cpm 2 in the circuit arrangement of fig1 a as its reference voltage . a fifth method is such that , when the on time ta is made variable with the lapse of time t as in the second method , the time tc is further made variable as a function of the time ta , i . e ., tc = f ( ta ), and thus , the time for the forced turning off , tc , is made variable according to the preceding time ta , so that the time tc becomes shorter the longer the time ta becomes in the present case , a circuit arrangement as shown in fig2 b can be employed in which a charging circuit with a presetermined time constant for the capacitor c &# 39 ; p is formed when the output signal from the comparator cmp1 in the circuit arrangement of fig1 a is a low l level as long as the output signal of the comparator cpm is held at a high h level , and a discharging circuit with a predetermined time constant for the capacitor c &# 39 ; p is formed when the output signal of the comparator cmp1 is switched to the high h level and for which a circuit is provided forcedly to reset the capacitor c &# 39 ; p when the switching element sw is turned off . the potential of capacitor c &# 39 ; p may be taken out through an operational amplifier and supplied ( at d ) to the comparator cmp2 in the circuit arrangement of fig1 a as its reference voltage value . in the described manner , as the battery voltage drops and the period of time during which the field coil current in the generator 3 is held on becomes longer , the system of the present invention causes the field coil current in the generator to be forcedly cut off temporarily to gradually prolong the period during which the generator is switched to the high power generation mode and thereby to allow the generator to perform soft or gradual generation . therefore , as shown in fig1 a and 15b , the usual sharp increase of the generated power quantity by the generator 3 can be eliminated even if a larger electrical load 4 is switched on . thus , the load on the engine becomes lighter and the sudden decrease in the number of revolutions ne of the engine is reduced . also , when idle up control of the engine occurs ( that is , when fuel is increased to bring the idle back up ), the response time t &# 39 ; up for the number of revolutions of the engine to rise to a predetermined level can be shortened and idle up of the engine with good response can be achieved . another alternative embodiment is shown in fig2 a - 22f . these figures show a system wherein the reference voltage on the comparator cmp is switched between the high and low voltage levels ( e . g . 14 . 5 v and 12 . 5 v ) so that the reference voltage for the comparator is set at the high or low voltage levels according to electrical load conditions and engine operating conditions . this system , as was the case discussed previously , includes means for detecting that the on - state of the field coil current for the generator will continue for a predetermined first period of time , includes means for forcibly switching the field coil current off for a predetermined second period of time when the foregoing protection is made , and includes means for varying the first period of time according to the state ( high or low ) of the reference voltage . turning now to fig2 a , this circuit or system includes a comparator ( cmp ) portion labelled a , including a comparator cmp1 for comparing a terminal voltage v b of the battery 1 with a reference voltage v s1 which is set at a low voltage ( for example , 12 . 5 v ), a comparator cmp2 for comparing the battery voltage v b with a reference voltage v s2 which is set at a high voltage ( for example , 14 . 5 v ), and an and gate g1 implementing the logical and operation over an inverted signal ( cs ) of a control signal cs which is the switching signal for the generator 3 for switching between the high powe generation level and the low power generation level and the output signal of the comparator cmp1 . the voltage levels v sl and v s2 can be considered to be like the solid line v s in fig6 a and the dashed line above v s in fig6 a respectively . the circuit further includes an and gate g2 implementing the logical and operation over the control signal cs and the output signal of the comparator cmp2 , and an or gate g3 implementing the or operation over the outputs of the and gates g1 and g2 , and a controller ( cnt ) portion b responsive to the output signal of the comparator a for causing the switching element sw , which controls electric current flowing through the field coil fc in the generator 3 , to switch on and off . thus , the control signal from the controller b is an on / off signal for the switching element sw . with the structure of the system as described above , if the battery voltage v b varies as indicated in fig3 a , for example , then in the case of the prior art , the controller b reads the output signal then output from the comparator a and causes , under its control , the switching element sw to properly switch on and off so as to hold the battery voltage v b at a predetermined reference voltage v s . referring to the comparator portion a of fig2 a , if the control signal cs is a low level l which is the signal for switching to the low power generation level , the low reference voltage v s1 on the comparator cmp1 is set in the comparator , and if the control signal cs is a high level h which is the signal for switching to the high power generation level , the high reference voltage v s2 on the comparator cmp2 is set . the circuit a is such that , if v b & lt ; v s1 or v s2 , the output signal of the comparator goes to the high level h and issues a command to the controller b for making or energizing the field coil fc , and if v b is greater than or equal to v s1 or v s2 , the output signal of the comparator a becomes the low level l and issues a break command for opening or deenergizing the field coil . however , when control is performed with such a simple arrangement to cause the switching element sw to turn on / off just according to the output signal of the comparator a , if a large electrical load 4 , such as an air conditioner , is turned on at the time t1 when the switching element sw is in the off state and the generator 3 is in the low power generation mode as shown in fig3 a , then , since the electrical load becomes larger and the generator 3 is switched to the high power generation mode , it takes a long time ton for the battery voltage v b to reach the reference voltage v s2 at the time t2 . at this time , as shown in fig4 a , the generated power quantity of the generator 3 abruptly increases according to the rush of current flowing into the electrical load 4 and as a result the engine revolutions ne decrease sharply . in the case idle up control of the engine 2 is made , the response time tup until the engine revolutions rise to a predetrmined level becomes considerably long . since , specifically , setting to the high reference voltage v s2 is made in the comparator a at that time , the variation in the load exerted on the engine 2 becomes greater . accordingly , the controller b in the present embodiment ( fig2 a ) is provided with means for detecting that the on state of the switching element sw has continued for a predetermined period of time , means to forcedly turn off the switching element sw temporarily when the above detection is made , and means for varying the above mentioned predeterined period of time and the forced turning off period of sw according to the set state in the comparator a of the reference voltage to be switched between the high voltage level and the low voltage level . fig1 which was discussed earlier shows an example of the structure of the controller b used in this embodiment also , but the detailed circuit is different from those previously shown and described . this new circuit is shown in fig2 b , along with the circuits of fig2 c - f which provide appropriate signals . referring again to fig6 a , various methds are implemented by the circuits of fig2 b - f to produce the forced turning off of sw by means of the timers whose timer times are ta and tc within the period ton from the time t1 when the battery voltage v b is lowered below the reference voltage v s1 to time t 2 when the voltage reaches the reference voltage v s2 . the first method is such that the time tc is made constant , and when the on command for the switchng element sw is output from the comparator a , the time ta is adapted to be shortened as long as the high reference voltage v s2 is set in the comparator a , whereby the ratio of the forced off period in the total period is made larger to suppress the power generation by the generator 3 . the implementation of this method is by the circuit of fig2 c ( with the circuit of fig2 b ). if the output signal s1 of the comparator a supplied to the input terminal in of the controller b ( fig2 a ) becomes the low level l , the capacitor c p ( fig2 c ) is brought to a discharged state , and if it becomes the high level h , this capacitor is brought to a state to be gradually charged at the time constant determined by r p and c p , but when the inverted signal of the control signal cs , which is supplied to the sg terminal of the controller b is at the low level l , the charging voltage starts virtually at ground potential , and when the cs signal is at the high level h , it is well remedied by such arrangement that the potential of the capacitor c 2 , the charging on which starts at the initial voltage determined by the zener voltage of the zener diode zd , is taken 7out or discharged through the operational amplifier 10 and supplied ( at a ) to the comparator cmp3 in the circuit arrangement in fig2 b as the reference voltage therefor . in the present case , the reference voltage for the comparator cmp4 in the circuit arrangement in fig2 b is provided from the voltage dividing point as shown in fig1 c . the second method is such that the time ta is made constant , and when an on command for the switching element sw is output from the comparator a , the time tc is adapted to be prolonged as long as the high reference voltage v s2 is set in the comparator a , and thus the ratio of the forced off period in the total period is made larger and the power generation quantity of the generator 3 is thereby suppressed . this second method is implemented by the circuit of fig2 d . when the output signal s1 of the comparator a input to the input terminal in of the controller b becomes the low level l , the capacitor c &# 39 ; p in fig2 d supplies the initial voltage to be determined by existence or nonexistence of the voltage drop given by the zener voltage of the zener diode zd supplied to the capacitor c &# 39 ; p , and as the signal s1 changes to the high level h , the capacitor c p is brought to a state to gradually discharge at the time constant determined by the capacitance c p and the resistance r &# 39 ; p . the voltage drop due to the zener diode zd becomes nil when the inverted signal cs of the control signal cs , which is input to the terminal sg of the controller b , becomes the low level l , and when the same becomes the high level h , it becomes existent . in this case , the potential at the voltage dividing point in the circuit of fig1 c can be supplied to the comparator cmp3 in the circuit arrangement in fig2 b as the reference voltage therefor . the third method is such that the time tc is made constant , and at the time when an on command for the switching element sw is output from the comparator a , the time ta is adapted to be shortened when switching from the low reference voltage v s2 in the comparator a . in the method as shown in fig2 e , when the output signal s1 of the comparator a to be supplied to the input terminal in of the controller b is at the low level l , the capacitor c p is supplied with the initial voltage determined by the zener voltage of the zener diode zd except when the inverted signal cs of te control signal cs is switched from the high level h to the low level l , and the capacitor is brought to the state to discharge at the time constant determined by r p and c p when the output signal sl becomes the high level h . on the other hand , when the signal cs is switched from the high level h to the low level l , the initial voltage for the capacitor c p is virtually lowered to ground potential . the potential of the capacitor c p can be taken out through the operational amplifier 10 and applied to the comparator cmp3 as the reference voltage therefor . the fourth method is such that the time ta is made constant , and at the time when an on command for the switching element sw is output from the comparator a , the time tc is adapted to be prolonged when switching from the low reference voltage v s1 to the high reference voltage v s2 in the comparator a . in this fourth method , as shown in fig2 f , when the output signal s1 of the comparator a which is input to the input terminal in of the controller b is at the low level l , the capacitor c &# 39 ; p supplies the initial voltage determined by the zener voltage of the zener diode zd to the capacitor c &# 39 ; p except when the inverted signal cs of the control signal cs is changed over , and when the signal s1 becomes the high level h , the capacitor is brought to the state to gradually discharge at the time constant determined by c p and r p . on the other hand , when the signal cs is switched from the high level h to the low level l , the initial voltage of c p is virtually lowered to + v cc . the potential on the capacitor c p of the rc timer unit can be taken out through the operational amplifier and applied to the comparator cmp4 in the circuit arrangement in fig2 b as the reference voltage ( b ) therefor . in the described manner , as the battery voltage drops and the period of time during which the field coil current of the battery 3 is held on becomes longer , the system of the present embodiment causes the power generation quantity of the generator 3 to be temporarily suppressed by force , and soft or gradual generation of the generator 3 may be performed avoiding exertion of an abrupt load on the engine . therefore , as shown in fig1 a , the sharp increase of the generated quantity by the generator 3 can be eliminated even if a large electrical load 4 is added . therefore , as shown in fig1 a , the sharp increase of the generated quantity by the generator 3 can be eliminated even if a large electrical load 4 is added . thus , the load on the engine becomes lighter and the sudden decrease in the number of revolutions ne of the engine is avoided and when idle up control of the engine occurs , the response time tup for the number of revolutions of the engine to rise to a predetermined level can be shortened and an idle up of the engine with good response can be accomplished . therefore , a significant advantage is obtained therefrom that the engine is effectively prevented from being subjected to an abrupt burden when the generator is switched to the high power generation made upon turning on of a large electrical load . the term &# 34 ; control period &# 34 ; is used herein to include the period being sensed , such as a period comprising the last on period ( t ( n - 1 ) in fig6 a ) plus the predetermined period or time ( such as td in fig6 a ), or a given or predetermined period of time alone , and / or other variations as described herein , or the like . while several embodiments of the present invention have been shown and described , various changes and modifications can be made without departing from the present concepts . | 7 |
the polyisocyanate used in the present invention may be any organic polyisocyanate having two or more isocyanate groups in the molecule , including diphenylmethane diisocyanate , toluene diisocyanate , and hexamethylene diisocyanate . the term of &# 34 ; organic polyisocyanate &# 34 ; herein includes unmodified organic polyisocyanates and modified organic polyisocyanates . a preferred organic polyisocyanate in the present invention is a bifunctional or more functional polymethylene polyphenylene polyisocyanate produced by phosgenation of an aniline / formaldehyde condensate ( hereinafter referred to as &# 34 ; polymeric mdi &# 34 ;): more preferred is a water - dispersible polymeric mdi having water dispersibility . it is well - known that the water - dispersible polymeric mdi is prepared , for example , by reacting a polymeric mdi with a monofunctional hydroxyl - containing substance such as a hydrophilic alkoxypolyalkylene glycol having a number - average molecular weight ranging from about 250 to about 4000 . japanese patent publication no . 2 - 58287 discloses such water - dispersible polymeric mdi which is commercially available as &# 34 ; wood cure - 300 &# 34 ; nco - content = 28 . 0 % to 30 . 5 % by weight : by nippon polyurethane industry co ., ltd .!. the organic polyisocyanate may be an isocyanate - terminated prepolymer derived by reaction of an organic polyisocyanate with a polyol . the preferable isocyanate - terminated prepolymer is prepared by the reaction of mdi and / or polymeric mdi with polyols having a number - average molecular weight ranging from 500 to 3000 and containing hydrophilic groups . these polyols include a polyether - polyol containing 50 mole % or more of ethylene oxide units ; a polyester -, polycarbonate - and polyether - polyol having anionic - polar groups such as sulfonates (-- so 3 m wherein m is an alkali metal , quaternary organic amine and the like ), carboxylates (-- coom wherein m is an alkali methal , quaternary organic amine and the like ) and the like . the preferable isocyanate - terminatated prepolymer may be a reaction product having an nco - content of 20 % to 30 % by weight , which is obtained by the reaction of mdi and / or polymeric mdi and the polyether - polyols containing 50 mole % or more of ethylene oxide units . the aqueous emulsion of a wax used in the present invention is an aqueous emulsion of a known wax - type releasing agent of a melting point ranging from 50 ° c . to 160 ° c ., including natural waxes such as montan wax , carnauba wax , rice wax , and paraffin wax ; synthetic waxes such as polyethylene wax , montan wax derivatives , paraffin wax derivatives , hardened castor oil , and stearic amide . a conventional emulsifier is preferably used for the emulsification . the solid content of the emulsion is preferably in the range of from 10 % to 50 % by weight . the organic phosphate ester derivative used in the present invention includes well - known water - soluble phosphate ester type internal releasing agents such as zelec un , a non - neutral phosphate salt alcohol produced by dupont co . ; and mold wiz int - 1858 and int - 1856 , a phosphate ester type internal releasing agent produced by axel plastics research laboratories co . a higher mold - releasability and more satisfactory properties of the board are achievable by use of a phosphate produced by neutralization with an alkanolamine of partial phosphate ester produced from phosphoric acid and an aliphatic alcohol . the aliphatic alcohol used may have 12 to 20 carbon atoms , including stearyl alcohol , and oleyl alcohol . the esterification of the phosphoric acid is preferably partial esterification to obtain a monoester , di - ester , or mixture thereof . the partial phosphate ester is neutralized with an alkanolamine to use as a component of the composition according to the present invention . the neutralization need not be precise , and the stoichiometric ratio is in the range of from 0 . 3 to 3 . 0 . incomplete nuetralization by alkanoamine or the presence of excess of alkanolamine is tolerated . the alkanolamine for the neutralization includes monoethanolamine , diethanolamine , and triethanolamine . the organic phosphate ester derivative may be a solution in water or another solvent . the lignocellulose type compression molded article is produced by spraying of the polyisocyanate composition to the lignocellulose type material and thermo - compressing the material . the molding can be conducted under any particle board molding conditions . the organic polyisocyanate , the aqueous wax emulsion , and the phosphate ester derivative may be sprayed by use of a mixture formed immediately before the application , or separately onto the lignocellulose type material . water may be optionally used in addition to the above three components . the application of the components to the lignocellulose type material is carried out by uniformly spraying a mixture of the components ( a ), ( b ), ( c ) and optionally ( d ) to the lignocellulose type material in a batch mixer or continuous mixer . alternatively , the components ( a ), ( b ), ( c ) and ( d ) are separately sprayed on the ligunocellulose type material in a batch mixer or continuous mixer in any order . it is preferable to use the continuous mixture . on the preparation of the mixture , the components ( a ), ( b ), ( c ) and ( d ) may be mixed in any order . however , it is preferable the component ( a ) is finally added . and it is preferable that the components ( b ) and ( c ) are previously mixed . it is preferable to use a mixture of the components ( a ), ( b ), ( c ) and ( d ). in production in a continuous line , the aqueous wax emulsion and the phosphate ester derivative are preferably mixed before the application . this preliminarily mixture is further mixed continuously with water by a static mixer followed by mixing with the organic polyisocyanate . the resulting mixture is sprayed onto the lignocellulose type material . u . s . pat . nos . 5 , 093 , 058 , 5 , 188 , 785 and 5 , 200 , 267 disclose continuous processes and apparatus for the process . the amounts of the components relative to the lignocellulose type material are respectively in the range of 5 to 20 parts by weight of the organic polyisocyanate , 0 . 5 to 4 . 0 parts by weight of solid matter of the aqueous wax emulsion , and 0 . 1 to 2 . 0 parts by weight of solid matter of the phosphate ester derivative based on 100 parts of the dry lignocellulose type material . it is preferable to add water in order to keep a moisture content of mat prior to the compression at a constant value . the amount of water to be added is calculated from the difference between the amount of water required to a set value of moisture content of mat and an amount of water contained in the lignocellulose type material and emulsions . the moisture content of mat ranges 5 to 35 % by weight , preferably 5 to 30 % by weight . by the process of the present invention , the adhesion of the material to the metal surface is prevented in thermo - compression molding of a lignocellulose type material such as wood chips , and wood fibers . furthermore , the wax which is solid at an ordinary temperature can be handled in a uniform liquid emulsion state , advantageously . the present invention is described by reference to examples without limiting the invention . in examples , the units , &# 34 ; parts &# 34 ; and &# 34 ;%&# 34 ;, are based on weight respectively . a preliminary mixture was prepared by mixing , by a laboratory mixer , 16 . 8 g of a montan wax emulsion , &# 34 ; mn - 30 &# 34 ; ( solid content : 30 %, orion kasei k . k . ); 1 g of a phosphate ester derivative , &# 34 ; mold wiz int - 1858 &# 34 ; ( solid content : 100 %: axel plastics research laboratories co . ); and 35 . 9 g of distilled water . to the resulting preliminary mixture 20 . 1 g of water - emulsifiable mdi , &# 34 ; wood cure - 300 &# 34 ; ( nippon polyurethane industry co ., ltd .) was added , and the composition a was obtained by thorough mixing , by a laboratory mixer . to 100 parts of dried chips , 22 . 0 parts of the above composition a was blended to be thermo - compression molded under the molding conditions below . the mold - releasability was checked by placing the iron panels &# 34 ; spcc - sb &# 34 ; ( nippon test panel k . k .) on the both surfaces of the board . as the results , the compression molded board could readily be released from the iron plates without adhesion of the chip to the iron plate . this board had a flexural strength of 288 kg / cm 2 according to jis a 5908 , and showed a thickness increase ratio of 6 . 2 % on absorption of water according to jis a 5901 . a preliminary mixture was prepared by mixing , by a laboratory mixer , 13 . 3 g of a carnauba wax emulsion , &# 34 ; bn - 50 &# 34 ; ( solid content : 50 %, orion kasei k . k . ); 1 . 0 g of a phosphate ester derivative , &# 34 ; mold wiz int - 1858 &# 34 ; ( solid content : 100 %: axel plastics research laboratories co . ); and 41 . 0 g of distilled water . to the resulting preliminary mixture 20 . 0 g of water - emulsifiable mid &# 34 ; wood cure - 300 &# 34 ; ( nippon polyurethane industry co ., ltd .) was added , and the composition b was obtained by thorough mixing , by laboratory mixer . to 100 parts of dried chips , 22 . 6 parts of the above composition b was blended to be thermo - compression molded under the same molded under the same molding conditions as in example 1 . the compression molded board could be released readily from the iron plates without adhesion of the chip to the iron plate . this board had a flexural strength of 288 kg / cm 2 , and showed a thickness increase ratio of 6 . 4 % on absorption of water . the thermo - compression molding was conducted in the same manner as in example 1 except that the water - emulsifiable mdi was replaced by a polymeric mdi , &# 34 ; millionate mr300 &# 34 ; ( nippon polyurethane industry co . ltd .). the compression molded board could be released readily from the iron plates without adhesion of the chip to the iron plate . this board had a flexural strength of 287 kg / cm 2 , and showed a thickness increase ratio of 6 . 2 % on absorption of water . the thermo - compression molding was conducted in the same manner as in example 1 except that the phosphate ester derivative was replaced by a non - neutral phosphate salt alcohol , &# 34 ; zelec un &# 34 ; ( solid content : 100 %; dupont co .). the compression molded board could be released readily from the iron plates without adhesion of the chip to the iron plate . this board had a flexural strength of 290 kg / cm 2 , and showed a thickness increase ratio of 6 . 3 % on absorption of water . the thermo - compression molding was conducted in the same manner as in example 1 except that the phosphate ester derivative was replaced by the one prepared by neutralizing 100 parts by weight of dioleyl phosphate with 25 parts by weight of triethanolamine ( mole ratio = 1 : 1 ). the compression molded board could be released readily from the iron plates without adhesion of the chip to the iron plate . this board had a flexural strength of 320 kg / cm 2 , and showed a thickness increase ratio of 5 . 0 % on absorption of water . a preliminary mixture was prepared by mixing , by a laboratory mixer , 33 . 2 g of a montan wax emulsion , &# 34 ; mn - 30 &# 34 ; ( solid content : 30 %, orion kasei k . k . ); and 24 . 5 g of distilled water . to the resulting preliminary mixture 19 . 9 g of water - emulsifiable mid &# 34 ; wood cure - 300 &# 34 ; ( nippon polyurethane industry co ., ltd .) was added , and the composition f was obtained by thorough mixing , by laboratory mixer . to 100 parts of dried chips , 23 . 4 parts of the above composition f was blended to be thermo - compression molded under the same molded under the same molding conditions as in example 1 . the composition molded board could not be pulled apart from the iron plates owing to firm adhesion to the iron plates . a preliminary mixture was prepared by mixing , by a laboratory mixer , 19 . 9 g of a carnauba wax emulsion , &# 34 ; bn - 50 &# 34 ; ( solid content : 50 %, orion kasei k . k . ); and 37 . 8 g of distilled water . to the resulting preliminary mixture 19 . 9 g of water - emulsifiable mid &# 34 ; wood cure - 300 &# 34 ; ( nippon polyurethane industry co ., ltd .) was added , and the composition g was obtained by thorough mixing , by laboratory mixer . to 100 parts of dried chips , 23 . 4 parts of the composition g was the blended . the mixture was thermo - compression molded under the same molding conditions as in example 1 . the compression molded board could not be pulled apart from the iron plates owing to firm adhesion to the iron plates . a preliminary mixture was prepared by mixing , by a laboratory mixer , 1 . 0 g of a phosphate ester derivative , &# 34 ; mold wiz int - 1858 &# 34 ; ( solid content : 100 %: axel plastics research laboratories co . ); and 47 . 5 g of distilled water . to the resulting preliminary mixture 20 . 4 g of water - emulsifiable mid &# 34 ; wood cure - 300 &# 34 ; ( nippon polyurethane industry co ., ltd .) was added , and the composition h was obtained by thorough mixing , by laboratory mixer . to 100 parts of dried chips , 20 . 3 parts of the above composition h was blended . the mixture was thermo - compression molded under the same molding conditions as in example 1 . the compression molded board could not be pulled apart from the iron plates owing to firm adhesion to the iron plates . a preliminary mixture was prepared by mixing , by a laboratory mixer , 3 . 4 g of a phosphate ester derivative , &# 34 ; mold wiz int - 1858 &# 34 ; ( solid content : 100 %: axel plastics research laboratories co . ); and 47 . 6 g of distilled water . to the resulting preliminary mixture 20 . 4 g of water - emulsifiable mid &# 34 ; wood cure - 300 &# 34 ; ( nippon polyurethane industry co ., ltd .) was added , and the composition j was obtained by thorough mixing , by laboratory mixer . to 100 parts of dried chips , 21 . 1 parts of the above composition j was added . the mixture was thermo - compression molded under the same molded under the same molding conditions as in example 1 . the thermo - compression molded board could be released readily from the iron plates without adhesion of the chip to the iron plate . this board had a flexural strength of 272 kg / cm 2 , and showed a thickness increase ratio of 18 . 3 % on absorption of water . the water resistance of the board was significantly lower than that of examples 1 to 3 . in 50 - ml sample bottle , were placed 7 . 5 g of montan wax of a melting point of 75 ° c . to 85 ° c ., and 12 . 5 g of 2 - ethylhexyl diphenylphosphate , and were heated up to 95 ° c . to form a solution . after formation of a homogeneous solution at this temperature , the heating was stopped , and the solution was left standing to cool spontaneously . at about 50 ° c . to 60 ° c ., the solution lost the fluidity . at ordinary temperature , the solution had no fluidity at all . | 2 |
the pruning methods according to the invention provide better results with respect to conventional techniques , for every s - random type interleaver . however , these methods provide optimal results if applied to s - random interleavers obtained with a progressive technique of permutation generation invented by the same inventors of this application , which will be now presented herebelow . in european patent application ep 1 257 064 a there was proposed an algorithm for the generation of s - random interleavers or , better stated , interleaver permutations , which , starting from a good s - random interleaver permutation of size k and spread s , creates , by extension , a larger or longer interleaver permutation , say of size n , with the same spread properties of the starting interleaver permutation . although this may be sufficiently acceptable for a small range of interleaver sizes , this constraint may lead to poor results if one has to construct interleavers in a wide range of sizes , as this leads to poor spreading properties of the larger interleavers . the incremental technique which will be now presented overcomes this limitation . while the algorithm according to the prior art in fact extracts at random an integer representing the position of the new element which is added to the interleaver , the technique which will be now described picks a number from a subset of positions that allows to improve the spread properties . if we start from a k - sized interleaver with a spread s , the next step in the extension process is to add new positions until we reach a spread s + 1 . thus we analyze the permutation and see which pairs of positions [ i ; j ] and [ π ( i ); π ( j )] correspond to the violations that do not permit to reach a spread equal to s + 1 . one easy way to overcome these violations is to choose an element with π ( k + 1 )= ψ , ψ ∈[ min ( π ( i ), π ( j ))+ 1 ; max ( π ( i ), π ( j ))], and then update all previous k elements or positions of the interleaver by incrementing of one all those greater than or equal to ψ . to eliminate or break , at each step , the maximum number of violations , an interval vector a is created , which contains all position pairs causing violations of the spread properties . each pair defines an interval , whose internal numbers are suitable for extraction ; then we can use the vector a to build a second vector , defined as the position vector b , which is proportional to the attitude of each position to break spread violations . the vector b is then sorted in descending order and the first element that does not introduce new spread violations is extracted . this technique permits to improve the spread properties in a very fast way , and to construct interleavers with large sizes having very good spreading properties with a computational complexity that may be competitive even with the direct s - random interleaver generation . the improved method for the construction of interleavers described above can be performed essentially by the algorithm disclosed herebelow in a pseudo - code formalism : starting from an interleaver permutation π having a size or length k and a spread s in : build the interval vector a with the ( s + 1 ) spread violations ; the intervals are [ min ( π ( i ), π ( j ))+ 1 ; max ( π ( i ), π ( j ))] build the position vector b pick ψ from b , such that it does not introduce new spread violations set π ( dim + 1 )= ψ ∀ k ≦ dim , if π ( k )≧ ψ , set π ( k )= π ( k )+ 1 obtain the inverse interleaver π − 1 build the interval vector a with the ( s + 1 ) spread violations ; the intervals are [ min ( i , j )+ 1 ; max ( i , j )] build the position vector b pick ψ from b , such that it does not introduce new spread violations set π − 1 ( dim + 1 )= ψ ∀ k ≦ dim , if π − 1 ( k )≧ ψ , set π − 1 ( k )= π − 1 ( k )+ 1 obtain the interleaver π set dim = dim + 1 if there are no more ( s + 1 ) spread violations set s = s + 1 the algorithm above allows to yield a wide range of interleavers with different sizes with good spreading properties . when the system at hand needs to obtain one of them “ on the fly ”, an easily implementable pruning algorithm is required . for instance , this means that new elements have to be inserted into the interleaver permutation in a way that allows to know their position and discard them very easily . according to the prior method disclosed in ep 1 257 064 a , this can be obtained for instance starting from a created n - sized interleaver and removing its last n - k positions . this , in turn , requires to use the elements of the position vector b to choose the elements π ( k + i ), i = 1 , . . . , n − k . that is in fact the pruning rule suggested in ep 1 257 064 a , and it complies very well with the therein aimed criterion of preserving for the extended interleavers the same spread properties of the shortest interleaver . on the contrary , it has serious drawbacks in other cases and in particular when applied to interleavers having an interleaver permutation or an interleaver law obtained by means of the innovative technique described above or the algorithm presented above . as it will be readily apparent form the following , the pruning method according to the present invention allows to obtain , starting from an initial s - random interleaver permutation stored in memory means and having a size n , i . e . formed of n elements , a final s - random permutation having a smaller size k & lt ; n , i . e . formed of k elements , by means of successive pruning operations or steps which , starting from the initial permutation , yield the final permutation through an iterative process carried out by means of electronic processing means with memory . in successive steps of said iterative process elements selected on the basis of predetermined criteria are discarded from the initial permutation . in particular , in the method according to the invention the final permutation is generated by utilizing a reference vector having a size equal to that of the initial permutation and thus comprising n elements ; said reference vector being generated by said processing means in such a way that at each pruning step if the element discarded from the initial permutation has been eliminated on the basis of a predetermined criterion , one element of said reference vector is generated such that its value and its position in the reference vector are indicative of the value of the elements discarded from the initial permutation . the method according to the invention can be performed in different variants , which will be described in a more detailed way in the following , to reduce the size of a large initial interleaver , named afterwards π 0 ( x ), that is stored in a read - only memory ( rom ), to obtain a shorter one , named π n ( x ), that is stored in a reserved random - access memory ( ram ) area . a good number of methods according to the invention are in general composed by three tasks : identification of the elements to be pruned , re - normalization , namely re - definition ( scaling ) of the value of part of the valid or surviving elements , and re - compacting of the interleaver . the basic pruning method according to the invention as defined above can be carried out for instance by means of the apparatus shown in fig1 , which comprises a microprocessor 1 with associated memory devices 2 and 3 . the memory devices indicated 2 are of the read - only ( rom ) kind and serve to store the n - sized initial or start interleaver π 0 and , possibly , its inverse π 0 − 1 , whereas the memory devices 3 can be either of the read - only ( rom ) type or of the random - access ( ram ) type and serve to store the reference or auxiliary vector ( s ), described in the following , and the final interleaver π n . the microprocessor 1 is coupled to random - access memory ( ram ) devices 4 through an address line 5 . said memory devices are used for implementing the algorithm for decoding the turbo - codes . said algorithm is based on the iterative performance of a variant of the so - called bcjr algorithm by so - called siso ( soft input soft output ) units : in the case of only two constituent convolutional codes , each iteration is composed of two half - iterations , in the first one of which the data are written and read in natural order from memory 4 , and in the second one of which data are written and read in the order determined by the interleaver permutation or interleaver law . in the pruning methods according to the invention , in those steps which we conventionally define as “ odd ” steps , i . e . the steps at which a pruning operation is made onto a permutation having an odd size , the elements of the interleaver which have the highest values are discarded , whereas in those steps which we conventionally define as “ even ” steps , i . e . the steps in which a pruning operation is made onto an interleaver permutation having an even size , the elements having the highest position indices , namely the last elements of the permutation , are eliminated . for a better understanding of the following remarks reference can be made to fig2 which gives a graphic representation of an initial interleaver permutation , indicated π , formed of 25 elements , and , therebelow , a representation of the corresponding inverse permutation π − 1 . at the end of the pruning process of the invention , as shown in fig2 , all the values discarded in the even steps and some of those deleted in the odd steps will form an end or tail group of consecutive deleted elements , while the other eliminated values will be scattered on the rest of the permutation . the pruned elements are distributed in a similar pattern also in the inverse interleaver π − 1 . the thresholds which separate the end or tail groups of consecutive discarded elements in the permutation π and in the inverse permutation π − 1 , respectively , are denoted as l 1 and l 2 . in various pruning methods according to the invention the main source of complexity lies in the re - normalization and re - compacting operations performed in the innermost loops . it is possible to decrease the number of required operations avoiding to perform the above - mentioned operations for each deleted element . this can be done by keeping track of the deleted elements updating the thresholds l 1 and l 2 , and building a reference or flag vector v f , which has been graphically represented by way of example in fig2 . the flag vector v f has a size n and comprises n binary elements or flags assuming each a predetermined value or state ( set to “ 1 ”, for instance ) when their position corresponds to the value of an element discarded from the initial permutation π as being placed at the last position of a permutation of odd size . such ‘ set ’ elements or flags of vector v f have been indicated “ x ” in the representation of fig2 . the values of the thresholds l 1 and l 2 , and the flag vector v f , obtained in a first phase of the pruning method , can be conveniently used in a second and a third phase for performing the re - normalisation of surviving or remaining elements of the permutation . this allows to lower significantly the overall computational complexity . in the following some techniques will be described , which rely on these principles , but differing in the way they exploit the flag vector v f . a preliminary remark is necessary to analyze the average complexity of said techniques : when pruning an n - sized interleaver to obtain a k - sized one , the threshold l 1 and l 2 can be approximated as : a first embodiment of the general method of the invention , that we will call now onward “ algorithm a ”, is composed essentially of three main cycles . in the first cycle , the flag vector v f is computed and the thresholds l 1 and l 2 are updated : set dim = n − 1 , l 1 = l 2 = n loop until dim & lt ; k if dim is even : set l 1 − l 1 − 1 loop until π 0 ( l 1 )& lt ; l 2 set l 1 = l 1 − 1 end of loop set v f ( π 0 ( li ))= 1 set l 2 = l 2 − 1 loop until v f ( l 2 )= 0 set l 2 = l 2 − 1 end of loop in the second cycle , after the permutation π 0 is copied to π n , the positions of the latter vector are re - normalized with the help of the de - interleaver π 0 − 1 and of the flag vector v f . copy the first l 1 positions of π 0 to π n set the number of positions to be discarded dp = l 2 − k and i = l 2 − 1 loop until dp = 0 if v f ( i ) is set , set dp = dp − 1 or else decrease π n ( π 0 − 1 ( i )) by dp set i = i − 1 end of loop scanning the interleaver as described here is equal to scan it starting from the elements with the highest values and ending with the elements with the lower values . finally , in the third cycle , the permutation π n is re - compacted by eliminating all the elements whose value exceeds k , or , equivalently , l 2 : set cnt = 0 and i = 0 loop until i = l 1 if π n ( i )& lt ; l 2 set π n ( cnt )= π n ( i ) and cnt = cnt + 1 set i = i + 1 end of loop the complexity of the algorithm a can as a whole be approximated as : a variant of the basic method of the invention , defined “ algorithm b ” in the following , applies the same principles of the previous one ( algorithm a ), but gets rid of the de - interleaver . the re - normalization step is performed with relatively low complexity , exploiting the computations already performed for the closest previous elements . in fact , the re - normalization is performed decreasing the value of the i - th element of π 0 by a number equal to the number of “ set ” flags contained in v f before the index π 0 ( i ). in this case for every of the k elements of the pruned interleaver , one should scan the flag vector v f for π 0 ( i ) positions . alternatively , if d is an integer greater than zero and lesser than n , we can find amongst the d previously updated elements the one , with index i d , such that π 0 ( i d ) is closest to π 0 ( i ). then the flag vector is to be scanned only for a number of positions equal to the difference between π 0 ( i d ) and π 0 ( i ), and decrease the current element of the number of flags in the said interval and of the difference between π 0 ( i d ) and π n ( i d ) therefore , firstly one has to obtain the thresholds l 1 and l 2 and the flag vector v f , as in the first cycle of the algorithm a , and then the first l 1 elements of π 0 , as in the second cycle of the algorithm a . then π n is re - normalized : set i = 0 loop until i = l 1 if π n ( i )& lt ; l 2 find in the d previous elements the i d - th element such that π 0 ( i d )& lt ; l 2 and that the difference δ = π 0 ( i d )− π 0 ( i ) is minimum . set n f = 0 if δ & gt ; 0 if δ & gt ; π 0 ( i ), count n f , i . e the number of flags in v f in the interval [ 0 ; π 0 ( i )] and set π n ( i )= π n ( i )− n f if δ ≦ π 0 ( i ), count n f , the number of flags in v f in the interval [ π 0 ( i ); π 0 ( i )+ δ ] and set π n ( i )= π n ( i )+ n f + π n ( i d )− π 0 ( i d ) if − δ & gt ; l 2 − π 0 ( i ), count n f , i . e . the number of flags in v f in the interval [ π 0 ( i ); l 2 ] and set π n ( i )= π n ( i )+ n f + k − l 2 if − δ ≦ l 2 − π 0 ( i ), count n f , the number of flags in v f in the interval [ π 0 ( i )+ δ ; π 0 ( i )] and set π n ( i )= π n ( i ) n f + π n ( i d )− π 0 ( i d ) finally , in the third cycle the re - compacting step is performed as already previously described . the overall complexity of this variant of the method can be approximated as : unlike algorithm a , this variant does not need the de - interleaver π 0 − 1 so a memory of 2n is required . this variant of the method according to the invention has a complexity that can be lowered to that of algorithm a by trading - off a small quantity of additional memory . in the previous variant ( algorithm b ) the re - normalization step is performed exploiting the information implicitly present in the updated values of the neighbouring elements . in this variant , defined algorithm c , we construct a small vector of ( np ) elements ( with p & lt ;& lt ; 1 ) named v p : the vector v p ( i ) contains the number of flags set in v f in the interval [ 0 ; i ( 1 +└ l 2 /( np )┘)], where └ x ┘ is the integer part of x . then the flag vector v f has to be scanned , for each of the k elements of the pruned interleaver , in the worst case for l 2 / np elements . then , as in the preceding two algorithms , we have to obtain the thresholds l 1 and l 2 and the flag vector v f and to copy to π n the first l 1 elements of π 0 . thereafter in the second cycle we construct the vector v p : set i = 0 and n f = 0 loop until i = l 2 if v f ( i )= 1 set n f = n f + 1 if ( 1 +└ l 2 /( np )┘) divides i , set v p ( i /( 1 +└ l 2 /( np )┘))= n f set i = i + 1 end of loop in the successive cycle , the vectors v p and v f are exploited to perform the re - normalization step : set i = 0 loop until i = l 1 set n f = 0 if π n ( i )& lt ; l 2 compute k = π n ( i )/( 1 +└ l 2 /( np )┘) and round it to the nearest integer m if m = np , set m = m − 1 if k ≧ m , compute the number of flags n f in v f in the interval ( m ( 1 +└ l 2 /( np )┘); π 0 ( i )) and set π n ( i )= π n ( i )− n f − v p ( m ) if k ≦ m , compute the number of flags n f in v f in the interval ( π 0 ( i ); m ( 1 +└ l 2 /( np )┘) and set π n ( i )= π n ( i )+ n f − v p ( m ) the total memory required by this algorithm amounts to ( 2 + p ) n ; it is easy to deduce from the above expression of the complexity that if p is increased , i . e . if the memory requirements grow , the complexity becomes lower . if extra cycles , i . e . operations of reading non - valid elements of the initial permutation , are tolerated , the traditional pruning method according to ep 1 257 064 a requires no beforehand computations but only to compare every element of the original interleaver with the new interleaver size . while in the first semi - iteration the siso module reads and writes data following the natural order of the addresses from the first k positions of the memory device , in the second half - iteration the data are read and written from the said memory device in the order determined by the interleaver and in that phase every element of the initial permutation greater than k is ignored . clearly , no ram is required . since the elements to be discarded are scattered on the whole length of the interleaver , in the worst case all the interleaver has to be scanned in order to perform interleaving . in a first variant of the method according to algorithm c , denoted as algorithm d , only the steps necessary to obtain l 1 , l 2 and the vector v f are performed , and , while computing v f , also the positions discarded in the odd steps are considered . thus the elements of the flag vector v f take a predetermined value ( for instance set to “ 1 ”) when their position corresponds to the value of an element discarded from the initial permutation . in the first semi - iteration the siso module reads and writes data following the natural order of the addresses avoiding the i - th position if v f ( i ) is “ flagged ”. similarly , in the second semi - iteration the data are read and written in the order of the initial permutation , avoiding the π 0 ( i )- th address if the corresponding element v f ( π 0 ( i )) is “ flagged ”. it is not necessary to scan the interleaver in its entire length , because , as previously explained , the last elements are discarded , so the number of extra - cycles is somewhat reduced , with respect to the previous case . a further variant of the method defined above as algorithm c , here denoted as algorithm e , avoids the computations each time necessary to obtain the flag vector v f , using a vector of n integers , named v aux , stored in a rom and containing the same information of v f . for each flag set to 1 , we store the step , i . e . the interleaver size or length , during which that position was flagged , so that , when writing / reading in natural ( scrambled ) order , the i - th address is discarded if v aux ( i ) is greater than k , and , similarly , when writing / reading in scrambled order , the π 0 ( i )- th address is discarded if v aux ( π 0 ( i )) is greater than k . we can now summarize the characteristics of the different pruning techniques that we have described so far . their complexity and their memory requirements are summarised in the following table . in the diagram shown in fig3 , which illustrates the frame error rate ( fer ) as a function of e b / n 0 , where e b is the energy per bit and n 0 is the spectral density of the gaussian white noise , there are compared the characteristics of two s - random interleavers having a length of 640 , obtained starting from an s - random interleaver generated by a standard technique with a length of 32768 and a spread s = 195 , with a standard pruning technique and with the new method , with an interleaver specially designed for that same length , and with the interleaver proposed by the umts standard . similarly , in fig4 there are compared the features of two s - random interleavers of length 5120 obtained starting from an s - random interleaver generated by the standard technique , with a length of 32768 and a spread s = 195 , with the standard pruning technique and the new method , with an interleaver specially designed for that length and with the interleaver proposed by the umts standard . naturally , the principle of the invention remaining the same , the form of embodiment and the particulars of construction can be widely modified with respect to what has been described and illustrated by way of non - limiting example , without departing from the scope of the invention as defined in the annexed claims . | 7 |
reference should now be made to the drawings wherein the same reference numerals are used throughout to designate the same or similar parts . it should be noted that the use of cardiopulmonary bypass , as shown in fig1 is for descriptive purposes , and should not be taken as a limitation to the use of the devices described hereinafter . it should also be noted that the term soft shell reservoir , venous bag and bag are used interchangeably . [ 0099 ] fig1 is a schematic representation of a system according to the present invention and showing the relative location of the venous reservoir in a typical cardiopulmonary bypass circuit . as shown , tubing 123 is inserted at one end by means of a cannula ( not shown ) in the vena cavae for obtaining venous blood from the heart ( not shown ) of patient 1102 . tubing 123 is coupled , as an example , to venous reservoir 1103 . the blood is drawn from venous reservoir 1103 via tube 135 by roller pump 1104 and pumped through a membrane oxygenator 1105 wherein oxygen is supplied to the blood and carbon dioxide is removed . the blood from the oxygenator is then conducted by means of tubing 157 to arterial filter 1107 and then via tubing 172 and an arterial cannula ( not shown ) back to the patient . as described in the prior art , the venous blood , here shown coming from the patient &# 39 ; s vena cavae , may contain air that must be eliminated before it is pumped back to the patient . this is one of the main functions of the venous reservoir . as shown , air entering venous reservoir 1103 rises to the top of said reservoir where it is removed by suction pump 1114 to cardiotomy reservoir 1115 . roller pump 1104 is usually one of 3 to five pumps composing a heart - lung machine , which is part of a hardware required for cardiopulmonary bypass . [ 0100 ] fig2 a , 2 b , 2 c , 2 d and 2 e illustrate line drawings of one preferred embodiment of the present invention . here , venous blood enters the venous reservoir 1819 via inlet tube 1 and is directed into first inlet chamber 2 , shown as a cutaway . first inlet chamber 2 preferably has a circular cross section with its walls formed of fine screen 3 typically having a pore size of 40μ to 150μ and having an effective open area that is preferably greater than 40 %. it is understood that though lower pore sizes result in higher resistance to blood flow , they prevent smaller bubbles from crossing the screen . it should also be understood that screen 3 is preferably heparin coated , to increase wettability and reduce clot formation . the top of chamber 2 is in fluid communication with gas purge port 4 . the bottom of chamber 2 is open and is in fluid communication with inlet tube 1 and , via expandable chamber 8 , with outlet tube 5 . preferably outlet tube 5 is located on the opposite side of , and lower than , inlet tube 1 . ( bentley patent ?) in one of the preferred embodiment , shown in fig2 a , first inlet chamber 2 has a larger inside diameter than inlet tube 1 ( e . g . 1 . 0 ″ v . 0 . 5 ″), said larger diameter serves to slow the velocity of the blood ( e . g . ¼ the inlet velocity ), and thus allow more time for any bubbles to rise to the top where they can be removed . slowing the blood also reduces the tendency of the flowing blood to carry the bubbles , especially the smaller ones , by reducing the drag on the bubbles by the moving blood . lower velocity also lowers the tendency of larger bubbles to break into smaller ones ; larger bubbles have a higher buoyancy and less of a chance of crossing screen 3 into expandable chamber 8 , and flowing out of the bag through outlet tube 5 shown in fig2 a . with sufficient pressure across screen 3 , the bubbles could cross into chamber 8 and travel to outlet 5 of the reservoir , a very undesirable outcome . to reduce that possibility , inlet chamber 2 is open at the bottom where debubbled blood can exit first inlet chamber 2 at 2 a . to improve flow conditions , the outlet of inlet tube 1 , 1 a , is preferably centered with the centerline of chamber 2 , as also shown in fig2 b ( cross - section 15 - 15 ′ in fig2 a ). also shown is one preferred embodiment of structure 28 that centers inlet tube 1 within chamber 2 formed by screen 3 . connector 28 , shown in fig2 a and as a cross section taken of fig2 a along line 15 - 15 ′ shown in fig2 b , lines up and connects inlet tube 1 to inlet chamber 2 . thus , in one preferred embodiment , connector 28 has a wheel cross - section with an internal circular structure 28 a connected via spokes 28 b to an external circular structure 28 c . the inside diameter of inside structure 28 a that allows interference fitting to the outside diameter of inlet tube 1 and the outside diameter of outside structure 28 c supports cylinder 6 . the space between internal structure 28 a and outside structure 28 c maintained by spokes 28 b forms a fluid communication between inlet chamber 2 and expandable chamber 8 as indicated by the downward facing arrow at the bottom of fig2 e . it should also be obvious that since screen 3 may be flimsy , it may need radial support , as for example internal cage 26 , see fig2 c ( cross section 16 - 16 ′ in fig2 a ) and 2 f . screen 3 can be attached to cage 26 by various means ( e . g . insert molding ) longitudinally and radially to 26 a or 26 b and longitudinally to ribs 26 c , for example , by adhesive . this would maximize the id of first internal chamber 2 to provide a smooth and straight vertical flow path thereby facilitating the upward motion of the bubbles . with this design , as is the case for present venous reservoir bags ( e . g . bentley , cobe , sarns / 3m , minntech ) most of the incoming blood would exit via screen 3 across which very few bubbles , if any , cross . however , present venous reservoir bags are made of four layers : the two outside layers being flexible pvc sheets and the two inside layers being a screen ( e . g . u . s . pat . no . 4 , 734 , 269 ). the screen is usually folded over with the fold being in the center of the venous reservoir bag and its edges sandwiched and sealed along at least two of edges of the two pvc outer layers . this design is simple but it provides no means to keep the internal surface of the external pvc walls from contacting the external wall of the screen . this contact reduces the effective screen area available for blood flow , especially at low blood volumes , causing further problems because more bubbles cross the screen at lower blood volumes . for example , tests conducted with the cobe venous reservoir bag ( model # vrb , cobe lakewood , colo .) showed that at a blood flow of 4 . 0 l / min and an air flow of 750 ml / min , the bubble count ( size & gt ; 50μ ) with a blood volume of 750 ml in the bag was 35 bubbles / sec as compared to 94 bubbles / sec when the blood volume was 500 ml . the baxter venous reservoir bag ( model # bmr - 1900 , baxter / bentley irvine , calif .) had similar results : the bubble count increased from 69 bubbles / sec to 160 bubbles / sec when the blood volume decreased from 750 to 500 ml . the present invention eliminates the problem of screen to wall contact by introducing means to maintain the wall of the venous reservoir bag away from the screen as well as to maintain a vertical column of blood within first inlet chamber 2 . this can be achieved by either incorporating the means into the disposable bag , or by interfacing a disposable bag with a nondisposable holder , the combination providing the aforementioned means . fig2 a illustrates one preferred embodiment of the disposable type . here , a semi rigid cylinder 6 with perforated wall is placed over screen 3 forming second inlet chamber 7 in fluid communication with expandable chamber 8 via said perforations as well as its open bottom at 6 a . the perforations can be effectively formed by using a tubular net with , for example 0 . 030 ″ to 0 . 100 ″ diameter strands forming a diamond shaped opening , see 6 in fig2 a , and can be obtained from nalle plastics inc . austin , tex . the tubular net can be made of polypropylene , polyester , nylon , or polyethylene . it must possess at least three properties : 1 ) sufficient stiffness ( either by rigidity of the material or thickness of the yarn ) and structure to keep walls 18 and 19 ( fig2 b , 2 c , 2 d ) of venous reservoir bag 1819 ( fig2 a ) away from screen 3 thereby maintaining chamber 7 ; 2 ) an opening to allow unhindered fluid communication between chamber 7 and expandable chamber 8 ; and 3 ) cause no undesired interaction with biological fluids . tubular net 6 preferably extends vertically from the bottom of venous reservoir 1819 at its inlet to the top of said reservoir and can be attached to the external wall of air - venting tube 4 for support . the inlet to cylinder 6 , 6 a , may extend below screen 3 providing free fluid communication between inlet 1 and expandable chamber 8 . with this design , experiments similar to those described for the cobe and baxter bags result in a steady bubble count of 60 at bag volumes of 500 and 1000 ml . [ 0104 ] fig2 e illustrates the blood path of the present invention . venous blood with some gas bubbles 23 enters the venous reservoir via inlet tube 1 . the inertial forces of the blood exiting outlet of tube 1 propel the blood and bubbles upward into first inlet chamber 2 . chamber 2 is preferentially lined up within ± 15 ° of the vertical line . this essentially vertical position , unlike prior art devices , provides the least resistance for gas bubbles to rise up chamber 2 to air - venting tube 4 where they are evacuated by suction applied to the outlet of tube 4 , port 4 b . as shown in fig2 a , screen 3 extends to the top of venous reservoir 1819 where it is sealed to gas venting tube 4 . this seal prevents blood from exiting at the top where it may drag bubbles out of inlet chamber 2 into expandable chamber 8 . should gas volume increase at tube 4 and displace blood volume at the top of chamber 2 , the gas could cross screen 3 and enter chamber 7 and chamber 8 . because screen wall 3 may get wet again before all the gas at the top of chamber 8 is removed , that gas can be trapped . purge tube 9 ( see fig2 a and 2 e ) is provided to allow gas to be purged from chambers 7 and 8 . for that purpose , the topmost entry point of tube 9 into chamber 8 is the highest point in chamber 8 ( e . g . point 8 a is higher than point 8 b ). tube 9 extends from air - venting tube 4 into chamber 8 , said extension preferably having holes 9 a in its wall to provide better fluid communication with chamber 8 along the entire length of tube 9 . holes 9 a allows air to enter tube 9 and be evacuated as described before . other holes may be punched into tube 9 to allow air to be evacuated at any blood level . the smaller diameter of tube 9 and the location of its outlet at the top of venting tube 4 reduces the chance of blood flowing ( with bubbles ) from chamber 2 to chamber 8 via tube 9 . the extension of tube 9 into chamber 8 also forms two channels , shown as 9 aa in fig2 cc , for air to travel along the tube upwards because the tube prohibits the opposite walls of the bag from making complete contact . channels 9 aa increase in size with increasing outside diameter of air removal tube 9 and thicker / stiffer walls 18 and 19 of bag 1819 . fig1 b and its associated view along 1 b - 1 b ′, fig1 bb , illustrate how the present invention provides air channels . fig1 a and its associated view along 1 a - 1 a ′, 1 aa illustrate how prior art shorter air removal tube ( e . g . prior art u . s . pat . no . 5 , 573 , 526 fig1 tubes 18 and 20 ) lack such channels . tube 9 extends downward into blood chamber 8 at least 40 % but preferably over 50 % of the height blood chamber 8 . as well known in the art , tube 9 can alternatively be sealed directly into chamber 8 and external to tube 4 . as shown , tube 9 is exposed to the same suction applied to air - venting tube 4 . with the present invention because , air moves freely to the top of bag 1819 where it can be purged easily . it therefore should be obvious that the degree of suction applied and the blood volume removed in order to purge the gas should be significantly lower than with present devices . the smaller blood volume removed , the lower flow required to remove the gas and the larger id of the purge line all contribute to significantly lower blood damage . this is especially true when stopcocks , which have very small id ( e . g ., 0 . 062 ″ and sometimes less ) and are used with present devices , are eliminated . the user may not easily determine the presence of bubbles or the blood level in first inlet chamber 2 due to the opacity of the blood and / or screen 3 . yet another innovation provides means to easily ascertain the presence of bubbles by increasing the id of air - venting tube 4 to at least ¼ ″ but preferably ⅜ ″ or greater . other venous reservoir bags have gas ports of ⅛ ″ id or smaller , which presents a high resistance to gas and blood flow . the increased port diameter of the present invention increases the ease by which bubbles rise up tube 4 for two reasons . first , gas bubbles move up easier in a liquid filled tube having a diameter larger than the diameter of the bubbles . second , a larger diameter tube accommodates larger bubbles with greater buoyancy , providing greater upward force on the bubbles relative to the capillary force within a liquid filled tube that inhibits their movement . thus , by having an exhaust tube with a larger diameter , the user could pull blood up into tube 4 . should air enter first inlet chamber 2 , it would travel up and replace the blood in tube 4 causing the visible blood level 4 d ( see fig2 a ) in tube 4 to drop , an indication that air entered the venous reservoir and must be removed . it should be understood that the process can be automated by incorporating level detector 10 radial to tube 4 , said detector 10 connected to a suction controller and / or alarm monitor via transmitter line 10 a . monitor / controller 12 alarms the user to air entering tube 4 and / or starts the required suction applied to the outlet of tube 4 , 4 b , to remove said air and raise the liquid level . once the level detector detects the rising liquid , it can stop the alarm and / or stop the suction used to remove the gas from the venous reservoir . monitor / controller 12 can , for example , control the speed of the pump providing suction . alternatively , it can open or close the tube providing suction ( not shown ) by a solenoid actuated tubing clamp . also , as described in reference to one way valve 422 in reference to fig4 preferably one - way valve 22 , placed just below outlet 4 b of tube 4 , prevents air from entering the reservoir if the reservoir empties and is exposed to the suction generated by arterial pump 1104 . further , defoamer sponge 24 , preferably incorporating anti - foam a and placed below valve 22 , may be used to break up blood in the form of foam that reaches the inlet of valve 22 . placement of defoamer 24 at the top of tube 4 provides the desirable defoaming action while limiting contact between the defoamer and the blood that rises to that level . as shown in fig2 a the large diameter of chamber 2 allows more time for the bubbles to rise to the top and causes less turbulence that could hinder the upward motion of the bubbles . most of the blood preferably flows from chamber 2 to chamber 7 across screen 3 , thereby assuring the upward motion of the bubbles . this preference is enhanced by cylinder 6 maintaining screen 3 free of contact with venous reservoir walls 18 and 19 , see fig2 c . typically , if wall screen 3 forms a cylinder with a 1 ″ diameter , then for an 8 ″ high structure , its surface area is 25in2 . this large effective area is available for blood flowing from inlet chamber 2 to expandable chamber 8 and is virtually independent of the blood volume in expandable chamber 8 . annular space 7 formed by cylinder 6 and screen 3 and better seen in fig2 c , serves to separate gas from the blood ; any bubbles that may have crossed wall 3 can still be buoyed upward to the top of chamber 7 where they can be removed by tube 9 . the blood then flows from expandable chamber 8 to outlet port 5 . should air enter chamber 8 , it can still float to the top of said chamber and be eliminated via tube 9 . fig2 cc , which is an enlargement of the circled section shown in fig2 c , illustrates how tube 9 forms air channels 9 aa , described in reference to fig1 b and 1 bb , thereby enhancing air removal by keeping walls 18 and 19 slightly apart along the length of tube 9 . thus with this design , there are three chambers for air elimination : chambers 2 , 7 , and 8 . a major reason a collapsible bag is used as a venous reservoir is to prevent air from being pumped out of the bag and into the patient should the venous reservoir empty . in present bags this is achieved by having the outlet port ( 5 in fig2 a ) at the lowermost point of the bag . this can be incorporated into the present invention . alternatively , the inlet of outlet tube 5 , 5 a , can be cut on a diagonal ( nominal 35 ° to 65 °) with its pointed end protruding into expandable chamber 8 and its low point in line with the periphery of the bag at 8 c , as shown in fig2 a . tube 5 should be made of relatively soft material ( e . g . 55 shore a ) and have a relatively large id / wall ratio ( e . g . 0 . 5 ″/ 0 . 062 ″= 8 ). since a larger id / wall ratio , as well as softer durometer wall , requires a lower pressure difference across the wall of the tube to collapse the tube , then the combination of higher ratio and lower durometer can be used to quantify the ease of said collapse , ( id / wall )/ durometer . thus , for the above example , ( 0 . 5 ″/ 0 . 062 ″)/( 55 )= 0 . 147 . this number is significantly higher than that obtained for the outlet tube typically used at the outlet of present venous reservoirs ( 0 . 5 ″/ 0 . 093 ″)/( 65 )= 0 . 082 . since the ease of tube collapse is related to ( id / wall ) 3 , ( see my u . s . pat . no . 5 , 215 , 450 : innovative pumping system for peristaltic pumps ), even a small change in that ratio causes a large change in ease of collapse . thus , the softer tubing and / or high id / wall ratio allows collapsing walls 18 and 19 of venous reservoir bag 1819 to gradually , rather than suddenly , impede the flow out of outlet tube 5 . once empty of liquids , the present aspect of the invention provides a looser seal about the outlet as compared to standard bags . thus , when inlet flow resumes , less volume is needed to open the outlet tube , thereby providing resumption of flow sooner than present venous reservoir bags . an experiment was conducted to determine the negative pressure developed between the outlet of venous reservoir 1103 and the inlet of pump 1104 when pump 1104 ( see fig1 ) was pumping at 6 . 0 l / min out of venous reservoir 1103 and the venous flow into the venous reservoir was less than 6 . 0 l / min . the reservoir was emptied and its outlet collapsed . also measured was the blood volume required in the venous reservoir to reopen the venous reservoir outlet . once emptied , the outlet of the cobe reservoir bag stayed closed until the volume in the bag increased to over 1 , 400 ml . during that time , the pump inlet pressure ( measured in line 435 in fig1 ) decreased to and remained at over − 600 mmhg . once the blood volume in the bag reached 1 , 400 ml , sufficient pressure was exerted to expand walls and release the collapsed outlet of the venous reservoir , thereby allowing resumption of blood flow from the venous reservoir to the pump inlet . a similar experiment with the baxter bag required an increase in blood volume of 400 ml before the high negative pressure at the pump inlet (− 580 mmhg ) was relieved and the bag outlet opened up . with the present invention , only 350 ml were required to open the venous reservoir outlet and reestablish flow , and the maximum negative pressure was only − 400 mmhg . as shown in fig2 a , 2 b , 2 c , 2 d , layers 18 and 19 are heat sealed ( e . g ., by radio frequency welding ) by a double margin along their upper and lower edges , by a relatively wide seal along their right edge and by a narrower seal along their left edge . anchoring holes ( eyelets ) 27 , used to hang bag 1819 , can be formed by punching holes through , and along , the top and bottom of the heat sealed surface . the preferred configuration includes a hole on both sides of inlet tube 1 , outlet tube 5 , and air - venting tube 4 , and in the upper corner of the bag opposite tube 4 to facilitate secure attachment of the bag to the frame , see fig2 a . it should be understood that various sizes of the venous reservoir can be made without necessarily affecting their performance ; for example , three popular sizes having capacities of 400 , 1200 , and 2000 ml are some of the possibilities . to simplify manufacturing and reduce costs of the hardware , all reservoir sizes can have the same footprint so each size can utilize the same frame . here , smaller capacity reservoirs have a smaller bag portion and larger peripheral area ( fig3 ). anchoring holes 21 a , 21 b , 21 c , 21 d , 21 e , 21 f , and 21 g used to attach each bag to the frame can be accommodated by corresponding adjustable supporting pins in the frame , for example , as well known in the art . [ 0113 ] fig7 a , 7 b , and 7 c illustrate another preferred embodiment of the present invention . here , rigid cylinder 72 replaces perforated cylinder 6 , shown in fig2 a , to provide annular space 77 as well as to serve as part of the wall of venous reservoir 772 . pliable venous reservoir walls 18 and 19 are sealed to rigid cylinder 72 on both sides of longitudinal slot 72 a , said slot better seen in fig7 b —( a cross sectional view of cylinder 72 along lines 25 and 25 ′ in fig7 a ) and 7 c ( a cross sectional view of cylinder 72 along lines 272 and 272 ′ in fig7 a ), providing fluid communication between annular space 77 and expandable outlet chamber 8 . to reduce stasis and provide smooth blood flow , the incline at the bottom of the rigid cylinder 72 , 72 d , matches the bottom incline of chamber 8 , 8 d . cylinder 72 ( fig7 b ) preferentially has longitudinal lips 72 b and 72 c along both sides of slot 72 a , said lips tapering and thinning as they extend outward . these lips serve to seal venous reservoir walls 18 and 19 about slot 72 a ( e . g ., by radio frequency welding ) as well as to form a smooth blood flow path from annular space 77 to expandable chamber 8 . it should be obvious that cylinder 72 preferentially is made of biocompatible , clear , rigid thermoplastic that can be easily sealed to venous reservoir walls 18 and 19 . a good choice would be rigid pvc . it should be obvious that screen 3 , air - venting tube 4 , outlet tube 5 , and expandable chamber 8 formed by walls 18 and 19 serve the same purpose described for the venous reservoir embodiment shown in fig2 a . [ 0114 ] fig7 d , which is an enlargement of the circled section shown in fig7 a , illustrates another preferred embodiment providing a fluid path between chamber 8 and air - venting tube 74 that allows air removal present in annular space 77 and expandable chamber 8 . here , cylindrical air - venting tube 74 has a notch 74 h , at its bottom , also seen in fig7 e , which is a view of fig7 d taken along cross section 26 - 26 ′ and fig7 f , which is a view of fig7 e taken along cross section 27 - 27 ′. as shown , the height of notch 74 h extends beyond the top of screen cage 26 , 26 b . the bottom of notch 74 h extends onto the highest point of chamber 8 , 8 a , which also preferentially corresponds to the highest point of screen 3 . thus , notch 74 h provides a fluid communication , see arrow 84 in fig7 d , between air - venting tube 74 and chamber 8 . notch 74 h replaces the function of tube 9 shown in fig2 a . as described so far , air removal is accomplished as it is by current techniques : suction pump 1114 ( see fig1 ) typically with ¼ ″ id tubing is used to remove the gas from the top of the venous reservoir . this arrangement works but requires constant vigilance and intervention by the user to control air removal . another innovative feature of the present invention is that air can be automatically eliminated from the reservoir with little or no user intervention required . three preferable designs for the air purge port use a hydrophobic membrane , a floating ball , or controlled suction . all three methods allow air to be removed with very little , or no blood loss . the user would have the option to connect wall suction or one of the sucker pumps as the suction source for the air purge port , preferably having some regulating means to adjust / limit the degree of suction . [ 0116 ] fig4 illustrates one preferred embodiment that achieves a large membrane area at the top of the venous reservoir . the design , with a cross section in the shape of an inverted “ v ” or “ u ”, achieves a large area and provides an inclined surface . membrane 45 has an inclined surface that facilitates clearing of any blood film off the surface of the membrane . gravity and wicking should encourage any such film to “ peel ” off the surface into the blood pool , thereby maintaining the membrane clearer and the gas transfer rate up . membrane support 425 can be incorporated as the top of a semi - rigid pvc frame formed into a protective “ roof ”. the inside surface of the roof - contacting membrane incorporates ridges 425 a , which are in unimpeded fluid communication with air - venting tube 44 . ridges 425 a also support membrane 45 and prevent it from deforming due to pressure differences across its wall . the membrane should meet a high gas flow elimination requirement ( at least 1 l / min at − 100 mmhg ). membranes preferably are made of ptfe ( e . g . durapel ™ from millipore , bedford , mass .) or polypropylene ( e . g . zintex ™ from w l gore , elkton , md . ), preferably having a pore size between 0 . 45μ and 1 . 0μ . the small pore provides a sterile barrier . the membrane is used to automatically remove air 423 that may accumulate at the top of the venous reservoir by applying suction ( from the hospital supply ) to air - venting tube 44 . hydrophobic microporous membrane 45 prevents the loss of blood 46 from the venous reservoir . one - way valve 422 may be placed at the outlet of air - venting tube 44 to prevent air from entering the reservoir if the reservoir empties and is exposed to the suction generated by arterial pump 1104 . membrane 45 has sufficient surface area to allow the removal of the expected volume of air entering the venous reservoir . studies have shown that membranes that clear air from water can function almost indefinitely ( many days ) and high suction can be applied without reducing gas transfer rate over time . ( however , over time , when the membrane is exposed to blood , especially when high suction is applied , a film overlays the membrane , resulting in a significant increase in resistance to gas flow . when applying lower suction ( preferably between − 50 and 200 mmhg ), the transfer rate of gas across the membrane does not decrease as fast as with high suction ( possibly due to less plasma penetration into the pores or lower holding force of the film ). therefore , removing air from blood requires a membrane with a larger area . the larger area compensates for the lower suction used to extend the life of the membrane and the lower transfer rates seen with blood as compared to water . another preferred embodiment , shown in fig5 a and 5 b , utilizes a tubular microporous membrane 55 in fluid communication with purge port 54 , said tubular membrane internally supported and sealed to perforated rigid housing 525 . perforated rigid housing 525 allows gas to cross membrane 55 and enter chamber 59 unimpeded . housing 525 is sealed at the bottom along 525 a . chamber 59 , formed by housing 525 , is in fluid communication with purge port 54 . annular space 57 is formed by circular membrane 55 and air - venting tube 4 . air - venting tube 4 could be in fluid communication with first inlet chamber 2 shown in fig2 a and preferably located on top of chamber 2 . normally annular space 57 is filled with blood . should air 523 enter line 1 ( see fig2 a ), it would rise up chamber 2 , as shown in fig2 f , enter annular space 57 ( fig5 a and 5 b ), across membrane 55 into chamber 59 ( fig5 a ), across port 522 a of one - way valve 522 , and be purged via purge port 54 . applying suction to purge port 54 facilitates air removal by increasing the pressure difference across membrane 55 . as with the “ roof ” design referenced in fig4 vertical placement of the tubular membrane 55 facilitates “ peeling ” of the blood layer of the surface of the membrane , thereby improving long - term gas transfer . the second preferred method to remove air utilizes a floating ball , which allows air but not blood to be removed through the purge port . as shown in fig6 a , housing 64 a forms chamber 67 that allows air bubbles to rise unhindered as previously described for chamber 2 and tube 4 in reference to fig2 a . housing 64 a incorporates ball cage 68 , floating ball 61 and unidirectional valve 622 . port 622 a of unidirectional valve 622 providing fluid communication between chamber 67 and gas exhaust port 64 , is open as long as air 623 is present in chamber 67 . when most of the air has been eliminated , the rising fluid level brings ball 61 to the top of chamber 67 , effectively closing port 622 a . in this position , any further withdrawal of fluid from the venous reservoir is prevented . when more air enters the reservoir , the blood level falls , ball 61 drops , and the applied suction removes air 623 . suction may be provided by a wall source or a suction pump , but preferably is controlled for the purpose described below . there are two forces maintaining ball 61 up against port 622 a keeping said port closed : the buoyancy of the ball and the suction force applied at the gas port ( fs ). fs = ( πd2s / 4 , where d is the inside diameter of air port 622 a in contact with ball 61 , and s is the negative pressure ( suction ) applied via air - venting tube 64 against said ball . the upward force , fs , must be less than the weight of the ball so that when the blood level drops , the weight of the ball overcomes fs and the ball falls . cage 68 , in general has a larger id than the od of ball 61 , see 68 a in fig6 a and 6 c , where fig6 c is a line drawing illustrating another view of the ball cage used in fig6 a taken along line 24 - 24 ′. cage 68 aligns the ball with air port 622 a . the bottom of cage 68 narrows down to an id smaller than the od of ball 61 , see 68 b fig6 a and 6 b , where fig6 b is a line drawing illustrating another view of the bottom of the ball cage used in fig6 a taken along line 23 - 23 ′. the smaller id 68 b serves to retain ball 61 within its chamber 67 and prevents it from falling into the venous reservoir . for this design , for example , ball 61 may be a 1 ″ solid polypropylene ball ( specific gravity sp = 0 . 90 ), or a hollow ball ( where sp is adjustable ). air port seal 622 a could , for example , be made of soft silicone and the id of the air port may be { fraction ( 1 / 32 )}″. to assure a good seal , the surface of the ball should have a fine finish , preferably with a tolerance of 0 . 001 ″ or better . the applied suction should be low to assure that ball 61 does not “ stick ” to gas port 622 a in the closed position , and to minimize blood damage . for example , a pressure of − 30 mmhg can be applied to remove the air . this degree of suction is sufficient to withdraw the air and maintain the liquid column within first and second inlet chambers 2 and 7 when flexible chamber 8 is less than full , see fig2 a . to prevent excess suction ( e . g . over − 150 mmhg ) from being applied , the line between air venting tube 64 and the suction source can include a t - connector 64 c with a suction regulating valve 632 attached at the inlet of side port 64 c ( fig6 d ). such valves are commercially available at various cracking pressures and are currently used for iv infusion sets ( e . g ., np medical , clinton , mass ., cost & lt ; $ 0 . 25 ). as well known in the art , a blood trap ( not shown ) may be incorporated so any blood that may enter the line would not progress to the suction source , and , in fact , excess lost may be returned to the patient . alternatively , the air - venting tube 64 may be connected at 64 b to cardiotomy reservoir 1115 ( see fig1 ), to which suction is applied . thus , any blood that may pass the ball valve system would go back to the patient via cardiotomy 1115 . safety is paramount . therefore , side port 64 d , having for example a female luer , in fluid communication with first inlet chamber ( e . g ., via chamber 67 in fig6 d ), is placed prior to either the ball or the membrane . port 64 d provides the user means to eliminate incoming air in a fashion similar to that of present devices , in case the membrane or ball malfunctions . another preferred method to remove air is a variation of the second method but without the floating ball valve combination . as shown in fig1 , the top of first inlet chamber 112 of venous reservoir 113 is extended into “ chimney ” 114 that serves to vent air and is connected to cardiotomy reservoir 15 , to which suction is applied at 15 a . the degree of suction should be sufficient to elevate the blood level into chimney 114 , even when the expandable chamber 118 is less than full . thus , any air 623 entering inlet tube 111 would float to the top of first inlet chamber 112 and enter chimney 114 . the air would then displace the liquid in chimney - 114 , coalesce with air volume 114 a that interfaces between the blood in chimney 114 and outlet 114 b of chimney 114 , and the additional suction would pull the liquid up the chimney to its original level . this system requires that chimney 114 have an id that facilitates upward movement of air bubbles , even large ones . the length of the chimney needs to be at least equal to the level of the expected liquid when suction is applied and expandable chamber 118 is full . beyond that height , the outlet of chimney 114 b can be connected via ¼ ″ id tube - 116 to the cardiotomy reservoir . air space 114 a below chimney outlet 114 b assures that the blood does not enter smaller diameter tube 116 . suction , applied at 15 a , can be provided by the wall source , or suction pump 1114 ( fig1 ) connected to cardiotomy reservoir 15 , said suction regulated to appropriate levels as well known in the art . as described in the description of the prior art , improved venous drainage can be achieved by applying some negative pressure on the venous blood . another aspect of the invention allows the user to apply suction with a collapsible reservoir . fig8 a , 8 b , and 8 c illustrate venous reservoir 772 , previously described in reference to fig7 a , 7 b , and 7 c , placed in generally elliptical , clear rigid , housing 88 . housing 88 is open both at its bottom , defined by border 88 a , and at its top , defined by border 88 b , said borders having sealing gaskets 82 and 81 respectively . disposable venous reservoir 772 incorporates rigid bottom cap 89 , said cap having lip 89 a with its inside diameter matching outside diameter of housing 88 to form a seal along gasket 82 . bottom cap 89 also is sealed to inlet tube 1 at 89 a and outlet tube 5 at 89 b . a similar arrangement is made at the top of venous reservoir 772 where rigid disk 72 d is sealed along top gasket 81 of housing 88 . thus , the user would slip chimney 74 of disposable venous reservoir 772 into the bottom of housing 88 , push it up and insert it through opening 88 d at the top of housing 88 . when lined up , rigid disk 72 d is pushed against gasket 81 and bottom cap 89 seals against gasket 82 . the bottom and top seals are reinforced and maintained by cap 89 held against housing 88 by snaps 88 e , 88 f , 88 g and 88 h that lock onto ridge 89 d of cap 89 . at the end of the case , snaps 88 e , 88 f , 88 g and 88 h , each of which is hinged at its midpoint ( e . g . see 88 i of hinge 88 f ) are pushed inward , as shown by respective arrows 812 and 811 for snaps 88 f and 88 e , causing the bottom of said snaps ( e . g . 88 j shown in fig8 b ) to move outward , see for example 88 e ′ in fig8 b , releasing said snaps from locking ridge 89 c and 89 j thereby allowing the removal of venous reservoir 772 . chamber 87 , formed between venous reservoir 772 and rigid housing 88 , communicates via port 88 c with vacuum regulator 813 , said regulator used to adjust the degree of suction applied to chamber 87 using knob 813 b . gauge 813 a can be used to indicate the applied suction . as described before , venous reservoir 772 responds to pressure differences across its walls 18 and 19 ( fig8 b ). thus , diminished blood flow from patient 1102 , see fig1 due to increased resistance to flow ( e . g . smaller cannula ) can be increased by applying suction to chamber 87 . the suction “ pulls ” walls 18 and 19 outward thereby pulling the blood into the blood chamber . for safety , housing 88 is sized to assure that venous reservoir 772 cannot over - expand beyond defined limits , said limits defined as a volume in blood chamber 8 that would result in a pressure measured at the top of blood chamber 8 being greater than 10 mmhg . thus , as chamber 8 of venous reservoir 772 expands , walls 18 and 19 move towards the walls of housing 88 until they make contact , see 18 a and 19 a in fig8 b . once contact is made , further outward motion of walls 18 and 19 is limited by rigid housing 88 . to facilitate the use of the system , housing 88 incorporates pole clamp 810 , said clamp provides a simple connection of said housing to a heart - lung machine . it should be understood that a rigid component , such as rigid cylinder 72 , incorporating into venous reservoir 772 , see fig7 a and 8 a , is required to facilitate both the introduction of said venous reservoir 772 into housing 88 , and the sealing of said reservoir against gasket 81 , shown in fig8 a . to enhance the ability of the user to see the blood in venous reservoir 772 , light 80 , shown in fig8 b , can be added to the back of housing 88 . [ 0124 ] fig9 a illustrates another embodiment for a nondisposable housing designed to allow venous augmentation with a collapsible venous reservoir . the concept is similar to that shown in fig8 a except that the seals and closure mechanism are different . here , venous reservoir 772 is placed in container 98 , said container having a back plate and four walls forming first open box , 98 e , which accommodates venous reservoir 772 . container 98 has a matching door 99 that is hinged at 99 f by pin 98 f to container 98 and is shown in fig9 b and 9 c . door 99 has a front plate and four walls forming second box 99 e that also accommodates venous reservoir 772 . to operate , venous reservoir 772 is placed in first box 98 e and door 99 is closed thereby sealing said venous reservoir , along gasket 92 , within space 909 formed by first box 98 e and second box 99 e . port 98 c in box 98 in fluid communication with the formed sealed space can be connected to a regulated vacuum source , much like the one described in reference to port 88 c shown in fig8 a and 8 b . it should be understood that for proper function , the venous reservoir is free to expand within the sealed space 909 thus formed . for free expansion of venous reservoir 772 , seals of the venous reservoir within container 98 and door 99 are achieved at inlet tube 1 , between 92 a and 99 a ( fig9 b ), air - venting tube 4 , at 92 b and 99 b ( fig9 c ), and along outlet tube 5 , at 92 c and 99 c ( fig9 b ). when door 99 is closed , the id of indentations 92 a and 99 a form a tight seal about the od of inlet tube 1 . similarly , indentations 92 c and 99 c form a tight seal about the outside of outlet tube 5 ( fig9 b ), and indentations 92 b and 99 b form a tight seal about the outside of air - venting tube 4 ( fig9 c ). to assure a tight seal , relievable latches 99 d and 99 f lock unto ridge 98 d , see fig9 a , 9 b and 9 c . to improve the seal along the inlet , outlet and gas exhaust port , each of said tubes preferably incorporates a secondary structure , see sealing structure 1 a in fig9 d for inlet tube 1 . sealing structure la has a flexible wall forming a wings 1 aa and 1 ab on the side of tube 1 , see fig9 e and 9 d . the wings are tapered , being thickest at the base and thinnest at the tips , see fig9 d . for effective sealing , gasket 92 accommodates wing 1 aa at thinner section 92 aa and wing 1 ab at thinner section 92 ab , said accommodation providing a seal between container 98 and door 99 along gasket 92 . gasket 92 , for example , can be made of a polyurethane sponge , which conform to the shape of said wings , see fig9 d . wing 1 a preferably is bonded or welded to tube 1 and is therefore disposed when venous reservoir 772 is disposed . similar designs can be incorporated into air - venting tube 4 and outlet tube 5 . [ 0126 ] fig9 f illustrates another preferred embodiment for sealing inlet tube 1 between housing 98 and door 99 . here , gasket 93 is attached to door 99 , said gasket having indentation 93 a to seal about the inlet tube 1 when door 99 is closed against housing 98 . this design also incorporates deeper indentation 98 a ′ in the housing , with a closed circumference greater than 225 ° and an inside diameter that is less than the od of inlet tube 1 . when the venous reservoir is loaded into the housing , flexible inlet tube 1 is pushed into indention 98 a ′ where it is retained within said indentation by a pressure fit . this allows the user to load air - venting tube 4 and outlet tube 5 . it should be obvious that purge port should be loaded first thereby having the venous reservoir hanging from the top while the other two tubes are lined up before door 99 is closed . [ 0127 ] fig1 a , 12 b , and 12 c illustrate another preferred embodiment that is identical to that described in fig8 a , 8 b and 8 c with two major exceptions . gas removal port 74 and its associated seal 72 d shown in fig8 a are replaced by gas removal tube 124 shown in fig1 a . tube 124 bends and extends to the bottom of bag 772 , see fig1 a , and exits in the same direction as inlet tube 1 and outlet tube 5 thereby eliminating the need for top seal 72 d . bag 772 in fig8 a has its gas removal port 74 extending straight up with its outlet ending above bag 772 and pointing opposite to said inlet and outlet tubing . having all three tubes of bag 772 extend beyond blood chamber 8 and in one direction and exit along the same plane allows all three tubes to be threaded , preferably during manufacturing , through bottom supporting plate , or cover 89 . thus , as shown in fig1 a , 12 b , and 12 c , inlet tube 1 is threaded through cover 89 and is sealed at 89 a , outlet tube 5 is threaded through cover 89 and is sealed at 89 b , and gas removal 124 is threaded through cover 89 and is sealed at 89 e . having all tubes extend beyond blood chamber sealed within single plate 89 significantly simplifies sealing bag 772 in housing 88 ; it allows sealing along a single plane of cover 89 against single o - ring 82 of housing 88 . it should be obvious that bottom plate 89 could incorporate perfusion connectors as described in reference to supporting plate 1389 in fig1 f . the other innovative design , shown in fig1 a and 12 b but not in fig8 a or 8 b , incorporates an opening 88 k in front wall 881 of housing 88 allowing the user to reach bag 772 without removing the bag from its housing . reaching bag 772 was the purpose of the external means provided by aforementioned u . s . pat . no . &# 39 ; 045 to massage the ssr with vibrator 36 . the present invention incorporates removable sealing means to front wall 881 of housing 88 , such as door 1288 , whose outside outline is shown as a dashed line in fig1 a and 12 b . door 1288 in its neutral state is supported by hinge 1202 hanging at on front wall 881 . the outside perimeter of opening 88 k , shown as a dotted line in fig1 a and 12 b , of front wall 881 is surrounded by flexible seal 83 . seal 83 assures that when door 1288 is closed , it seals opening 88 k from atmospheric pressure . to open door 1288 , the user would release any negative pressure in closed chamber 87 then open door 1288 by pulling handle 1288 a shown in fig1 b . closure of door 1288 against seal 83 can be facilitated by tilting front wall 881 either by design , or by tilting entire housing 88 , thereby allowing gravity to hold door 1288 against wall 881 . design correctly , using gravity to push door 1288 against seal 83 can eliminate clamps that may be necessary otherwise . gravity closing would allow hinged door 1288 , if it were not secured to rigid housing 88 , to also serve as a pressure relief valve should vacuum fail . as well known in the art of doors , mechanisms to maintain door 1288 open , or even temporarily remove the door , can be easily incorporated in the usual manner . to assure that vacuum is not applied accidentally , door closure is preferably designed such a complete seal occurs only when vacuum is applied and the user temporarily pushes against the door . the seal formed by the initial pushing force provided by the user , is then maintained once vacuum build within chamber 87 . [ 0129 ] fig1 a and 13 b illustrate another preferred embodiment of a soft shell reservoir with the very innovative features : top loading of the reservoir into its holder and easy secure sealing of the bag for vacuum assist . venous bag 1366 is preferably made by rf welding polyvinylchloride or polyurethane film having thickness of 0 . 015 to 0 . 020 ″ along perimeter 1310 , to form expandable chamber 138 with walls 1318 and 1319 . folded screen 1303 ( e . g . medifab from tetko inc . depew n . y ., a polyester mesh with a pore size of 105μ and a 52 % opening ) is placed with fold ( preferably not creased ) 1303 a facing downward and sealed along its vertical sides by welding its side edges between walls 1318 and 1319 along periphery 1310 . screen fold 1303 a defining the bottom of screen 1303 , preferably is placed at least ½ ″ from the bottom of blood chamber 138 . the top free edges 1303 b and 1303 c of screen 1303 , shown in fig1 b , face upward and , at least partially , are not sealed along the top periphery 1310 a and therefore an opening into pouch formed by fold 1303 a and the two sealed sides of screen 1303 . the screen placement defines four sections , within expandable chamber 138 . bottom or outlet section 138 a defined as the section of blood chamber between screen fold 1303 a and blood outlet tube 1305 . mid or inlet section 138 b defined as the section of blood chamber between the top of screen 1303 and its fold 1303 a . in inlet section 138 b , blood is completely surrounded by screen 1303 . top , or bubble removal section 138 c , is defined as the section of blood chamber 138 above inlet section 138 b , between the top of screen 1303 and sealed top periphery 1310 a . bubble removal section 138 c has no screen . the “ in - between ” section , 138 d , is the section between walls 1318 and 1319 and screen 1303 . the four sections are in fluid communication with each other . as shown , four tubes enter bag 1366 . inlet tube 1301 and infusion tube 1306 are in direct fluid communication with inlet section 138 b . air removal tube 1304 is in direct fluid communication with inlet section 138 b and air removal section 138 c . outlet tube 1305 is in direct fluid communication with outlet section 138 a . tubes 1301 , 1306 and 1304 enter from the top of blood chamber 138 , are sealed along top perimeter of sealed section 1310 a , pass through air removal section 138 c , two screen edges 1303 b and 1303 c of screen 1303 and into inlet section 138 b . all tubes , except outlet tube 1305 , preferably have holes along their length positioned in inlet section 138 b . gas removal tube 1304 also has holes , 1304 aa , along its length stationed in both air removal section 138 c and inlet section 138 b . inlet tube 1301 preferably enters blood chamber 138 at a top corner of blood chamber 138 and extends to the bottom of inlet section 138 b , preferably diagonally to a bottom corner opposite said top corner . blood enters inlet tube 1301 at its inlet end 1301 a in a downward direction , said inlet being above said blood chamber 138 and changes direction as it flows within curved inlet tube 1301 . outlet end 1301 d of inlet tube 1301 is preferably sealed , forcing blood out exiting holes 1301 b . exit holes 1301 b are preferably located only along the top length of tube 1301 situated in inlet section 138 b that faces air removal section 138 c , see fig1 a . thus , venous blood , entering inlet tube 1301 in a downward flow at inlet 1301 a , is diverted from a downward flow to a more horizontal flow and then in an upward direction through exit holes 1301 b . the diversion in flow occurs within inlet tube 1301 distal to inlet 1301 a . the upward blood flow pushes bubbles towards air removal section 138 c . a venous bag for an adult patient would preferably have inlet tube 1301 , said tube preferably having an id of 0 . 5 ″ and exit holes 1301 b with a diameter of 0 . 5 ″ or larger . blood entering inlet section 138 b preferentially flows to outlet section 138 a via screen 1303 , said screen , once wet , allowing liquid through but retaining bubbles within inlet section 138 b . bubbles are pushed upwards by the direction of the blood exiting holes 1301 b and by buoyancy . bubbles rise towards air removal section 138 c and then to access holes 1304 a of air removal tube 1304 , where they are removed , is obstructed when wall 1318 collapses against its opposing wall , as happens with prior art ssr when blood volume is low . with the present ssr , as described in reference to fig2 cc and fig1 b and 1 bb , channels are formed along the outside diameter of tubes 1301 , 1306 , and 1304 providing a pathway for bubbles to move upward to air removal section 138 c and on to access holes 1304 a of air removal tube 1304 . air removal efficiency is further improved by extending tube 1304 , and preferably also infusion tube 1306 , from the top of blood chamber 138 downward into inlet section 138 b , at least 50 % of the vertical distance between the top and the bottom of inlet section 138 b but preferably over 80 % of the height inlet chamber 138 b . if no screen is used , then said extension downward from the top of blood chamber 138 is at least 50 % of the height of blood chamber 138 . as shown in fig1 a , air removal tube 1304 preferably extends in a diagonal direction within blood chamber 138 b thereby providing a longer air removal channel than that possible with said tube extending only vertically . tube 1306 serving as an infusion line , may be closed at its top and just serve as a spacer that provides air bubbles a pathway to air removal section 138 c when low blood volume tends to collapse the blood chamber . in fact additional intermediate gas purge tubes ( not shown ), similar to tubes 1304 and 1306 may be incorporated in a similar manner to provide more numerous air removal channels . having air channels from the bottom of the screen to the air removal section , not only eliminates the front plate of prior art venous reservoir , but also allows chamber 138 of bag 1366 to take its natural tear drop shape , much like that shown in fig1 b . the teardrop shape provides a larger area of the screen ( the bottom ) for blood flow unhindered by contact with the walls of the bag . to assure that air bubbles can travel along the entire horizontal length of air removal section 138 c towards air removal tube 1304 , spacer 138 cc may be placed along the top of blood chamber 138 . spacer 138 cc prevents the flexible wall forming blood chamber 138 from completely collapsing against its opposing wall when the blood chamber is partially empty . as with the aforementioned air channels provided by tube 1304 , preventing said complete collapse increases the efficiency of gas from the top of blood chamber 138 . another innovative design feature requires that the open ends of the all tubes of venous reservoir 1366 be above blood chamber 138 . inlet tube 1301 , gas removal tube 1304 and infusion tube 1306 enter blood chamber 138 from its top . outlet tube 1305 exits outlet blood chamber 138 a in a direction that facilitates outlet flow to exit in an upward direction . for example , as shown in fig1 a , tube 1305 exits outlet pocket 138 aa , the lowest portion of outlet 138 a , in a horizontal direction thereby requiring only 90 ° turn for changing the normally downward outlet flow to the desirable upward flow . here the venous reservoir also incorporates supporting plate 1389 having a first and second planar surfaces , with said first planar surface facing blood chamber 138 . the tubes of venous reservoir : inlet tube 1301 at 1389 a , outlet tube 1305 at 1389 b , gas removal tube 1304 at 1389 c , and infusion tube 1306 at 1389 d can be threaded through , solvent bonded and sealed during manufacturing to supporting plate 1389 . : ( inlet tube 1301 at 1389 a , outlet tube 1305 at 1389 b , gas removal tube 1304 at 1389 c , and infusion tube 1306 at 1389 d .) supporting plate 1389 can serve to support bag 1366 by dropping it into holder 1388 , as is done with prior art hard shell reservoir ( e . g . baxter holder p / n hsrh for hard shell reservoir p / n hsr4000 ). for this purpose , the perimeter of supporting plate 1389 is preferably larger than the perimeter of venous reservoir 1366 . inlet 1305 a of outlet tube 1305 tube may also be designed to prevent pocket 138 aa , shown in fig1 a , from prematurely collapsing ( i . e . while there is still blood in outlet chamber 138 a ) and uncollapsing once blood returns to outlet chamber 138 a . this is achieved by having the inlet of tube 1305 cut longitudinal to form a scoop - shape whose walls provide the resilience to maintain the walls of bag 1366 of section 138 aa apart from each other . a similar design was described in reference the inlet 5 a of outlet tube 5 shown in fig2 a . another advantage of having all the tubes for the ssr entering from its top is that the bottom of the bag is unhindered by tubing and can be placed lower on to the floor thereby allowing greater gravity drainage . it should be obvious that other designs of ssr 772 shown in fig1 a can be made without compromising the spirit of the present invention . for example , fig1 d is a line drawing of the bottom part of another preferred embodiment of a ssr , ssr 1362 . fig1 dd is a line drawing of a cross section taken of fig1 d along line 133 - 133 ′. ssr 1362 is identical to ssr 1366 shown in fig1 a and 13 b except its outlet section 1368 a is shaped as a funnel and its outlet tube 1365 enters said outlet section through back wall 1362 a via an angled connection . here , as for outlet 138 a of bag 1366 , outlet tube 1365 exits outlet section 1368 a at lowest point , pocket 1368 aa . the angled connection can be made utilizing , for example , a halkey - roberts semi rigid connector # 727ac ( st . petersburg , fla .) rf welded to wall 1362 a and then connecting outlet tube 1365 to said connector . this design with an angle connector eliminates the need for outlet tube 1365 to be bent , as is the case for the design of outlet tube 1305 shown in fig1 a . though not illustrated , it is also possible to have outlet tube 1305 contained within blood chamber 138 and exiting at the top of bag 1366 . [ 0139 ] fig1 e is a line drawing of the bottom part of another preferred embodiment of a ssr , ssr 1372 . fig1 ee is a line drawing of a cross section taken of fig1 e along line 134 - 134 ′. ssr 1372 is identical to ssr 1366 shown in fig1 a and 13 b except its outlet tube 1375 enters its outlet section 1378 a through back wall 1372 a via an angled connection . here , as for outlet 138 a of bag 1366 , outlet tube 1375 exits outlet section 1378 a at lowest point , pocket 1378 aa . the angled connection can be made utilizing , for example , a halkey - roberts semi rigid connector # 727ac ( st . petersburg , fla .) rf welded to wall 1372 a and then connecting outlet tube 1375 to said connector . this design with a semi rigid angle connector eliminates the need for outlet tube 1375 to be bent , as is the case for the design of outlet tube 1305 shown in fig1 a .? [ 0140 ] fig1 a , and 13 b also illustrate a line drawing of one preferred embodiment of a ssr holder that in combination with supporting plate 1389 of venous bag 1366 can form a closed housing that can be used for vavd . container 1388 can , in one embodiment , consist of continuous vertical walls ( e . g . an extruded ellipsoid tube ), a bottom and open top 1388 f forming an internal chamber having an effective internal diameter ( e . g . for an ellipsoid the effective diameter being a function of the major and minor diameters .) open top 1388 f preferably has a smaller opening than that of container 1388 , said opening sized to at least allow venous reservoir 1366 with its blood chamber 138 empty , to be dropped into container 1388 . the internal diameter of container 1388 is sized to prevent blood chamber 138 from over extending beyond aforementioned desirable limits . the perimeter of cover 1389 preferably is larger than opening 1388 f so as to close said opening 1388 f of container 1388 and form sealed chamber 1309 . when positioned properly , supporting plate , or cover , 1389 closes said opening 1388 f forming housing 1309 . in one embodiment , cover 1389 preferably has two protrusions along its perimeter , 1389 e and 1389 f , said protrusions forming a channel between accepting open perimeter 1388 a of container 1388 . this combination lines up cover 1389 and container 1388 , provides a better seal , and hinders cover 1389 from sliding off container 1388 . rim 1388 a along the open perimeter of housing 1388 may incorporate sealing gasket 1382 against which cover 1389 can seal when vacuum is applied to chamber 1309 . when regulated vacuum is applied , via port 1308 shown in fig1 b , ssr 1366 can be used to enhance venous drainage , as described in aforementioned vavd . for vavd , the cross section of container 1388 is preferably ellipsoid , a shape that accommodates the general shape of ssr 1366 and provides mechanical strength . it also serves to line up top of bag 1366 with its supported bottom , as well as preventing cover 1389 from rotating and thereby preventing the bag from twisting . twisting along the vertical axis is also minimized by guides 1388 c and 1388 b extending from the bottom of container 1388 , accepting bag 1366 . preferably , guides 1388 b and 1388 c support bag 1366 via outlet tube 1305 , which is stiffer than pliable wall 1319 and 1318 . container 1388 preferably should be made from crystal clear , rigid , scratch resistance , tough material such as polycarbonate that can withstand an internal pressure of at least − 250 mmhg . since cover 1389 is disposable , it can be made from less expensive material , such as polyvinyl chloride , and need not be clear or scratch resistance . cover 1389 required the physical strength to withstand the expected pressure differences across its wall when used for vavd , preferably supporting a minimum internal pressure of − 200 mmhg . structures such as ribs 1389 f , shown in fig1 a , can be used to reinforce cover 1389 . reducing opening 1388 f by extending 1388 g shown in fig1 b , to “ just ” allow loading of venous reservoir , reduces the area of cover 1389 that is exposed to vacuum and therefore reduces its required strength . the top loaded ssr 1366 , compared to the bottom loaded design shown in fig8 b , has significant advantages . ssr 1366 can be easily placed in the housing with one hand . once placed , it stays in the holder / housing without clamps ( e . g . 88 g and 88 h in fig8 a ). with top loading / support , the weight ( gravity ) of the blood in bag 1366 pulls down cover 1389 against seal 1382 rather than pulling away , thereby using gravity , at least partially , to initiate a seal between cover 1389 and container 1388 . also , the support on top and the weight ( blood volume ) on the bottom tend to “ straightens out ” bag 1366 . top loading also provides a single flat plane to seal the bag and its associated tubing within housing 1388 . this feature is extremely important to assuring simplicity , reliability , and cost effectiveness . making one of the walls of the of the housing a disposable rather than the entire housing as shown in fig9 of pct &# 39 ; 16893 , reduces costs significantly . further reduction in costs is achieved by making the disposable wall , a wall with a small area ( e . g . top or bottom wall ). a smaller area requires lower force to support the same pressure difference and therefore allows use of thinner cover . top loaded ssr has two additional advantages . first , when placing venous reservoir 1366 into its holder by hanging it by it supporting plate 1389 , blood in blood chamber 138 tends to settle at the bottom of blood chamber 138 lowering the center of gravity towards the bottom of the venous reservoir and far below , supporting plate 1389 . thus , supported at its top and pulled down by weight of the blood , gravity is used to assist in maintaining the venous reservoir in a vertical position . second , cover 1389 responds to pressure differences across its wall in a useful manner . thus , when suction is applied to chamber 1309 , cover 1389 pulls tighter against seal 1382 ; the additional sealing force approximating the product of the area of 1389 exposed to the vacuum applied and the level of vacuum . for example , for a cover 2 ″ wide and 7 . 5 ″ long , when a suction of − 50 mmhg (− 1 psi ) the sealing force would be 15 lbs . similarly , should the vacuum fail , and cover 1389 was not secured to ridged housing 1388 , a build up of pressure within chamber 1309 would provide a force to open cover 1389 to relief pressure should it rise above atmospheric . accidental pressure build up due to failed vacuum supply can also be achieved by introducing a small “ leak ” that prevents total sealing yet is small enough to allow suction in the operating room to overcome that leak and provide the desired regulated vacuum . such a leak could for example be between 100 and 500 cc / min . it is obvious that the safety features described with respect to fig8 b apply to bag 1366 and housing 1388 shown fig1 a . for example , housing 1388 is sized to assure that venous reservoir 1366 cannot over - expand beyond defined limits , said limits defined as a volume in blood chamber 138 that would result in a pressure measured at the top of blood chamber 138 of + 10 mmhg . should blood chamber 138 of venous reservoir 1366 expand , walls 1318 and 1319 would move outward until they make contact with the vertical walls of housing 1388 , as shown for walls 18 a and 19 a in fig8 b . once contact is made , further expansion of walls 1318 and 1319 is limited by the vertical walls of rigid housing 1388 . for non - vavd applications container 1388 need not be sealed . for example , front wall 1388 e of housing 1388 shown in fig1 b , can be minimized or eliminated to allow the user to reach bag 1366 without removing the bag from the holder . this still provides a venous reservoir featuring easy top loading and connections of the inlet tube , outlet tube , and purge port to the extracorporeal circuit made by an end user from the top of the venous reservoir . top connections are easier to make in the operating room than the side or bottom connections required with prior art soft shell venous reservoirs . it should also be obvious that bag 1366 can incorporate additional tubing ( e . g . for cardiotomy return ) in a manner similar to that shown for inlet tube 1301 and / or outlet tube 1305 . the advantage of top loading being maintained as long as said additions allow top cover 1389 to be used as shown . to simplify changing from a closed housing and open front wall housing , front wall 1388 e of housing 1388 , can be designed as a removable wall as described in detail in reference to door 1288 of housing 88 in fig1 a and 12 b . the aforementioned design of ssr incorporating a disposable supporting plate adds little cost compared to the added convenience and shorter set up time making it economical to use the bag for standard or vavd procedures . this reduces cost of inventory and simplifies the user &# 39 ; s set up and learning curve . it should be emphasized that all the designs for sealing a venous reservoir having at least one flexible wall within a rigid housing for example , as described in reference to fig8 b , 9 b , 10 b , 12 b , or 13 b , allow the introduction of a venous reservoir into a rigid container without compromising the sterility of the blood contacting surfaces of the venous reservoir . as well known in the art , the blood contacting surfaces of a venous reservoir consist of at least the inside walls of the blood chamber as well as that of the inlet , the outlet , and the air removal tubes . thus , the present invention overcomes one of the major obstacles , though not mentioned as such in the description of the prior art , inherent in prior art ssr intended to be sealed within a housing , see aforementioned u . s . pat . no . &# 39 ; 045 and pct &# 39 ; 08734 . cover 1389 may also incorporate tubing connectors 1389 aa , 1389 bb , 1389 cc , and 1389 dd , shown in fig1 f , that facilitate assembly of bag tubing and eliminate the need for separate tubing connectors . thus , inlet tube 1301 is sealed ( e . g . solvent bonded ) to the bottom of inlet connector 1389 aa , said inlet connector providing fluid communication between itself and said inlet tubing . similarly , outlet tube 1305 is sealed to the bottom of outlet connector 1389 bb , said outlet connector forming fluid communication between itself and said outlet tubing . to further enhance the functionality of outlet connector 1389 bb , unidirectional valve 1305 c may be placed within outlet connector 1389 bb . one - way valve 1305 is a safety feature that prevents back flow from the arterial line , 157 shown in fig1 should arterial pump 1104 stop . air removal tube 1304 is sealed to the bottom of air removal connector 1389 cc , said connector forming fluid communication between itself and said air removal tubing . like connector 1389 bb , air removal connector 1389 cc may incorporate unidirectional valve 1304 c . this valve assures that air cannot enter the bag via connector 1389 cc . lastly , infusion tube 1306 is sealed ( e . g . solvent bonded ) to the bottom of infusion connector 1389 dd , said infusion connector forming fluid communication between itself and said infusion tubing . an additional advantage of incorporating rigid connectors into cover 1389 : they provide physical strength to the cover further preventing buckling under high vacuum . [ 0150 ] fig1 f also illustrates means that assure the pressure on the gas side 1105 c of microporous oxygenator 1105 , not fall below that of chamber 1309 . this is achieved by applying the same suction to the outlet of gas port of oxygenator 1105 as is applied to chamber 1309 of fig1 a . thus , vacuum is provided by vacuum regulator 813 via tube 818 to three - way valve 1391 . three - way valve 1391 channels the regulated vacuum to tube 1390 a , said tube in fluid communication with chamber 1309 , seen in fig1 a and 13 b , via connector 1308 placed in housing wall 1388 , see fig1 f . valve 1391 also channels the regulated vacuum to tube 1390 b , said tube in fluid communication with gas side chamber 1105 b of oxygenator 1105 . tube 1390 b is also in fluid communication with one - way valve 1392 , caged in structure 1393 a having opening 1393 b to atmosphere , said one - way valve opening when pressure in tube 1390 b exceeds atmospheric pressure . a similar one - way valve 1394 , is in fluid communication with tube 1390 a connecting suction port 1308 of housing 1388 to said three - way valve 1391 . valve 1394 opens when the pressure in tube 1390 a exceeds atmospheric pressure . both valves 1392 and 1394 provide safety and assure that in the event vacuum , applied to either tube 1390 a or 1390 b , fail , the pressure in said tubes not be built but rather exhaust to atmosphere . it is important the valves 1392 and 1394 have very low cracking pressure , preferably below 10 mmhg . it is also important that these valves present a low resistance to gas flow , preferably requiring no more than 10 mmhg pressure drop at an air flow of 10 l / min . similarly , vacuum regulator 813 , when used to apply suction to oxygenator 1105 , should accommodate gas flows exceeding that expected for oxygenator 1105 , or 12 l / min for adults . three - way valve 1391 preferably allows the user to apply suction to chamber 1309 via tube 1309 a but not to oxygenator 1105 , apply suction to both chamber 1309 and oxygenator 1105 , or not to apply suction to either chamber 1309 or oxygenator 1105 . applying suction to the gas side of the oxygenator can reduce o 2 transfer rate because the partial pressure of o 2 , po 2 , on the gas side is lowered by the percentage decrease in total pressure on the gas side . thus , when suction of − 50 mmhg is applied to the gas side , the total pressure is lowered by 50 / 760 or 7 % thereby nominally reducing the o 2 exchange by 7 %. considering that the percent o 2 used in the sweep gas is less than 100 %, it is possible to compensate for decreased total pressure by increasing the % of o 2 in the sweep gas . to avoid reduction in o 2 exchange , it is desirable to apply suction to the gas side only when there is none or very low blood flow . low blood flow can be indicated by low pressure on the blood side . to achieve this desirable result , suction applied to the gas side of the oxygenator is throttled with valve 1391 , said valve responding to pressure readings taken of arterial line 157 shown in fig1 . for example , when the pressure in line 157 falls below 100 mmhg ( a pressure indicating low blood flow ), a signal is sent to direct valve 1391 to apply suction to gas exhaust line 1390 b of oxygenator 1105 shown in fig1 f . it should be pointed out that the decrease in o 2 exchange due to suction application on the gas side ( i . e . reduction in po 2 ) is compensated by longer residence time of the blood ( lower blood flow ). applying vacuum to the gas side has no adverse affect on co 2 exchange . the scope of the invention should not be limited to the aforementioned embodiments . the invention can be extended to other embodiments as illustrated with the venous reservoir having a single flexible wall assigned to cordis dow corp and made by c . r . bard ( u . s . pat . no . 4 , 424 , 190 ). currently , there are no means to apply suction to the venous blood utilizing this bard venous reservoir . with the present invention , applying suction to this design of a venous reservoir is simple . fig1 a , a three dimensional view , 10 b , a cross sectional view of 103 , and 10 c , a cross sectional view along lines 10 c and 10 c ′ shown in fig1 b , all illustrate a modification of the venous reservoir component shown in fig1 of pat . no . &# 39 ; 190 . blood enters venous reservoir 103 at inlet 101 into chamber 102 , said chamber formed by rigid wall 1019 and flexible wall 1018 , shown in a semi - full position . wall 1018 is also shown in an almost empty position as indicated by dashed line 1018 ′. flexible wall is sealed to rigid wall 1019 along periphery 1019 a , said seal made by solvent bonding , rf welding , ultrasonic welding or other appropriate method . air entering expandable blood chamber 102 is extracted via gas exhaust port 104 . gas exhaust port 104 may incorporate an automated gas removal means , as shown for example , utilizing a hydrophobic membrane as described in reference to fig5 a . blood exits via outlet tube 105 . for augmented venous return , the present invention adds face plate 108 that seals the external surface of flexible wall 1018 along periphery 108 a of face plate 108 , forming sealed pressure chamber 107 . the seal 108 a and seal 1019 a therefore can sandwich the free ends of flexible wall 1018 and can be made simultaneously . gas port 108 b is in fluid communication with sealed pressure chamber 107 , and is preferably connected to vacuum regulator 813 shown and previously described in reference to fig8 a and 12 a . faceplate 108 , is preferably clear and rigid such as clear pvc , polycarbonate , polyethylene terephtalate ( pet ), polyethylene terephtalate glycol ( petg ), polyester , or alike . faceplate 108 does not have to be biocompatible because it does not contact blood . it should be clear that by incorporating sealing means between faceplate 108 and flexible wall 1018 , similar to those described in reference to fig8 a , faceplate 108 could be made nondisposable . whether disposable or not , faceplate 108 forming pressure chamber 107 allows the user to apply suction to chamber 107 via port 108 b , said suction transmitted to the blood via flexible wall 1018 thereby providing augmented venous return . [ 0153 ] fig1 b shows nondisposable cover 108 rests within lip 1019 aa of disposable rigid structure 1019 where it is held lightly . when vacuum is applied to suction port 108 b of nondisposable cover 108 , the user would hold cover 108 against periphery 1019 a of structure 1019 . seal material 1082 a , located along the periphery of cover 108 , is then compressed therebetween forming sealed chamber 107 . the suction within chamber 107 would pull disposable structure 1019 and nondisposable cover 108 together . thus , the pressure difference across faceplate 108 is used for forming a tighter seal and holding cover 108 . as described in reference to cover 1389 shown in fig1 a , should vacuum fail , any pressure buildup in chamber 107 would push faceplate 108 open to relieve said pressure . it should be understood that a comprehensive description of each of the applications of the invention is beyond the scope of a patent application and therefore the aforementioned descriptions are given as illustrations and should not be used to limit the intent , spirit , or scope of the invention . with that in mind , | 8 |
hereinafter , the preferable embodiments of the present invention will be described with reference to the appended drawings . fig1 is a schematic drawing which shows a typical image forming apparatus which employs the image heating apparatus in one of the embodiments of the present invention . this image forming apparatus is a color laser printer which employs an electrophotographic process . a referential code 101 designates a photosensitive drum as an image bearing member , for example , an organic photosensitive member , an amorphous silicon based photosensitive member , and the like , and is rotationally driven in the counterclockwise direction , indicated by an arrow mark , at a predetermined process speed ( peripheral velocity ). as the photosensitive drum 101 is rotationally driven , it is uniformly charged the predetermined polarity and potential level by a charging apparatus 102 such as a charge roller . then , the charged surface of the photosensitive drum 101 is exposed to a laser beam 103 outputted in a scanning manner , while being modulated with image formation information , from a laser optics box ( laser scanner ) 110 . more specifically , the laser optics box 110 scans the peripheral surface of the photosensitive drum 101 with the laser beam 103 , which it outputs , while modulating ( turning on or off ) the beam 103 with sequential electric digital signals which reflect image formation information , and which are sent from an unillustrated image signal generating apparatus such as an image reading apparatus . as a result , an electrostatic latent image which reflects the image formation information is formed on the peripheral surface of the photosensitive drum 101 . designated by a referential code 109 is a mirror for deflecting the laser beam from the laser optics box 110 , onto the specific points on the peripheral surface of the photosensitive drum 101 which are to be exposed . in an image forming operation in which a full - color image is formed , a target image , that is , a full - color image , is separated into primary color components . first , a latent image which corresponds to a first color component , for example , yellow component , of the target image , is formed through the scanning exposure . the thus formed latent image is developed into an image formed of yellow toner ( yellow toner image ) through the operation of a yellow component developing device 104 y , which is one of the four color component developing devices 104 . then , the yellow toner image is transferred onto the peripheral surface of an intermediary transfer drum 105 , in a primary transfer station t 1 , that is , the place where contact is made between the photosensitive drum 101 and intermediary transfer drum 105 ( where the gap between the photosensitive drum 101 and intermediary transfer drum 105 is smallest ). after the transfer of the toner image onto the peripheral surface of the intermediary transfer drum 105 , the peripheral surface of the photosensitive drum 101 is cleaned by a cleaner 107 ; the residue , such as the toner which remains on the photosensitive drum 101 after the transfer , on the peripheral surface of photosensitive drum 101 , is removed by the cleaner 107 . the above described process cycle which comprises the charging , scanning or exposing , developing , primary transferring , and cleaning processes is also carried out for a second component ( for example , magenta component , for which a magenta component developing device 104 m is operated ), a third component ( for example , cyan component , for which a cyan component developing device 104 c , and a fourth component ( for example , black component , for which a black component developing device 104 bk is operated ), in a sequential order . as a result , four color toner images , that is , a yellow toner image , a magenta toner image , a cyan toner image , and a black toner image , are sequentially placed in layers on the peripheral surface of the intermediary transfer drum 105 , forming a full - color image of the target full - color image . the intermediary transfer drum 105 comprises a metallic drum , an elastic layer placed on the peripheral surface of the metallic drum , and a surface layer coated on the elastic layer . the elastic layer has an intermediary electrical resistance , whereas the surface layer has a high electrical resistance . the intermediary transfer drum 105 is disposed so that its peripheral surface is placed actually or virtually in contact with the peripheral surface of the photosensitive drum 101 . it is rotationally driven in the clockwise direction , indicated by an arrow mark , at the same peripheral velocity as the photosensitive drum 101 , and bias , that is , difference in electrical potential level , is provided between the metallic drum of the intermediary transfer drum 105 , and the photosensitive drum 101 . as a result , the toner images on the photosensitive drum 101 are transferred onto the intermediary transfer drum 105 by the difference in electrical potential level . the color toner images formed on the peripheral surface of the intermediary transfer drum 105 are transferred , in a secondary transfer station t 2 , that is , the contact nip between the intermediary transfer drum 105 and a transfer roller 106 , onto the surface of a recording medium p sent into the secondary transfer station t 2 from an unillustrated sheet feeding portion with predetermined timing . more specifically , the transfer roller 106 supplies the recording medium p with electrical charge , the polarity of which is opposite to that of the toner , from the back side of the recording medium p . as a result , the four color toner images , which synthetically form a single full - color image , are transferred together from the peripheral surface of the intermediary transfer drum 105 onto the recording medium p , starting from the leading end of the recording medium p , as the recording medium p is conveyed forward . after passing through the secondary transfer station t 2 , the recording medium p is separated from the peripheral surface of the intermediary transfer drum 105 , and then is introduced into a fixing apparatus 100 ( image heating apparatus ), in which the unfixed toner images are thermally fixed to the recording medium p . thereafter , the recording medium p is discharged into an unillustrated delivery tray located outside the image forming apparatus . the fixing apparatus 100 will be described later in more detail . after the transferring of the color toner images onto the recording medium p , the intermediary transfer drum 105 is cleaned by a cleaner 108 ; the residue , such as the toner particles , paper dust , and the like , left behind on the intermediary transfer drum 105 after the transfer , is removed by the cleaner 108 . when not activated , the cleaner 108 is not kept in contact with the intermediary transfer drum 105 ; it is placed and kept in contact with the intermediary transfer drum 105 during the secondary transfer process in which the color toner images are transferred from the intermediary transfer drum 105 onto the recording medium p . also , the transfer roller 106 is not kept in contact with the intermediary transfer drum 105 when not activated ; it is pressed against the intermediary transfer drum 105 , with the recording medium p pinched between the transfer roller 106 and intermediary transfer drum 105 , during the secondary transfer process in which the color toner images are transferred from the intermediary transfer drum 105 onto the recording medium p . the image forming apparatus in this embodiment is enabled to operate also in a monochromatic printing mode ; for example , it is capable of creating a black - and - white image . it is also enabled to operate in a double - sided printing mode , and a multilayer printing mode . in a double - sided printing mode , after a set of toner images is formed on one of the two surfaces of the recording medium p , and the recording medium p is discharged from the fixing apparatus 100 , the recording medium p is turned over through an unillustrated recirculating mechanism , and sent back into the secondary transfer station t 2 , in which another set of toner images is transferred onto the other side of the recording medium p . thereafter , the recording medium p is again introduced into the fixing apparatus 100 , in which the second set of toner images is fixed to the recording medium p . then , the recording medium p , both sides of which bear a fixed image at this point , is outputted as a double - side print . in a multilayer printing mode , after a set of toner images is formed on one of the two surfaces of the recording medium p , and the recording medium p is discharged from the fixing apparatus 100 , the recording medium p is again sent into the secondary transfer station t 2 without being turned over through the unillustrated recirculating mechanism . in the secondary transfer station t 2 , another set of toner images is transferred onto the very surface of the recording medium p , to which the first set of toner images has been already fixed . thereafter , the recording medium p is introduced again into the fixing apparatus 100 , in which the second set of toner images is fixed , and the recording medium p is outputted as a multilayer print . next , an image heating apparatus in accordance with the present invention will be described with reference to fig1 - 3 . the image heating apparatus in accordance with the present invention is such an image heating apparatus ( fixing device ) that comprises a cylindrical fixing film ( fixing belt ) as a heating member , in which heat can be electromagnetically induced . it employs an electromagnetic heat induction system , and a pressure roller driving system . fig1 is a schematic sectional view of the essential portion of the thermal image fixing apparatus 100 as an image heating apparatus in accordance with the present invention , at a plane parallel to the side walls of the thermal image fixing apparatus 100 ( at the line ( 1 )—( 1 ) in fig2 ). fig2 is a schematic front view of the essential portion of the apparatus in fig1 with some portions of the apparatus unillustrated . fig3 is a schematic , longitudinal sectional view of the apparatus in fig1 with some portions of the apparatus unillustrated ( at the line ( 3 )—( 3 ) in fig1 ). this apparatus 100 can be roughly divided into three members : first , second , and third members . the first member is a film guiding member 2 , which is a trough - like member , and is approximately semicircular in cross - section . in fig1 the film guiding member 2 looks like a cylindrical member , the left half of which is missing . the second member is a cylindrical fixing film 1 , which is loosely fitted around the film guiding member 2 , and a film guiding member 9 disposed in a manner to cover the left side of the film guiding member 2 , and in which heat can be electromagnetically induced . the third member is a pressure roller 5 , which is disposed below the film guiding member 2 so that it forms a nip n against the bottom surface of the film guiding member 2 , with the fixing film pinched between the pressure roller 5 and the film guiding member 3 . on the inward side of the film guiding member 2 , a combination of an exciter coil 3 and a magnetic core 4 is disposed as a magnetic field generating means . the pressure roller 5 comprises a metallic core 5 a , and an elastic layer 5 b coated , in the form of a roller coaxial with the metallic core 5 a , around the metallic core 5 a . the material for the elastic layer 5 b is elastic , heat resistant material such as silicone rubber , fluorinated rubber , fluorinated resin , or the like . it is rotationally supported between the side walls of the unillustrated chassis of the image apparatus ; the longitudinal ends of the metallic core 5 a are supported by bearings . the film guiding member 2 , around which the fixing film 1 is fitted , is disposed on the top side of the pressure roller 5 . it is kept under the downward pressure generated by a pair of pressure applying mechanisms 8 and 8 , which apply pressure to the correspondent longitudinal ends of a rigid stay 6 put through the space on the inward side of the film guiding member 2 . with this arrangement , the bottom surface of the film guiding member 2 , and the upwardly facing surface of the pressure roller 5 , are pressed against each other , with the fixing film 1 pinched between the two surfaces , forming the fixing nip n . the pressure roller 5 is rotationally driven by a motor , which constitutes a driving means m ( fig1 ), in the counterclockwise direction indicated by the arrow mark . as the pressure roller 5 is rotationally driven , the rotational force from the pressure roller 5 acts on the fixing film 1 due to the presence of the friction between the pressure roller 5 and the outwardly facing surface of the fixing film 1 , in the fixing nip n . as a result , the fixing film 1 is rotated around the film guiding members 2 and 9 in the clockwise direction indicated by the arrow mark , at a peripheral velocity approximately equal to the peripheral velocity of the pressure roller 5 , with the inwardly facing surface of the fixing film sliding on the bottom surface of the film guiding member 2 while remaining in contact therewith , within the fixing nip n ( pressure roller driving system ). in order to improve the slidableness of the inwardly facing surface of the fixing film 1 against the bottom surface of the film guiding member 2 within the fixing nip n , in other words , in order to reduce the friction between the two surfaces within the fixing nip n , the bottom surface of the film guiding member 2 is provided with a slippery member 10 , which is correspondent in position to the fixing nip n . as for the material for the slippery member 10 , a plate of pi ( polyimide ), a plate of alumina coated with glass , or the like , is used , which is superior in heat resistance , and on which the fixing film 1 easily slides . in order to further improve the slidableness , lubricant such as grease is coated on the inwardly facing surface of the fixing film 1 , in addition to the provision of the slippery member 10 , so that the lubricant is provided between the slippery member 10 and the fixing film 1 , within the fixing nip n . designated by referential codes 7 and 7 are flanges fitted one for one in the longitudinal ends of the film guiding member 2 . the flanges control the deviation of the fixing film 1 in the longitudinal direction of the film guiding member 2 ; as the fixing film 1 deviates in the longitudinal direction of the film guiding member 2 from its normal position , it comes in contact with one of the flanges by its corresponding edge , being thereby prevented from further deviation . the flanges 7 and 7 may be structured so that they rotate following the rotation of the fixing film 1 . thus , while the pressure roller 5 is rotationally driven , and the fixing film 1 rotates following the rotation of the pressure roller 5 , heat is electromagnetically induced within the fixing film 1 , as the heating member , by the magnetic field generated by the power supplied to the exciter coil 3 from an exciter circuit 12 . as a result , the temperature of the fixing nip n is increased to , and kept at , a predetermined level . in this state , the recording medium p , on which a toner image t ( unfixed ) has been formed , is sent into the fixing nip n from the image forming means , between the fixing film 1 and pressure roller 5 , with the recording medium p surface with the toner image facing upward , that is , facing the fixing film 1 , and then is passed through the fixing nip n along with the fixing film 1 , being pinched between the fixing film 1 and the pressure roller 5 so that the recording medium p surface with the toner image is kept tightly in contact with the outwardly facing surface of the fixing film 1 . the portion of the fixing film 1 , in which heat is actually generated by the function of the magnetic field generating means when the fixing film 1 is standing still , is the right - hand side of the fixing film 1 , which is adjacent to the exciter coil 3 and magnetic core 4 ( fig1 ). while the recording medium p is conveyed through the fixing nip n , being pinched therein , along with the fixing film 1 , the unfixed toner image t on the recording medium p is fixed to the recording medium p by being heated by the heat electromagnetically induced in the fixing film 1 . after being passed through the fixing nip n , the recording medium p is separated from the peripheral surface of the rotating fixing film 1 , and is conveyed further to be discharged . also after being passed through the fixing nip n , the thermally fixed toner image t on the recording medium p cools down to become a permanently fixed image . fig5 is a schematic drawing which shows the laminar structure of the fixing film 1 . the fixing film 1 in this embodiment is a piece of laminar film , and comprises a heat generating layer 1 a , an elastic layer 1 b laminated on the outwardly facing surface of the heat generating layer 1 a , and a mold releasing layer 1 c laminated on the outwardly facing surface of the elastic layer 1 b . the heat generating layer 1 a is formed of metallic film or the like , and functions as the base layer of the fixing film 1 in which heat is electromagnetically induced . a primer layer may be provided between the heat generating layer 1 a and elastic layer 1 b , and between the elastic layer 1 b and mold releasing layer 1 c , to glue the three layers together . in the approximately cylindrical fixing film 1 , the heat generating layer 1 a constitutes the inwardly facing layer , and the mold releasing layer 1 c constitutes the outwardly facing layer . as described above , as an alternating magnetic flux acts on the heat generating layer 1 a , eddy current is generated within the heat generating layer 1 a . as a result , heat is generated within the heat generating layer 1 a . since the fixing film 1 is rotationally driven , heat is electromagnetically induced through the entirety of the fixing film 1 , and the recording medium p passed through the fixing nip n is heated by the thus generated heat . consequently , the toner image 5 is thermally fixed to the recording medium p . as for the material for the heat generating layer 1 a , ferromagnetic material such as nickel , iron , ferromagnetic sus , nickel - cobalt alloy , or the like , is desirable . as for the thickness of the heat generating layer 1 a , a range of 1 - 100 μm is desirable because of the relationship between the electromagnetic energy absorbency of the film and the rigidity of the film . the elastic layer 1 b is a layer necessary to cause the heating surface ( surface of the mold releasing layer 1 c ) to conform to the unevenness of the recording medium p or toner layer so that the image is prevented from becoming uneven in glossiness . as for the material for the elastic layer 1 b , material such as silicone rubber , fluorinated rubber , fluoro - silicone rubber , or the like , which is superior in heat resistance and thermal conductivity , is used . the elastic layer 1 b is desired to be in a range of 10 - 500 μm in thickness , and to have a hardness of no more than 60 degrees ( jis - a : jis - k , a - type tester ). the mold releasing layer 1 c is in a range of 1 - 100 μm in thickness . as for the material for the mold releasing layer 1 c , fluorinated resin ( pfa , ptfe , fep ), silicone resin , fluoro - silicone rubber , fluorinated rubber , silicone rubber , or the like , which is superior in mold releasing property and heat resistance , is used . in order to further improve the efficiency with which heat is supplied to the recording medium p , the free surface ( the heat generating layer surface which faces opposite to the elastic layer 1 b ) of the heat generating layer 1 a of the fixing film 1 may be covered with a heat insulating layer 1 d , as shown in fig6 . as for the material for the heat insulating layer 1 d , heat resistant resin , for example , fluorinated resin ( pfa , ptfe , fep ), polyimide , polyamide - imide , peek , pes , pps , or the like , is desirable . the thickness of the heat insulating layer 1 d is desired to be within a range of 10 - 1 , 000 μm . with the provision of the heat insulating layer 1 d , the heat generated in the heat generating layer 1 a is prevented from conducting inward of the loop of the fixing film 1 . therefore , the efficiency with which the heat is supplied toward the recording medium p side is improved , compared to a fixing film without the heat insulating layer 1 d . consequently , power consumption is reduced . the film guiding member 2 must assure that the exciter coil 3 is electrically insulated from the fixing film 1 . therefore , material such as phenol resin , polyimide , polyamide , polyamide - imide , peek , pes , pps , pfa , ptfe , fep , lcp , or the like , which is excellent in electrically insulating property and heat resistance , is used as the material for the film guiding member 2 . the film guiding member 2 plays a role in pressing the fixing film 1 against the pressure roller 5 in the contact area ( fixing nip n ), supporting the combination of the exciter coil 3 and magnetic core 4 as the magnetic field generating means , supporting the fixing film 1 , and assuring stability in the rotational conveyance of the fixing film 1 . the film guiding member 9 is the same as the film guiding member 2 in terms of material . it also supports the fixing film 1 , and assures stability in the rotational conveyance of the fixing film 1 . the exciter coil 3 is a coil constituted of a plurality of pieces of fine copper wire , which are individually coated for electrical insulation , are bound together , and are wound together a few times . in this embodiment , polyimide is used as the heat resistant and electrically insulating coating material for the wires of the exciter coil 3 . the number of times the exciter coil 3 is wound is eight ( eight turns ). the exciter coil 3 is formed ( wound ) so that it conforms to the inward surface of the film guiding member 2 to make it possible to generate heat in as large an area of the heat generating film as possible . the diameter of each piece of fine wire , and the cross sectional size of the bundle of the fine wires , and the like , are determined by the amount of the electrical current to be flowed through the exciter coil 3 . in this embodiment , 98 pieces of bundled fine wires with a diameter of 0 . 2 mm ( approximately 3 . 1 mm 2 in the cross sectional size of the bundle ) are used . to the exciter coil 3 , the exciter circuit 12 is connected . this exciter circuit 12 is enabled to generate high frequency waves in a range of 20 khz to 500 khz with the use of a switching power source . the exciter coil 3 generates an alternating magnetic flux by being supplied with alternating current ( high frequency current ) which is supplied from the exciter circuit 12 . the magnetic core 4 is a core high in magnetic permeability . it is t - shaped in cross section . as for the material for the magnetic core 4 , ferrite , permalloy , or the like , which is used as the material for a transmission core , is desirable , preferably , ferrite which is small in loss even when the frequency is no less than 100 khz . the temperature of the fixing nip n is controlled by a temperature controlling system inclusive of a temperature detecting member 11 ( apparatus temperature detecting means in fig1 ). more specifically , the electrical current supply to the exciter coil 3 is controlled by the temperature controlling system so that the amount of the heat electromagnetically induced within the fixing film 1 is controlled . as a result , the temperature of the fixing nip n is maintained at a predetermined level . the temperature detecting member 11 is a temperature sensor , such as a thermistor , for detecting the temperature of the fixing film 1 . in this embodiment , the temperature detecting member 11 is disposed within the loop of the fixing film 1 , elastically in contact with the inwardly facing surface of the fixing film 1 , on the downstream side of the fixing nip n in terms of the rotational direction of the fixing film 1 . the information regarding the temperature of the fixing film 1 measured by the temperature sensor 11 is inputted as the apparatus temperature information into a control circuit 13 . the current supply to the exciter coil 3 is controlled according to the thus inputted temperature information to control the amount of the heat electromagnetically induced in the fixing film 1 so that the temperature of the fixing nip n is kept at the predetermined level . as described above , both longitudinal ends of the rigid pressure application stay 6 put through the space on the inward side of the film guiding member 2 are pressed downward by the pressure generated by the pressure applying mechanisms 8 and 8 , so that the bottom surface of the film guiding member 2 is pressed against the upwardly facing surface of the pressure roller 5 , with the fixing film 1 pinched between the two surfaces , to form the fixing nip n . the pressure applying mechanisms 8 and 8 disposed one for one at both longitudinal ends of the rigid pressure application stay 6 are enabled to vary the amount of the pressure they apply . each pressure applying mechanism 8 comprises a pressure generating spring 8 a , a spring seating member 8 b , an oval cam 8 c ( pressure adjusting member ), a cam shaft 8 d , a driving mechanism 8 e , and the like . the pressure generating spring 8 a is disposed so that its bottom end is seated against the upwardly facing surface of the corresponding longitudinal end of the rigid pressure application stay 6 , and the top end of the pressure generating spring 8 a is seated against the spring seating member 8 b disposed above the pressure generating spring 8 a . the oval cam 8 c is placed in contact with the spring seating member 8 b . the cam shaft 8 d is rotated by the driving mechanism 8 e to rotate the cam 8 c . the pressure generating spring 8 a is disposed in the compressed state between the upwardly facing surface of the corresponding longitudinal end of the rigid pressure generation stay 6 and the cam 8 c . the reactive force from the compression of the pressure generating spring 8 a acts as the pressure which applies to the recording medium p within the fixing nip n . the driving mechanism 8 e comprises a clutch solenoid , or the like . it is controlled by the control circuit 13 to intermittently rotate the cam shaft 8 d by 90 degrees to intermittently rotate the cam 8 c by 90 degrees . the left and right pressure generating mechanisms 8 and 8 are intermittently rotated by 90 degrees in synchronous phase . as the oval cam 8 c is intermittently rotated by 90 degrees so that the major axis of the oval cam 8 c becomes vertical as shown in fig1 - 3 , in other words , so that the oval cam 8 c is positioned to cause the high lift portion of the cam 8 c to be in contact with the spring seating member 8 b , the amount by which the pressure generating spring 8 d is compressed increases , creating pressure application state b , in which pressure is applied to the recording medium p by the amount ( for example , 30 kgf ) necessary for the proper thermal fixation of a toner image in the fixing nip n . when the oval cam 8 c is laid sideways , in other words , when the oval cam 8 c is positioned so that the low lift portion of the over cam 8 c is caused to be in contact with the spring seating member 8 b , the amount by which the pressure generating spring 8 a is compressed is relatively small , creating pressure application state a , in which the pressure which applies to the recording medium p within the fixing nip n is smaller ( for example , 10 kgf ) than that in the above described pressure application state b . the pressure applied in the pressure application state a is greater than zero . in other words , the image fixing apparatus 100 in this embodiment is enabled to apply two different levels of pressures to the recording medium p . further , in order to assure that a toner image is properly fixed to special purpose recording medium , such as high gloss paper or thick paper , the image fixing apparatus 100 in this embodiment is set up so that the pressure applied in the pressure application state b by this fixing apparatus 100 is greater , compared to the pressure applied by a conventional fixing apparatus . next , this fixing apparatus will be described regarding the driving control . fig7 is a flow chart which shows a method for controlling the fixing apparatus in this embodiment . upon receiving a fixing operation initiation instruction , that is , an instruction for initiating an image heating operation ( step 1 ), the control circuit 13 confirms the state of pressure application ( step 2 ). when the apparatus is not in the pressure application state a , the control circuit 13 controls the pressure applying mechanisms 8 and 8 so that the fixing nip n is placed in the pressure application state a , that is , the low pressure application state , by the pressure adjusting members ( cams ) 8 c and 8 c ( step 3 ). while a power source is off , or the apparatus is on standby , the fixing nip n is placed in the pressure application state a , that is , the low pressure state , by the pressure adjusting members 8 c and 8 c to prevent deformation or the like . next , the control circuit 13 rotationally drives the pressure roller 5 by the driving means m while keeping the fixing nip n in the pressure application state a , and flows rated current through the exciter coil 3 from the exciter circuit 12 to begin electromagnetically inducing heat in the fixing film 1 ( step 4 ). as the pressure roller 5 is rotationally driven , the rotational force from the pressure roller 5 acts on the fixing film 1 due to the presence of the friction between the pressure roller 5 and the outwardly facing surface of the fixing film 1 , in the fixing nip n . as a result , the fixing film 1 is rotated around the film guiding members 2 and 9 , while being heated , with its inwardly facing surface sliding on the slippery member 10 and film guiding member 2 , tightly in contact therewith , at a peripheral velocity approximately equal to the rotational speed of the pressure roller 5 . the fixing film 1 is rotated and heated for a predetermined length of time ( for example , 15 seconds ), with the fixing nip n kept in the pressure application state a , and then , the pressure application state is changed from the state a to the state b by the operation of the pressure adjusting member ( step 5 6 ). thereafter , the fixing apparatus is controlled so that the temperature within the fixing nip n remains at a predetermined level ( for example , 180 ° c .) suitable for image fixation ; the fixing apparatus is controlled so that the fixing apparatus remains in the state in which image fixation is possible ( step 7 ). naturally , when the temperature in the fixing nip n is low , the friction between the fixing film 1 and pressure roller 5 is relatively high . in particularly , when grease is present between the filing film 1 and pressure roller 5 , the friction between the fixing film 1 and guiding member 2 is relatively high because the viscosity of the grease is higher when temperature is lower . however , with the provision of the above described arrangement for apparatus control , when a fixing apparatus is started up , it is possible to reduce the torque required when starting up the fixing apparatus , in order to assure that fixing film properly slides . therefore , even when a fixing apparatus is started up in a low temperature environment in which higher torque is required to start up a fixing apparatus , it is assured that the fixing film 1 smoothly slides ; the pressure roller 5 is prevented from being rotated . in other words , with the provision of the above described arrangement for apparatus control , the amounts of the pressure , as well as the sizes of the contact areas , between the fixing film 1 and slippery member 10 , and between the fixing film 1 and the outwardly facing surface of the film guiding member 2 , can be reduced by reducing the amount of the pressure applied by the pressure applying members , in other words , by placing a fixing nip n in the pressure application state a ( steps 2 and 3 ), so that the frictional resistance at the aforementioned contact areas is reduced to reduce the torque required at the time of starting up a fixing apparatus . therefore , the slidableness of the fixing film 1 is assured to prevent the fixing film 1 from failing to move . further , the fixing film 1 is rotated and heated , while the fixing nip n is kept in the state a ( step 4 ), for a predetermined length of time to increase the temperature of the fixing film 1 . as the temperature of the fixing film 1 increases , the temperature of the slippery member 10 and grease also increases , making it easier for the fixing film 1 to slide . therefor , the torque required for rotational driving the fixing film 1 further reduces . after the elapsing of the predetermined length of time necessary to assure that the fixing film 1 smoothly slides , the fixing nip n is placed in the pressure application state b ( step 5 6 ), to increase the amount of the pressure applied by the pressure applying members so that a proper amount of pressure is generated in the fixing nip n . thus , when a fixing apparatus which requires high fixing pressure is started up in a low temperature environment , it is possible to reduce the amount of the initial torque necessary for the startup . therefore , it is possible to prevent the occurrences of inconveniences . for example , it is possible to prevent the fixing film 1 from failing to slide , to prevent warm - up time from becoming excessively long , or to prevent the fixing film 1 from being damaged . in addition , with the provision of the above described arrangement for apparatus control , high fixing pressure necessary when forming an image on special purpose recording medium , such as high gloss paper or thick paper , can be easily obtained , and therefore , it is possible to prevent the problem that a toner image fails to be properly fixed . further , it is possible to prevent the motor from breaking down due to an excessive amount of external load . table 1 shows the amount of the initial torque measured when the fixing apparatus in this embodiment is started up in a low temperature environment , and the results of the evaluation of the images fixed to thick paper . table 1 also presents the results of two cases in which the fixing pressure was not adjusted by the pressure application members 8 c and 8 c , that is , in which the fixing apparatus was kept in the high pressure state ( comparative example 1 : equivalent to pressure application state b ) and low pressure state ( comparative example 2 : equivalent to pressure application state a ). as is evident from table 1 , in the case of comparative example 1 , the required initial torque was in a range of 15 - 25 kgf · cm , which was rather high , causing the fixing film 1 to remain standing still for a while when the fixing apparatus was started up in a low temperature environment . as a result , the problems occurred ; for example , it took a long time for the fixing apparatus to warm up , and / or damages occurred to the fixing film 1 . in the case of comparative example 2 , the required initial torque was 8 kgf · cm , which did not prevent the fixing film from moving . however , the amount of the fixing pressure was not sufficient , and therefore , fixed images were not good ; they suffered from fixation failure . on the contrary , in the case of the fixing apparatus in this embodiment , the required initial torque was 8 kgf · cm , and the fixing film 1 did not fail to move . as a result , images were satisfactorily fixed . in other words , according to the present invention , even in the case of a fixing apparatus which requires a higher amount of fixing pressure , its fixing film can be prevented from failing to move , by adjusting the pressure applied to the fixing nip when the fixing apparatus is started up in a low temperature environment , as in the case of the fixing apparatus in this embodiment . therefore , it is possible to prevent such problems that warm - up time is long , and / or that the fixing film is damaged . when the fixing apparatus in this embodiment is started up in a low temperature environment , it reaches 150 ° c . or higher , which is high enough to assure that the fixing film smoothly slides by being assisted by the grease , slippery member 10 , and the like , in 15 seconds after power begins to be supplied thereto . the length of 15 seconds , which is set for the fixing apparatus in this embodiment , is determined based on the length of time necessary for the fixing apparatus to reach a specific temperature level ( 150 ° c . in this embodiment ) which assures that the fixing film smoothly slides . these values ( temperature , time ) vary depending upon the configuration of an individual fixing apparatus ( torque , total thermal capacity , fixing pressure ), amount of supplied power , and the like , and therefore , they are optionally set according to these factors . fig8 is a flow chart which shows the method for controlling a fixing apparatus , in another embodiment of the present invention . in this embodiment , the fixing apparatus is controlled so that the pressure applied by the pressure application members is switched according to the temperature detected by the temperature detecting member 11 . more specifically , upon reception of an instruction for initiating a fixing operation ( step 1 ), the control circuit 13 determines , based on the temperature detected and inputted by the temperature detecting member 11 , whether or not the temperature t detected at the beginning of the fixing operation is no more than a predetermined temperature t 1 ( for example , 70 ° c .) ( step 2 ). when the detected temperature t is no more than the referential temperature t 1 , the rotating and heating of the fixing film are started , with the fixing nip n placed in the pressure application state a ( when the fixing nip n is in the pressure application state b , the pressure application state of the fixing nip n is switched to the state a , whereas the fixing nip n is in the pressure application state a , it is left in the same state ), and the rotating and heating of the fixing film are continued until the detected temperature t reaches the referential temperature t 1 ( steps 3 , 4 , and 5 ). as the detected temperature t reaches the referential temperature t 1 , the pressure application state of the fixing nip n is switched from the state a to the state b by activating the pressure adjusting members 8 c and 8 c ( step 6 ), and the temperature is controlled so that it reaches a proper fixation temperature ( 180 ° c .) ( steps 8 and 9 ). then , after the proper fixation temperature is reached , that is , after satisfactory fixation becomes possible , an actual fixing operation is started ( steps 9 and 10 ). on the other hand , when the temperature t detected at the beginning of a fixing operation is no less than the predetermined referential temperature t 1 ( response in step 2 is yes ), the rotating and heating of the fixing film are started , with the fixing nip n placed in the pressure application state b ( when the fixing nip n is in the pressure application state a , the pressure application state of the fixing nip n is switched to the state b , whereas the fixing nip n is in the pressure application state b , it is left in the same state ) ( steps 6 , 7 , and 8 ), and the temperature is controlled so that it reaches the proper fixation temperature ( 180 ° c .) ( steps 8 and 9 ). then , after the proper fixation temperature is reached , that is , after satisfactory fixation becomes possible , an actual fixing operation is started ( steps 9 and 10 ). configuring and controlling a fixing apparatus as described above makes it possible to reduce the initial torque required when starting up the fixing apparatus , to assure that the fixing film smoothly slides . therefore , even when the fixing apparatus is started up in a low temperature environment , it is possible to prevent the fixing film from failing to move . further , when the apparatus temperature t detected at the beginning of the driving of the apparatus is no less than the predetermined referential temperature t 1 , it is unnecessary for the pressure application state of the fixing nip n to be switched to the low pressure application state a . in other words , the step for switching the pressure application state can be eliminated , and therefore , the apparatus can be readied faster for an actual fixing operation . in the case of the above described embodiment , the fixing apparatus was configured so that the pressure adjustment , rotational driving of the fixing film , and heating of the fixing film , were started after the confirmation of the pressure application state , temperature detection , and the like , which were carried out upon reception of the instruction for initiating a fixing operation . however , a fixing apparatus may be configured so that the pressure adjustment is made at the beginning of the rotational driving of a fixing apparatus , according to the structure ( film , slippery member , pressure roller , and the like ), cumulative usage time , and / or the like , of the fixing apparatus . in other words , a fixing apparatus may be structured so that the referential fixing film temperature , according to which the pressure applied by the pressure applying members is adjusted , can be varied depending on the ambient temperature and / or cumulative usage time , for example . further , in this embodiment , the referential temperature t 1 is set at a temperature ( 70 ° c . ), which is lower than the fixation temperature ( 180 ° c .). however , the referential temperature t 1 may be rendered the same as the fixation temperature as indicated by the control flow chart in fig9 . also , a fixing apparatus may be structured so that the pressure application state of the fixing nip n is switched to the pressure application state a during the post - rotation period which occurs at the end of an fixing operation . with such an arrangement , it is possible to eliminate the time otherwise necessary for the pressure adjusting mechanism operation , at the beginning of a fixing operation . the post - rotation period means the period immediately after the last recording medium has been put through the fixing apparatus 100 in a continuous printing mode ( when in a single copy mode , it is the period immediately after the single copy has been passed through the fixing apparatus 100 ). in this post - rotation period , the driving of the main motor is continued for a while after the passing of the last recording medium through the fixing apparatus 100 , to cause the apparatus to carry out predetermined post - image formation procedures . after this post - rotation period , the driving of the main motor is stopped , and the apparatus is placed on standby to be kept on standby until an instruction for initiating the next operation is inputted . further , the pressure applied during the pressure application state a may be further reduced to 4 kgf , for example , so that paper jam or the like can be dealt with while the fixing nip n is in the pressure application state a . further , from the viewpoint of reducing the amount of the load which applies to the motor , it is effective to make the rotational speed of the driver roller slower during the starting up than during the fixing operation , so that the amount of the initial torque required when starting up the fixing film is further reduced . next , another embodiment of the present invention will be described . in this embodiment , the film heating type fixing apparatus employs a ceramic heater as a heating member . the fixing apparatus 100 in this embodiment , which is shown in fig1 , can be roughly divided into a film guiding member 20 , a ceramic heater 15 as a heating member , a fixing film 1 a , and a pressure roller 5 as a pressuring member . the film guiding member 20 is a trough - like member , and is approximately semicircular in cross - section . it is heat resistant and heat insulating . it is provided with a groove , which longitudinally extends along the approximate center line of the bottom surface of the film guiding member 20 . the ceramic heater 15 is fixedly fitted in the groove of the film guiding member 20 . the fixing film 1 a is a cylindrical ( endless ) piece of heat resistant film , and is loosely fitted around the film guiding member 20 inclusive of the ceramic heater 15 . the film guiding member 20 inclusive of the ceramic heater 15 is pressed upon the pressure roller 5 , forming a nip n , with the fixing film 1 a pinched between the downwardly facing surface of the ceramic heater 15 and the pressure roller 5 . in this embodiment , the ceramic heater 15 , or the film guiding member 20 inclusive of the ceramic heater 15 , constitutes the aforementioned first member , and the fixing film 1 a constitutes the second member . the pressure roller 5 is the third member . the pressure roller 5 is an elastic pressure roller . it comprises a metallic core 5 a , and an elastic layer 5 b placed on the peripheral surface of the metallic core 5 a to reduce the hardness of the pressure roller 5 . the material for the elastic roller 5 a is silicone rubber or the like . the pressure roller 5 is rotationally supported between the unillustrated front and rear plates of the apparatus chassis ; its longitudinal ends are supported by bearings . the peripheral surface of the elastic layer 5 b may be coated with fluorinated resin such as ptfe , pfa , or fep to improve the surface properties of the pressure roller 5 . the film guiding member 20 , around which the fixing film 1 a is fitted , is disposed above the pressure roller 5 , with the ceramic heater 15 side facing downward . through the space on the inward side of the film guiding member 20 , a rigid pressure application stay 21 is put through , and a pair of pressure applying mechanisms 8 are positioned between the longitudinal ends of the pressure application stay 21 and a pair of spring seating members provided on the apparatus chassis side , one for one , so that the pressure application stay 21 is kept under downward pressure . with this arrangement , the downwardly facing surface of the ceramic heater 15 on the film guiding member 20 side is pressed against the upwardly facing surface portion of the pressure roller 5 , with the fixing film 1 a between the two surfaces , forming the fixing nip n . the pressure roller 5 is rotationally driven by a driving means m , in the counterclockwise direction indicated by an arrow mark . as the pressure roller 5 is rotationally driven , the rotational force from the pressure roller 5 acts on the fixing film 1 a due to the presence of the friction between the pressure roller 5 and the outwardly facing surface of the filing film 1 a . as a result , the fixing film 1 a is rotated around the film guiding members 20 in the clockwise direction indicated by an arrow mark , at a peripheral velocity approximately equal to the peripheral velocity of the pressure roller 5 , with the inwardly facing surface of the fixing film 1 a sliding on the downwardly facing surface of the ceramic heater 15 while remaining tightly in contact therewith within the fixing nip n ( pressure roller driving system ). in order to reduce the friction which occurs between the bottom surface of the ceramic heater 15 , that is , the surface on which the fixing film 1 a slides in the fixing nip n , and the inwardly facing surface of the fixing film 1 a , the bottom surface of the ceramic heater 15 is provided with a slippery member 15 d , which is similar to the slippery member 10 of the fixing apparatus in the preceding embodiment . further , lubricant such as heat resistant grease is provided between the slippery member 15 d and the inwardly facing surface of the fixing film 1 a . in response to a print start signal , the rotation of the pressure roller 5 is started , along with the heating up of the ceramic heater 15 . after the rotational speed of the fixing film 1 a rotated by the rotation of the pressure roller 5 becomes constant , and the temperature of the ceramic heater 15 reaches a predetermined level , a piece of recording medium p , as an object to be heated , on which a toner image t is borne , is introduced between the fixing film 1 a and pressure roller 5 , with the toner bearing surface of the recording medium p faced toward the fixing film 1 a , in the fixing nip n . then , the recording medium p is passed , along with the fixing film 1 a , through the fixing nip n , while being pressed upon the bottom surface of the ceramic heater 15 . while the recording medium p is passed through the fixing nip n , the heat from the ceramic heater 15 is given to the recording medium p through the fixing film 1 a . as a result , the toner image t is thermally fixed to the surface of the recording medium p . after passing through the fixing nip n , the recording medium p is separated from the surface of the fixing film 1 a to be further conveyed . in order to reduce the thermal capacity of the fixing film 1 a so that the fixing apparatus starts up quickly , the thickness of the fixing film 1 a is desired to be no more than 100 μm , preferably , no more than 50 μm and no less than 20 μm . the material for the fixing film 1 a may be heat resistant ptfe , pfa , or fep , which may be used in a single layer , or in the form of compound , laminar film . in the case of the latter , ptfe , pfa , fep , or the like , is coated on the outwardly facing surface of a base layer of peek , pes , pps , or the like . in this embodiment , the fixing film 1 a comprises a cylindrical base film formed of polyimide , and a layer of ptfe coated on the outwardly facing surface of the base film . it is 25 mm in diameter . the ceramic heater 15 as a heating member is a linear heating member with low thermal capacity . it is disposed perpendicular to the moving direction of the fixing film 1 a and recording medium p . in this embodiment , the ceramic heater 15 basically comprises a substrate 15 a , a heat generating layer 15 b , and a protective layer 15 c . the substrate 15 a is formed of aluminum nitride ( ain ) or the like . the heat generating layer 15 b is extended on the surface of the substrate 15 a in the longitudinal direction of the substrate 15 a ; more specifically , electrically resistive material such as ag / pd ( silver / palladium ) is coated , approximately 10 μm thick and approximately 1 - 5 mm wide , by screen printing , or the like . the protective layer 15 c is formed of glass , fluorinated resin , or the like , and is placed on the heat generating layer 15 b . the slippery member 15 d is placed on the back surface on the substrate 15 a , that is , the surface opposite to the front side where the heat generating layer 15 b and protective layer 15 c are located . an electrical current is flowed between the longitudinal ends of the heat generating layer 15 b of the ceramic heater 15 , the heat generating layer 15 b generates heat , quickly raising the temperature of the heater 15 . the temperature of the heater 15 is detected by a temperature sensor 22 , and is used by a control circuit to control the amount of power supplied to the heat generating layer 15 b , so that the heater temperature is kept at a predetermined level . the ceramic heater 15 is fixedly fitted in the groove extended along the approximate longitudinal center line , in the bottom surface of the film guiding member 20 , with the protective layer 15 c side facing upward . the structure of the pressure applying mechanism 8 , and control for switching between the pressure application states a and b , are the same as those in the preceding embodiment . the same effects as those provided by the fixing apparatus in the preceding embodiment can be also provided by the fixing apparatus in this embodiment , which is different in heating means from the fixing apparatus in the preceding embodiment . as long as the material for the substrate 15 a itself of the ceramic heater 15 is excellent in terms of its slidableness against the fixing film 1 a , it is unnecessary to provide the substrate 15 a with the slippery member 15 d ; the surface of the substrate 15 a itself may be used as the surface on which the fixing film 1 a slides . the ceramic heater 15 as a heating member of the fixing apparatus in this embodiment may be replaced with a plate of such material as iron , in which heat can be electromagnetically induced . in such a case , the fixing apparatus is provided with a combination of an exciter coil and a magnetic core , as a magnetic field generating means , and heat is electromagnetically induced in , for example , an iron plate , to be given to the recording medium p through the fixing film 1 a , in the fixing nip n . the structure of a fixing apparatus as a heating apparatus does not need to be limited to such a structure as the structure of the fixing apparatus 100 in the preceding embodiments , which employed a pressure roller driving system . for example , referring to fig1 , a fixing film 1 , that is , an endless piece of film in which heat can be electromagnetically induced , may be stretched around a film guiding member 23 , a driver roller 31 , and a tension roller 32 . in this case , a fixing nip n is formed between the bottom surface of the film guiding member 23 and a pressure roller as a pressuring member , by the pressure from a pressure applying mechanism 8 , with the fixing film 1 pinched between the bottom surface of the film guiding member 23 and the pressure roller 5 . in this case , fixing film 1 is rotationally driven by the driver roller 31 , and the pressure roller 5 functions as a follower roller . on the inward side of the film guiding member 23 , a combination of an exciter coil 3 and a magnetic core 4 is provided as a magnetic field generating means . the portion of the bottom surface of the film guiding member 23 , which corresponds to the fixing nip n , is provided with a slippery member 10 to reduce the friction between the inwardly facing surface of the fixing film 1 and the bottom surface of the film guiding member 23 . further , lubricant such as heat resistant grease is provided between the slippery member 10 and the inwardly facing surface of the fixing film 1 , in the fixing nip n . the structure of the pressure applying mechanism 8 , and control for switching between the pressure application states a and b , are the same as those in the preceding embodiments . the same effects as those provided by the fixing apparatuses in the preceding embodiments can be also provided by the fixing apparatus in this embodiment , which is different in heating means from the fixing apparatuses in the preceding embodiments . as described above , according to the present invention , a fixing apparatus is structured so that while the fixing apparatus is started up , the pressure application state in the fixing nip n is kept in , or switched to , the pressure application state a , in which the pressure in the fixing nip n is smaller than the pressure in the fixing nip n in the pressure application state b , so that the torque required to start up the fixing apparatus is reduced . therefore , even in the case of a fixing apparatus in which the pressure applied to an object to be charged , while heating the object , is set relatively high , it is assured that the aforementioned first and second members smoothly slide against each other , even in a low temperature environment , so that the second member is prevented from failing to move . thus , it is possible to prevent the occurrence of the inconveniences associated with a conventional , film heating type fixing apparatus . for example , it is possible to reduce the warm - up time , and / or to prevent the fixing film as the second member from being damaged . further , according to the present invention , initially , the pressure application state of the fixing nip n is kept in , or switched to , the state a . then , after the elapsing of a predetermined length of time , that is , after the apparatus temperature climbs to a predetermined level , the pressure application state of the fixing nip n is switched to the state b , in which a predetermined higher amount of pressure is applied in the fixing nip n while heating an object to be heated . therefore , it is assured that the object to be heated is properly pinched in , and carried through , the fixing nip n , to be properly heated . in other words , a thermal , image fixing apparatus in accordance with the present invention assures that a recording medium is properly conveyed to produce a high quality image . it is obvious that the structure of the pressure applying mechanism 8 does not need to be limited to the structure in this embodiment . for example , a fixing apparatus may be structured so that the pressure application state can be adjusted in three or more steps , or even steplessly . further , when the fixing film 1 in which heat is electromagnetically induced is used for thermally fixing only a monochromatic image or a single - pass multicolor image , the elastic layer 1 b may be eliminated . the material for the heat generating layer 1 a may be a mixture of resinous material and metallic filler . the fixing film 1 may be formed of a heat generating layer alone . the fixing film 1 and fixing film 1 a , as the second member , do not need to be in the endless form or rotational form . for example , they may be in the form of a web , which can be repeatedly rolled back and forth . the pressing member 5 as the third member does not need to be in the form of a roller ; for example , it may be in the form of a rotational belt , or the like . a means for electromagnetically inducing the heat for controlling the temperature in the fixing nip n by generating heat may be provided on the pressuring member 5 side to supply the recording member p with thermal energy from the pressuring member 5 side . the usage of a heating apparatus in accordance with the present invention is not limited to the usage as an image heating apparatus such as those in the preceding embodiments . it can be widely used as a thermal means , or an apparatus , for heating a wide range of objects . for example , it can be used an image heating apparatus for improving the surface properties , such as glossiness , of a resultant copy , by heating the recording medium on which an image is borne , an image heating apparatus for temporarily fixing an image , an image heating apparatus for drying an object , a thermal laminating apparatus , and the like . while the invention has been described with reference to the structure disclosed herein , it is not confined to the details set forth , and this application is intended to cover such modifications or changes as may come within the purposes of the improvements or the scope of the following claims . | 6 |
the polyaryleneamines according to the first aspect of the present invention are characterized by having a structural unit represented by the general formula ( 1 ), in which ar 1 and ar 2 are each independently an aromatic group having 6 - 24 carbon atoms . preferred examples of the aromatic group having 6 - 24 carbon atoms include substituted or unsubstituted phenyl , biphenyl , anthracenyl , naphthyl and fluorenyl groups . specific examples of ar 1 include the following : substituted or unsubstituted phenyl groups such as phenyl , 2 - methoxyphenyl , 3 - methoxyphenyl , 4 - methoxyphenyl , 2 - methylphenyl , 3 - methylphenyl , 4 - methylphenyl , 2 - hydroxyphenyl , 3 - hydroxyphenyl , 4 - hydroxyphenyl , 2 - trifluoromethylphenyl , 3 - trifluoromethylphenyl , 4 - trifluoromethylphenyl , 2 , 6 - dimethylphenyl , 3 , 6 - dimethylphenyl , 2 , 3 - dimethylphenyl , 3 , 4 - dimethylphenyl , 2 , 4 - dimethylphenyl , 3 , 5 - dimethylphenyl , 3 -( trifluoromethoxy ) phenyl , 4 -( trifluoromethoxy ) phenyl and 3 , 4 -( methylenedioxy ) phenyl ; biphenyl groups such as 2 - biphenyl , 3 - biphenyl and 4 - biphenyl ; naphthyl groups such as 1 - naphthyl , 2 - naphthyl , 2 - methylnaphthyl and 4 - methylnaphthyl ; and 9 - anthracenyl , 2 - fluorenyl , etc . exemplary structures of ar 2 are listed below . ## str2 ## where r 2 is a hydrogen atom , an alkyl group having 1 - 5 carbon atoms or a trifluoromethoxy group ; m is an integer of 1 or 2 ; ## str3 ## where r is an alkyl group having 1 - 4 carbon atoms . among the polyaryleneamines of the invention , those that have a structural unit represented by the following general formula ( 15 ) are particularly preferred , since they have high heat resistance : ## str4 ## where r is h or ch 3 and n is an integer of 1 - 5 . if higher heat resistance is particularly important , the polyaryleneamines of the invention preferably have ar 2 bound in para positions . if higher solubility in solvents and better moldability are more important , the polyaryleneamines may contain bonds in the meta and / or ortho position . as long as they have the repeating unit represented by the general formula ( 1 ), the polyaryleneamines of the invention may be a homo - or copolymer . polyaryleneamines composed of at least ten repetitions of the structural unit ( 1 ) are particularly preferred since they have high resistance to heat and solvents . other examples of the polyaryleneamines of the invention are those that are composed of a repeating unit represented by either the following general formula ( 3 ): ## str5 ## or the following general formula ( 7 ): ## str6 ## the polyaryleneamines represented by the general formula ( 3 ) are such that a diphenylether residue and an aniline derivative residue alternate in the polyaryleneamines having the structural unit represented by the general formula ( 1 ). the polyaryleneamines represented by the general formula ( 7 ) are such that a diphenyl sulfide residue and an aniline derivative residue alternate in the polyaryleneamines having the structural unit represented by the general formula ( 1 ). exemplary aniline derivative residues include 3 - toluidine , aniline , 3 - fluoroaniline , 4 - fluoroaniline , 2 - toluidine , 4 - toluidine , 2 - anisidine , 3 - anisidine , 4 - anisidine , 3 - ethylaniline , 4 - ethylaniline , 2 , 4 - dimethoxyaniline , 2 , 5 - dimethoxyaniline , 2 , 3 - dimethylaniline , 2 , 4 - dimethylaniline , 2 , 4 , 6 - trimethylaniline , 4 - cyanoaniline , 4 - aminomethyl benzoate , 4 - nitroaniline , 3 , 4 - difluoroaniline , 3 , 4 , 5 - trifluoroaniline , 2 , 3 , 4 , 5 - tetrafluoroaniline and 2 , 3 , 4 , 5 , 6 - pentafluoroaniline . among these , the aniline , 3 - toluidine and 4 - fluoroaniline residues are particularly preferred since they contribute to the production of highly heat - resistant polyaryleneamines . the polyaryleneamines of the invention that are composed of the repeating unit represented by the general formula ( 3 ) have high melting points and those having melting points higher than 245 ° c . are particularly useful as heat - resistant resins . the polyaryleneamines of the invention that are composed of the repeating unit represented by the general formula ( 7 ) also have high melting points and those having melting points higher than 275 ° c . are particularly useful as diverse heat - resisting materials . the polyaryleneamines of the invention that are composed of the repeating unit represented by the general formula ( 3 ) or ( 4 ) may have any sufficient weight average molecular weights to be entitled to the designation of &# 34 ; polymers &# 34 ;. in view of the high mechanical and other characteristics that can be provided , the polyaryleneamines have preferably weight average molecular weights of 1 , 000 - 1 , 000 , 000 as calculated for polystyrene ; in view of the good processing characteristics that can be additionally provided , weight average molecular weights of 5 , 000 - 50 , 000 are more preferred . the polyaryleneamines of the invention may be produced by any methods . according to one method , an arylamine represented by the following general formula ( 9 ): ( where ar 1 is an aromatic group having 6 - 24 carbon atoms ) and / or an arylenediamine derivative represented by the following general formula ( 10 ): ## str7 ## ( where ar 1 and ar 2 are each independently an aromatic group having 6 - 24 carbon atoms ) is aminated with an aryl dihalide represented by the following general formula ( 11 ): ( where ar 2 is an aromatic group having 6 - 24 carbon atoms ; and x is cl , br , f or i ) in the presence of both a base and a catalyst composed of a trialkylphosphine and / or an arylphosphine and a palladium compound , whereby the desired polyaryleneamine can be produced efficiently . according to a modification of the process just described above , an aniline represented by the following general formula ( 12 ): ## str8 ## ( where r 1 - r 5 are each independently a hydrogen atom , an alkyl group having 1 - 20 carbon atoms , a thioalkyl group having 1 - 20 carbon atoms , an alkoxy group having 1 - 20 carbon atoms , a fluorine atom , a carbonyl group , a carboxyl group , a sulfonyl group , a sulfoxyl group , a nitro group or a cyano group ) is reacted with an aryl dihalide represented by the following general formula ( 13 ): ## str9 ## ( where x is cl , br or i ; a is o , s , so 2 , co , ch 2 or c ( ch 3 ) 2 ) to produce a polyaryleneamine composed of a repeating unit represented by the following general formula ( 14 ): ## str10 ## where a is o , s , so 2 , co , ch 2 or c ( ch 3 ) 2 ; r 1 - r 5 are each independently a hydrogen atom , an alkyl group having 1 - 20 carbon atoms , a thioalkyl group having 1 - 20 carbon atoms , an alkoxy group having 1 - 20 carbon atoms , a fluorine atom , a carboxyl group , a sulfonyl group , a sulfoxyl group , a nitro group , or a cyano group . specific examples of the arylamine represented by the general formula ( 9 ) which is to be used in the process described above include : anilines such as 3 - toluidine , aniline , 2 - fluoroaniline , 3 - fluoroaniline , 4 - fluoroaniline , 2 - toluidine , 4 - toluidine , 2 - anisidine , 3 - anisidine , 4 - anisidine , 3 - ethylaniline , 4 - ethylaniline , 2 , 4 - dimethoxyaniline , 2 , 5 - dimethoxyaniline , 2 , 3 - dimethylaniline , 2 , 4 - dimethylaniline , 2 , 4 , 6 - trimethylaniline , 4 - cyanoaniline , 4 - aminomethyl benzoate , 4 - nitroaniline , 3 , 4 - difluoroaniline , 3 , 4 , 5 - trifluoroaniline , 2 , 3 , 4 , 5 - tetrafluoroaniline and 2 , 3 , 4 , 5 , 6 - pentafluoroaniline ; and 2 - naphthylamine , 2 - aminobiphenyl , 4 - aminobiphenyl , etc . specific examples of the arylenediamine derivative represented by the general formula ( 10 ) which is to be used in the process described above include the following : n , n &# 39 ;- diphenylphenylenediamine , n , n &# 39 ;- di ( 2 - methoxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - methoxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - methoxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 - methylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - methylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - methylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 - hydroxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - hydroxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - hydroxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 - trifluoromethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - trifluoromethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - trifluoromethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 , 6 - dimethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 , 6 - dimethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 , 3 - dimethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 , 4 - dimethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 , 4 - dimethylphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - trifluoromethoxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - trifluoromethoxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - trifluoromethoxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 3 - biphenyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - biphenyl ) phenylenediamine , n , n &# 39 ;- di ( 1 - naphthyl ) phenylenediamine , n , n &# 39 ;- di ( 2 - naphthyl ) phenylenediamine , n , n &# 39 ;- di ( 3 , 4 - methylenedioxyphenyl ) phenylenediamine , n , n &# 39 ;- di ( 2 - methylnaphthyl ) phenylenediamine , n , n &# 39 ;- di ( 4 - methylnaphthyl ) phenylenediamine , n , n &# 39 ;- di ( 9 - anthracenyl ) phenylenediamine and n , n &# 39 ;- di ( 2 - fluorenyl ) phenylenediamine . specific examples of the aryl dihalide represented by the general formula ( 11 ) which is to be used in the process described above include : dibromobenzenes such as 1 , 4 - dibromobenzene , 1 , 2 - dibromobenzene , 1 , 3 - dibromobenzene , 2 , 5 - dibromotoluene , 3 , 5 - dibromotoluene , 1 , 4 - dibromo - 2 , 5 - dimethylbenzene , 1 , 3 - dibromo - 5 -( trifluoromethoxy ) benzene , 1 , 4 - dibromobiphenyl , 9 , 10 - dibromoanthracene , n - methyl - 3 , 6 - dibromocarbazole , n - ethyl - 3 , 6 - dibromocarbazole , n - propyl - 3 , 6 - dibromocarbazole , n - butyl - 3 , 6 - dibromocarbazole and 2 , 7 - dibromofluorene ; dichlorobenzenes such as 1 , 4 - dichlorobenzene , 1 , 2 - dichlorobenzene , 1 , 3 - dichlorobenzene , 2 , 5 - dichlorotoluene , 3 , 5 - dichlorotoluene , 1 , 4 - dichloro - 2 , 5 - dimethylbenzene , 1 , 3 - dichloro - 5 -( trifluoromethoxy ) benzene , 1 , 4 - dichlorobiphenyl , 9 , 10 - dichloroanthracene , n - methyl - 3 , 6 - dichlorocarbazole , n - ethyl - 3 , 6 - dichlorocarbazole , n - propyl - 3 , 6 - dichlorocarbazole , n - butyl - 3 , 6 - dichlorocarbazole and 2 , 7 - dichlorofluorene ; diiodebenzenes such as 1 , 4 - diiodobenzene , 1 , 2 - diiodobenzene , 1 , 3 - diiodobenzene , 2 , 5 - diiodotoluene , 3 , 5 - diiodotoluene , 1 , 4 - diiodo - 2 , 5 - dimethylbenzene , 1 , 3 - diiodo - 5 -( trifluoromethoxy ) benzene , 1 , 4 - diiodobiphenyl , 9 , 10 - diiodoanthracene , n - methyl - 3 , 6 - diiodocarbazole , n - ethyl - 3 , 6 - diiodocarbazole , n - propyl - 3 , 6 - diiodocarbazole , n - butyl - 3 , 6 - diiodocarbazole and 2 , 7 - diiodofluorene ; and difluorobenzenes such as 1 , 4 - difluorobenzene , 1 , 2 - difluorobenzene , 1 , 3 - difluorobenzene , 2 , 5 - difluorotoluene , 3 , 5 - difluorotoluene , 1 , 4 - difluoro - 2 , 5 - dimethylbenzene , 1 , 3 - difluoro - 5 -( trifluoromethoxy ) benzene , 1 , 4 - difluorobiphenyl , 9 , 10 - difluoroanthracene , n - methyl - 3 , 6 - difluorocarbazole , n - ethyl - 3 , 6 - difluorocarbazole , n - propyl - 3 , 6 - difluorocarbazole , n - butyl - 3 , 6 - difluorocarbazole and 2 , 7 - difluorofluorene . other examples of the aryl dihalide represented by the general formula ( 11 ) which is to be used in the invention include the following : 4 , 4 &# 39 ;- dihalogenodiphenylethers such as 4 , 4 &# 39 ;- dichlorodiphenylether , 4 , 4 &# 39 ;- dibromodiphenylether , 4 , 4 &# 39 ;- diiododiphenylether , 4 - chloro - 4 &# 39 ;- bromodiphenylether , 4 - chloro - 4 &# 39 ;- iododiphenylether and 4 - bromo - 4 &# 39 ;- iododiphenylether ; 4 , 4 &# 39 ;- dihalogenodiphenyl sulfides such as 4 , 4 &# 39 ;- dichlorodiphenyl sulfide , 4 , 4 &# 39 ;- dibromodiphenyl sulfide , 4 , 4 &# 39 ;- diiododiphenyl sulfide , 4 - chloro - 4 &# 39 ;- bromodiphenyl sulfide , 4 - chloro - 4 &# 39 ;- iododiphenyl sulfide and 4 - bromo - 4 &# 39 ;- iododiphenyl sulfide ; 4 , 4 &# 39 ;- dihalogenodiphenyl sulfones such as 4 , 4 &# 39 ;- dichlorodiphenyl sulfone , 4 , 4 &# 39 ;- dibromodiphenyl sulfone , 4 , 4 &# 39 ;- diiododiphenyl sulfone , 4 - chloro - 4 &# 39 ;- bromodiphenyl sulfone , 4 - chloro - 4 &# 39 ;- iododiphenyl sulfone and 4 - bromo - 4 &# 39 ;- iododiphenyl sulfone ; 4 , 4 &# 39 ;- dihalogenodiphenyl ketones such as 4 , 4 &# 39 ;- dichlorodiphenyl ketone , 4 , 4 &# 39 ;- dibromodiphenyl ketone , 4 , 4 &# 39 ;- diiododiphenyl ketone , 4 - chloro - 4 &# 39 ;- bromodiphenyl ketone , 4 - chloro - 4 &# 39 ;- iododiphenyl ketone and 4 - bromo - 4 &# 39 ;- iododiphenyl ketone ; 4 , 4 &# 39 ;- dihalogenodiphenylmethanes such as 4 , 4 &# 39 ;- dichlorodiphenylmethane , 4 , 4 &# 39 ;- dibromodiphenylmethane , 4 , 4 &# 39 ;- diiododiphenylmethane , 4 - chloro - 4 &# 39 ;- bromodiphenylmethane , 4 - chloro - 4 &# 39 ;- iododiphenylmethane and 4 - bromo - 4 &# 39 ;- iododiphenylmethane ; and 2 , 2 - di ( 4 - halogenophenyl ) propanes such as 2 , 2 - di ( 4 - chlorophenyl ) propane , 2 , 2 - di ( 4 - bromophenyl ) propane and 2 , 2 - di ( 4 - iodophenyl ) propane . the amounts of the arylenediamine derivative and / or arylamine to be added in the process of the invention are not limited to any particular values . to produce polyaryleneamines of higher molecular weights , the arylenediamine derivative is preferably added in an amount of 0 . 9 - 1 . 1 moles per mole of the aryl dihalide whereas the arylamine is preferably added in an amount of 0 . 4 - 0 . 6 moles per mole of the aryl dihalide . to the extent that will not deviate from the objects of the invention , the arylenediamine derivative and the arylamine may be used in admixture or they may be used in combination with a third component . in the process of the invention , the amination reaction is allowed to proceed in the presence of a catalyst composed of a trialkylphosphine and / or an arylphosphine and a palladium compound . the trialkylphosphine and the arylphosphine may be used either alone or in admixture . the palladium compound to be used in the process of the invention is not limited to any particular type and may be exemplified by the following : tetravalent palladium compounds such as sodium hexachloropalladate ( iv ) tetrahydrate and potassium hexachloropalladate ( iv ); divalent palladium compounds such as palladium ( ii ) chloride , palladium ( ii ) bromide , palladium ( ii ) acetate , palladium ( ii ) acetylacetonate , dichlorobis ( benzonitrile ) palladium ( ii ), dichlorobis ( acetonitrile ) palladium ( ii ), dichlorobis ( triphenylphosphine ) palladium ( ii ), dichlorotetramminepalladium ( ii ), dichloro ( cycloocta - 1 , 5 - diene ) palladium ( ii ) and palladium ( ii ) trifluoroacetate ; and zero - valent palladium compounds such as tris ( dibenzylideneacetone ) dipalladium ( o ), tris ( dibenzylideneacetone ) dipalladium ( o ) chloroform complex and tetraquis ( triphenylphosphine ) palladium ( o ). the amount in which the palladium compounds are to be used in the process of the invention is not limited in any particular way but they are typically used in amounts of 0 . 00001 - 20 . 0 mol %, as calculated for palladium , per mole of the halogen atoms in the starting aryl dihadide ; in view of the high cost of the palladium compounds , they are preferably used in amounts of 0 . 001 - 5 . 0 mol %, as calculated for palladium , per mole of the halogen atoms in the starting aryl dihalide . the trialkylphosphine to be used as a component of the catalyst in the process of the invention is not limited in any particular way and may be exemplified by triethylphosphine , tricyclohexylphosphine , triisopropylphosphine , tri - n - butylphosphine , triisobutylphosphine , tri - sec - butylphosphine and tri - tert - butylphosphine . among these , tri - tert - butylphosphine is particularly preferred , since it exhibits high catalytic activity in the reaction . the arylphosphine to be used in the process of the invention also is not limited in any particular way and may be exemplified by triphenylphosphine , tri ( o - tolyl ) phosphine , tri ( m - tolyl ) phosphine , tri ( p - tolyl ) phosphine , binap , trimesitylphoshine , diphenylphosphinoethane , diphenylphosphinopropane and diphenylphosphinoferrocene . the amounts in which the trialkylphosphine and / or arylphosphine are to be used in the process of the invention are not limited to any particular values and they may typically be used in the range of 0 . 01 - 10 , 000 moles per mole of the palladium compound . in view of the high cost of the trialkylphosphine and arylphosphine , they are preferably used in the range of 0 . 1 - 10 moles per mole of the palladium compound . the catalyst to be used in the process of the invention consists of the palladium compound and the trialkylphosphine and / or arylphosphine . the two catalytic components may be added independently to the reaction system ; alternatively , a complex of the two components may first be prepared and then added to the reaction system . the base to be used in the process of the invention also is not limited in any particular way and may be exemplified by inorganic bases such as sodium or potassium carbonates and alkali metal alkoxides , and organic bases such as tertiary amines . among these , alkali metal alkoxides are preferred as exemplified by sodium methoxide , sodium ethoxide , potassium methoxide , potassium ethoxide , lithium - tert - butoxide , sodium - tert - butoxide and potassium - tert - butoxide . these may be added as such to the reaction system or , alternatively , they may be added to the reaction system after in situ preparation from an alkali metal or an alkali metal hydride and an alcohol . the amount in which the base is to be used in the process of the invention is not limited to any particular value but it is preferably used in at least one half of a mole per mole of the halogen atoms in the aryl dihalide to be added to the reaction system ; in view of the ease in performing post - treatments after the end of the reaction , it is particularly preferred to use the base in an amount ranging from 1 . 0 to 5 moles per mole of the halogen atoms in the aryl dihalide . the process of the invention is generally performed in an inert solvent . any inert solvents that do not very much interfere with the intended reaction may be used without any particular limitations and examples include : aromatic hydrocarbon solvents such as benzene , toluene and xylene ; ether solvents such as diethyl ether , tetrahydrofuran and dioxane ; and acetonitrile , dimethylformamide , dimethyl sulfoxide and hexamethyl phosphoric triamide . among these , aromatic hydrocarbon solvents such as benzene , toluene and xylene are particularly preferred . the process of the invention is preferably performed in an inert gas atmosphere such as nitrogen or argon at atmospheric pressure . it should , however , be noted that the process can also be performed under superatmospheric pressure . any reaction conditions that are capable of producing the desired polyaryleneamines may be employed in the process of the invention without any particular limitations ; to give just one example , the reaction temperature ranges preferably from 20 to 300 ° c ., more preferably from 50 to 200 ° c ., and the reaction time may range from several minutes to 72 hours . when the aniline represented by the general formula ( 12 ) and the aryl dihalide represented by the general formula ( 13 ) are reacted to produce a polyaryleneamine composed of the repeating unit represented by the general formula ( 14 ), the reaction temperature may preferably be selected from the range of 20 - 250 ° c ., more preferably from the range of 50 - 150 ° c ., with the reaction time being selected from the range of several minutes to 20 hours . the polyaryleneamine of the invention is composed of the repeating unit represented by the general formula ( 1 ) and in its structure , the aryl residue and the aniline derivative residue alternate to provide a higher melting point and improved heat resistance . therefore , the polyaryleneamine of the invention is salient as a heat - resisting structural material . the polyaryleneamine of the invention may be used independently as a resin material ; if desired , it may be used in admixture with fillers such as glass fiber , carbon fiber , talc , calcium carbonate and mica , or various types of stabilizers including antioxidants and photostabilizers . the polyaryleneamine of the invention may also be used as a polymer alloy or blend with other polymers including general - purpose resins such as polyethylene , poly ( vinyl chloride ) and polystyrene , engineering plastics such as polypropylene and modified polyphenylene ether , and super engineering plastics such as polyphenylene sulfide , polyphenylene sulfide ketone , polyimides , polyether imides and liquid - crystal polymers . the polymer of the invention comprises a series of triarylamine structures capable of efficient positive hole transport and , hence , it holds promise for use as a positive hole transport material in organic electroluminescent ( el ) devices . the following examples are provided for the purpose of further illustrating the present invention but are in no way intended to limit its scope . a four - necked flask ( 200 ml ) equipped with a condenser tube and a thermometer was charged with 2 . 6 g ( 0 . 01 mol ) of n , n &# 39 ;- diphenylphenylenediamine , 2 . 36 g ( 0 . 01 mol ) of p - dibromobenzene , 2 . 69 g ( 1 . 4 eqs . as compared to bromine atoms ) of sodium tertiary butoxide and 60 ml of o - xylene at room temperature . to the mixture , 11 . 2 mg ( 0 . 5 mol %) of palladium acetate and 4 eqs . as compared to palladium compound of tritertiary butylphosphine were added in a nitrogen atmosphere . subsequently , the mixture was heated to 120 ° c . in a nitrogen atmosphere and reaction was performed at 120 ° c . for 3 h . after the end of the reaction , 60 ml of water was added to wash the reaction product , from which the solids was recovered by filtration . the recovered solids was washed again with 20 ml of water and subsequently dried under vacuum to give a yellow powder in an amount of 4 . 03 g ( yield : 92 . 8 %). tg / dta showed that the powder had a melting point of 325 . 6 ° c . the powder was also subjected to elementary and ir analyses and the results are respectively shown in table 1 and fig1 . table 1______________________________________ c h n______________________________________found ( wt %) 86 . 19 5 . 37 8 . 44 cal &# 39 ; d ( wt %) 86 . 23 5 . 39 8 . 38______________________________________ with all data taken together , the powder was a polyaryleneamine having high melting point . a four - necked flask ( 200 ml ) equipped with a condenser tube and a thermometer was charged with 2 . 14 g ( 0 . 02 mol ) of 3 - toluidine , 9 . 44 g ( 0 . 04 mol ) of p - dibromobenzene , 10 . 75 g ( 1 . 4 eqs . as compared to bromine atoms ) of sodium tertiary butoxide and 60 ml of o - xylene at room temperature . to the mixture , 51 . 8 mg ( 0 . 25 mol %) of a tris ( dibenzylideneacetone ) dipalladium chloroform complex ( product of aldrich ) and 4 eqs . as compared to palladium compound of tri - tertiary butylphosphine were added in a nitrogen atmosphere . subsequently , the mixture was heated to 120 ° c . in a nitrogen atmosphere and reaction was performed at 120 ° c . for 3 h . after the end of the reaction , 60 ml of water was added to wash the reaction product , from which the solids was recovered by filtration . the recovered solids was washed again with 20 ml of water and subsequently dried under vacuum to give a yellow powder in an amount of 3 . 75 g ( yield : 89 . 4 %). tg / dta showed that the powder had a melting point of 327 . 6 ° c . the powder was also subjected to elementary and ir analyses and the results are respectively shown in table 2 and fig2 . table 2______________________________________ c h n______________________________________found ( wt %) 86 . 15 6 . 05 7 . 80 cal &# 39 ; d ( wt %) 86 . 19 6 . 08 7 . 73______________________________________ with all data taken together , the powder was a polyaryleneamine having high melting point . reaction and post - treatments were performed under the same conditions as in example 2 , except that the amount of p - dibromobenzene was reduced from 9 . 44 g ( 0 . 04 mol ) to 4 . 72 g ( 0 . 02 mol ) and sodium tert - butoxide was reduced from 10 . 75 g to 5 . 38 g ( 1 . 4 eqs . as compared to bromine atoms ). upon vacuum drying , a yellow white powder formed in an amount of 3 . 41 g ( yield : 94 . 2 %). tg / dta showed that the powder had a melting point of 327 . 6 ° c . the powder was also subjected to elementary and ir analyses and the results are respectively shown in table 3 and fig3 . table 3______________________________________ c h n______________________________________found ( wt %) 86 . 19 6 . 08 7 . 73 cal &# 39 ; d ( wt %) 86 . 14 6 . 14 7 . 72______________________________________ reaction and post - treatments were performed under the same conditions as in example 3 , except that 2 . 14 g ( 0 . 02 mol ) of 3 - toluidine was replaced by 2 . 22 g ( 0 . 02 mol ) of 4 - fluoroaniline . upon vacuum drying , a yellow white powder formed in an amount of 3 . 60 g ( yield : 97 . 3 %). tg / dta showed that the powder had a melting point of 331 . 3 ° c . the powder was also subjected to elementary and ir analyses and the results are respectively shown in table 4 and fig4 . table 4______________________________________ c h n f______________________________________cal &# 39 ; d ( wt %) 77 . 84 4 . 32 7 . 57 10 . 27 found ( wt %) 77 . 78 4 . 49 7 . 52 10 . 21______________________________________ reaction and post treatments were performed under the same conditions as in example 3 , except that 4 . 72 g of p - dibromobenzene was replaced by 6 . 24 g of 4 , 4 &# 39 ;- dibromobiphenyl . upon vacuum drying , a yellow white powder formed in an amount of 5 . 10 g ( yield : 99 . 0 %). tg / dta showed that the powder had a melting point of 268 . 0 ° c . the powder was also subjected to elementary and ir analyses and the results are respectively shown in table 5 and fig5 . table 5______________________________________ c h n______________________________________cal &# 39 ; d ( wt %) 88 . 72 5 . 84 5 . 44 found ( wt %) 88 . 60 5 . 97 5 . 43______________________________________ reaction and post treatments were performed under the same conditions as in example 3 , except that 4 . 72 g ( 0 . 02 mol ) of p - dibromobenzene was replaced by an equal amount of m - dibromobenzene . upon vacuum drying , a yellow white powder formed in an amount of 3 . 35 g ( yield : 92 . 5 %). tg / dta showed that the powder had a melting point of 281 . 2 ° c . the powder was also subjected to elementary and ir analyses and the results are respectively shown in table 6 and fig6 . table 6______________________________________ c h n______________________________________cal &# 39 ; d ( wt %) 86 . 19 6 . 08 7 . 73 found ( wt %) 86 . 15 6 . 14 7 . 74______________________________________ reaction and post treatments were performed under the same conditions as in example 3 , except that the amount of the poalladium catalyst was increased from 0 . 25 mol % to 2 . 5 mol % ( 518 mg ) and that tri - ortho - tolylphosphine rather than tri - tertiary butylphosphine was used in an amount of 4 eqs . as compared to the palladium catalyst . upon vacuum drying , a yellow white powder formed in an amount of 2 . 72 g ( yield : 75 . 1 %). reaction and post treatments were performed under the same conditions as in example 3 , except that the amount of the palladium catalyst was increased from 0 . 25 mol % to 0 . 5 mol % ( 103 . 6 mg ) and sodium tert - butoxide was reduced from 10 . 75 g to 5 . 38 g ( 1 . 4 eqs . as compared to bromine atoms ) and that tricyclohexylphosphine rather than tri - tertiary butylphosphine was used in an amount of 4 eqs . as compared to the palladium catalyst . upon vacuum drying , a yellow white powder formed in an amount of 2 . 94 g ( yield : 81 . 2 %). a four - necked flask ( 200 ml ) equipped with a condenser tube and a thermometer was charged with 2 . 14 g ( 0 . 02 mol ) of 3 - toluidine , 6 . 56 g ( 0 . 02 mol ) of 4 , 4 &# 39 ;- dibromodiphenylether , 4 . 61 g ( 1 . 2 eqs . as compared to bromine atoms ) and 80 ml of o - xylene at room temperature . to the mixture , 103 . 5 mg ( 0 . 5 mol %) of tris ( dibenzylideneacetone ) dipalladium and 4 eqs . as compared to palladium compound of tri - tertiary butylphosphine were added in a nitrogen atmosphere . subsequently , the mixture was heated to 120 ° c . in a nitrogen atmosphere and reaction was performed at 120 ° c . for 3 h with stirring . after the end of the reaction , 60 ml of water was added to wash the reaction product , which was separated into oil and water phases in a separating funnel and the organic phase was concentrated under vacuum to give a solution in orange color . the solution was added dropwise to a 1 : 5 mixture of thf and methanol , whereupon a white powder precipitated . the white powder was recovered by filtration and dried under vacuum to give a white powder in an amount of 4 . 20 g ( yield : 73 . 0 %). the polymer had a melting point of 249 . 4 ° c . ( as measured with tg / dta 220 of seiko instruments , inc .) gpc analysis using thf as an eluant ( with hlc 8120 of tosoh corp .) showed that the polyaryleneamine had an average molecular weight of 19 , 600 as calculated for polystyrene . the polyaryleneamine was subjected to nmr analysis ( with gsx - 400 of jeol ltd . ), ir analysis ( with dr - 8000 of shimadzu corp .) and elementary analysis ( with chn corder mt - 5 of yanaco ); the results of the respective analyses are shown in fig7 and 8 and table 7 . table 7______________________________________ c h n o______________________________________found ( wt %) 83 . 4 5 . 6 5 . 3 5 . 7 cal &# 39 ; d ( wt %) 83 . 5 5 . 5 5 . 1 5 . 9______________________________________ a four - necked flask ( 200 ml ) equipped with a condenser tube and a thermometer was charged with 2 . 22 g ( 0 . 02 mol ) of 4 - fluoroaniline , 6 . 56 g ( 0 . 02 mol ) of 4 , 4 &# 39 ;- dibromodiphenylether , 4 . 61 g ( 1 . 2 eqs . as compared to bromine atoms ) of sodium tertiary butoxide and 80 ml of o - xylene at room temperature . to the mixture , 103 . 5 mg ( 0 . 5 mol %) of tris ( dibenzylideneactone ) depalladium and 4 eqs . as compared to palladium compound of tri - tertiary butylphosphone were added in a nitrogen atmosphere . subsequently , the mixture was heated to 120 ° c . in a nitrogen atmosphere and reaction was performed at 120 ° c . for 3 h with stirring . after the end of the reaction 60 ml of water was added to wash the reaction product , which was separated into oil and water phases in a separating funnel and the organic phase was concentrated under vacuum to give a solution in orange color . the solution was added dropwise to a 1 : 5 mixture of thf and methanol , whereupon a white powder precipitated . the white powder was recovered by filtration and dried under vacuum to give a white powder in an amount of 4 . 45 g ( yield : 97 . 3 %). the polymer had a melting point of 252 . 9 ° c . ( as measured with tg / dta 220 of seiko instruments , inc .) gpc analysis using thf as an eluant ( with hlc 8120 of tosoh corp .) showed that the polyaryleneamine had an average molecular weight of 19 , 800 as calculated for polystyrene . the polyaryleneamine was subjected to nmr analysis ( with jnm - sx270 of jeol ltd . ), ir analysis ( with dr - 8000 of shimadzu corp .) and elementary analysis ( with chn corder mt - 5 of yanaco ); the results of the respective analyses are shown in fig9 and 10 and table 8 . table 8______________________________________ c h n o , f______________________________________found ( wt %) 77 . 49 4 . 30 4 . 99 13 . 22 cal &# 39 ; d ( wt %) 77 . 98 4 . 33 5 . 05 12 . 64______________________________________ a four - necked flask ( 200 ml ) equipped with a condenser tube and a thermometer was charged with 1 . 86 g ( 0 . 02 mol ) of aniline , 6 . 56 g ( 0 . 02 mol ) of 4 , 4 &# 39 ;- dibromodiphenylether , 4 . 61 g ( 1 . 2 eqs . as compared to bromine atoms ) of sodium tertiary butoxide and 80 ml of o - xylene at room temperature . to the mixture , 103 . 5 mg ( 0 . 5 mol %) of tris ( dibenzylideneacetone ) dipalladium and 4 eqs . as compared to palladium compound of tri - tertiary butylphosphine were added in a nitrogen atmosphere . subsequently , the mixture was heated to 120 ° c . in a nitrogen atmosphere and reaction was performed at 120 ° c . for 3 h with stirring . after the end of the reaction , 60 ml of water was added to wash the reaction product , from which the solids was recovered by filtration . the recovered solids was washed with 30 ml each of water , thf and methanol . subsequent vacuum drying gave a white powder in an amount of 4 . 05 g ( yield : 78 . 2 %). the polymer had a melting point of 259 . 4 ° c . ( as measured with tg / dta 220 of seiko instruments , inc .) the polymer was also subjected to ir analysis ( with dr - 8000 of shimadzu corp .) and elementary analysis ( with chn corder mt - 5 of yanaco ); the results are respectively shown in fig1 and table 9 . table 9______________________________________ c h n o______________________________________found ( wt %) 83 . 38 5 . 00 5 . 38 6 . 24 cal &# 39 ; d ( wt %) 83 . 40 5 . 02 5 . 40 6 . 18______________________________________ a four - necked flask ( 200 ml ) equipped with a condenser tube and a thermometer was charged with 2 . 14 g ( 0 . 02 mol ) of 3 - toluidine , 6 . 88 g ( 0 . 02 mol ) of 4 , 4 &# 39 ;- dibromodiphenyl sulfide , 4 . 61 g ( 1 . 2 eqs . as compared to bromine atoms ) of sodium tertiary butoxide and 80 ml of o - xylene . in a separate step , a complex was formed from 103 . 5 mg ( 0 . 5 mol %) of tris ( dibenzylideneacetone ) dipalladium and 4 eqs . as compared to palladium compound of tri - tertiary butylphosphine . the thus prepared complex was used as a catalyst and its solution in o - xylene was added to the mixture in the flask through a syringe in a nitrogen atmosphere . subsequently , the flask was heated to 120 ° c . in a nitrogen atmosphere and reaction was performed at 120 ° c . for 3 h with stirring . after the end of the reaction , 60 ml of water was added to wash the reaction product , from which the solids was recovered by filtration . the recovered solids was washed with 30 ml each of water , thf and methanol . subsequent vacuum drying gave a white powder in an amount of 5 . 22 g ( yield : 93 . 1 %). the polymer had a melting point of 275 . 5 ° c . ( as measured with tg / dta 220 of seiko instruments , inc .) the resulting polyaryleneamine was subjected to elementary analysis ( with chn corder mt - 5 of yanaco ) and ir analysis ( with dr - 8000 of shimadzu corp . ); the results of the respective analyses are shown in table 10 and fig1 . table 10______________________________________ c h n s______________________________________found ( wt %) 78 . 80 4 . 99 4 . 89 11 . 28 cal &# 39 ; d ( wt %) 78 . 89 5 . 19 4 . 84 11 . 08______________________________________ as will be understood from the foregoing description , the present invention provides novel polyaryleneamines that have tertiary arylamino groups connected serially and which are useful as structural materials improved in heat resistance , solvent resistance and other properties . the invention also provides a process for efficient production of the polyaryleneamines . therefore , the invention will offer great benefits to the industry concerned . | 2 |
fig1 illustrates an architecture in which a system and method for installing computer network service components on a client may operate , according to an embodiment of the invention . various aspects of embodiments of the invention may be described in the general context of computer code or machine - useable instructions , including computer - executable instructions such as program modules , being embodied on computer - storage media and being executed by a computer or other machine . computer - storage media include both volatile and nonvolatile media , removable and nonremovable media , and contemplate media readable by a processor . media examples include ram , rom , eeprom , flash memory or other memory technology , cd - rom , digital versatile discs ( dvd ), holographic media or other optical disc storage , magnetic cassettes , magnetic tape , magnetic disk storage , and other magnetic storage devices . as illustrated in that figure fig1 , a user may operate a client 102 using a user interface 116 such as a graphical user interface ( gui ) or other to initiate and guide an installation process of one or more components for services of their choosing . as illustrated , the user may initiate the service installation process by inserting media 104 such as a cd - rom into the client 102 , or , in embodiments may access a network 106 such as the internet or other network 106 or a combination of the two , in embodiments , the client may host and execute an installation engine 120 to manage the distribution of new service components to the client 102 and / or the user &# 39 ; s subscription account . the service components which the user may choose to install or initiate on client 102 or associated account may include a range of network access features , services and media . the service components may include , for example , one or more email accounts , or a web site hosting service , for instance with a certain amount of storage ( e . g . 10 mb or other ) for new or existing accounts . the service components may likewise include utilities and tools , such as anti - spam filters for email or other communications channels , anti - virus tools for client 102 or other machines , or the provisioning of internet access itself , via network 106 or otherwise . the service components managed according to embodiments of the invention may likewise encompass media and other services , such as digital photo or other file sharing , music download service , video download service or other media delivery services . the service components may likewise include web or other services such as financial , medical , educational or other portals , or other personal or business resources . in embodiments , the selection and installation of eligible services may include the installation of corresponding application components , interfaces or resources , such as web browsers , media players including audio or video codecs , email clients , or other components or services . according to embodiments as shown in fig1 , when the user inserts media 104 or accesses a web site via network 106 , installation logic may be started which analyzes and delivers content and components to client 102 or otherwise which matches the user &# 39 ; s subscription status . according to embodiments in one regard , the client 102 may communicate with installation server 108 to facilitate that provisioning . installation server 108 may be or include a local or remote server which may in turn communicate with a subscription database 110 , to identify appropriate service components for the requesting user . toward that purpose , subscription database 110 may host resources including an available component list 112 , a subscriber services list 114 and other data or connections . when the installation engine 120 is notified that a new installation event has begun , the installation engine may prompt the user for user id , login or other account or identification information . for instance , an existing user desiring to update or upgrade services may enter their existing user name or account name , while a new user may enter a new user or account name to be activated . installation engine 120 may authenticate the user &# 39 ; s entered account and other information as appropriate , for instance by performing a lookup of that information against subscription database 110 . this authorization process may in one regard be performed before components , code or other data may be installed onto client 102 or activated in an associated account , thereby again avoiding unnecessary or inappropriate delivery of undesired components . after the initiating user has been authenticated , the installation engine 120 may access the subscription database 110 to reference an available component list 112 , to begin to isolate eligible components for that user . available component list 112 may include or interface to , for example , a list or set of service components which are available to the user based on their geographic location , market or co - branding preferences , language requirements or other governing criteria or factors . for instance , the available component list 112 may indicate that for user x updating their service components in , for illustration south america , certain services such as internet telephony may be available , or that eligible components must include services delivered in spanish , portuguese , english or other languages . in embodiments , marketing terms or conditions , such as the user &# 39 ; s agreement to use their telephone company &# 39 ; s affiliated cellular telephone or network - enabled data service , may narrow the set of services in and presented by the available component list 112 . likewise in cases a user &# 39 ; s age or other criteria may affect or filter the services stored to or accessed from available component list 112 . the installation engine 120 may likewise access the subscribed services list 114 for the initiating user , which data may also be stored in subscription database 110 . the subscribed services list 114 may contain a list , table or other data structure recording the services and components which a user may currently subscribe to , or which are awaiting activation or are currently in other status . thus for a given user , the subscribed services list 114 may contain selections or components such as email , web hosting , music downloads , internet banking or email payment service , or other services or components . those services or components may in embodiments be or include some services or components whose subscription is free of charge , and others which involve a monthly or other subscription fee . for example some services , such as on - demand music download , may incur a per - track download charge . some services in subscribed services list 114 may be dependent on subscription to other services , such as anti - spam tools which may depend on email service . other subscription arrangements , charges and combinations are possible . the installation engine 120 may in embodiments compare the components in the available component list 112 for the initiating user against the subscribed services list 114 , to generate a set of eligible components based on the matching components from that data . according to embodiments illustrated in fig1 , the installation server 108 may likewise communicate with a component store 128 hosting a set of software or service components 130 available in available component list 112 or otherwise , to permit accessing or downloading of those components and resources by authorized clients . in embodiments the set of software or service components 130 may be stored in or distributed from other local or remote storage resources , depending on configuration . upon initiation of a service installation and the isolation of eligible components via the subscription database 110 , as illustrated in fig2 the user may be presented with a set of installation options 118 on user interface 116 . those installation options 118 may again and as illustrated include services or components such as email , web hosting , anti - virus or other utilities , music , video or other download options , or other services or resources . after the user &# 39 ; s selections from the set of installation options 118 are made , the installation engine 120 may initiate the building of those components on client 102 or otherwise . for example , a new or updated media player may be installed to client 102 . the components to be installed may in embodiments be retrieved or delivered from media 104 , from the component store 128 , from both media 104 and component store 128 , or via other channels or resources . in embodiments , components transmitted from installation server 108 may be communicated through application or service - aware protocols , for example activex ™, java ™, xml ( extensible markup language ) or other code , data or resources . the installation engine 120 may communicate with installation server 108 to update the user &# 39 ; s subscribed services list 114 , to reflect those newly chosen or installed components or services for that user &# 39 ; s account or profile . in embodiments , the user may likewise remove or unsubscribe from given components , when desired . fig3 illustrates a logical architecture for the installation engine 120 and other resources , according to an embodiment of the invention . as shown the installation engine 120 may execute an installation script or processing which is in one regard dependent on user authorization and that user &# 39 ; s subscription status . according to that processing in one regard , the installation engine 120 may commence a non - silent installation when a user inserts media 104 , accesses network 106 or takes other steps to begin the addition or subtraction of components to or from a new or existing user subscription or account . the user &# 39 ; s subscribed services list 114 , or desired or selected components or services and associated component permits may be checked against available component list 112 to determine the intersection of those components . in embodiments , component requirements , such as geographic , language , or in some cases , machine - specific criteria for client 102 ( such as minimum available storage ) or other requirements may be checked . again after the set of eligible components are generated , they may be passed to the user interface 116 . in embodiments the installation engine 120 and user interface 116 may also receive or present a set of default selections , such as components commonly chosen or subscribed to in the user &# 39 ; s location or at the user &# 39 ; s given service level . according to the logical architecture as shown , the set of eligible services and other data may be communicated to the installation server 108 , which in embodiments and as illustrated in fig3 may host a network access service such as a soap ( simple object access protocol ) service 122 , to facilitate the transmission of component objects selected out by the initiating user . in arrangements as shown , the installation server 108 may access component store 128 or other resources to access or retrieve a set of market - specific components 124 , associated xml code or data as well as one or more default component package 126 to transmit to client 102 via installation engine 120 . those default components may for instance be selected and accessed when the user interface 116 permits the user to choose an abbreviated installation process which accepts default services or components . overall installation processing according to embodiments of the invention is illustrated in further regard in fig4 . in step 402 , processing may begin . in step 404 , installation may be initiated by reading installation media such as a cd - rom or other removable or other media , by initiating access to an installation web site or a download from a web site , or other channels . in step 406 , a client software containing an installation engine , such as microsoft network ( msn ) or other media or other client software , may be installed , for instance onto the hard drive of client 102 or other client or device . in instances where the client 102 already has a media client installed , that installation may be omitted , or updating to current versions may take place . in step 408 , a subscriber signup or login process may be initiated , for instance by prompting the user for a username , password , security - enabled account login such as a microsoft passport ™ account , or other account setup , authorization , verification or authentication routines . in step 410 , an available component list 112 for the user may be retrieved , for example from subscription database 110 . the available component list 112 may be filtered or conditioned based on subscriber status information for that user , such as geographic location , language , market or co - branding limitations or preferences , age restrictions ( for example , in a multiuser family account ), or other factors . in step 412 , service component permits for the user may be acquired , for instance by accessing the user &# 39 ; s subscribed services list 114 or otherwise . in step 414 , the permits or authorizations for various service components for that user may be compared against the available component 112 to identify and extract those services that are desired , permitted and available to the user . in step 416 , setup options based on those filtered services may be displayed to the user . for example , the user may be asked to select a degree of anti - spam protection , for instance low , medium or high . other services and selections may be presented . in step 418 , the user &# 39 ; s selections or other inputs may be received in installation engine 120 or other installation logic . in step 420 , the generated set of final component services may be installed in client 102 or other client or device . in step 422 , any post - installation setup or confirmation may be launched , for example to display a welcome screen to the user inviting them to log in to one or more service . in step 424 , processing may repeat , return to a prior processing point , jump to a further processing point or end . the foregoing description of the invention is illustrative , and modifications in configuration and implementation will occur to persons skilled in the art . for instance , while the invention has generally been described in terms of subscriber status data stored and accessed from a single subscription database 110 , in embodiments data regarding one or more users may be shared or distributed across multiple databases or data hosts . in embodiments all or part of that data may be stored in client 102 , itself . further , while the invention has generally been described in embodiments wherein the installation engine 120 may be hosted in client 120 , in embodiments the installation engine 120 or similar logic may be hosted or may execute in other local or remote resources , including the installation server 108 . similarly , while the invention has in embodiments been generally described as involving subscriptions covering individual users , in embodiments the subscriptions to services and corresponding installation management may be for groups of users or organizations . other hardware , software or other resources described as singular may in embodiments be distributed or shared , and similarly in embodiments resources described as distributed may be combined . the scope of the invention is accordingly intended to be limited only by the following claims . | 7 |
fig1 shows an external rotor 22 for an external - rotor motor 20 as depicted in fig7 . external rotor 22 has a rotor cup 24 that is usually manufactured from plastic or a lightweight metal . the parts that are facing toward rotor cup 24 will be referred to hereinafter , by analogy with medical terminology , as “ proximal ,” and the parts facing away from rotor cup 24 as “ distal .” mounted in the center of rotor cup 24 , i . e . on its hub 36 , is proximal end 26 of a shaft 28 at the distal end of which is provided an annular groove 30 that serves , as shown in fig2 , for mounting of a snap ring 32 . the distal end of shaft 28 is labeled 34 . shaft 28 has a cylindrical cross section , and its diameter is constant over practically the entire length . located on hub 36 is an axial projection 38 that protrudes in the distal direction away from hub 36 and has a depressed region 39 in its center . a magnetic yoke in the form of a sheet - metal ring 40 made of soft iron is mounted in rotor cup 22 , and on the ring &# 39 ; s inner side is located a ( usually flexible ) ring 44 made of permanent - magnetic material , usually a so - called rubber magnet , i . e . a mixture of ferromagnetic particles and an elastomer . ring 44 is magnetized in the radial direction with the requisite number of magnetic poles , e . g . with four poles as is common practice in the art . as shown in fig2 , a variety of components are pre - installed on shaft 28 prior to the assembly of motor 20 . beginning at projection 38 , the first is a compression spring 48 of approximately conical shape whose proximal , larger - diameter end lies in depression 39 . following spring 48 in the distal direction is an annular retaining member in the form of a retaining washer 50 , as described in more detail below with reference to fig8 and 9 . spring 48 preferably is not in contact against this retaining member 50 . retaining member 50 is followed by a proximal rolling bearing 52 comprising an outer ring 54 and an inner ring 56 . the latter is displaceable in the axial direction on shaft 28 with a small clearance . the distal end of spring 48 is in contact against the proximal end of inner ring 56 . rolling bearing 52 is followed in the distal direction by a spacer 58 , which is guided displaceably on shaft 28 by means of a radially inwardly protruding projection 59 , and whose proximal end is in contact , as depicted , against the distal end of outer ring 54 . spacer 58 is followed by a distal rolling bearing 60 comprising an outer ring 62 that is in contact with its proximal end against spacer 58 , and comprising an inner ring 64 that is displaceable in the axial direction on shaft 28 with a small clearance and is in contact with its distal end , as depicted , against snap ring 32 when motor 20 is completely assembled . ( optionally , a spacer or the like can also be located between snap ring 32 and rolling bearing 60 , e . g . in order to compensate for tolerances .) it is immediately apparent that by pressing with a force f in the proximal direction on distal rolling bearing 60 , spring 48 can be compressed and the two rolling bearings 52 and 60 , spacer 58 , and retaining washer 50 can be displaced in the proximal direction on shaft 28 , so that inner ring 64 is no longer in contact against snap ring 32 but becomes spaced away from it . in this case projection 38 of rotor cup 24 comes into contact against retaining washer 50 and allows an axial force to be transferred via the latter , in the distal direction , onto retaining washer 50 , outer ring 54 , spacer 58 , and outer ring 62 when rotor cup 24 is pressed downward , i . e . in the distal direction , by a force k upon assembly . this is depicted below in fig6 . fig3 shows bearing support tube 70 of external - rotor motor 20 , which tube is usually manufactured from plastic or a lightweight metal . in this embodiment it has at the bottom a flange 72 that serves to mount motor 20 , e . g . to mount it on a fan housing or some other device to be driven . bearing support tube 70 has on its outer side a shoulder 74 , and adjacent thereto in the proximal direction a circumferential surface 76 that tapers toward the top in frustoconical fashion . on its inner side 78 , bearing support tube 70 has six longitudinal ribs 80 that end at a distance d from the closed distal end 82 of bearing support tube 70 . they are followed in the distal region by a total of eight ribs 84 whose proximal ends form , during assembly , a stop for outer ring 62 of distal ball bearing 60 ( see fig7 ). these ribs 84 taper in the proximal direction so that distal end 34 of shaft 28 has sufficient room during assembly ( see fig6 ). the bearing support tube has projections 86 at its upper , proximal end ( see fig6 ). fig5 shows the manner in which a stator lamination stack 90 is mounted on bearing support tube 70 . lamination stack 90 has for this purpose a coil former 92 made of plastic into which a stator winding 94 is wound . a circuit board is indicated at 93 . fig5 shows two winding ends 95 , 96 that are soldered respectively onto an associated metal pin 98 and 97 . coil former 92 has , as depicted , an inwardly protruding projection 100 with which it is pressed onto outer side 76 of bearing support tube 70 . fig6 shows a snapshot , so to speak , during the “ marrying ” operation in which shaft 28 of rotor 22 , with rolling bearings 52 , 60 located thereon , is introduced for the first time into inner recess 78 ( see fig3 ) of bearing support tube 70 . in this context , a force k is applied in the distal direction onto rotor 22 , and because outer rings 54 , 62 of rolling bearings 52 , 60 are pressed with a press fit into ribs 80 ( see fig3 ) of bearing support tube 70 , spring 48 is compressed by force k so that shaft 28 is displaced in the distal direction within ball bearings 52 , 60 , and projection 38 pushes via retaining washer 50 on outer ring 54 of ball bearing 52 , and via spacer 58 also on outer ring 62 of ball bearing 60 , and thus presses the two ball bearings 52 , 60 into bearing support tube 70 . as depicted in fig6 , spring 48 is only partly compressed in this process in order to prevent damage to it . the pressing - in operation continues until outer ring 62 of distal ball bearing 60 is in contact against the proximal ends of ribs 84 . in this context , as depicted , retaining member 50 is displaced in bearing support tube 70 in the distal direction , i . e . downward , and digs into the material of bearing support tube 70 so that the entire bearing arrangement is latched or locked in bearing support tube 70 . if an attempt were made to pull rotor 22 out of bearing support tube 70 oppositely to force k , retaining member 50 would only dig that much more deeply into the material of bearing support tube 70 , so that the attachment here is therefore extraordinarily secure . there are , of course , many different solutions and components for a permanent latching system of this kind , and retention member 50 that is depicted therefore represents only a preferred embodiment . after the pressing - in operation is complete , force k is removed and the result then is as shown in fig7 , i . e . spring 48 again presses shaft 28 upward in the proximal direction until snap ring 32 is again in contact against inner ring 64 of distal rolling bearing 60 . the marriage is then complete . spring 48 now clamps the two inner rings 56 , 64 of rolling bearings 52 , 60 against one another , which is favorable in terms of quiet operation of motor 20 . fig8 and 9 show a preferred embodiment of a retaining member 50 . this has in the middle an opening 110 for the passage of shaft 28 and of the distal end of compression spring 48 . opening 110 is located in a flat part 112 that is adjoined toward the outside by a frustoconical portion 114 whose upper ( in fig8 ) end 116 digs into the material of bearing support tube 70 upon assembly because its diameter is greater than the inside diameter of bearing support tube 70 . portion 114 could be divided , by slots that extend in the axial direction , into a plurality of individual prongs . in this case an annular retaining member of this kind can also be referred to as a prong washer or prong ring . it is usually not necessary , however , to provide such individual prongs . it can also be very advantageous to implement spring 48 and retaining member 50 together as a single component . these parts can , for example , be welded together , or spring 48 can be machined directly out of the material of retaining washer 50 . in other ways as well , many variants and modifications are possible in the context of the present invention . | 5 |
with reference now to the drawings , as best the present invention provides an electrical wiring harness specifically designed for use on the main landing gear of a jet aircraft as best illustrated in fig1 - 5 . more particularly , a modern jet aircraft , such as the canadair regional jet referenced as 100 , includes left and right main landing gear systems , referenced as 102 - l and 102 - r respectively . fig2 is a partial view of the left main landing gear 102 l and depicts the landing gear in a partially deployed configuration . fig3 is a partial detailed view of the lower portion of the main landing gear with the wheels removed . fig4 and 5 depict inboard side views of the left and right main landing gear in fully deployed ( e . g . down ) configuration with the wheels removed . each left and right main landing gear system , 102 - l and 102 - r , have inboard and outboard wheels , referenced as 104 - ib and 104 - ob respectively . each of the wheels includes a brake temperature sensing system (“ bts ”), a weight - off - wheels sensing system (“ wow ”), and an anti - skid system . accordingly , each main landing gear requires two electrical harnesses such as the prior art harnesses depicted in fig1 - 5 . more particularly , the prior art harnesses include an inboard harness 106 - ib and an outboard harness 106 - ob , for routing electrical wiring from sensors and other electrical components associated with the inboard and outboard landing gear systems to monitoring and control systems located onboard the aircraft . the prior art inboard and outboard harnesses comprise unitary structures that run from the aircraft &# 39 ; s landing gear wheel well down the landing gear structure to the inboard and outboard wheels . as noted hereinabove , a failure associated with any one part of the prior art harnesses requires replacement of the entire harness thus grounding the aircraft for many hours while the defective harness is replaced . with reference now to fig6 - 13 there is depicted a modular main landing gear electrical wiring harness 10 for use on the landing gear of a jet aircraft according to a preferred embodiment of the present invention . as more fully disclosed herein , modular main landing gear wiring harness 10 incorporates advanced structural and functional features for preventing moisture intrusion and for preventing corrosion . harness 10 is particularly designed to allow operators easier troubleshooting and replacement of various harness systems . landing gear harness 10 includes a main harness sub - assembly 20 , a brake temperature monitoring sub - assembly 30 , a weight - off - wheels sub - assembly 40 , and an anti - skid sub - assembly 50 . as depicted in fig6 a , and 7 b , main sub - assembly 20 is the main connection point between the airframe of the aircraft and the remaining sub - assemblies that traverse downward along the main landing gear . main sub - assembly 20 has a large mil - spec connector 22 at a proximal end thereof , and two smaller mil - spec connectors 24 and 26 forming a y - junction at a distal end thereof . main sub - assembly 20 provides a conduit that houses all of the relevant wires for the weight - off - wheels , brake temperature monitoring system and anti - skid system sub - assemblies . large mil - spec connector 22 mates with a corresponding mil - spec connector ( not shown ) positioned in the airframe of the aircraft . the two smaller mil - spec connectors 24 and 26 mate with corresponding mil - spec connectors . more particularly , mil - spec connector 24 is attached to a corresponding mil - spec connector 42 on the weight - off - wheels sub - assembly 40 , and mil - spec connector 26 is attached to a corresponding mil - spec connector 32 on the brake temperature monitoring system sub - assembly 30 . as best depicted in fig9 , the weight - off - wheels (“ wow ”) sub - assembly 40 includes connector 42 at a proximal end thereof that is normally connected to mil - spec connector 24 on main sub - assembly 20 , and a proximity sensor 44 at a distal end thereof . proximity sensor 44 functions in accordance with the hall principle and is capable of generating a “ signal near ”, “ signal neutral ” and “ signal far ” indication . each signal is sent via the harness back to a control box ( not shown ) located in the avionics bay of the aircraft . this information is filtered and then sent to the flight control deck where it relays pertinent information to the pilot . the sensor is mounted directly to the main landing gear in a method as to indicate the position of the landing gear relative to the ground . the signal near is generated when the target is in direct view of the sensor indicating the full weight of the aircraft is on the landing gear , because the aircraft is on the ground . the signal neutral , which indicates a target in transit , is generated when the landing gear is transitioning from the full weight on wheels position to full weight off wheels as the aircraft became airborne . the signal far , which indicates that the original target transitioned through the full range of motion and at the end of its travel , indicates that the full weight of the aircraft is off of the wheels . as best depicted in fig6 and 8 , the brake temperature monitoring system (“ btms ”) sub - assembly 30 is a harness that has a first mil - spec connector 32 at a proximal end thereof end coupled to the corresponding mil - spec connector 26 on the main harness sub - assembly 20 . at the distal end of the btms sub - assembly 30 is a first mil - spec connector 34 that attaches to a thermal couple ( not shown ) installed on the main wheel brake assembly , and a second mil - spec connector 36 that attaches to the anti - skid sub - assembly 50 . the harness has wires for both the anti - skid sub - assembly and the btms sub - assembly . the btms sub - assembly includes pre - calibrated chromel and alumel wires that translate heat readings from a thermal couple installed in the main wheel brake assembly up through the harness sub - assembly to the main harness sub - assembly , and eventually to a control box in the avionics bay that filters the information and provides a warning to the flight control deck should the temperature of the main wheel brake assembly exceed its operating limitations . this warning allows the crew time to release the brakes and allow them to cool prior to blowing out either the tires and / or fusible plugs located in the wheel rims . mil - spec connector 36 is connected to a corresponding mil - spec connector 52 on the anti - skid sub - assembly 50 . as best depicted in fig6 and 10 , the anti - skid sub - assembly 50 is a small harness comprised of tubing with a first mil - spec connector 52 connected to a corresponding mil - spec connector 36 on the btms sub - assembly 30 . anti - skid sub - assembly 50 is routed through a neoprene grommet ( not shown ) inserted into the main gear wheel axle assembly and transitioned through the interior of the axle to the wheel speed sensor that is located at the end of the axle assembly . the wheel speed sensor is maintained in a stationary position inside the inner dimension of the axle and has a rotating boss at one end and a mil - spec connector at the other . that mil - spec connector ( not shown ) attaches to the corresponding mil - spec connector 54 on the anti - skid sub - assembly 50 and the rotating boss fits into a corresponding recess on the back side of the main wheels hub cap assembly . as the main wheel spins , the hubcap also spins which in turn spins the wheel speed sensor . signals from the sensor are transmitted up through the anti - skid sub - assembly 50 through btms sub - assembly 30 onto main harness sub - assembly 20 . from there these signals are again transmitted to a control box located in the avionics bay of the aircraft were the signal is filtered and interpreted . unlike previous signals , software in the control box will control , through electronic pulses , hydraulic fluid that will engage and disengage in rapid succession the main wheel brakes in an effort to prevent them from locking the wheels and causing damage to the tires and / or to the airframe . the landing gear harness assembly of the present invention is preferably configured for both an inboard configuration and an outboard configuration , wherein the only difference is that the main sub - assembly 20 has a longer overall dimension in the outboard configuration than the main sub - assembly 20 used in the inboard configuration . the additional length of main sub - assembly 20 in the outboard configuration enables the harness to be routed over the landing gear structural members to an outboard position . conversely the main sub - assembly for an inboard configuration is shorter than its outboard counterpart . the dimensional difference allows the harnesses to accommodate the landing gear movement as the gear retracts toward the centerline of the aircraft . therefore , the inboard harness must traverse a smaller radius than the outboard harness . as should now be apparent , a significant aspect of the present invention relates to the modular aspect of the harness . by providing a modular harness troubleshooting is simplified , and individual harness sub - assemblies may be easily removed and replaced without requiring that the aircraft be taken out of service to replace the entire harness assembly as is required with non - modular harnesses of the prior art . more particularly , the harness of the present invention has received faa certification to allow for interchangeability of the three main sub - assemblies , namely the wow , btms , and as sub - assemblies , between all four positions , e . g . left landing gear inboard and outboard , and right landing gear inboard and outboard . accordingly , the modular harness sub - assemblies are capable of being used as replacement parts for both the left hand and right hand — inboard and outboard positions on the landing gear . as a result of the interchangeability of the sub - assemblies the landing gear harness spare parts inventory required to service a particular jet aircraft is reduced by approximately 60 % over inventory requirements for prior art harnesses . an additional significant aspect of the present invention relates to the use of composite connectors that meet the requirements of mil - c - 38999 . the composite connectors have added strength , reduce overall weight and increase corrosion resistance . more particularly , the connectors use gold plated pins and sockets which increase conductivity as well as corrosion resistance . in addition , the wire used in the harness assembly is silver coated copper , instead of the tin coated wires used in the prior art harnesses . furthermore , the harness incorporates sealing thermal fit tubing with an adhesive lining to seal all openings in the joints at various transition areas of the harness . by covering various transition areas of the harness , not only are these areas protected against moisture contamination , but also added strain relief is provided to help against damage from servicing and vibration . as best illustrated in fig1 , a further significant aspect of the present invention relates to the incorporation of abrasion resistant thermal tubing on portions of harness 10 . more particularly , harness 10 includes abrasion resistant sleeves , referenced as 60 for shielding the underlying tubular harness structure from abrasion . the ability to shield portions of the harness from abrasion is considered particularly important since the present inventor has discovered that repeated extension and retraction of the landing gear causes the wiring harness to rub against portions of the landing gear structure thereby leading to failure . as best illustrated in fig1 , the landing gear wiring harness of the present invention is further adapted to include part number identification labels such that each sub - assembly is easily identifiable . labeling each sub - assembly with an identification label is considered particularly important given the modular nature of the wiring harness of the present invention as each of the above - referenced sub - assemblies may be disconnected and removed from the aircraft . the instant invention has been shown and described herein in what is considered to be the most practical and preferred embodiment . it is recognized , however , that departures may be made therefrom within the scope of the invention and that obvious structural and / or functional modifications will occur to a person skilled in the art . | 1 |
in the following detailed description of the preferred embodiments , reference is made to the accompanying drawings that form a part hereof , and in which are shown by way of illustration specific embodiments in which the invention may be practiced . it is to be understood that other embodiments may be utilized and structural changes may be made without departing from the scope of the present invention . many logic designs are created in a high - level hdl such as verilog or vhdl . thorough testing of the device is an important part of the design process and involves the performance of many tests , each of which may include a number of individual tasks . these tasks are typically defined once and called multiple times in the performance of one or more tests . for example , verilog supports tasks that can be defined once , but are called many times to perform a common task , such as a microprocessor read or write . even though tests are typically performed on a number of separate parts of the dut , many tests must still be run sequentially to make sure no task collisions occur . typically , the highest risk of a task collision is at the microprocessor interface . since several tests might be able to test different parts of the logic device simultaneously , it would make sense to run the tests concurrently so that the time spent during simulation is minimized if task collisions could be avoided . fig1 shows an example of how the problem of task collisions in an hdl testbench environment have been handled in the past . step 101 defines the various tests in the hdl testbench . in steps 103 , 105 and 107 the tests are run sequentially , i . e ., at a different time to ensure that task collisions are avoided . the method of the present invention enables multiple hdl tests to be run simultaneously . to avoid the possibility of a task collision , the present invention enables each task to be performed and completed before other , potentially conflicting , tasks are allowed to perform . to implement the invention of the present application , one must determine how many clock cycles the tasks in question will take to complete and how many tests will be performed at the same time . once this has been determined , unique timeslots can be assigned to one or more of the tests to be performed simultaneously such that each timeslot will allow for tasks of a test to be completed during the designated timeslot . in this way , advantageously , a number of tests can be performed at the same time , and result in considerable time savings in an hdl verification process . fig2 illustrates a method of running simultaneous hdl tests according to the present invention . step 201 defines the various tests to be performed in the top level of the testbench and assigns a timeslot to each test . each task may be evaluated to determine whether it may collide with a task of another test . if the task may potentially collide with any other task , the task is put in the timeslot corresponding to the timeslot assigned to the test to which it belongs . thus , the task should be defined to include a discrete timeslot symbol or input variable to let it know which timeslot it is to use . the number of bits of the input variable will depend on the number of timeslots required . if the task is certain not to collide with any other task a timeslot is not necessary and may be skipped for that task . after determining the number of clock cycles needed to perform the longest task , timeslots are created by generating a counter in step 202 in the top level test bench of the hdl . for simplicity , a single counter is used to count both timeslots and time . the number of bits in the counter should be sufficient to allow enough time for the longest task of any of the tests to be completed and also to count the number of timeslots needed for the tests to be performed simultaneously . for example , if the longest task takes 10 clock cycles to be performed , and there will be two timeslots , the counter should have at least 5 bits . as many tests as there are timeslots available can be run simultaneously . if more tests are to be run simultaneously additional bits can be added to the counter . for example , to allow for up to 8 timeslots , and a timeslot of up to 16 clock cycles , the counter should have at least 7 bits . in this case , the bottom least significant 4 bits may be used to provide the time to make sure the task can be completed in the up to 16 clock cycles and the top most significant 3 bits at step 204 will allow for 8 different timeslots . these can be used to make sure that the tests 206 , 212 and 214 running concurrently will not have task collisions . when a task is called , the assigned timeslot must be passed to it . at step 206 , test 1 , which has been assigned timeslot 1 , is called . the process checks at step 208 to see if timeslot 1 is indeed available . if it is not , test 1 waits at step 208 until the timeslot is available . once timeslot 1 becomes available , the task executes at 210 . if another task is to be executed as a part of test 1 , the process again checks to see if timeslot 1 is available . if the assigned timeslot is not yet available , the process again waits for timeslot 1 . when timeslot 1 is available , the additional task is executed at step 213 . the process continues in the same manner until all of the tasks of the test have been completed . in this way , during testing , if the verification process calls another task that might cause a task collision , the task will wait for its designated timeslot . in this example , the passed - in variable timeslot for each task will wait until it matches the top 3 bits in the counter , which is the counter at the top - level test bench . the same procedure applies for tests 2 to test n . test 2 begins at step 212 and waits for timeslot 2 to become available at 209 . when timeslot 2 is available , the task executes at step 215 . likewise , test n begins at step 214 and waits for timeslot n to become available at 217 . when timeslot n is available , the task executes at 219 . in this way each test can proceed simultaneously and tasks can be executed in assigned timeslots and will not collide with tasks called from any other tests . not all tasks , of course , will run the risk of a task collision . if any one or more of the tasks for a test would not conflict with tasks to be performed by another simultaneous test there is no need to assign the task a timeslot . in that case , the task will execute without going through the step of determining if a timeslot is available . although specific embodiments have been illustrated and described herein , it will be appreciated by those of ordinary skill in the art that any arrangement which is calculated to achieve the same purpose may be substituted for the specific embodiments shown . this application is intended to cover any adaptations or variations of the present invention . therefore , it is intended that this invention be limited only by the claims and the equivalents thereof . | 6 |
as will become apparent from the following description , the present invention is beneficial when applied to rapid prototyping systems that utilize lasers in the fabrication of articles from computer readable representations of those articles , such as those created by computer - aided - design ( cad ) or computer - aided - manufacturing ( cam ) systems . it is contemplated that the present invention is particularly beneficial when applied to rapid prototyping methods that are based upon a thermal mechanism . as is well - known in the art , selective laser sintering is a rapid prototyping approach that uses a thermal mechanism to form the article , in that particles of powder in selected locations of each of a sequence of layers are fused to one another at locations that receive laser energy . the fusing or binding of particles at the selected locations takes place through one of a number of thermal mechanisms , including sintering ( in its traditional sense ), melting and resolidification , initiation of a chemical reaction ( including thermosetting ), or some other thermally based mechanism ; for purposes of this description , and as consistent in the rapid prototyping field , all of these mechanisms will be referred to as “ sintering ”. accordingly , the following description will be directed to a selective laser sintering system . it is of course to be understood that the present invention may be used to benefit in other types of rapid prototyping systems that involve a thermal mechanism . fabrication of a cross - section of the desired article or articles is effected by laser 110 , which provides a beam which is directed by scanning system 142 in the manner described in the u . s . patents referred to hereinabove and as will now be described relative to fig3 . laser 110 includes , in addition to a laser itself , such conventional control elements as described in the above - referenced u . s . pat . no . 4 , 863 , 538 , including for example a front mirror assembly , and focusing elements such as diverging and converging lenses . the type of laser 110 used depends upon many factors and in particular upon the type of powder that is to be sintered . for many types of conventional powders , a preferred laser is a 100 watt co 2 type laser with controllable power output , although lasers having as low as 25 watt power output are useful with some materials . laser 110 , when on , emits laser beam 105 that travels generally along the path shown by the arrows in fig3 . computer 140 and scanning system 142 control the direction of laser beam 105 as it impinges target surface 104 . in this preferred embodiment of the invention , computer 140 includes a controlling microprocessor for scanning system 142 and further includes a system for storing a computer readable representation of the article or articles being produced , such as a cad / cam data base or data files generated from such a database , at least in slice - by - slice form if not in entirety , to define the dimensions of the article or articles being produced . a conventional personal computer workstation , such as a microprocessor - based personal computer that includes floating point capabilities , is suitable for use as computer 140 in the preferred embodiment of the invention . computer 140 generates signals on lines aim to scanner processor 103 , in scanning system 142 , to direct laser beam 105 across target surface 104 according to the cross - section of the article to be produced in the current layer of powder . laser power control system 150 controls the power of laser 110 in response to control signals from computer 140 and feedback signals from scanner processor 103 ; an example of advanced laser power control that may be used in connection with this embodiment of the invention is described in the above - incorporated u . s . pat . no . 6 , 151 , 345 . scanning system 142 includes prism 144 for redirecting the path of travel of laser beam 105 ; the number of prisms 144 necessary for directing laser beam 105 to the proper location is based on the physical layout of the apparatus . alternatively , as is well known in the art , one or more fixed mirrors can be used in place of prism 144 for directing laser beam 105 , depending upon the particular layout of system 100 . scanning system 142 further includes a pair of mirrors 146 , 147 , which are driven by respective galvanometers 148 , 149 . galvanometers 148 , 149 are coupled to their respective mirrors 146 , 147 to selectively orient the mirrors 146 , 147 and control the aim of laser beam 105 . galvanometers 148 , 149 are mounted perpendicularly to one another so that mirrors 146 , 147 are mounted nominally at a right angle relative to one another . scanner processor 103 in scanning system 142 controls the movement of galvanometers 148 , 149 to control the aim of laser beam 105 within target surface 104 , in response to the signals on lines aim from computer 140 that are generated according to the computer readable representation produced from a cad / cam data base , which defines the cross - section of the article to be formed in the layer of powder at target surface 104 . other scanning systems may alternatively be used in connection with this invention , including , for example , an x - y gantry system that delivers energy beams by way of a fiber optic cable . referring now to fig4 the operation of computer 140 in controlling laser beam 105 according to the preferred embodiment of the invention will be described in detail . this operation begins with several processes ( not shown in fig4 ) in which parameters are established for a given build cycle . as known in the art , a build cycle refers to a cycle of operation of the system of fig3 in which one or more articles are formed in layerwise fashion in one instance of part bed 107 . for this build cycle , as conventional in the art , the desired powder material is selected by the human user . computer 140 in turn reads a file to load various build parameters such as laser power , part bed temperature , and the like . the process begins with the enabling of scan direction optimization by the human user of selective laser sintering system 100 in process 200 . the optimization of scan directions is contemplated to be an optional feature in selective laser sintering , and as such is expected to be selectable for each build cycle by the user . if scan direction optimization is not enabled , generation of the fill vectors for each layer of powder will be performed in the conventional manner . following enabling of the optimization of the scan direction in process 200 , certain build parameters are set by the human user , and stored in the memory of computer 140 , in process 201 . these build parameters include those that are necessary to define the scanning of laser beam 105 in the build cycle , including the thickness of the powder layers to be dispensed , and the scan fill spacing , or pitch , between adjacent raster scan lines . other related parameters such as laser spot size , scan speed , and the like may also be set in process 201 , if not previously stored in computer 140 . in process 202 , the human user of system 100 arranges , with the assistance of computer 140 , the article or articles to be fabricated within part bed 107 in this build cycle . of course , if multiple articles are to be fabricated , these articles are arranged to fit within part bed 107 . it will be apparent to those skilled in the art having reference to this specification that processes 200 , 201 , 202 may be performed in any order . individual layers , and individual cross - sections of the articles to be formed in those individual layers , are now processed beginning with process 204 . in process 204 of fig4 computer 140 receives a computer readable representation of the articles to be formed in the current selective laser sintering build cycle , and generates the set of outline and fill vectors to be traced in each layer of powder , referenced to a coordinate system of target surface 104 at the top layer of powder in part bed 107 . the generation of the vectors in process 204 may be performed in real - time during the build itself , for example by generating the vectors for the next layer during the selective laser sintering of a prior layer , or alternatively process 204 may be carried out as a batch operation , for all layers in the build cycle prior to initiating selective laser sintering . in addition , all or part of process 204 may be performed by computer 140 in system 100 , or alternatively by a separate off - line computer . for purposes of this description , process 204 will be described as a real - time process , performed by computer 140 . referring now to fig5 process 204 for generating the fill vectors for one or more cross - sections of articles to be formed in each of the layers of the build cycle , according to the preferred embodiment of the invention , will be described in detail . for purposes of this description , the current layer of powder for which computer 140 is generating the fill vectors will be referred to as layer k , and the current article cross - section upon which computer 140 is operating will be referred to as cross - section j . it is of course understood that multiple article cross - sections within the same layer may belong to different articles , or to the same article , depending upon the particular geometries of the desired articles . as will become apparent from the following description , according to the preferred embodiment of the invention , the vectors for each layer are generated substantially one layer at a time , for the current ( or next ) layer k of powder that is to be selectively sintered by laser beam 105 . to conserve memory , therefore , process 220 is first performed , according to the preferred embodiment of the invention , to discard the stored vectors for a previous layer ( e . g ., k - 1 or earlier ) from the memory of computer 140 , once those stored vectors have been used in selective laser sintering . the layer for which the vectors are discarded may be the immediately prior layer to the current layer , or may be for a layer even further back in the process , depending upon the memory resources of computer 140 and any “ pipelining ” of the vector generation that is implemented . according to this preferred embodiment of the invention , a set of contour vectors are then defined for current cross - section j in current layer k , in process 222 . these contour vectors will be defined relative to an x - y coordinate system applied to the target plane of system 100 , with the origin of this coordinate system ( and the assignment of the x and y axis directions ) being arbitrarily assigned . typically , in a two - mirror scanning system as described above relative to system 100 in fig3 the fast scan axis ( i . e ., the x - axis ) will be parallel to the line traced by laser beam 105 when mirror 147 is rotated and mirror 146 is held fixed , while the slow scan axis ( e . g ., the y - axis ) will be parallel to the line traced by laser beam 105 when mirror 146 is rotated and mirror 147 is held fixed . once the contour of cross - section j in layer k is defined by computer 140 in process 222 , process 225 is next performed to evaluate and test the fill scan time for this cross - section at multiple rotational angles , so that the scan time of this cross - section can be optimized according to the preferred embodiment of the invention . in summary , computer 140 will effectively simulate the scanning of the current cross - section j in current layer k at several rotations from its position as arranged in process 202 . the results of these simulations will determine an optimal orientation for the fast scan axis in the scanning this cross - section j ; this optimal orientation is that at which the shortest scan fill time is obtained . attention is now directed to fig6 and 7 , relative to which the steps of process 225 according to the preferred embodiment of the invention will be described in detail . [ 0039 ] fig6 illustrates an exemplary set of angles of rotation in the x - y plane corresponding to target surface 104 at the top layer of powder in part bed 107 of system 100 . in this example , eight possible rotations are shown , ranging from a rotation of + 90 ° to a rotation of − 67 . 5 ° including no rotation ( i . e . rotation of 0 °). the sample rotations in this example are separated by 22 . 5 °, or one - sixteenth of a rotation . the other angles ( rotations from + 112 . 5 ° to − 90 °) opposing the eight rotations from + 90 ° to − 67 . 5 °, and need not be included in process 224 , because their associated scan times will be identical to those of their corresponding opposites . referring now to fig7 process 225 begins with the selection of certain parameters to be used in the testing or simulation . because process 225 is a simulation or calculation , the actual structural strength of the object is not pertinent , and thus the spacing of the fill scans in process 225 can be expanded from that which will actually be used . it is therefore contemplated that a fair comparison of the scan times can be derived by simulating the time required to scan a fraction of the actual scans that will be carried out . in process 234 , therefore , the user selects a sample ratio , which is the ratio of the number of scans to be evaluated in process 225 for the current cross - section , relative to the number of scans that selective laser sintering system 100 will actually carry out in fabricating the cross - section . it is contemplated that a ratio of 1 : 2 will often provide an accurate relative measure of the fill scan times of the various rotations , while still reducing the computational time and resources of the simulation . also in process 234 , the user of computer 140 selects the incremental angle of rotation between simulated rotations ; in the example of fig6 the incremental angle δ is 22 . 5 °. the iterative simulation and calculations of sample fill times begins with process 236 , in which current x - section j is “ rotated ” by angle φ m according to a rotation index m . as noted above , the angle of rotation φ m includes no rotation , or φ m = 0 °. in process 238 , computer 140 calculates the time that would be required to fill carry out a fill scan of cross - section j of layer k , when rotated by the current angle φ m . this calculation of process 238 is performed for the number of scans determined by the sample ratio selected in process 234 , but otherwise is intended to sum the time required for the particular scan itself along the fast scan direction ( x - direction ), plus the incrementing in the slow scan axis ( y - direction ). for improved accuracy , additional time for each scan line can include acceleration and deceleration times at the ends of the vectors , as described in the above - incorporated u . s . pat . no . 6 , 085 , 122 , and any time required for scanning the laser beam outside of the outline of cross - section j . these factors are important in the actual simulation and calculation of process 238 , considering that approximately the same scan fill area is subsumed by cross - section j , regardless of the orientation of the fill scan lines , which indicates that the actual true scan time is constant over the various rotations . however , because of the overhead time involved in connection with each linear scan , regardless of its length , the number of scans is preferably minimized in determining the optimum cross - section orientation for selective laser sintering . [ 0042 ] fig8 a illustrates an exemplary cross - section 252 0 , in its position in the x - y plane as arranged in process 220 ; in other words , at a rotational angle φ m of 0 °. in this representation of fig8 a , the sampled fill scan lines are parallel to the x - axis . these sampled fill scan lines are separated relatively widely from one another , as described above , considering that process 238 is a simulation only , and therefore the derived scans need not be so closely spaced as to form a unitary cross - section . indeed , it is preferred to not store the actual simulated fill scans themselves in the memory of computer 140 for cross - section 252 0 , beyond the completion of process 238 , to conserve the memory resources of computer 140 . in addition , there is no need to center or otherwise translate the position of cross - section 252 for purposes of the calculation , thus saving additional computational resources . in process 238 , computer 140 calculates an estimate of the time that would be required to scan cross - section 252 0 in the manner illustrated in fig8 a , and stores this estimate in its memory . computer 140 next determines whether any remaining rotational angles are to be estimated for current cross - section j . if so ( decision 239 is yes ), index m for rotational angle φ m is incremented ( or decremented , if appropriate ), in process 240 , and control returns to processes 236 , 238 for the rotation of current cross - section j and the calculation of its estimated sample fill scan time , respectively . [ 0044 ] fig8 b and 8 c illustrate two other exemplary rotated cross - sections 252 + 1 , 259 − 1 , for comparison with non - rotated cross - section 252 0 . in fig8 b , cross - section 252 + 1 is rotated in a positive angular direction by one incremental angle δ , which in this example is 22 . 5 °. as evident from fig8 b , the simulated scan lines are again parallel to the x - axis . in fig8 c , cross - section 252 1 is illustrated as rotated from non - rotated cross - section 252 0 by one incremental angle δ in the negative angular direction , which in this example is − 22 . 5 °. again , its sampled simulated scan lines are parallel to the x - axis . it is of course contemplated that , in performing process 225 to test the scan fill time of the rotated cross - sections , computer 140 may alternatively rotate the angle of the simulated scan lines while maintaining the orientation of the cross - section fixed , rather than rotating the angular orientation of the cross - section and maintaining the scan direction fixed . according to this embodiment of the invention , and using currently available cad routines , iteratively rotating the cross - section itself is more computationally efficient . upon determining that all desired rotations of current cross - section j have been simulated and their estimated fill scan time stored ( decision 239 is no ), one additional simulation is performed according to the preferred embodiment of the invention . in process 242 , computer 140 refers to the contour of current cross - section j as generated in process 222 , and determines the angle at which the longest outline vector segment is oriented in that current cross - section . once this angle is found , computer 140 then rotates cross - section j by the arithmetic inverse of this angle , so that a rotated cross - section is derived in which the longest outline vector segment is parallel to the simulated scan lines ( in this example , parallel to the x - axis ). referring to the example of fig8 a , the longest outline vector of cross - section 252 is the longer side of the rectangle , which is at an angle approximately − 18 ° from the x - axis ; in this example , therefore , process 242 will rotate cross - section 252 by an angle of + 18 °. the sampled simulated fill scan time is then calculated for this rotation , and the result stored in memory , by computer 140 in process 242 . referring back to fig5 following the calculation of estimated fill scan times for each of the desired trial rotations of current cross - section j in process 225 , computer 140 interrogates these stored estimated fill scan times to identify the minimum estimate , and the rotation associated with that minimum estimated fill scan time , in process 226 . referring back to the example of fig8 a through 8 c , among the three exemplary rotated cross - sections 252 , cross - section 252 + 1 has the minimum fill scan time , considering that it is intersected by fewer scan lines than the others . however , because cross - section 252 is rectangular , the rotation parallel to the longest side as used in process 242 , will provide the true minimum , and therefore , in this example , the optimum angle of rotation is approximately 18 °. in process 228 , the actual fill scans are generated for current cross - section j , based upon the rotation selected in process 226 , and stored in the memory of computer 140 for use in the actual selective laser sintering process . these fill scans are rotated from the nominal fast scan axis ( e . g ., the x - axis ) by the arithmetic inverse of the angle of rotation φ m associated with the rotation selected in process 226 , so that , in the selective laser sintering process , current cross - section j will be scanned at the optimum angle of rotation φ m determined in process 226 . in addition , the spacing of the fill scans derived in process 228 corresponds to the value of the fill scan spacing parameter l selected and stored in process 218 . [ 0049 ] fig8 d illustrates the result of process 228 as applied to cross - section 252 , based upon its optimal rotation . as shown in fig8 d , cross - section 252 ′ is at a non - rotated position , in other words corresponding to non - rotated cross - section 252 0 shown in fig8 a . however , the fill scans in cross - section 252 ′ are not parallel to the x - axis as in the estimates of fig8 a through 8 c , but instead are rotated from the x - axis by the inverse of its optimum rotation . in this example , because the selected optimal cross - section 252 + 1 , was at a rotation of + 18 °, each of the fill scans in cross - section 252 ′ of fig8 d are rotated from the x - axis by − 18 °. preferably , as described in the above - incorporated application ser . no . ______ entitled “ selective laser sintering with interleaved fill scan ”, or alternatively in united kingdom patent application 0118652 . 7 , filed jul . 31 , 2001 , also incorporated herein by this reference , the fill scans for current cross - section j that are generated in process 228 are not only separated from one another by the value of fill scan spacing parameter l , but are positioned relative to the x - y coordinate plane and not to the boundary of cross - section j itself . in addition , the positions of the fill scans are offset from one another , in successive layers k , by one - half the value of fill scan spacing parameter l to maximize the structural strength of the object as formed by selective laser sintering . upon generating and storing the fill scans for current cross - section j in layer k at the optimal rotation in process 228 , decision 229 is performed by computer 140 to determine whether additional cross - sections remain for which fill scans are to be generated . if so ( decision 229 is yes ), index j for cross - sections within the current layer is incremented in process 230 , and control returns to process 222 for the generation of the outline contour vectors and optimized fill scans for the next cross - section . the skilled reader will recognize that , if multiple cross - sections are present in the current layer k , each cross - section has its own optimized scan direction derived independently from that of the other cross - sections in that layer k . fig9 illustrates , in plan view , rectangular cross - sections 250 a , 250 b , 250 c , 250 d at target surface 104 , with their fill scans 62 shown as generated according to the preferred embodiment of the invention described above . cross - sections 250 of fig9 correspond to the same shape , size , and position as cross - sections 50 of fig2 . comparison of fill scans 62 for cross - sections 250 with fill scans 62 of cross - sections 50 illustrate the optimization provided by the present invention . each of cross - sections 250 have the minimum number of scans ( e . g ., four ), regardless of their orientation . in contrast , for cross - sections 50 of fig2 which each have fill scans 62 in the same fast scan direction , parallel to the x - axis , only cross - section 50 a ( which happens to be oriented with its longest sides parallel to the x - axis ) is optimized ; cross - sections 50 b , 50 c , 50 d all require many more than the optimized , minimum , number of fill scans 62 . upon determining that no additional layers remain to be processed ( decision 229 is no ), the generation of fill vectors for the current build cycle is complete . control then passes to the first instance of process 206 ( fig4 ), to begin the actual layerwise fabrication of the article or articles by way of selective laser sintering . alternatively , as discussed above , process 204 may be performed as a batch operation for all layers of the build cycle prior to initiating the actual build , or may alternatively be performed in real - time during the build . referring back to fig4 in combination with fig3 the method of fabricating an article according to the preferred embodiment of the invention continues with the dispensing of a layer of powder at the surface of part bed 107 in process 206 , for example by the translation of counter - rotating roller 118 ( fig1 ) to form the powder layer with minimal shear stress , as described in the above - incorporated u . s . pat . no . 5 , 076 , 869 . other systems for dispensing a layer of powder may alternatively be used , including , for example , the delivery of a volume of powder from above the surface of part bed 107 , and in front of a moving roller or scraper . once the powder is dispensed , laser beam 105 is directed by computer 140 and scanning system 142 to selectively sinter the outline of the cross - sections in the current layer of powder in process 208 , if vector outlining is to be performed . in process 210 , one of the article cross - sections in the current layer of powder at the surface of part bed 107 is raster scanned by laser beam 105 , under the control of computer 140 and scanning system 142 , according to the fill scan vectors generated for that cross - section in that layer in process 204 . as discussed above , the direction of fill scan for each article cross - section in the current layer is optimized for the fastest scan time . because of the independence in scan direction optimization among the various cross - sections , multiple cross - sections in any given layer are likely scanned in different fast - axis directions . decision 211 is therefore performed to determine whether additional article cross - sections in this current layer remain to be raster scanned ; if so ( decision 211 is yes ), control passes back to process 210 to perform the fill scan for that next cross - section . upon completion of the raster , or fill , scanning for each cross - section within the current layer in process 210 ( decision 211 is no ), process 212 is optionally performed to vector - outline each article cross - section in the current layer . alternatively , each cross - section may be outlined immediately prior to or after its fill scanning , after the fill scanning of another cross - section in that layer , or prior to the fill scanning of any one of the cross - sections in the current layer . computer 140 then executes decision 213 to determine whether additional layers remain to be selectively sintered in the current build cycle . if so ( decision 213 is yes ), control passes to process 214 , in which computer 140 increments index k of the layers , and initializes index j to refer to a first cross - section within that next layer . control then passes back to process 204 , for generation of the optimized fill vectors for the cross - sections in this next layer . as is well - known in the art , extremely thin layers , for example on the order of a few tenths of a millimeter thick , are typically used in selective laser sintering . with such thin layers , in many cases the shape of article cross - sections often does not drastically change from layer to layer . accordingly , it is contemplated that the optimized fill scan calculations according to the preferred embodiment of the invention need not necessarily be performed for every layer , but may alternatively be applied periodically to layers in the sequence . such sampling of the layers in optimizing the scan direction will be especially useful in systems that have limited computational capacity for computer 140 , or in which computer 140 is burdened by other tasks involved in the selective laser sintering build cycle . further in the alternative , computer 140 may analyze the article or articles involved in the build cycle , and apply a rule - based or other adaptive algorithm to determine which specific layers in the build ought to be processed for scan direction optimization ; for example , computer 140 may identify those layers at which significant changes in the article cross - sections are present . following the generation of optimized fill vectors for the next layer , process 206 is next performed , to dispense the next layer of powder over the previously sintered layer . processes 208 and 210 then control laser beam 105 to fill scan and vector outline the cross - sections in this new layer , in the manner described above . the process continues , via decision 213 , until the build cycle is complete ( decision 213 is no ). cool down of part bed 107 including the sintered article or articles is then carried out as appropriate for the material used , followed by removal of the loose powder from around the articles . post processing , such as an anneal or infiltration of the articles with another material to improve the properties of the article , is then performed as desired , completing the fabrication of the articles . the present invention provides important advantages in selective laser sintering , particularly in improving the efficiency and manufacturing capacity of selective laser sintering systems . it is contemplated that the overall build cycle time can be significantly reduced through the implementation of this invention . this improvement in build cycle time is available at little cost , other than computational resources of the system computer . considering the significant advances in the capability of modern microprocessors and computer systems , it is therefore contemplated that adequate computational resources are available for use according to this invention . while the present invention has been described according to its preferred embodiments , it is of course contemplated that modifications of , and alternatives to , these embodiments , such modifications and alternatives obtaining the advantages and benefits of this invention , will be apparent to those of ordinary skill in the art having reference to this specification and its drawings . it is contemplated that such modifications and alternatives are within the scope of this invention as subsequently claimed herein . | 1 |
referring now to the drawings , the present purification apparatus , shown generally at 10 , includes an ozone generator , shown generally at 12 , and a transfer assembly , shown generally at 14 . ozone generator 12 includes a housing body 16 and a housing cover 18 which is adapted to be joined or connected to the housing body by coupling threaded inserts 20 through complimentary cover holes 22 with threaded screws ( not shown ). with housing cover 18 secured to housing body 18 , ozone generator 12 is in the form of a compact , closed unit . located within the space 24 between the housing body 16 and housing cover 18 is an ozone - producing corona discharge chip electrode 26 . ozone - containing gases produced from air , which enters housing body 16 through air inlet 27 in the housing , by chip electrode 26 exit the housing through housing outlet 28 , which can be an integral part of the housing body 16 . the air inlet may , and preferably does , include a particulate filter , for example , of conventional construction . both the housing body 16 and housing cover 18 can be made from any suitable material or materials of construction . preferably , these components are made of polymeric material . the ozone generator 12 typically has a length in a range of about 4 inches to about 10 inches , a width in a range of about 1 inch to about 6 inches and a thickness of about 0 . 5 inch to about 4 inches . an electrical transformer 30 , of conventional design , is included within space 24 . electrical transformer 30 processes line power , e . g ., 120v , from source 32 through power cord 33 into power suitable for use by chip electrode 26 . transformer 30 is a “ step up ” transformer in that the chip electrode 26 uses power having a voltage in the range of about 3000 to about 5000 volts and a frequency in the range of about 18 khz to about 20 khz . a series of electrical connectors 33 , 34 and 36 are included within space 24 and are adapted to connect electric wires so as to provide electric power from source 32 ultimately to chip electrode 26 . these connectors are adapted to be easily removed to allow maintenance of generator 12 . a variable potentiometer 37 is provided and is used to control or adjust the ozone output of generator 12 . the top 38 of housing cover 18 includes a transparent window 40 through which the spa owner can visually observe chip electrode 26 , which glows when ozone is being produced . this glow diminishes over time as the chip electrode 26 becomes less effective in producing ozone . thus , the spa owner , by observing chip electrode 26 , is provided with an indication as to when ozone generator 12 should be replaced . atmospheric air from air inlet 27 is directed to come in contact with the chip electrode 26 to produce an ozone - containing gas which passes through housing outlet 28 . in addition , the housing cover 18 includes two end tabs 44 and 46 , each of which includes a through hole 48 through which screws can be passed to secure the ozone generator 12 in place in a suitable stationary position . ozone generator 12 operates as shown in fig1 . spa 50 includes a quantity of heated and circulating water 52 , for example , about 500 to 1000 gallons in volume . the spa 50 is equipped with a water circulating system in which water from the spa passes through spa outlet 54 into conduit 56 through spa pump 58 , spa filter 60 and spa heater 62 . eventually the pumped , filtered and heated water is passed back to the spa 50 through return lines 64 and 66 . in the present invention , piping segment 70 ( a part of conduit 56 ), downstream of heater 62 is divided to provide a bypass line , shown generally at 72 . bypass line 72 includes a venturi assembly 74 , of generally conventional construction , which acts as an ozone adductor to suction ozone - containing gases from ozone generator 12 into bypass line 72 . the combined ozone - containing gases and water is returned to the main water conduit 56 , as shown in fig1 . a valve 78 , of conventional design , is located in water conduit 79 and can be adjusted to control the amount of water passed through bypass line 72 . the ozone - containing gases from ozone generator 12 are passed through housing outlet 28 and through ozone conduit 80 into the water flowing through bypass line 72 . the suction created by venturi assembly 74 causes ozone to flow through ozone conduit 80 . ozone conduit 80 includes a water trap loop 82 located above venturi assembly 74 . this water trap loop 82 acts to protect the ozone generator from being exposed to water in line 56 and bypass line 72 . in addition , ozone conduit 80 includes a check valve 84 , of conventional construction , which effectively prevents fluid flow in the ozone conduit back to the ozone generator 12 . this feature inhibits , or even substantially prevents , any water from line 56 and bypass line 72 from entering ozone generator 12 . apparatus 10 functions as follows . when it is desired to purify / sanitize the water 52 in spa 50 , operation of the pump 58 and ozone generator 12 is initiated . this causes water 52 to flow from spa 50 through line 56 into pump 58 , filter 60 , heater 62 into piping segment 70 . at this point , a minor amount , that is less than about 50 %, of the total water passing through segment 70 is caused to flow through bypass line 72 and venturi assembly 74 . this causes ozone - containing gases being generated by ozone generator 12 to pass through ozone conduit 80 into the water in bypass line 72 , which is ultimately returned to the spa via return line 64 and 66 . sufficient ozone is produced in accordance with the present invention to purify / sanitize the water 52 in spa 50 and / or to maintain such water in the desired purified / sanitized state . the present ozone generator provides a very compact structure which : is easily and conveniently mounted for use in a spa / jetted tub application ; requires relatively reduced amounts of maintenance ; is cost effective to produce and use ; and effectively and efficiently produces ozone in sufficient quantities to perform the desired spa / jetted tub purification / sanitation service . while this invention has been described with respect to various specific examples and embodiments , it is to be understood that the invention is not limited thereto and that it can be variously practiced within the scope of the following claims . | 2 |
to further clarify the concept of the present invention , the presently preferred embodiments of the invention will be described . it is to be understood that the invention is not limited to the details of the illustrated embodiments . it is also to be understood that the invention may be embodied with various changes , modifications and improvements , which may occur to those skilled in the art , without departing from the spirit of the invention . referring first to fig1 ( a )- 1 ( g ), reference numeral 2 denotes a first patterned sheet member which is prepared from a metallic sheet . the first sheet member 2 has a generally comb - like configuration whose outer profile is formed by etching , as indicated in fig1 ( a ) and 1 ( b ). the patterned sheet member 2 has two mutually spaced - apart thin - walled - portions 2a , and three non - etched portions 2b ( thick - walled portions ) in the form of elongate strips of the comb - like configuration . the non - etched portions 2b are spaced apart from each other in the direction of their width . the thin - walled portions 2a have a thickness which is one half of the nominal thickness of the sheet member 2 ( i . e ., one half of the thickness of the non - etched portions 2b ). a second patterned sheet member 4 is prepared from another metallic sheet having the same thickness as that of the first patterned sheet member 2 . as shown in fig1 ( c ) and 1 ( d ), the second sheet member 4 has three thin - walled portions 4a and two non - etched or thick - walled portions 4b , which are located differently from the portions 2a , 2b of the first sheet member 2 . the non - etched portions 4b are spaced apart from each other in the direction of their width . the thin - walled portions 4a also have a thickness which is one half of the nominal thickness of the sheet member 4 . the first and second patterned sheet members 2 and 4 are partially superposed on each other such that the thin - walled portions 2a and 4a engage or contact the non - etched portions 4b and 2b , respectively , so as to accurately position the two sheet members 2 , 4 relative to each other , as indicated in fig1 ( e ), 1 ( f ) and 1 ( g ). thus , the two sheets 2 , 4 are assembled together into a patterned structure 10 , wherein the two sheets 2 , 4 cooperate with each other to define a plurality of elongate rectangular voids in the form of slits 8 having a very small width . as is seen from fig1 ( g ), the thus prepared minutely patterned structure , which has a generally planar shape , has an overall thickness which is about 1 . 5 times as large as the nominal thickness of the patterned sheet members 2 , 4 . referring next to fig2 ( a )- 2 ( g ), there is shown another embodiment of this invention . this embodiment uses a first and a second patterned sheet member 12 , 14 which have the same outer profiles as the corresponding first and second sheet members 2 , 4 of the preceding embodiment . unlike the sheet members 2 , 4 , however , the sheet members 12 and 14 have first thin - walled portions 12a , 14a , and second thin - walled portions 12b , 14b , respectively . these first and second thin - walled portions 12a , 14a , and 12b , 14b have different thicknesses . more specifically , the thickness of the first thin - walled portions 12a , 14a is one third of the nominal thickness of the sheet members 12 , 14 , i . e ., one third of non - etched or thick - walled portions 12c , 14c of the sheets , while the thickness of the second thin - walled portions 12b , 14b is two thirds of the nominal thickness of the sheet members 12 , 14 . the non - etched portions 12c of the sheet 12 are spaced apart from each other in the direction of their width , and the non - etched portions 14c of the sheet 14 are also spaced apart from each other in the direction of their width . the first and second patterned sheet members 12 , 14 are superposed on each other such that the first thin - walled portions of one of the two sheet members engage or contact the second thin - walled portions of the other sheet member . thus , a patterned structure 20 is prepared from the two sheet members 12 , 14 , as shown in fig2 ( e )- 2 ( g ). in this embodiment , the overall thickness of the patterned structure 20 is substantially equal to the nominal thickness of the component sheet members 12 , 14 , as indicated in fig2 ( g ). reference is now made to fig3 ( a ), 3 ( b ) and 3 ( c ) which show a further modified embodiment of the invention , in which only one of two patterned sheet members 22 , 24 , namely , only the sheet member 22 has a thin - walled portion 22a . the first sheet member 22 is prepared from a metallic sheet . the metallic sheet is first etched such that the etched sheet has an outer profile as shown in fig3 ( a ). then , the etched metallic sheet is subjected to an etching operation so as to form the thin - walled portion 22a whose thickness is one half of the nominal thickness of the metallic sheet . thus , the first patterned sheet member 22 is produced , with two rectangular cutouts 23 formed therethrough in the first etching of the metallic sheet such that each cutout 23 is defined by two adjacent non - etched strip portions 22b which are spaced apart from each other in the direction of their width . these cutouts 23 cooperate with strip portions 25 of the second patterned sheet member 24 to define a plurality of elongate rectangular voids in the form of slits 28 which will be described . the second patterned sheet member 24 is prepared from another metallic sheet , so that the sheet member 24 having the strips 25 has an outer profile as shown in fig3 ( b ). the first and second patterned sheet members 22 , 24 are superposed on each other such that the portion of the second sheet member 24 from which the strips 25 extend is in contact with the thin - walled portion 22a of the first sheet member 22 , and such that the cutouts 23 of the first sheet member 22 cooperate with the strips 25 of the second sheet member 24 to define the slits 28 indicated above . thus , the two sheet members 22 , 24 are assembled together into a patterned structure 26 having the narrow slits 28 , as shown in fig3 ( c ). the slits 28 are formed on opposite sides of each strip 25 of the second sheet member 24 which is aligned with the longitudinal centerline of the corresponding elongate cutout 24 of the first sheet member 22 . referring next to fig4 ( a )- 4 ( c ), there is illustrated a still further embodiment of the present invention which uses a first and a second patterned sheet member 32 , 34 . each of these two sheet members 32 , 34 is prepared by etching from a single metallic sheet . both of the sheet members 32 , 34 have a plurality of rectangular cutouts 36 having a relatively large size . the first sheet member 32 has an etched thin - walled portion 32a , and a plurality of non - etched or thick - walled portions 32b which overlap the cutouts 36 . similarly , the second sheet member 34 has an etched thin - walled portion 34a , and a plurality of non - etched or thick - walled portions 34b overlapping the cutouts 36 . the thickness of the thin - walled portions 32a , 34a is one half of the nominal thickness of the sheet members 32 , 34 . these first and second patterned sheet members 32 , 34 are superposed on each other such that the non - etched portions 32b of the first sheet member 32 are fitted in the respective cutouts 36 of the second sheet member 34 while the non - etched portions 34b of the second sheet member 34 are fitted in the respective cutouts 36 of the first sheet member 32 . further , the thin - walled portions 32a , 34a of the two sheet members 32 , 34 are held in contact with each other . as a result , there is produced a planar patterned structure 40 having an array of small rectangular openings or voids 38 which are spaced apart from each other . a still further modified embodiment of the invention is illustrated in fig5 ( a ) through 5 ( h ), wherein each of two stainless steel sheets 42 , 44 as electrically conductive sheets has mutually spaced - apart apertures 45 , each of which have length portions which have different widths . described more specifically , the apertures 45 and thin - walled portions 46 are formed in each stainless steel sheet 42 , 44 , by an etching operation , as in the preceding embodiments . each aperture 45 has a relatively wide central portion 45a , and relatively narrow opposite end portions 45b , 45b on both sides of the central portion 45a . the ends of the opposite end portions 45b are defined by the thin - walled portions 46 . as a result , the apertures 45 define a plurality of mutually spaced - apart , generally elongate electrode portions 48 , each of which has a relatively narrow central portion 48a , and relatively wide opposite end portions 48b , 48b which terminate in the thin - walled portions 46 . the width of the relatively narrow end portions 45b of the aperture 45 is made equal to that of the relatively wide end portions 48b of the electrode portion 48 . the thickness of the thin - walled portions 46 is one half of the thickness of the electrode portions 48 . the two stainless steel sheets 42 , 44 are superposed on each other such that the wide end portions 48b of the electrode portions are snugly fitted in the corresponding narrow end portions 45b of the apertures 45 , whereby an electrode assembly 50 as shown in fig5 ( e ) is prepared . | 8 |
referring now to the drawings wherein reference numerals are used to designate parts throughout the various figures thereof , there is shown in fig1 a section view of the planar magnetron rolled into a cylindrical configuration 10 suitable for operation as an ion source . the same figure can also be interpreted as a sectional view of a rectangular geometry to be discussed later . a magnetic field strength of about 200 gauss appears parallel to the cathode 12 midway between the pole pieces 14 . in this region an intense , donut - shaped negative glow 16 should form with a radial thickness of about 1 cm . the axial length is controlled by the magnetic gap width . a cathode 12 , cylinder diameter of about 3 cm , may be sufficient to form the discharge . the radial dimensions are governed by an electron cycloid diameter of about 1 cm for a 400 ev primary electron in a field of 200 gauss . the cathode cylinder 12 is terminated outside of the re - entrant magnetic field by anode end caps 18 . an axial anode 20 extends down the center of the ion source . in general , the dimensions of the source scale to the magnetic gap size used . for example , the inside diameter could be about 3 gap widths and the inside length could be about 4 gap widths . the diameter of the anode , if in the form of a rod down the center , should be very small compared to the inside diameter of the source . in an alternate embodiment , the axial anode 20 can be eliminated and the anode formed as plates 21 or 23 ( shown in dotted lines ) or both . the shape of the anode is not critical , but it must be outside the region of intense magnetic field . ions are extracted from an aperture 22 cut in the cathode 12 . the ions , originating in a cathode sheath of thickness x , exit the cathode with an energy of 400 ev . then they are accelerated to a final energy of ev o by an electrode spaced a distance d from the cathode . according to present concepts , the extraction fields should form an analytic continuation of the space charge limited fields in a flat cathode sheath . if not , the beam will be severely defocussed and dissipated . the entire region of extraction is governed by child &# 39 ; s law . if v g = 400 volts is the discharge voltage , then to transport a constant current we require that : ## equ2 ## thus , the spacing of the extraction electrodes is given in terms of the sheath thickness which is a function of the ion current density j , and the operating voltages . the cathode 12 is formed as a double - walled cylinder so that cooling water can be circulated from an inlet 24 , through a hollow jacket 26 , and through an outlet 28 . permanent magnets 30 are mounted outside the pole pieces 14 . the tips of the pole pieces 14 are tapered toward the region of the plasma to direct the lines of magnetic field . an outer jacket 32 of magnetic material forms a magnetic shield and serves as a yoke for the magnetic field . the arrangement for the extraction of the beam is shown in fig2 . the discharge chamber is grounded . an extractor electrode 40 is formed of graphite and operated at - 6 kv . electrodes 40 , 42 and 44 form an einzel lens . third electrode 44 is connected to extractor electrode 40 , and a voltage of - 1 kv is applied to the einzel electrode 42 . a faraday cup 46 operated at - 6 kv is used to measure currents . a suppressor electrode 48 is placed in front of the faraday cup to suppress electrons from the faraday cup and operated at a few volts below the faraday cup 46 . ceramic rings 50 and bolts 52 are used to space and hold the electrodes . pumpout holes 54 are needed at intervals to remove gases . an electrical schematic of the extraction arrangement is shown in fig3 . adjustment of both the voltage on the einzel 42 and the arc current in the magnetron ion source is necessary to obtain optimum focussing . then the extractor current is less than the beam current and there is practically no current on the third electrode . under these conditions beam current is proportionate to extraction voltage to the 3 / 2 power and arc current is proportionate to beam current . the entire arrangement is enclosed in a vacuum chamber ( not shown ). to accommodate the extraction electrode system , the gap between the pole pieces was made about 0 . 7 inch . the beam aperture was made 0 . 2 inches diameter which corresponds to an area of about 1 / 5 cm 2 . thus , a beam current of 1 ma at 6 kv represents a density at the aperture of 5 ma / cm 2 . if current is proportioned to voltage to the 3 / 2 power , than an extraction voltage of 15 kv will give an ion current density of 20 ma / cm 2 at an arc current of 2 . 4 a . for some applications such as ion implantation in semiconductors , a slit - shaped aperture is needed , about 3 mm wide × 3 cm long . to maintain high ion current density per ampere of arc current it is necessary to align the slit parallel to the edges of the pole pieces normal to the magnetic flux to retain a narrow magnetic gap . with a cylindrical source as previously described , the slit would have the curvature of the wall which tends to cause rapid beam divergence in the wide direction . as it may be difficult to focus divergence in the wide direction , it is convenient to use a cell of rectangular cross - section so that the slit may lie in a flat wall , as shown in fig5 . the currents to the beam forming electrodes in tests of the cylindrical embodiment are shown in fig4 as a function of arc current . the arc is matched at 0 . 8 amps with most of the extracted current going into the beam . various cathode liners 60 may be used to extract different ion beams . a discharge limiting liner 62 of graphite can be used to further confine the discharge . for example , a boron - carbide liner can be used to extract a boron ion beam , or an aluminum liner may be used to extract an aluminum ion beam . if ions of the feed gas are only of interest , the chamber may be lined with graphite which has a low sputtering yield . this invention is uniquely suitable for generating an ion beam from solid materials . however , its desirable properties are also achieved using suitable gases as beam material sources . when a gaseous source is used the magnetron ion source is preferably lined with graphite or titanium which has a low sputtering yield . this invention is not limited to the preferred embodiments and alternatives heretofore described , to which variations and improvements may be made including mechanically and electrically equivalent modifications , changes and adaptations to component parts , without departing from the scope of production of the present patent and true spirit of the invention , the characteristics of which are summarized in the appended claims . | 7 |
fig1 shows a motor vehicle 1 , which is equipped with a device 11 for the assisted parking of a motor vehicle 1 into a parking space . device 11 can also be used to implement the method according to the present invention . device 11 includes an electronic control unit 12 , a travel transducer 13 , for example , in the form of a wheel pulse counter ( riz ), a steering angle sensor 14 , which , if indicated , may also have a yaw rate sensor assigned to it , as well as a so - called human machine interface 15 in the form of a display . display 15 may be the display of a navigation system , of an instrument cluster or of a central display . furthermore , device 11 is provided with sensors 16 in the form of ultrasonic sensors , which are situated on both sides of the vehicle in the region of a rear axle of motor vehicle 1 , as well as with distance sensors 17 situated at the front and rear sides of the vehicle . travel transducer 13 , steering angle sensor 14 , display 15 , ultrasonic sensors 16 and distance sensors 17 are each connected to electronic control unit 12 . a parking operation that can be performed using device 11 is shown in fig2 through 8 , the respective parking situation being represented for the driver of motor vehicle 1 on display 15 in a so - called bird &# 39 ; s eye view . represented for this purpose are , on the one hand , a parking space 20 selected for a parking operation and measured using ultrasonic sensors 16 , and motor vehicle 1 in its current position x as well as in its position x ′ situated in parking space 20 . in addition , a setpoint parking path 21 and an actual parking path 22 are represented on display 15 . further , the maneuver required to adhere to setpoint parking path 21 is displayed in written form and with the aid of arrows . in the first parking phase shown in fig2 , the driver is asked to back up in a straight line by a suitable prompt in a text field 23 such as e . g . “ back up straight ”. thereupon the driver backs up motor vehicle 1 parallel to the alignment of parking space 20 until he arrives at a first steering reversal point and a signal is output or a gong sounds , as shown in fig3 . for this purpose , e . g . the instruction “ back up straight until signal tone sounds ” is displayed in text field 23 . when the signal tone sounds , the driver stops the motor vehicle , whereupon display 15 , as shown in fig4 , displays the request “ turn steering wheel to the right until signal tone sounds ” in text field 23 . thus a first steering action occurs at a standstill . subsequently , the driver of the motor vehicle must now back up further at the set steering angle until a new signal tone or gong sounds . the driver is requested to do so by the instruction “ back up until signal tone sounds ” in text field 23 of the display shown in fig5 . once motor vehicle 1 has stopped , a second steering action is performed at a standstill , again a signal tone or gong sounding once the correct steering wheel position has been reached . the request to do so occurs with the instruction “ turn steering wheel to the left until signal tone sounds ” in text field 23 of display 15 as shown in fig6 . once the corresponding movement of the vehicle has occurred , which can be seen on display 15 shown in fig7 , the parking operation concludes with the request in text field 23 “ back up until signal tone sounds ”. this backing up process until the renewed sounding of a signal tone occurs at the steering angle selected in the preceding step . with the sounding of the latter signal tone or gong , motor vehicle 1 is correctly situated in the parking space . this is indicated to the driver as shown in fig8 and is communicated by a message “ parking operation concluded ” in text field 23 . if necessary or if desired , the driver may then additionally straighten out the wheels . if the parking space is very tight and the motor vehicle is very close to a vehicle adjacent to the rear of the vehicle , then the driver may be asked via device 11 to straighten out the wheels and drive forward a bit so that motor vehicle 1 comes to rest at the center of parking space 20 . the estimated parking path is represented alongside setpoint parking path 21 as a function of the current steering angle . the driver &# 39 ; s task is to bring the estimated parking path and the setpoint parking path into superposition by steering . the alignment of motor vehicle 1 regarding an optimum initial yaw angle with respect to the longitudinal extension of a parking space is now explained with reference to fig9 through 13 . for this purpose , as shown in fig9 by a block diagram , the dimensions of the respective parking space are ascertained using ultrasonic sensors 16 , the measurement data 30 being analyzed in real - time in control unit 12 together with vehicle data 30 , which may be supplied by a wheel pulse counter , by a steering angle sensor and the like . using a so - called human machine interface 31 , for example a display , the current yaw angle 32 is then communicated to the driver . this is then able to correct the steering angle in a step 33 such that vehicle data 30 are modified accordingly and motor vehicle 1 is able to assume the desired initial yaw angle . in addition to the use of ultrasonic sensors 16 , a yaw angle sensor of an electronic stability program ( esp ) may be also be calibrated and used as additional vehicle information . fig1 shows the aids for driver 32 represented on display 15 . in fig1 a , motor vehicle 1 deviates from a parallel position . this may be corrected by turning the steering wheel to the left . an arrow 41 pointing to the left flashes on in color to indicate the required maneuver . in fig1 b , motor vehicle 1 is in a position parallel to the extension of the parking space such that neither arrow 41 nor an arrow 42 used for requesting a right turn of the steering wheel flashes on . in fig1 c , motor vehicle 1 must be steered to the right in order to set a yaw angle of 0 °. in order to prompt driver 32 to do this , arrow 42 pointing to the right flashes . fig1 shows a situation in which a parking space 20 adjoining a curb 44 is measured . for this purpose , vehicle 1 drives past parking space 20 along a path 45 , on which it is kept by the functionality represented in fig9 and 10 , such that parking space 20 is measured with the aid of ultrasonic sensors 16 in the region of the rear axle of motor vehicle 1 and , if applicable , with the aid of ultrasonic sensors 46 in the region of the front axle of motor vehicle 1 . first a motor vehicle 47 adjoining parking space 20 and then curb 44 are used to determine the yaw angle of the motor vehicle . fig1 depicts a situation , in which a parking space 20 is located between two motor vehicles 47 and 48 , there being no curb in this case . using its ultrasonic sensors 16 and 46 , motor vehicle 1 finds its orientation in parked vehicles 47 and 48 . if vehicles 47 and 48 are situated obliquely in their respective parking spaces , then a reference line 49 is produced using the points of vehicles 47 and 48 that jut out furthest into the street . fig1 shows a special case of parking into a parking space 20 that is situated in a curve . here motor vehicle 1 is aligned parallel to motor vehicles 47 and 48 parked adjacent to parking space 20 or parallel to a curb 44 , parallel in this case meaning that a constant distance is maintained with respect to obstacle - constituting motor vehicles 47 and 48 or to curb 44 . | 1 |
referring to fig1 to 3 of the drawings , the automatic controller 1 comprises infrared sensor 21 , mcu 22 , flushing power selection 23 , liquid / solid waste flushing mode selection 24 , amplifier 25 , and a one - in - two - out two - series electromagnetic - controlled valve 26 according to the preferred embodiment of the present invention . the mcu 22 is installed with one flushing procedure for liquid waste and three flushing procedures for solid waste in different flushing power , which could be access through the flushing power selection 23 . the flushing mode selection 24 is designed for switching between automatic and manual flushing control . the manual flushing control guarantees the automatic control flushing process to function applicably even if the automatic flushing system collapses . the mcu 22 of the present invention is exchangeable with the programmable logic device to program the desired procedures according to different usages and each user &# 39 ; s requirements . the following list illustrates the detail settings of the flushing power selection of the present invention : for example , when an object is entered into a detection area , the mcu 22 generates a pulse signal per second . when an object stays in the detection area for 5 minutes , the mcu generates 5 pulse signals and so starts to operate . a v 1a of the electromagnetic - controlled valve 26 will first closed and a one second rinsing process starts for rinsing the toilet bowl . at the same time , the mcu starts to calculate and will sending command for liquid waste flushing process if less than 60 pulse signals are generated and detected . then the v 1b of the electromagnetic - controlled valve 26 releases for three second for flushing , and the v 1a sprays water for two second to rinse the toilet bowl . when more than 60 pulse signals are generated and detected by the mcu , the mcu will initiate a solid flushing waste process comprising the steps of flushing the toilet bowl , draining the toilet bowl , and refilling flushing water or blocking any odor smell . referring to fig2 and fig3 of the drawings , the mcu 22 transmits a series of pulse signals 210 , with frequency 1 hz and 10 % duty cycle , to the infrared sensor 21 . after the series of pulse signals 210 is amplified by the signal - amplifying circuit , it is emitted by the infrared emitter 211 . the infrared receiver 212 of the infrared sensor 21 would detect any feedback infrared signals if any object is within the adjustable detection range of the infrared sensor 21 . once the feedback signals are being amplified by the signal - amplifying circuit after received , the mcu 22 would check and discriminate according to the pre - installed decision rules . the amplifier 25 could be the triode amplifying circuit to set between the mcu 22 and the electromagnetic - controlled valve 26 , or simply using pulse - triggered electromagnetic - controlled valve which could be switch on by applying a positive voltage equal to or longer than 50 microsecond and switch off by applying a negative voltage equal to or longer than 50 microsecond . the pulse - amplifying circuit and the pulse - switching bridge circuit are showing in the fig4 and the pulse high and low widths are set by the mcu 22 . referring to fig1 of the drawings , the flushing system of a plumbing fixture in the present invention comprises automatic controller 1 , electromagnetic - controlled a valve 2 , electromagnetic - controlled b valve 3 , unidirectional valves 4 and 5 , upper jet 6 , and lower jet 7 . the realization of the two - aqueduct flushing system of a plumbing fixture is achieved by using both electromagnetic - controlled a valve 2 and b electromagnetic - controlled b valve 3 to control the flow in each aqueduct . the design of combining a water intake with two water outlets into a single water valve greatly reduce the size of the flushing control apparatus , and with supplementary unidirectional valves 4 and 5 on the aqueducts , this design is even feasible on the flush toilet . the unidirectional valves 4 and 5 are installed on the aqueducts between the electromagnetic - controlled valves 2 and upper jet 6 , and electromagnetic - controlled valves 3 and lower jet 7 , respectively . this installation provides the safety control which prevents the flushing water from being contaminated by the toilet water in the toilet bowl due to the failure of shutting electromagnetic - controlled valves 2 and 3 timely or the vacuum between electromagnetic - controlled valves 2 and 3 and the jets 6 and 7 , respectively , resulting in the siphon phenomenon . when the flushing system is not in process of flushing , the loophole of the unidirectional valve is not occluded and connects to the atmosphere . once the electromagnetic - controlled valve switches on and starts flushing water into the aqueduct , the hydraulic pressure lifts the seal in the unidirectional to obstruct the loophole against the atmospheric pressure so that the flushing water is toward the jet without overflowing into the loophole causing leakage problem . after the electromagnetic - controlled valve switches off and stops flushing water into the aqueduct , the seal in the unidirectional valve descends by gravity and atmospheric pressure , which the airway of the loophole is not occluded , again . even the siphon phenomenon occurs for some reason , it would only draw in the atmosphere from the loophole of the unidirectional valve , which provides an airway block to ensure that the contaminated water is not accessible to the electromagnetic - controlled valve . while the pressure of the residue of the flushing water does not suffice for pushing outward through the jet , it remains in the bent part of the aqueduct , which , provides as a block between the toilet water and the electromagnetic - controlled valve , another protection design . referring to fig6 to 8 of the structural drawings , two electro - magnetic - controlled valves are designed to join on the same platform to form a set of one - in - two - out two - series electromagnetic - controlled valves according to the preferred embodiment of the present invention . the width of the above electromagnetic - controlled valve is 50 millimeters so that the discharge quantity of the flushing water is sufficient enough to qualify the design requirement . the main body of the valve with a 12 or 24 volts low voltage dc current , built up by one - step injection molding , greatly improves the convenience of installation , as compared with the most common valve : equilibrium electromagnetic water valve without on / off function . according to the fig6 of the preferred embodiment of the present invention , pulse - triggered electromagnetic - controlled valves a and b consist of the permanent magnet 61 , the spring 62 , the coil 63 , the armature 64 , the seal 65 , the washer 66 , decompression void 67 , o - ring 68 , valve core 69 , and valve 60 . when the valve core 69 and the valve 60 are separated to switch on the valve itself , the positive voltage is applied to the coil 63 to polarize the armature 64 to have the attracting force with the permanent magnet 61 in opposite polarity against the pulling force of the string 62 . when the valve core 69 and the valve 60 are shut to switch off the valve itself , the negative voltage is applied to the coil 63 to polarize the armature 64 in the same polarity with the permanent magnet 61 and , consequently , repel away from each other . the switch - on interval for polarization requires only 0 . 05 sec to complete , which means a single 6 - volt alkaline battery could last approximately two and a half year without the need for replacement . the fig7 shows an optional structure for a set of one - in - two - out two - series electromagnetic - controlled valves without decompression void . if the volume saving is the first priority , an more compact structure is available in integrating the unidirectional valve with the set of one - in - two - out two - series electromagnetic - controlled valves according in fig8 . the mcu 22 does not send any command signals until receiving 5 infrared pulse signals from the infrared sensor 21 . after the infrared sensor 21 detects an object is within the detection range for 5 seconds , in this case , the electromagnetic - controlled a valve 2 switches on for 1 second to flush the inner surface of the plumbing fixture . if the object stays within the detection range for longer than 60 seconds , the flushing system discriminates the solid waste flushing procedure should be executed . if shorter than or equal to 60 seconds , the liquid waste flushing procedure is executed . the solid waste flushing procedure with medium flushing power is as follows : 1 ). the electromagnetic - controlled a valve 2 switches on for 3 seconds to let the upper jet 6 flush . 2 ). the electromagnetic - controlled b valve 3 switches on for 4 seconds to let the lower jet 7 flush . 3 ). the electromagnetic - controlled a valve 2 switches on for 2 seconds to let the upper jet 6 refill both the water in the toilet bowl and the water in the bent part of the aqueduct . the liquid waste flushing procedure is as follows : 1 ). the electromagnetic - controlled b valve 3 switches on for 3 seconds to let the lower jet 7 flush . 2 ). the electromagnetic - controlled a valve 2 switches on for 2 seconds to let the upper jet 6 flush . the present invention provides a two ways electromagnetic valve with an upper outlet and an lower inlet system . the flushing effect is effective and has an advantage of saving water . the construction of the present invention is simplified whereas the number of pipe elements is reduced and the installation is more convenience . the electromagnetic valves may be as small as 50 mm in size which is easy to arrange in different position . the two inlets are incorporated under one electromagnetic valve which can be manufactured in one mounding and hence is more convenience for manufacture . the mcu may store four different flushing processes suitable for operation under different pressure conditions for different area such that different individual &# 39 ; s needs are met . the mcu can also analyze the action of an object to determine whether a liquid waste flushing process or a solid waste flushing process is suitable for each situation , thus achieving the purpose of saving water . the volume of flushing water used may be controlled between 2 . 8 and 3 . 2 liter . since the system is operated under pulse signal system , the work is not high and is suitable for long time period . the present invention is safe and reliable , and easy to install . a unidirectional value is also used for defining an enclosed environment such that any gas or water is stopped and a hygiene environment can be maintained . one skilled in the art will understand that the embodiment of the present invention as shown in the drawings and described above is exemplary only and not intended to be limiting . it will thus be seen that the objects of the present invention have been fully and effectively accomplished . it embodiments have been shown and described for the purposes of illustrating the functional and structural principles of the present invention and is subject to change without departure form such principles . therefore , this invention includes all modifications encompassed within the spirit and scope of the following claims . | 8 |
hereinafter , one embodiment of the present invention will be described with reference to the accompanying drawings . in addition , in the following description , unless particularly limited , “ forward ” and the “ backward ” mean forth and back in the traveling direction of a vehicle body , and the “ up ” and the “ down ” mean up and down in the vertical direction . fig1 is a perspective view of a vehicle body 1 adopting the present invention . fig2 is an enlarged perspective view of the section a of fig1 . in these drawings , reference numeral 2 denotes a roof panel provided in a roof part of the vehicle body 1 , reference numeral 3 denotes a roof side panel combined with a side part of the roof panel 2 in the width direction of the vehicle , reference numeral 4 denotes a front window glass arranged in front of the roof panel 2 , and reference numeral 5 denotes a front pillar panel provided continuously with the front side of the roof side panel 3 to support a side part of the front window glass 4 . fig3 is a sectional view along the line b - b of fig2 . fig4 is a sectional view along the line c - c of fig2 . as shown in these drawings , a junction between the roof panel 2 and the roof side panel 3 is bent in a stepped shape and projects into a vehicle room . the junction between the roof panel 2 and the roof side panel 3 is formed with a junction groove 6 having a substantially u - shaped cross - section along the longitudinal direction of the vehicle body . fig5 is a sectional view along the line d - d of fig2 . as shown in fig5 , an inner edge of the front pillar panel 5 that is formed continuously with a front part of the roof side panel 3 extends in the width direction of the vehicle , and is bent in the shape of the letter “ l ” to form a glass support 7 . the glass support 7 is a part that is depressed in a stepped shape from the part of the front pillar panel 5 exposed to the outside of the vehicle , and a side edge of the front window glass 4 is fixedly supported by this part . a long roof garnish 8 made of resin is attached to the junction groove 6 of the roof of the vehicle body . a window garnish 9 made of resin along a side part of the front window glass 4 is attached to the glass support 7 of the front pillar panel 5 . the whole roof garnish 8 is formed so as to have a nearly definite width . the window garnish 9 , as shown in fig2 , has a rear end region 10 a formed so as to have the same width as the roof garnish 8 and connected with the roof garnish 8 , and a general region 10 b located in front of the rear end region 10 a and formed so as to be narrower than the width of the roof garnish 8 . the rear end region 10 a of the window garnish 9 is fixedly positioned in a vehicle body member along with the front end of the roof garnish 8 at a front end of the junction groove 6 of the roof of the vehicle body . fig6 is a sectional view along the line e - e of fig2 . fig7 is an exploded perspective view of the junction between the roof garnish 8 and the window garnish 9 . as shown in these drawings , a base member 11 including a welding fixed part 11 a welded to the vehicle body and a bolt support 11 b supported by the welding fixed part 11 a is fixedly welded to the front end of the junction groove 6 . a stepped bolt 12 is fixed to the center of the bolt support 11 b . the stepped bolt 12 includes a cylindrical locking shaft 13 that projects upward from the base member 11 ( bolt support 11 b ), and an male thread 15 that projects upward from an upper end of the locking shaft 13 via a stepped part 14 . an end of the roof garnish 8 and an end of the window garnish 9 are locked by the locking shaft 13 . the projection height of the locking shaft 13 from the base member 11 is the same as the thickness of when the end of the roof garnish 8 and the end of the window garnish 9 overlap each other . a locking hole 16 for regulating the positional deviation of a front edge of the roof garnish 8 is formed in a position separated from the fixed position of the stepped bolt 12 of the base member 11 towards the rear of the vehicle body . in the present embodiment , the base member 11 and the stepped bolt 12 constitute a positioning locking part . the roof garnish 8 , as shown in fig3 and 6 , has a garnish body part 17 exposed upward of the junction groove 6 , and a plate - like core 18 that is a reinforcing member provided on the backside of the garnish body part 17 . a connecting piece 19 having a substantially u - shaped cross - section and extending forward is formed on a lower surface of a front end of the garnish body part 17 . a tip of the connecting piece 19 is formed with a u - shaped groove 20 that can be engaged with the locking shaft 13 of the stepped bolt 12 from a direction perpendicular to the shaft ( from the rear side of the vehicle body ). a locating projection 21 ( stopper part ) located on an extension line of the center of width of the u - shaped groove 20 is formed on the lower surface of the connecting piece 19 . the locating projection 21 can be fitted into the locking hole 16 of the base member 11 . the core 18 that reinforces the garnish body part 17 extends forward along the lower surface of the connecting piece 19 , and the tip of the core has a shape extending along the edge of the u - shaped groove 20 of the connecting piece 19 . in other words , the tip of the core 18 is formed with a u - shaped groove having the same shape as the u - shaped groove 20 of the connecting piece 19 . accordingly , the tip of the core 18 reinforces the edge of the u - shaped groove 20 . the core 18 is formed with a through hole 28 through which the locating projection 21 passes . the locating projection 21 projects below the core 18 through the through hole 28 . as shown in fig6 and 7 , a concave part 23 is provided in the broad rear end region 10 a of the window garnish 9 so as to form an oblong opening 23 a of rectangular shape in the surface of the garnish body part 22 exposed upward of the junction groove 6 . an attachment hole 24 that can be fitted to the locking shaft 13 of the stepped bolt 12 is formed almost in the central part of a bottom wall in the concave part 23 , and a boss 25 that projects upward is provided at a peripheral edge of the attachment hole 24 . after the u - shaped groove 20 of the roof garnish 8 and the attachment hole 24 of the window garnish 9 are locked by the locking shaft 13 , a nut ( female thread member ) 30 is screwed into the male thread 15 of the stepped bolt 12 that has passed through the attachment hole 24 , as shown in fig4 and 6 . the end of the roof garnish 8 and the end of the window garnish 9 are fixedly positioned in the vehicle body by fastening of the nut 30 in a state where they are caused to overlap each other . after the nut 30 is fastened , a cover member 29 is attached to the opening 23 a of the concave part 23 . in the garnish attachment structure of the present embodiment , even when either the roof garnish 8 or the window garnish 9 is attached in advance , both the garnishes 8 and 9 can be easily and accurately attached to the vehicle body . for example , when the roof garnish 8 is attached in advance , first , the u - shaped groove 20 of the connecting piece 19 of the front end of the roof garnish 8 is fitted to the locking shaft 13 of the stepped bolt 12 on the base member 11 from the rear side of the vehicle body . in this state , the locating projection 21 on the rear surface of the connecting piece 19 is fitted into the locking hole 16 in the base member 11 . next , with the front end of the roof garnish 8 being positioned , other parts of the roof garnish 8 are fixed within the junction groove 6 with a clip or a bolt . thereafter , the attachment hole 24 of the rear end region 10 a of the window garnish 9 is fitted to the locking shaft 13 of the stepped bolt 12 from above . when the attachment hole 24 is fitted to the locking shaft 13 of the stepped bolt 12 , the rear end region 10 a of the window garnish 9 is positioned in the vehicle body , and is overlapped on the tip of the connecting piece 19 of the roof garnish 8 . next , with the rear end region 10 a of the window garnish 9 being positioned , other parts of the window garnish 9 are fixed to the front pillar panel 5 by clipping , etc . moreover , the part that is obtained by overlapping the window garnish 9 and the roof garnish 8 is fixed to the vehicle body by screwing the nut 30 into the male thread 15 of the stepped bolt 12 . conversely , when the window garnish 9 is assembled in advance , the attachment hole 24 of the rear end region 10 a of the window garnish 9 is fitted to the locking shaft 13 of the stepped bolt 12 from above . next , with the rear end region 10 a being positioned and locked , other parts of the window garnish 9 are fixed to the front pillar panel 5 by clipping , etc . thereafter , the u - shaped groove 20 of the connecting piece 19 of the roof garnish 8 is hidden in the lower surface of the rear end region 10 a of the window garnish 9 and is fitted to the locking shaft 13 of the stepped bolt 12 from the rear side of the vehicle body , and the locating projection 21 on the rear surface of the connecting piece 19 is fitted into the locking hole 16 of the base member 11 . next , other parts of the roof garnish 8 are fixed within the junction groove 6 with a clip or a bolt . the nut 30 is screwed into the male thread 15 of the stepped bolt 12 , and the overlapping part of both the garnishes 8 and 9 is fixed to the vehicle body . as described above , in the case of this garnish attachment structure , even if the order in which the roof garnish 8 and the window garnish 9 are attached is changed , they can be attached to a vehicle body without any problem . therefore , the order in which both the garnishes 8 and 9 are attached can be changed flexibly according to a manufacturing line . for this reason , it is possible to rapidly cope even with a change in the place of manufacture , etc . further , in the present embodiment , the overlapping part of the roof garnish 8 and the window garnish 9 is fixed to the stepped bolt 12 by fastening of the nut 30 . however , since the height of the locking shaft 13 of the stepped bolt 12 that is locked in a state in which the ends of both garnishes 8 and 9 overlap each other is set the same as the thickness of when both garnishes 8 and 9 overlap each other , assembling work can be safely and efficiently performed without any fear that the overlapping part of both garnishes 8 and 9 is fastened by excessive force . moreover , in the present embodiment , the locating projection 21 is provided so as to protrude from the lower surface of the connecting piece 19 of the roof garnish 8 , and the locking hole 16 into which the locating projection 21 is fitted is formed in the base member 11 . therefore , when the roof garnish 8 is moved to the front , thereby causing the u - shaped groove 20 to engage the locking shaft 13 , the position of the roof garnish 8 in the forward - and - backward direction can be positioned easily and accurately . particularly if the locating projection 21 is made relatively easily deformable structure , the locating projection 21 can be surely fitted into the locking hole 16 even when the connecting piece 19 of the roof garnish 8 is hidden in the lower surface of the rear end region 10 a of the window garnish 9 . further , in the present embodiment , the edge of the u - shaped groove 20 of the connecting piece 19 of the roof garnish 8 is reinforced by the core 18 . therefore , deformation of the u - shaped groove 20 at the time of positioning can be reliably prevented , and the positioning accuracy of the roof garnish 8 and the assembling workability can be improved . in addition , the invention is not limited to the above embodiment , and various design changes can be made without departing from the scope thereof . for example , although the above embodiment has been described in that the front end of the roof garnish 8 is engaged with the locking shaft 13 from the forward - and - backward direction and the rear end of the window garnish 9 is engaged with the locking shaft 13 from the up - and - down direction . however , contrary to this , the front end of the roof garnish may be engaged with the locking shaft from the up - and - down direction , and the rear end of the window garnish may be engaged with the locking shaft from the forward - and - backward direction . | 1 |
many of the network architectures existing on vehicles today are not simply ethernet based due to various considerations . for example , military standards such as mil - std - 1553 and commercial standards like arinc 429 , take into account factors such as failure immunity , robustness and functional criticality . alternatively , there currently exist network architectures much faster than the predominant 10 / 100 baset ethernet , like firewire and usb , which are suitable for data transfers up to 400 - 800 mbps . equipping a vehicle to handle wireless transfers must take into account the diverse range of pre - existing and alternative communications media used to move data amongst vehicle network devices . the vehicle microserver bridge router ( vmbr ) 100 , outlined in fig1 allows data transfers across the wireless media , and also the routing 101 , bridging 102 and on - vehicle storage 103 104 of any of the static data hosted on inter - vehicle and other operatively connected network devices , data such as operational software updates , maps and other pertinent operational databases , device fault data , performance data and operational reports , etc . that may be stored in existing on - vehicle computers and network equipment . for functionality such as voqa or moqa , which may not be associated with an existing vehicle computer , the apparatus can effectively handle the routing and storage onto on - board storage media . the data content either originates from networked ground station computers or vehicle computers . the invention performs these functions by requesting and retrieving the stored data and emulating a legacy method which would be functionally equivalent to the method described in a previous embodiment of the invention for the arinc 615 interface 105 113 on commercial aircraft , of which this invention is a continuation . most vehicle computers in existence today have a limited storage medium such as nvm or eeprom with various ways to retrieve or overwrite the data , e . g ., rs232 serial dump via test connector . an application programmable interface ( api ) for the many types of vehicle communication bus architectures ( as depicted in fig1 ) conditions the data packets and operates as a query and data transfer engine for each vehicle communication bus interface , working in conjunction with the specific host bus adapter ( s ) for that device interface ( s ). in the case of a mil - std - 1553 bus 106 architecture , for example , the vmbr 100 would emulate a bus controller to poll , request and transfer data to and from devices connected to the 1553 bus 106 . likewise for either a firewire network 108 or a rs - 232 device ( s ) 109 such as a global positioning system ( gps ) that requires database updates and also provides periodic outputs that the vmbr can utilize in performing its routing , packetization and communication function . the methods described are generally non - time deterministic , describing a process to remotely or automatically request or transfer data via a wireless communication link ; however , the type of data described falls into the specific category of vehicle operation and performance — typical data structures targeted for movement to and from the vehicle include operational and database program updates to the on - board vehicle computers , stored performance and fault log downloads to ground - based operations centers , etc . one notable data type considered as operational data for download is recorded video and audio data stored on - board as a result of security monitoring or an emergency event , which can be used subsequently at a later time for training purposes and legal substantiation . the vmbr 100 has the additional capability of encoding and decoding , compressing and de - compressing data intended for wireless transmission and reception . this is considered an extension of the routing and data conditioning function that delivers packetized data to the appropriate vmbr interface 110 or interfaces shown in fig1 . the vehicle microserver bridge router ( vmbr ) apparatus , an extension of the apparatus described in application ser . no . 10 / 042 , 374 , provides a complete on - vehicle direct interface capability to a ground - based spread spectrum communications link , along with interfacing capability to existing on - vehicle rf and satellite communications such as hf , vhf , gps , narrowband and broadband satellite links . the typical formats include mil - 1553 , arinc 429 , ethernet , rs - 232 . optical fiber , firewire or a host of other communication bus structures . the apparatus is structured to bridge data to and from its internal host bus architecture 112 to the appropriate vehicle device ( s ) 110 communication bus format , route and / or store data packets to and from a noc 300 via a wireless data link 114 and the transportation vehicle 200 500 . appropriate application layer information to accompany the wireless link data packets that assist in maximizing bandwidth , both on the ground station platform and vehicle platform , will be discussed in the following paragraphs . the apparatus &# 39 ; primary function is to properly handle data updates or downloads required for a particular on - vehicle device or computer connected either directly , through a hub / switch or series of hubs / switches , or if an on - vehicle wireless lan is installed , any devices operatively connected to such a lan . a download is defined as a vehicle to noc wireless transfer of data packets from an on - vehicle network device to a noc , with the intermediate step of bridging , routing and / or storing the packets of information on - board the vehicle for later retrieval , depending on predetermined priority criteria , such as an emergency situation declared , company policy and procedures , automatic report generation , etc ., which requires a level of on - vehicle backup and redundancy . an embodiment of the invention that utilizes transmission / reception techniques such as multiple input multiple output orthogonal frequency division multiplexing ( ofdm ) being currently developed for fixed non une of sight general users at distances up to 40 - 50 kilometers could be applied to the vehicle data services link in a novel way . the following ‘ stores ’, ‘ data flows ’ and ‘ data manipulations ’ would be required : 1 ) gps database ( if available , for use by operatively connected vehicle clients ) 2 ) route plans and schedules ; for land vehicles , estimated or actual departure and arrival times , distance to and distance from intermediate waypoints ; for aircraft , navigation databases with entered flight plan , if available 3 ) rf coverage maps ( if available , for use by operatively connected vehicle clients ) 2 ) track , altitude , speed , geographical coordinates ( aircraft ), rate of climb / descent , if available ; direction , speed and coordinates ( land vehicles ) 3 ) vehicle users , if known through methods such as smart card presentation upon entry ; default user policy criteria status is assigned by the appropriate lower level user nocs for those who have not customized their preferences prior to going mobile . 3 ) multiple base station assignment to vehicle along route , if applicable and depending on priority level , for handoff coordination . 1 ) iterative correction for geographic position errors when multiple base station coordination is available ( triangulation method using received signal strength ( rss ) from vehicle ) against vehicle position output 2 ) adaptive channel management and multiple base station transmissions when multiple input multiple output polarization diversity antennas and associated signal modulation and processing techniques are applicable . 3 ) transmit power variation along with beaming forming for adaptive array antennas , if ability exists to follow predicted track and adjust beam direction and strength to achieve best bit error rate . as track exceeds range of coverage , appropriate handoff would occur based on noc information . the base station assesses user bandwidth allocation and priority . for example , coordinated two - tiered priority system ( user / emergency ) could be handled at the wireless link application layer . establishing excessive hierarchical dependency structures at the noc should not be required for the user / noc / data type relationship with this simplified structure . the number of nocs associated with the top three levels should always be very small compared to the potential number in levels iv and v . the dumping of bandwidth for general category users theoretically would only occur at the access points currently activated for communicating with the vehicle . a hierarchy for bandwidth allocation is suggested . on the ground station side , this consists of choice of signal path or paths between base station networks and user and the use of adaptive antenna beam focusing and signal strength adjustments 503 and / or multiple diversity antenna placements 504 . ii — regional alert — e . g ., amber alert , all points bulletin , regional transportation vehicle ( malfunction , medical , on - board incident ) an embodiment of the invention is presented where optimum bandwidth is desired on predictable , repeatable vehicle routes , at a time when man deployment is assumed to be in its infancy , i . e ., total area coverage continually scales up , but is never completely pervasive , with the assumption that there is no overlapping coverage between mans . the man is assumed to be a mix of small range , individual , enterprise ‘ hotspots ’, larger range mobility hotspots using any combination of diversity and adaptive antenna arrays and even wider area metropolitan area coverage hotspot or hotspots , which provide generic coverage when localized coverage has either been redirected or is not available to individual user . — the following is an example of how the two - tiered priority system would be handled : a regional bus carrier has just entered manhattan across the george washington bridge from new jersey when an unruly passenger becomes a source of concern to the safety of the driver and other passengers . the driver declares an emergency via a panic button that activates 2 firewire 800 ( 800 mb throughput ) cameras , along with a broadcast of the vehicle &# 39 ; s gps position . due to the fact that this is a public safety alert , in addition to the routing of the vehicle data to the bus carrier &# 39 ; s central noc , the nypd noc would take over operational control , thereby categorizing the user priority at the highest level and the emergency priority at the second highest level , due to the fact that a regional transportation vehicle is involved . this situation would constitute the highest level two - stage priority defined ( outside of an on - going or imminent terrorist attack ), meaning that all available bandwidth resources would be directed for use by users associated with the alert , including local hotspots within range of the vehicle and its priority users ( 802 . 11b / a ) 201 , man coverage ( 802 . 16e , 802 . 20 ) 202 203 and backhaul coverage ( 802 . 16a ) 204 . a base station setup embodied onto a vehicle such as a helicopter could create a portable and mobile base station function to perform as an access point with backhauling capability . as an example , in responding to a major municipal incident , the mobile base station could allow immediate communication access , including video feeds to public safety nocs or even a news station from individuals using mobile wireless cameras , e . g ., at a major fire , where the location may be obstructed by large buildings on all sides . it has previously been established that critical vehicle operations data such as foqa , moqa and voqa and its dissemination and control is addressed in the preferred embodiments of this invention . these data types are not time constrained , as they should be recorded and stored on - board vehicle computers for convenient delivery when within range of an access point , according to the particular responsible noc &# 39 ; s data distribution and usage procedures . occasionally , there are emergency or procedural situations where the data delivery becomes more urgent and low - latency , handoff management and range extension is required , e . g ., upon landing of an aircraft may require extensive data downloads with only a short turn around prior to the next departure . although vehicle storage should always be active for later retrieval , another added benefit during the unlikelihood of a potentially catastrophic event — that a video / audio stream , voip or vehicle performance data could be transmitted to ground stations by extending the wireless link to the vehicle platform using the methods described in previous paragraphs and exemplified in fig2 - 5 . eventually a flight or bus trip across country could intersect active wifi coverage areas that only require a coordinated handoff mechanism and extended antenna diversity and adaptive antenna array systems to minimize dropouts of data seen at the vehicle . until that occurs , the proposed system and method can provide session updates ( noc / vehicle / base station ) while a vehicle of interest follows a predicted track 205 501 502 within the vicinity of an access point , i . e . base station ( s ). | 7 |
one embodiment of an activity measuring and indicating circuit suitable for use in the inventive shoe is shown schematically in fig1 . the values of the components in the schematic of fig1 are listed in table i . ( in table i , k = 1000 , m = 1 , 000 , 000 , and μ = 1 × 10 - 6 .) although it is desirable to use the circuit of fig1 ( or its equivalent , such as in a custom asic application specific integrated circuit !) and the values of the components listed in table i , one skilled in the art would understand the function of the circuitry and be able to make various modifications of the circuitry and substitutions of components upon reading the description of the circuitry that follows . for example , criteria for selecting resistors and capacitors are discussed in more detail in another portion of this specification . other diodes types may be substituted for d1 - d4 , however , 1n4148 diodes were chosen because of their very low cost . the use of a hex inverter ic helps to keep the parts count low . other hex inverter ics ( integrated circuits ) could be substituted for the 74hc14 , but this particular component was chosen because of its extremely low standby power consumption , very low cost , and operation at voltages as low as 2 volts . other logic types could be used , although any substituted inverter should be one with hysteresis . it is also recognized that circuitry different from that illustrated in fig1 but that essentially duplicates all or most of the functions described herein may be substituted for the circuit of fig1 . table i______________________________________list of components for the circuit of fig1 component value______________________________________all resistors 1 / 8 watt , 5 % r1 , r2 2 . 2 mωr3a 39 kωr3b 39 kωr4 4 . 7 mωr5 330 kωr6 220 kωr7 3 . 3 mωr8 , r9 , r10 180 ωc1 0 . 01 μfc2 2 . 2 μfc3 0 . 47 μfd1 , d2 , d3 , d4 1n4148d5 , d6 , d7 red ledsu1 schmitt trigger inverter ( 74ho14 ) v . sub . cc lithium battery dl2430______________________________________ switch s1 is a switch having open and closed positions , and which is normally open . switch s1 is closed by application of foot pressure by the wearer of the shoe , and thus acts as an electrical transducer that responds to the activity of a person wearing the shoe . preferably , switch s1 is a pressure sensitive switch that is not responsive to activity , such as movement of the shoe , while the shoe is not being worn . preferably , the switch is located and configured to be responsive to footstrikes rather than mere motion of the shoe . if switch s1 is placed in the heel of a shoe , for example , it is preferable for the weight of the wearer to close the switch and keep it closed upon contact of the heel of the shoe with the ground . however , the switch should open when the weight of the wearer is removed from the switch , such as when the heel leaves the ground . initially , both terminals of capacitor c1 are at + v cc potential , because of the connection of both terminals to the v cc supply through resistors r1 and r2 , respectively . thus , the input signal to inverters u1a and u1c are high ( at or near v cc ), causing their outputs to be low ( at or near zero volts ). in this condition , the outputs of u1a and u1b ( which are sections of a hex inverter 74hc14 , which provides six inverters u1a - u1f per discrete package ) are low . therefore , diodes d1 , d2 , and d3 are non - conducting , and the voltage on the positive terminal of c2 is zero because of its connection to ground through the series - connected resistors r5 , r6 , and r7 . similarly , the voltage across c3 is zero , because of the connection of r4 across c3 . the output of u1b is therefore high , but the outputs of u1d , u1e , and u1f are also high . because led1 , led2 , and led3 are each connected between outputs in a high state , there is no voltage across them ( or at least , not enough voltage to cause significant conduction ), and therefore , they are not energized . when the wearer engages in an activity such as walking , running , or jumping , the pressure of the wearer &# 39 ; s foot against the inside of the shoe causes switch s1 to be repeatedly opened and closed . upon closure of switch s1 , the high - impedance inputs of u1a and u1c go to a low value momentarily , until either switch s1 opens or the charge on c1 is restored through resistor r2 , with time constant r2c1 . the time constant r2c1 is selected to be short enough so that it is less than the time between impacts of the shoe against the ground while a person wearing the shoe is running very rapidly . time constants less than about 50 ms are satisfactory for this purpose , and in this embodiment , r2c1 has been chosen to be 22 ms . the actual value selected is not particularly critical ( as long as it meets the criteria defined by shoe impacts ), although selection of a different time constant will influence the values of other components in the circuit , as will be explained below . when the input of u1a goes low momentarily , its output will go high momentarily , causing diode d2 to conduct and capacitor c2 to charge through resistor r3 ( which , in the circuit of fig1 comprises the parallel combination of two resistors r3a and r3b ) and diode d2 with a time constant determined by the product of the capacitance of c2 and r3 and the series combination of r5 , r6 , and r7 . because the series combination of r5 , r6 , and r7 is large compared to r3 , the time constant for charging c2 is essentially r3c2 , or about 86 ms in this circuit embodiment . because the period of time that the output of u1a is high is so short for each closure of s1 , several closures of s1 are required before c2 is charged to a high enough voltage to drive the output of u1d low . in the meantime , the charge on c2 is slowly bled off through the series combination of r5 , r6 , and r7 , so unless the repeated closures of s1 occur relatively frequently , there will not be enough charge accumulated on c2 to drive the output of u1d ( or u1e or u1f ) to a low state . it will be observed that , when s1 is opened , such as when pressure on s1 is relieved by the shoe leaving the ground , capacitor c1 will again reach v cc potential at both terminals , with a time constant equal to ( r1 + r2 ) c1 . input over voltage and under voltage protection is inherent in the 74hc14 ic , which has internal input protection diodes to clamp the input voltage to be within one diode drop of v cc or ground . let us assume now that c2 has acquired a sufficient voltage to drive the output of ( at least ) u1d low . for led1 to conduct and to energize , its anode must be at a higher voltage with respect to its cathode . thus , either diode d1 or diode d4 , which act logically together as an &# 34 ; or &# 34 ; gate , must also be conducting . diode d1 conducts briefly ( for a time period set by capacitors c1 and r2 ) at each closure of switch s1 , while capacitor c2 is charged . if capacitor c2 is sufficiently charged to cause the output of u1d to go low when switch s1 closes , led1 will flash briefly for an amount of time when switch s1 is closed to produce an activity signal because of the pulsed high level at the output of u1a . ( isolating diodes d1 and d4 ensure that a high logic level at either the output of u1a or u1b can allow led1 and the other leds to light .) thus , if the wearer is jumping up and down frequently enough , walking briskly , or running , enough charge can build up on capacitor c2 to allow ( at least ) led1 to flash . it will thus be apparent that inverter u1a , diode d2 , resistor r3 and capacitor c2 comprise , because of the finite length of the activity signal that is generated with each switch s1 closure , a processor that is responsive to the frequency of occurrences of the activity signal from electrical transducer s1 . the signal generated by this processor is a voltage produced on c2 that corresponds to a measure of activity of the person wearing the shoe . with each closure of switch s1 , capacitor c3 is charged through diode d3 ( which isolates c3 from output of u1c when the output is low ). capacitor c3 is sufficiently charged with each such closure ( in contrast to c2 , which , because it is in series with resistor r3 , requires a number of closures to become fully charged ) to cause the output of u1b to go to a low logic state . this low logic state persists until capacitor c3 is sufficiently discharged by leakage through resistor r4 , at which time the output of u1b returns to a high state . it takes less time for u1b to return to a high state than to discharge c2 because of the respective discharge time constants of c2 and c3 . therefore , when the output of u1b goes high , if there is a sufficient residual charge remaining on c2 , ( at least ) led1 will light and remain lit until c2 is sufficiently discharged to cause it to be extinguished . it is thus evident that c2 and r3 comprise an integrator responsive to the signal generated by the closings of switch s1 . resistors r5 , r6 , and r7 form a divider network . if the charge lost from c2 between the closings of switch s1 is less than the amount added as a result of the pulsed output of u1a upon each switch s1 closure , the voltage on c2 will gradually increase until it becomes high enough to cause the output of u1d to go low . if the closures are frequent enough , the charge will continue to increase until the voltage on c2 is sufficient to cause the output of u1e to go low . if the closures are still more frequent , the voltage on c2 will eventually increase until the output of u1f goes low . thus , voltage divider r5 , r6 and r7 set thresholds for activity levels , because led1 , led2 , and led3 will light up ( either in response to a pulsed switch closure or upon the output of u1b returning to a high state after a sufficiently long gap occurs between closures , such as when the activity of the wearer has ended ), depending upon there having been a sufficient number and frequency of switch s1 closures . thus , the led1 , led2 , and led3 comprise an indicator having separately energizable elements that activate at different threshold levels of activity in response to a coded indicator signal . the coded indicator signal in this circuit is coded by the voltage present on c2 and is decoded by the voltage divider comprising r5 , r6 , and r7 and the respective inputs to u1d , u1e , and u1f to provide a perceptible indication of the measure of activity of a person wearing the shoe having the activity meter circuit . in this embodiment , a visual indication is provided , although other types of indications , such as audible indications , could be provided as an alternative , or in addition to , the visual indication . the indication is given a period of time after the activity has ended , because the indicator is enabled only after capacitor c3 has sufficiently discharged , which occurs sometime after the activity ceases . it is desirable to make the flashes of led1 , led2 , and led3 that can occur with each switch closure relatively brief . it is also desirable to light the leds for a more extended period only after a brief but identifiable lapse of activity , and to limit the extended period to a few seconds . these criteria can be met by proper selection of the circuit time constants associated with capacitors c1 , c2 , and c3 . it is further desirable to use high input impedance gates throughout the circuit as well as the largest practical resistance values . however , resistors r8 , r9 , and r10 should conduct enough current when in circuit with their respective leds to allow the leds to light up to a desired brightness level consistent with a reasonable level of power consumption . for example , the component values listed in table i produce brief , but quite visible blinks lasting a small fraction of a second with each switch closure when c2 has been sufficiently charged . also , a delay is provided of about 2 to 3 seconds after a gap in activity before the leds light for the extended time period . with the listed components , there is also an approximately 6 second time period after the extended time period begins before all of the leds are extinguished , although this period can vary somewhat depending upon the final voltage reached by c2 . the specified components also set activity levels such that , if switch s1 is depressed about once every two seconds , in 6 to 8 seconds capacitor c2 is charged sufficiently to light led1 ; if s1 is depressed about once per second , led1 and led2 will be lit ; and if s1 is depressed once about every half second , led1 , led2 , and led3 will all be lit . ( these correspond to frequencies of 0 . 5 , 1 . 0 , and 1 . 9 depressions per second , respectively .) also , the various charging and discharging time constants are set by the specified components so that the extended - time led display ( i . e ., the display that occurs after a gap in activity ) represents a display of the highest activity level that occurred before the gap in switch s1 closures occurred . when an activity indicator is added to a shoe as an active decoration or novelty , the need for absolute accuracy of its operation may be offset by aesthetic considerations . therefore , high precision measurement of activity is not required , allowing inexpensive components with relatively broad tolerances to be used . aesthetic considerations concerning the lighting of led1 , led2 , and led3 and battery life may often be important factors in the selection of relative charging and discharging time constants for capacitors c1 , c2 , and c3 . considerations that go into the proper selection of component values , and particularly time constant values , may be summarized as follows : first , a time constant is selected for the combination of r2c1 . this time constant is not particularly critical , but must be somewhat less than the minimum time expected between switch closures of s1 . it is also desirable that the time constant be long enough to allow a visible flash of the leds during an activity period . as indicated above , satisfactory results are obtained with a time constant of about 22 ms . next , a value of c1 is selected that is consistent with physical size limitations , inasmuch as the circuit is intended to be embedded in a shoe . the value of r2 may then be determined based on the value of c1 selected and the time constant chosen . the value of r2 ( or equivalently , c1 ) may require some adjustment to account for the hysteresis of the inverter gates u1a and u1c , although the combined effects of the hysteresis and the exponential charging of capacitor c1 tend to produce pulses at the outputs of u1a and u1c that have a length close to the actual time constant r2c1 that is chosen . these combined effects , together with the general noncriticality of the activity measurement , tend to reduce the need for adjustment of component values . to reduce inventory costs , it is desirable for r1 to have the same resistance as r2 . however , r1 should be large enough so that , if a person is standing and thus applying sufficient pressure to close switch s1 , the flow of current through r1 and switch s1 does not result in a significant drain on the battery . if it does , r1 should be increased . in such a case , consideration may also be given to increasing r2 and decreasing c1 accordingly . capacitor c2 is charged through resistor r3 and diode d2 . the current through d2 when c2 is charging in the circuit of fig1 results in a 0 . 65 v drop across d2 , but is reduced to about 0 . 2 - 0 . 3 v because of the reduced current that flows through d2 as c2 reaches a maximum charge in this circuit ( about 2 . 7 - 2 . 8 v ). the voltage across c2 as the activity level circuit is activated determines the input voltage applied to u1d . resistors r5 , r6 , and r7 are selected based upon the voltage across c2 at the desired activity level thresholds , and the threshold input levels of the corresponding inverters . the time constant r3c2 is selected to be several times larger than r2c1 ( in this case , about 86 ms ), so that with increased rapidity of switch closures of s1 , increasing charge is gradually accumulated on c2 . if switch s1 is activated at a constant rate , the charge on capacitor c2 is periodically replenished through the series combination of diode d2 and capacitor r3 , but is also continuously drained through resistors r5 , r6 and r7 . eventually , the discharge rate between switch closures reaches an equilibrium with the charging rate supplied by the pulses that occur with each switch closures . thus , the charge on capacitor c2 reaches a steady - state condition with an equilibrium value of voltage ( that varies relatively slightly between switch closures ). resistors r5 , r6 , and r7 are selected so that their total value allows the input to u1d to rise to its threshold value ( i . e ., the voltage at which the output goes low ) at the desired minimum activity level , which in the circuit of fig1 is about 0 . 5 switch closures per second . the allocation of the total resistance between r5 , r6 , and r7 is made so that u1e and u1f reach their threshold values when c2 reaches its equilibrium at 1 . 0 , and 1 . 9 closures per second in the circuit of fig1 . thus , led1 , led2 , and led3 illuminate at footstrike rates of 0 . 5 , 1 . 0 , and 1 . 9 footstrikes per second . of course , different or additional activity levels may be selected as desired . time constant r4c3 is related to the time before a final indication of activity is given after the activity stops , and should be about one to three seconds . when the switch closures stop , capacitor c2 is discharged , and thus , if inverters u1d , u1e , and u1f had no hysteresis , the maximum activity level reached might not be properly indicated if the time constant r4c3 were too large . however , because of the hysteresis of inverters u1d , u1e , and u1f , the voltage at the input of these inverters has to drop below the threshold voltage that was reached at their input before the output goes high again . because of this fact , the time constant r4c3 can be on the order of seconds , and is , in fact , about 2 . 2 seconds in the circuit of fig1 . ( the hysteresis of inverter u1b also has to be taken into consideration in determining how long a delay occurs before the final activity display is activated .) the circuit is configured so that , after u1b and d4 go high , the anodes of led1 , led2 , and led3 remain high , until another closure of switch s1 . however , the series resistance of resistors r5 , r6 , and r7 is selected to discharge c2 so that a low enough voltage across c2 is reached to extinguish leds a few seconds after the final activity display , thus conserving battery power . many modifications of the circuit are possible within the scope of the invention . for example , the number and colors of the leds may be varied , or , with appropriate substitution of circuitry , other visible indicators may be used , such as el panels or liquid crystal displays . ( el panels may be especially desirable in some applications because of the wide variety of available colors and ease of producing decorative patterns . however , el displays require more complex driving circuitry .) various types of switches s1 may be used , although membrane switches are preferred for their durability , ease of manufacture , sensitivity , and unobtrusiveness to the wearer when disposed in ( for example ) the heel of a shoe . piezoelectric generators may be used instead of switches with appropriate modifications to the circuitry , and may advantageously serve as a source of power as well , possibly eliminating the need for a separate battery to power the circuitry . much of the circuitry may be placed in a single asic ( application specific integrated circuit ) with ease , possibly substituting standard gates for the isolation diodes as dictated by convenience . this asic could incorporate the 74hc14 hex schmitt trigger inverter as well as 5 resistors and 4 diodes , if the circuitry of fig1 were to be used . the diodes can be replaced with logic gates , if that results in further cost reductions . three of the outputs require 180 ohm , 1 / 16 w resistors to duplicate the circuit of fig1 ( the value and wattage rating may vary depending upon the led current required to light the leds to the desired brightness , the type of leds used , and the supply voltage ). the remaining resistors carry very little current and thus can have a very low power rating ( the smallest possible power rating consistent with current manufacturing techniques is sufficient ). the 74hc14 has a maximum threshold voltage of 2 . 2 v , while operating at 3 vdc . preferably , in an asic , the threshold should be reduced to 1 . 7 v , with a resultant hysteresis voltage of 0 . 5 v . with these specifications , the asic will have a very low operating current ( preferably less than 0 . 25 ma ) when the input to the inverters is between 0 - 3 vdc , and the supply voltage is 3 . 0 vdc . quiescent power is preferably similar to or less than that of the discrete implementation ( which itself has been measured in a number of test units as being less than 0 . 1 microamperes at 25 ° c . ), and should not exceed 2 microamperes at room temperature ( 25 ° c .) for extended battery life . ( the 74hc14 used in the discrete implementation described herein draws 3 . 0 microamperes maximum quiescent supply current at 5 . 5 volts at 85 ° c .) it is preferred that the asic operate reliably over a voltage range of 2 - 5 vdc , and that it have a low - cost surface - mount package to reduce manufacturing costs and the amount of space required for embedding the circuitry in a shoe . the reduced power consumption of the circuit of fig1 results in a large number of operating cycles being obtained from one 200 or 300 mah lithium cell . it has been demonstrated that , using a dl2430 , 300 mah lithium cell , the circuit will operate for over 88 , 000 cycles , each cycle being 5 seconds of fast running and an &# 34 ; off &# 34 ; period of 25 seconds . it has further been demonstrated that , using a dl2032 , 200 mah lithium cell , the circuit will operate for over 60 , 000 cycles , each cycle being 5 second of fast running and an &# 34 ; off &# 34 ; period of 25 seconds . a higher light intensity is possible with the same average current if the circuit is modified to provide high current pulse operation of the led . for leds , a wider viewing angle generally implies a lower luminous intensity . it is desirable to select leds that maximize both viewing angle and luminosity to maximize visibility of the activity display . high output &# 34 ; superbright &# 34 ; red leds such as model no . and120cr available from purdy electronics corp ., sunnyvale , calif . are desirable for this application . these leds are available with a forward voltage of 2 . 0 v at 10 ma current , with a specified operating temperature of - 10 ° c . to 60 ° c ., in at least four different varieties having luminous intensities and viewing angles at 20 ma as shown in table ii . of course , other types and colors of leds may be substituted , depending upon the effect desired . low cost leds that are available from many manufacturers may be used when manufacturing costs are a concern . red indicator leds are generally preferred for their visibility , but leds of other colors may be used to provide desired lighting effects . table ii______________________________________led luminous intensity and viewing angle at 20 maluminous intensity , mcd viewing angle , deg . ______________________________________100 19750 30680 50400 60______________________________________ switch s1 can be any small microswitch , tilt switch , inertia switch , or any other form of switch that provides contact closures the frequency of which can be made to vary in accordance with an activity of the wearer . most preferably , however , s1 is a subminiature , printed circuit board mountable , tactile pushbutton switch of the single pole , single throw ( spst ), normally open , momentary variety , having the specifications indicated in table iii . table iii______________________________________switch s1 specificationsspecification value______________________________________initial contact resistance 200 milliohm maximumcontact rating 20 - 50 ma @ 12 vdcoperating cycles 1 × 10 . sup . 6 - 2 × 10 . sup . 6 mech . and elect . operating temp . - 10 ° c . to 60 ° c . maximum dimensions 0 . 5 × 0 . 5 × 0 . 18 inches______________________________________ it should be understood that , while it is desirable that the above specifications for the leds and the switch be met , those skilled in the art would be able to make such substitutions for the specified components as may be deemed necessary or desirable for availability , manufacturing , aesthetic , or other reasons . fig2 shows a circuit board 10 on which is mounted an asic 102 containing many of the functional components of fig1 . the tactile switch s1 is preferably mounted at one end of circuit board s1 . lithium battery 104 is mounted in a battery holder 106 to supply the needed voltage v cc to asic 102 and in a manner that does not interfere with the operation of tactile switch s1 . capacitors c2 and c3 may also be mounted on circuit board 10 in a manner that does not interfere with operation of switch s1 . led1 , led2 , and led3 are connected to the circuit board by means of external wiring , which may be run either in the sole of a shoe , or in its sidewalls . the leds themselves are mounted on the shoe in any externally visible location , preferably one in which they are easily visible to the wearer of the shoe . fig3 shows one preferred way in which the circuit board of fig2 may be embedded in a typical athletic shoe so that it becomes a shoe 20 with a built - in activity meter in accordance with the invention . circuit board 10 is preferably mounted inside the heel portion 112 of the sole 110 of shoe 20 , and more preferably mounted inside the heel portion of the midsole . mounting may be accomplished by any suitable method , such as by molding . this location of the circuit board 10 is preferred when button 100 of switch s1 is located on the circuit board as shown in fig2 because with this configuration , the heel of a wearer &# 39 ; s foot will activate switch s1 when the wearer is stepping , walking , jumping , or running . any other mounting combination may be used for switch s1 in shoe 20 may be used that causes the circuit to be activated by these activities . preferably , in the configuration shown in fig3 button 100 is covered by a sock liner ( not shown in fig3 ) such as is normally inserted into an athletic shoe , to provide comfort for the wearer . because athletic shoes , and especially children &# 39 ; s athletic shoes are often replaced as they are outgrown or worn out , it is not required that circuit board 10 be accessible after installation , as the expected battery life is compatible with the anticipated useful life of the shoe . however , the circuit board 10 , or portions thereof , may be made accessible for battery replacement , such as by removal of the sock liner , and by providing access in the top of heel portion 112 through which the battery powering circuit board 10 may be reached . by way of example , the battery ( which may be physically attached to circuit board 10 , or optionally contained in a battery holder or compartment separate from , but electrically connected to circuit board 10 ) may reside in an upwardly opening recess or cavity positioned under the sock liner . wires 120 , 122 , 124 , 126 , 128 , and 130 from circuit board 10 may be routed ( and molded ) in sole portion 110 of shoe 20 and inside the upper 114 , 116 of shoe 20 to supply power to led1 , led2 , and led3 . these leds are shown in fig3 as being mounted in locations on the upper 114 and toe portion 116 of upper 114 so that they are visible to the wearer . any other suitable location may be used for the leds or other indicators ; for example , panels 118 are shown in which could be mounted three electroluminescent displays which could be used in lieu of or in addition to the leds . alternately , the leds could be mounted in a translucent diffusion panel or cover , such as a molded clear plastic to which a frosted surface has been applied . such diffusion panels or other suitable means may be used to increase the angles from which the leds are clearly visible . the output of the circuit board could be applied to indicator displays other than simple lighting devices such as leds . for example , the outputs could be applied to another circuit that converts and displays the outputs into an alphanumeric format . for example , the additional circuitry could provide a simple &# 34 ; 0 &# 34 ;, &# 34 ; 1 &# 34 ;, &# 34 ; 2 &# 34 ;, &# 34 ; 3 &# 34 ; display for activity levels on an lcd display , for example , where &# 34 ; 0 &# 34 ; might be assigned as an indicator of no activity , or activity insufficient to reach the first detected level . more complex conversions are also possible , particularly if the activity sensing circuitry is modified to allow it to indicate more than three levels of activity . as discussed above , those skilled in the art would be able to make many modifications of the specific embodiments of the invention discussed herein without departing from the spirit of the invention . for this reason , the scope of the invention should not be considered as being limited to the examples presented in detail herein , but should be determined by reference to the claims below and the full range of equivalents permitted under applicable law . | 0 |
u . s . pat . nos . 7 , 409 , 610 b1 ; 7 , 484 , 144 b2 ; and 7 , 630 , 259 b1 , the teachings of all of which are incorporated herein by reference in their entireties , describe alternative approaches for configuration - logic - based bist testing for fpga memories . in these approaches , the clock frequency applied during ram test is not matched to or even close to the ram functional frequency ( also known as “ at - speed configuration frequency ”) specification , thereby limiting the ability of these test approaches to provide enough stress to the ram under test for screening random delay defects . unlike other memory bist approaches , the current approach provides a “ shadow - bist ” capability to a configuration logic memory preload operation that , in some cases , could have zero delay penalty for testing . other memory test approaches tend to add test time for testing the memory blocks , and test time translates directly to test cost and product cost . a memory bist engine can be added to the bitstream engine in the configuration logic of an fpga to allow back - to - back configuration ( preload ) and read - back of ( i . e ., writing to and reading from ) embedded block rams at higher than at - speed configuration frequency in an attempt to match or exceed the rated frequency specification of the embedded ram ( assumed higher than that for the configuration logic ), since it is well understood that random delay defects can be stressed more at higher frequencies versus at lower frequencies . exceeding the rated frequency specification may be a requirement for testing the embedded memory under stress conditions designed to screen weak memory arrays . such testing may be targeted toward customers demanding extremely low defect levels or toward applications where the device with the embedded memory will be operated in a harsh environment such as outer space . if the rated frequency of the ram block is lower than the rated frequency of the configuration logic , then this approach of successive writes and reads would need to be done at a lower frequency , resulting in some additional modifications in the configuration logic clock distribution ( e . g ., more clock division ). in this case , however , the divided - down frequency of the configuration logic bitstream engine could end up being slightly lower than the rated frequency of the ram , thereby making it possible to use this invention . in one possible implementation , the higher frequency of back - to - back memory operations can be achieved by using an embedded pll in the bitstream engine to produce two times the at - speed configuration frequency using a slower - speed reference clock . back - to - back configuration and read - back does not add any overhead to the configuration time since the write and read operations are performed back - to - back without slowing down the write frequency . back - to - back configuration and read - back at high frequency can be used to produce high stress conditions on the memory cells and can be used to screen fpgas with defective or weak embedded block ram bits . back - to - back configuration and read - back can be used as a test ( e . g ., bist ) feature or as a customer feature allowing customers to verify the preloaded ram data ( if any ) downloaded from their application bitstream , without any additional effort and without any delay penalty . fig1 shows a simplified block diagram of a portion of an fpga 100 that supports bist testing of an exemplary block of embedded random access memory ( ram ) 110 according to one possible embodiment of the disclosure . to support that bist testing , fpga 100 has bist engine 120 and write / read - back ( w / rb ) bus 122 . embedded memory 110 is part of the fpga &# 39 ; s hard ip ( intellectual property ), while bist engine 120 is implemented in the fpga &# 39 ; s configuration logic as part of the bitstream engine that handles the writing of data ( including both bist data and configuration data ) into the fpga . routing interface ( i / f ) 130 provides the fpga &# 39 ; s programmable logic ( also known as soft ip or fabric ) 140 with access to embedded memory 110 . in particular , fabric 140 can write data to embedded memory 110 via routing i / f 130 and input register 112 either directly using path 113 or via ( 2 × 1 ) input multiplexer 114 . in addition , fabric 140 can read data from memory 110 via output register 116 and ( 2 × 2 ) output multiplexer 118 . note that the other input to input multiplexer 114 is connected to w / rb bus 122 and that one of the two outputs from output multiplexer 118 is also connected to w / rb bus 122 . to perform bist testing , bist engine 120 writes a set of data into embedded memory 110 via w / rb bus 122 , input multiplexer 114 , and input register 112 and then reads that same data from embedded memory 110 via output register 116 , output multiplexer 118 , and w / rb bus 122 . bist engine 120 then compares a local copy of the data that it sent to embedded memory 110 with the data read - back from embedded memory 110 to determine if there are any differences . if one or more differences ( e . g ., bit flips ) are detected , then bist engine 120 determines that a bist error has occurred . as described further below , depending on how bist engine 120 is configured ( e . g ., programmed ), the bist engine 120 will either terminate bist testing upon the first detection of a bist error or it will continue bist testing while counting the number of bist errors detected during the current bist testing session . as also described further below , bist engine 120 is specifically designed to perform bist testing using a back - to - back ( b2b ) write / read - back ( w / rb ) mode that operates faster than the configuration speed , that is , faster than the normal operating speed at which the fpga configuration bitstream engine writes data to and / or reads data from embedded memory 110 . in one exemplary implementation , bist engine 120 performs the b2b w / rb mode at two times the configuration speed . fig2 shows a block diagram representing one possible implementation of some of the circuitry involved in bist testing of embedded memory 110 shown in fig1 in which the bist testing is performed at two times the configuration speed . in particular , phase - lock loop ( pll ) 210 , bist controller 220 , comparator 230 , error counter 240 , address generator 250 , and data generator 260 may be considered to be part of bist engine 120 of fig1 , while input address bus 270 , input data bus 280 , and output data bus 290 may be considered to be part of w / rb bus 122 of fig1 . note that , as drawn in fig2 , input and output registers 112 and 116 of fig1 are assumed to be part of embedded memory 110 and that multiplexers 114 and 118 of fig1 are not shown in fig2 . bist controller 220 , which could be implemented in hardware ( e . g ., using asic circuitry ) or in software ( e . g ., using programmable circuitry ), controls the operations of the other components of bist engine 120 . in operation , pll 210 receives a relatively low - frequency reference clock and generates ( at least ) two faster output clocks : a configuration speed ( cs ) clock 212 and a two - times - configuration - speed ( 2 × cs ) clock 214 that is twice the speed of cs clock 212 . bist controller 220 receives and uses the cs clock 212 and the 2 × cs clock 214 to control bist testing of embedded memory 110 . in particular , during bist testing , at every cycle of cs clock 212 , bist controller 220 causes ( i ) address generator 250 to load a new memory address value into the memory &# 39 ; s address register addr via input address bus 270 and / or ( ii ) data generator 260 to load a new set of data values into the memory &# 39 ; s input data register input data via input data bus 280 . until the next cycle of cs clock 212 , the address value stored in the address register addr and the data value stored in the input data register input data are not changed . note that the address register addr and input data register input data are part of input register 112 of fig . furthermore , bist controller 220 uses 2 × cs clock 214 to control the write - enable signal we for embedded memory 110 such that ( i ) write operations are performed at configuration speed and ( ii ) a single read operation is performed between every two consecutive write operations . for example , for every cycle of the cs clock 212 , the write - enable signal we is high for the half of the cycle and low for the other half of the cycle . when the we signal is high , embedded memory 110 is in write mode , which means that the data values currently stored in the input data register input data will be written into embedded memory 110 at the address value currently stored in the address register addr . when the we signal is low , embedded memory 110 is in read mode , which means that the data values currently stored in embedded memory 110 at the address value currently stored in address register addr will be read from embedded memory 110 via output data register output data and output data bus 290 . note that the output data register output data is part of output register 116 of fig1 . optionally , another address generator and / or data generator can be added that generates only bist - mode addresses and data for possible additional coverage . these generators can be multiplexed in with the input address and data generators used during user - mode or during manufacturing test ( some of which may be off - chip — e . g ., customer boot prom during user mode , or ate memory during manufacturing test ). because , during bist testing , bist controller 220 toggles the we signal two times ( e . g ., first on and then off ) during each cycle of the cs clock 212 , this means that data is written to embedded memory 110 at - speed , but before the next bist write operation is performed , the data from the previous bist write operation is read from embedded memory 110 . note that each bist write operation may involve a set of data comprising one or more bits , where the size of each set of data may either be fixed or configurable , depending on the fpga design . for each bist read operation , comparator 230 performs a bit - by - bit comparison between the data values written into embedded memory 110 during the first half of the current configuration - speed clock cycle and the data values read from embedded memory 110 during the second half of the current configuration speed clock cycle . if any one or more corresponding pairs of bits do not match , then comparator 230 determines that a bist error occurred and therefore sets comparison output signal compare to fail ( e . g ., low ). otherwise , comparator 230 determines that a bist error did not occur and therefore sets ( or maintains ) comparison output signal compare to pass ( e . g ., high ). depending on the design and / or configuration of the fpga , error counter 240 can be used to count the number of bist errors that have occurred during the current session of bist testing as the output signal error_count . note that a typical bist testing session comprises a sequence of many bist write operations over as many consecutive cs clock cycles . alternatively , the fpga may be designed and / or configured such that bist testing is terminated upon the first detection of a bist error , in which case the output error_count generated by error counter 240 would never exceed one . fig3 shows a representation of a finite state machine ( fsm ) 300 that may be implemented by a bist controller analogous to bist controller 220 of fig2 to control the bist testing of an embedded memory having no input and output registers ( for data , address , or write - enable signals ) according to one possible implementation of the disclosure . note that the depiction of fsm 300 in fig3 follows the mealy convention in which inputs are identified before the slash (/), and outputs after the slash . as shown in fig3 , fsm 300 comprises the following four states : 1 ) reset : during which the bist circuitry is initialized for implementation of a next bist testing session ; 2 ) preload : during which a write operation is performed ; 3 ) read - back : during which a read operation is performed and the memory output data register is loaded ; and 4 ) error : where the bist circuitry is parked following detection of a bist error that terminates bist testing . the following are definitions of the different variable names and operations used in fig3 : preload_readback_bist : an input control signal provided by the configuration logic to the bist controller to start a bist testing session . initialize addr , data , and counter : control signals that initialize address generator 250 , data generator 260 , and error counter 240 of fig2 . incr_addr / incr_data : signals similar to conventional address and data register increment signals that a bitstream engine requires to write preload data sequentially into embedded block ram addresses . sof : stop on fail signal instructs the bist controller whether to go to the “ error ” state upon detection of the first bist error . this signal is a static option selected by the application / user , or it could be hardcoded . if sof = 0 , then the bist controller continues bist testing until the last address , while error counter 240 keeps a running count of the total number of detected bist errors . cmp_enable : signal produced by the bist controller that turns on comparator 230 following each read operation . compare : multi - bit signal generated by comparator 230 to indicate whether the most - recent comparison passed , failed , or is ongoing . incr_counter : signal that instructs error counter 240 to increment the value of its error_count output . if any bit errors occur in the current comparison performed by comparator 230 , then incr_counter is asserted . we : write enable signal for the embedded memory . in this state diagram , the we signal controls whether embedded memory 110 is in write or read mode . alternative implementations may have separate read and write enable signals that are externally controllable and can be made non - overlapping . addr_done : signal produced by address register 250 to indicate the end of address generation for the current bist testing session . bist_done : signal output by the bist controller 220 to indicate that the current bist testing session has completed . fig4 shows a representation of a finite state machine 400 that may be implemented by bist controller 220 of fig2 to control the bist testing of embedded memory 110 , which does have input and output registers for data , address , and write - enable signals , according to one possible implementation of the disclosure . as shown in fig4 , fsm 400 comprises seven states : reset , preload , read - back , and error states similar to those in fsm 300 of fig3 plus the following three additional states : 5 ) load memory input registers : during which the memory input data register , memory address register , and write - enable register are loaded with initial values with the write - enable register is set to its write - mode value ; 6 ) wiggle write - enable register : during which the write - enable register is set to its read - mode value ; and 7 ) compare : during which the memory output and input data registers are compared . in addition to the same variable names and operations used in fsm 300 of fig3 , fsm 400 also uses : load memory output data register ( load_modr ): this signal allows the memory output data register to be loaded with data read out from the embedded memory . fig5 shows a representation of another finite state machine 500 that may be implemented by bist controller 220 of fig2 to control the bist testing of embedded memory 110 , according to another possible implementation of the disclosure . fsm 500 is a modified version of fsm 400 of fig4 , in which the “ wiggle we register ” state is eliminated and its operation merged with the “ load memory input register ” state , resulting in fewer states in the state diagram and , consequently , less logic to implement in silicon . fig6 shows a representation of yet another finite state machine 600 that may be implemented by bist controller 220 of fig2 to control the bist testing of embedded memory 110 , according to yet another possible implementation of the disclosure . fsm 600 is an improvement over fsm 400 of fig4 and fsm 500 of fig5 . although it uses the same states as fsm 500 , it uses one less state transition to go from read to the next write operation , thereby causing higher stress during testing . those skilled in the art will understand that other fsm implementations and even non - fsm implementations ( such as with asynchronous logic ) are possible . in some implementations , w / rb bus 122 of fig1 is a hard - wired , dedicated , low - latency bus through which the configuration logic of the fpga can directly communicate with the embedded ram block for both reads and writes at configuration speed . furthermore , bist engine 120 can be designed to function as the bist master for bist testing of many ( e . g ., hundreds ) of different blocks of embedded memory in an fpga using the same w / rb bus 122 for each embedded memory block . in this way , bist testing can be performed in fpgas without the latency issues and without the congestion issues of conventional bist solutions . depending on the particular implementation and / or configuration of the fpga , the data for bist testing may be generated on - chip or off - chip . for off - chip bist data generation , address generator 250 and data generator 260 of fig2 would be implemented off - chip rather than being part of bist engine 120 of fig1 . the disclosure has been described in the context of bist testing in which a single read operation is performed between every two consecutive write operations , where the write operations are performed at - speed . in alternative implementations , two or more read operations could be performed between every two consecutive write operations . inserting multiple read operations between successive write operations could be used to test data - retention faults under stress conditions . for example , an sram bit cell with a broken pmos load transistor will lose its charge if read multiple times back to back after a write operation . such a faulty bit cell might not be detected if only one read operation is performed after each write operation . in other alternative implementations , one or more read operations could be performed between every two consecutive write operations , where the write operations are performed at speeds slower than configuration speed for the configuration logic , as long as the average number of write and read operations performed during two consecutive configuration - speed clock cycles is greater than two . in general , according to embodiments of the present disclosure , the timing between a write operation and an immediately following read operation is faster than the speed of the configuration logic and is within allowable stress limits for the ram being tested . although the disclosure has been described in the context of embedded memory that uses a single control signal ( i . e ., the write - enable ( we ) signal ) to control whether the embedded memory is in write mode or read mode , in other implementations , two or more control signals ( e . g ., a we signal and a distinct read enable ( re ) signal ) may be used to configure the embedded memory into its different operating modes . in such cases , the state machine would need to be modified to include additional states for the different modes of read and write operations . although the disclosure has been described in the context of bist testing , which is typically performed by the manufacturer in the factory before releasing the fpga to the customer , the fpga may also be able to be configured to enable the customer or other users to perform analogous testing . although the disclosure has been described in the context of testing of embedded memory in fpgas , the disclosure may also be implemented in the context of testing embedded memory in other suitable ic devices , such as asics and microprocessors . it should be appreciated by those of ordinary skill in the art that any block diagrams herein represent conceptual views of illustrative circuitry embodying the principles of the invention . similarly , it will be appreciated that any flow charts , flow diagrams , state transition diagrams , pseudo code , and the like represent various processes which may be substantially represented in computer readable medium and so executed by a computer or processor , whether or not such computer or processor is explicitly shown . unless explicitly stated otherwise , each numerical value and range should be interpreted as being approximate as if the word “ about ” or “ approximately ” preceded the value or range . in this specification including any claims , the term “ each ” may be used to refer to one or more specified characteristics of a plurality of previously recited elements or steps . when used with the open - ended term “ comprising ,” the recitation of the term “ each ” does not exclude additional , unrecited elements or steps . thus , it will be understood that an apparatus may have additional , unrecited elements and a method may have additional , unrecited steps , where the additional , unrecited elements or steps do not have the one or more specified characteristics . it will be further understood that various changes in the details , materials , and arrangements of the parts which have been described and illustrated in order to explain embodiments of this invention may be made by those skilled in the art without departing from embodiments of the invention encompassed by the following claims . the use of figure numbers and / or figure reference labels in the claims is intended to identify one or more possible embodiments of the claimed subject matter in order to facilitate the interpretation of the claims . such use is not to be construed as necessarily limiting the scope of those claims to the embodiments shown in the corresponding figures . it should be understood that the steps of the exemplary methods set forth herein are not necessarily required to be performed in the order described , and the order of the steps of such methods should be understood to be merely exemplary . likewise , additional steps may be included in such methods , and certain steps may be omitted or combined , in methods consistent with various embodiments of the invention . although the elements in the following method claims , if any , are recited in a particular sequence with corresponding labeling , unless the claim recitations otherwise imply a particular sequence for implementing some or all of those elements , those elements are not necessarily intended to be limited to being implemented in that particular sequence . reference herein to “ one embodiment ” or “ an embodiment ” means that a particular feature , structure , or characteristic described in connection with the embodiment can be included in at least one embodiment of the invention . the appearances of the phrase “ in one embodiment ” in various places in the specification are not necessarily all referring to the same embodiment , nor are separate or alternative embodiments necessarily mutually exclusive of other embodiments . the same applies to the term “ implementation .” the embodiments covered by the claims in this application are limited to embodiments that ( 1 ) are enabled by this specification and ( 2 ) correspond to statutory subject matter . non - enabled embodiments and embodiments that correspond to non - statutory subject matter are explicitly disclaimed even if they fall within the scope of the claims . | 6 |
examples of substrates are those which have groups on their surface that are reactive with functional groups associated with the organometallic coating . examples of such groups are oxide and / or hydroxyl groups . examples of other groups are carbonyl , carbonate and amide . non - limiting examples of such substrates are those which inherently have such groups on their surface or which form such groups by subsequent treatment such as exposure to the environment or a plasma treatment . examples of materials which form metal oxide surfaces upon exposure to ambient conditions include steels , including stainless steels , iron , and metals which acquire a non - ablating oxide coating upon exposure to the ambient environment , for example , tantalum , titanium , titanium alloys , aluminum , and aluminum alloys . additional examples of materials that acquire an oxide layer upon exposure to the ambient conditions are ceramic materials , for example , silicon nitride . also suitable in the method of the present invention are materials which have an oxide coating imparted to them , for example , thick film oxide insulators in semiconducting devices , and those which can be derivatized to have an oxide surface , for example , gallium arsenide , gallium nitride , and silicon carbide . other examples include conducting oxides , such as indium tin oxide , deposited on a glass substrate . also , metal oxides can be deposited on polymer substrates , for example , “ stacked ” metal oxides on polymer substrates to provide anti - reflective properties . examples of polymer substrates are those that contain oh or oxide groups , such as acrylic copolymers made from one or more monomers that contain hydroxyl groups . also , composite inorganic / organic polymers such as organo polymers containing entrained silica and / or alumina may be used . surprisingly , it has been found that certain polymers that do not adhere well to organometallic coatings such as the titanium and zirconium organometallic coatings in the aforementioned u . s . pat . no . 6 , 645 , 644 adhere very well to the organometallic coatings of the present invention . examples of such polymers are polycarbonates including aromatic and aliphatic polycarbonates , polyurethanes , polyesters , polyepoxides , acrylic polymers and copolymers ( without hydroxyl groups ) and polysiloxanes . the polymer can be in the form of a polymer substrate or a polymer coating on a different substrate , for example , a metal or metal oxide with a polymer surface coating , and a polycarbonate substrate such as an ophthalmic lens with a polysiloxane hard coat on its surface . preferably , the polymer surface is oxidized such as by subjecting the polymer to an atmospheric plasma treatment in the presence of air before application of the organometallic coating . the organometallic film or coating that is applied to the substrate is derived from an organo metal in which the metal has electrons in the f electron orbital such as metals selected from period 6 of the periodic table of elements ( lanthanide series ). examples of suitable metals include la , hf , ta , and w , with ta being preferred . an example of another suitable metal is niobium . the organo portion of the metal is preferably an alkoxide containing from 1 to 18 , preferably 2 to 8 carbon atoms such as ethoxide , propoxide , isopropoxide , butoxide , isobutoxide and tertiary butoxide . the alkoxides may be in the form of simple esters and polymeric forms of the esters . for example , with the preferred metal ta , the simple esters would be ta ( or ) 5 where r is c 1 to c 18 alkyl . polymeric esters would be obtained by condensation of the alkyl esters mentioned above and typically would have the structure ro —[ ta ( or ) 3 — o —] x r where r is defined above and x is a positive integer . besides alkoxides , other ligands can be present such as acetyl acetonates . also , ligands such as chloride , acetylacetonate , alkanolamine and lactate , etc . may be present . the organometallic compound may be used neat and applied under vacuum , by chemical vapor deposition techniques , or it may be dissolved or dispersed in a diluent and applied by coating techniques described below . examples of suitable diluents are alcohols such as methanol , ethanol and propanol , aliphatic hydrocarbons , such as hexane , isooctane and decane , ethers , for example , tetrahydrofuran and dialkylethers such as diethylether . also , adjuvant materials may be present in the organometallic composition . examples include stabilizers such as sterically hindered alcohols and acids , surfactants and anti - static agents . the adjuvants if present are present in amounts of up to 30 percent by weight based on the non - volatile content of the composition . the concentration of the organometallic compound in the composition is not particularly critical but is usually at least 0 . 01 millimolar , typically from 0 . 01 to 100 millimolar , and more typically from 0 . 1 to 50 millimolar . the organometallic treating composition can be obtained by mixing all of the components at the same time with low shear mixing or by combining the ingredients in several steps . the organometallic compounds are reactive with moisture , and care should be taken that moisture is not introduced with the diluent or adjuvant materials and that mixing is conducted in a substantially anhydrous atmosphere . the organometallic composition can be applied to the substrate surface by conventional means such as immersion coating such as dipping , rolling , spraying or wiping to form a film . the diluent is permitted to evaporate . this can be accomplished by heating to 50 - 200 ° c . or by simple exposure to ambient temperature , that is , from 20 - 25 ° c . it is believed that the resulting film is in the form of a polymeric metal oxide in multilayer form with unreacted alkoxide and hydroxyl groups . this is accomplished by depositing the film under conditions resulting in hydrolysis and self - condensation of the alkoxide . these reactions result in a polymeric coating being formed that provides cohesive strength to the film . the conditions necessary for these reactions to occur is to deposit the film in the presence of water , such as a moisture - containing atmosphere . the resulting film has some unreacted alkoxide groups and / or hydroxyl groups for subsequent reaction and possible covalent bonding with an overlayer material . however , for readily co - reactive groups , ambient temperatures , that is , 20 ° c ., may be sufficient . although not intending to be bound by any theory , it is believed the polymeric metal oxide is of the structure : where m is the metal of the invention , r is an alkyl group containing from 1 to 30 carbon atoms ; x + y + z = v , the valence of m ; x is at least 1 , y is at least 1 , z is at least 1 ; x = v − y − z ; y = v − x − z ; z = v − x − y ; n is greater than 2 , such as 2 to 1000 . for optical applications , the resulting film typically has a thickness of 5 to 100 nanometers . for other applications , thicker films can be used . when the organometallic compound is used neat and applied by chemical vapor deposition techniques in the absence of moisture , a thin metal alkoxide film is believed to form . polymerization , if any occurs , is minimized and the film may be in monolayer configuration . when the organometallic compound is subjected to hydrolysis and self - condensation conditions as mentioned above , thicker films are formed . the process of the present invention can be used to provide a film or layer that is continuous or discontinuous , that is , in a pattern on the substrate surface . non - limiting examples include spraying the composition onto the surface of the substrate in pre - determined areas , for example , by ink - jet printing or stenciling . other methods may be found by adapting printing techniques , including stamping , lithographing and gravure printing a coating solution onto the substrate in a pattern . as mentioned above , an overlayer or a different film can be applied to the organometallic film . such an overlayer material preferably contains groups that are reactive with the alkoxide and / or hydroxyl groups , such as hydroxyl groups or acid groups or derivatives thereof . preferably , the overlayer is an organic acid or a derivative thereof . the acid may be a carboxylic acid , a sulfonic acid or a phosphorus acid , such as a phosphoric acid , phosphonic acid or a phosphinic acid . by derivatives of acids are meant functional groups that perform similarly as acids such as acid salts , acid esters and acid complexes . the organo group of the acid may be monomeric , oligomeric or polymeric . for example , the organo acid may be a monomeric , phosphoric , phosphonic or phosphinic acid . examples of monomeric phosphoric acids are compounds or a mixture of compounds having the following structure : wherein x is 1 - 2 , y is 1 - 2 and x + y = 3 , r is a radical having a total of 1 - 30 , preferably 6 - 18 carbons , where r ′ is h , a metal such as an alkali metal , for example , sodium or potassium , alkyl including substituted alkyl having 1 to 50 carbons , preferably 1 to 4 carbons such as methyl or ethyl , including substituted aryl having 6 to 50 carbons ; preferably , a portion of r ′ is h . the organic component of the phosphoric acid ( r ) can be aliphatic ( e . g ., alkyl having 2 - 20 , preferably 6 - 18 carbon atoms ) including an unsaturated carbon chain ( e . g ., an olefin ), or can be aryl or aryl - substituted moiety . example of monomeric phosphonic acids are compounds or mixture of compounds having the formula : wherein x is 0 - 1 , y is 1 , z is 1 - 2 and x + y + z is 3 . preferably , r and r ″ are each independently a radical having a total of 1 - 30 , preferably 6 - 18 carbons . r ′ is h , a metal , such as an alkali metal , for example , sodium or potassium or an amine or alkyl including substituted alkyl having 1 to 50 carbon atoms , preferably lower alkyl having 1 - 4 carbons such as methyl or ethyl , or aryl including substituted aryl having 6 to 50 carbons . preferably at least a portion of r ′ is h . the organic component of the phosphonic acid ( r and r ″) can be aliphatic ( e . g ., alkyl having 2 - 20 , preferably 6 - 18 carbon atoms ) including an unsaturated carbon chain ( e . g ., an olefin ), or can be an aryl or aryl - substituted moiety . example of monomeric phosphinic acids are compounds or mixture of compounds having the formula : wherein x is 0 - 2 , y is 0 - 2 , z is 1 and x + y + z is 3 . preferably , r and r ″ are each independently radicals having a total of 1 - 30 , preferably 6 - 18 carbons . r ′ is h , a metal , such as an alkali metal , for example , sodium or potassium or an amine or alkyl including substituted alkyl having 1 to 50 carbon atoms , preferably lower alkyl having 1 - 4 carbons , such as methyl or ethyl , or aryl including substituted aryl having 6 to 50 carbons . preferably a portion of r ′ is h . the organic component of the phosphinic acid ( r , r ″) can be aliphatic ( e . g ., alkyl having 2 - 20 , preferably 6 - 18 carbon atoms ) including an unsaturated carbon chain ( e . g ., an olefin ), or can be an aryl or aryl - substituted moiety . examples of organo groups which may comprise r and r ″ include long and short chain aliphatic hydrocarbons , aromatic hydrocarbons and substituted aliphatic hydrocarbons and substituted aromatic hydrocarbons . examples of substituents include carboxyl such as carboxylic acid , hydroxyl , amino , imino , amido , thio , cyano , and fluoro . representative of the organophosphorous acids are as follows : amino trismethylene phosphonic acid , aminobenzylphosphonic acid , 3 - amino propyl phosphonic acid , o - aminophenyl phosphonic acid , 4 - methoxyphenyl phosphonic acid , aminophenylphosphonic acid , aminophosphonobutyric acid , aminopropylphosphonic acid , benzhydrylphosphonic acid , benzylphosphonic acid , butylphosphonic acid , carboxyethylphosphonic acid , diphenylphosphinic acid , dodecylphosphonic acid , ethylidenediphosphonic acid , heptadecylphosphonic acid , methylbenzylphosphonic acid , naphthylmethylphosphonic acid , octadecylphosphonic acid , octylphosphonic acid , pentylphosphonic acid , phenylphosphinic acid , phenylphosphonic acid , bis -( perfluoroheptyl ) phosphinic acid , perfluorohexyl phosphonic acid , styrene phosphonic acid , dodecyl bis - 1 , 12 - phosphonic acid , poly ( hexafluoropropyl ) phosphonic acid . in addition to the monomeric organophosphorous acids , oligomeric or polymeric organophosphorous acids resulting from self - condensation of the respective monomeric acids may be used . to provide hydrophobic properties to the overlayer , the organic acid or derivative thereof is preferably a fluorinated material , typically a perfluorinated oligomer having a number average molecular weight of less than 2000 . the perfluorinated material can be a perfluorinated hydrocarbon of the following structure : where r f is a perfluorinated alkyl group or a perfluorinated alkylene ether group and p is 2 to 4 , preferably 2 . where y is f or c n f 2n + 1 ; m is 4 to 20 and n is 1 to 6 . where a is an oxygen radical or a chemical bond ; n is 1 to 6 ; y is f or c n f 2n + 1 ; w is h , f , c n h 2n or c n f 2n ; b is 2 to 10 , m is 0 to 6 , and p is 0 to 18 . where r and r ″ are a hydrocarbon or substituted hydrocarbon radical having up to 200 , such as 1 to 30 and 6 to 20 carbons , r can also include the perfluoroalkyl groups mentioned above , and r ′ is h , a metal such as potassium or sodium or an amine or an aliphatic radical , for example , alkyl including substituted alkyl having 1 to 50 carbons , preferably lower alkyl having 1 to 4 carbons such as methyl or ethyl , or aryl including substituted aryl having 6 to 50 carbons . examples of fluorinated materials are esters of perfluorinated alcohols such as the alcohols of the structure : where y is f or c n f 2n + 1 ; m is 4 to 20 and n is 1 to 6 . examples of suitable esters are stearates and citrates of such alcohols . such materials are available from e . i . du pont de nemours and company under the trademark zonyl fts and zonyl tbc . for application to the surface of the substrate , the overlayer material is dissolved in a liquid diluent . the concentration of the overlayer material is typically dilute , for example , no greater than 10 percent on a weight / volume basis for solid overlayer material and 10 percent on a volume / volume basis for oil and liquid overlayer material , and preferably is within the range of 0 . 01 to 1 . 0 percent . the percentages are based on total weight or volume of the solution . examples of suitable diluents are hydrocarbons such as hexane isooctane and toluene ; ketones such as methyl ethyl ketone ; alcohols such as methanol and ethanol ; ethers such as tetrahydrofuran . fluorinated solvents such as nonafluorobutylmethyl ether and fluorinated solvents available as hfe - 7100 , supplied by 3m innovative products and perfluorinated ethers supplied by solvay solexis under the trademark galden are preferred for use with the fluorinated material . the fluorinated solvents can be used in admixtures with the other solvents mentioned above . the fluorinated solvents or diluents are different from the fluorinated materials in that the fluorinated solvents or diluents are not film formers , whereas the fluorinated materials are . preferably , the vapor pressure of the diluent is high , permitting rapid evaporation at room temperature ( 20 - 25 ° c .). the overlayer material can be dissolved easily upon adding the overlayer material to the diluent . the solution of the overlayer material can be applied to the surface of the optical article by dipping , rolling , spraying or wiping . after application of the overlayer material , the diluent is permitted to evaporate , with or without wiping during evaporation , preferably at ambient temperature , or optionally by the application of heat . the resultant layer typically is thin , having a thickness of about 10 - 100 nanometers or less . the fluorinated overlayers are hydrophobic , having a water contact angle greater than 70 °, typically from 75 - 1300 . the water contact angle can be determined using a contact angle goniometer such as a tantec contact angle meter model cam - micro . the following examples show various coated articles and methods for their preparation in accordance with the invention . all parts are by weight unless otherwise indicated . one milliliter of a 0 . 25 % solution of tantalum isopropoxide in isopropanol was dispensed onto a tissue (“ kimwipe ” manufactured by kimberly clark ) and rubbed on a polycarbonate lens which had a polysiloxane - based hardcoat for five seconds . then , one milliliter of a 0 . 2 % solution of poly ( hexafluoropropyleneoxide )- monophosphonic acid p ( hfpo ) pa in 5 % hfe - 7100 ( 3m innovative products ), 94 % soltrol - 10 ( cp chem ) and 1 % orange oil fragrance ( citrus and allied ) was sprayed onto the tantalum alkoxide - coated lens surface . over a period of 30 seconds , the solvent layer began to repel from the lens surface as the fluoropolymer coating reacted with the tantalum alkoxide . any visibly remaining coating or solvent was then gently wiped from the surface using a microfiber cloth ( hilco optiwipe ). water contact angle ( wca ) measurements were taken initially , and after abrading the surface with a microfiber cloth ( hilco optiwipe ) at 150 g / cm 2 ( table 1 ). to show that the organotantalum coating was still active after abrasion , the p ( hfpo ) pa coating was reapplied and the wca increased back to the initial level ( table 1 ). one milliliter of a 0 . 25 % solution of aluminum isopropoxide in isopropanol was dispensed onto a tissue (“ kimwipe ” manufactured by kimberly clark ) and rubbed on a polycarbonate lens which had a polysiloxane - based hardcoat for five seconds . then , one milliliter of a 0 . 2 % solution of poly ( hexafluoropropyleneoxide )- monophosphonic acid in 5 % hfe - 7100 ( 3m innovative products ), 94 % ethanol ( univar ) and 1 % orange oil fragrance ( citrus and allied ) was sprayed onto the aluminum alkoxide - coated lens surface . over a period of 30 seconds , the solvent layer began to repel from the lens surface as the fluoropolymer coating reacted with the aluminum alkoxide layer . any visibly remaining coating or solvent was then gently wiped from the surface using a microfiber cloth ( hilco optiwipe ). water contact angle measurements were taken initially , and after abrading the surface with a microfiber cloth ( hilco optiwipe ) at 150 g / cm 2 ( table 1 ). to show that the organoaluminum coating was inactive after abrasion , the p ( hfpo ) pa coating was reapplied and the wca did not increase ( table 1 ). one milliliter of a 0 . 25 % solution of zirconium propoxide in isopropanol was dispensed onto a tissue (“ kimwipe ” manufactured by kimberly clark ) and rubbed on a polycarbonate lens which had a polysiloxane - based hardcoat for five seconds . then , one milliliter of a 0 . 2 % solution of poly ( hexafluoropropyleneoxide )- monophosphonic acid in 5 % hfe - 7100 ( 3m innovative products ), 94 % ethanol ( univar ) and 1 % orange oil fragrance ( citrus and allied ) was sprayed onto the zirconium alkoxide - coated lens surface . over a period of 30 seconds , the solvent layer began to repel from the lens surface as the fluoropolymer coating reacted with the zirconium alkoxide layer . any visibly remaining coating or solvent was then gently wiped from the surface using a microfiber cloth ( hilco optiwipe ). water contact angle measurements were taken initially , and after abrading the surface with a microfiber cloth ( hilco optiwipe ) at 150 g / cm 2 ( table 1 ). to show that the organozirconium coating was inactive after abrasion , the p ( hfpo ) pa coating was reapplied and the wca did not increase ( table 1 ). one milliliter of a 0 . 5 % solution of titanium n - butoxide in isopropanol was dispensed onto a tissue (“ kimwipe ” manufactured by kimberly clark ) and rubbed on a polycarbonate lens which had a polysiloxane - based hardcoat for five seconds . then , one milliliter of a 0 . 2 % solution of poly ( hexafluoropropyleneoxide )- monophosphonic acid in 5 % hfe - 7100 ( 3m innovative products ), 94 % ethanol ( univar ) and 1 % orange oil fragrance ( citrus and allied ) was sprayed onto the titanium alkoxide - coated lens surface . over a period of 30 seconds , the solvent layer began to repel from the lens surface as the fluoropolymer coating reacted with the titanium alkoxide layer . any visibly remaining coating or solvent was then gently wiped from the surface using a microfiber cloth ( hilco optiwipe ). water contact angle measurements were taken initially , and after abrading the surface with a microfiber cloth ( hilco optiwipe ) at 150 g / cm 2 ( table 1 ). to show that the organotitanium coating was inactive after abrasion , the p ( hfpo ) pa coating was reapplied and the wca did not increase ( table 1 ). in this example , no organometallic coating step was employed . one milliliter of a 0 . 2 % solution of poly ( hexafluoropropyleneoxide )- monophosphonic acid in 5 % hfe - 7100 ( 3m innovative products ), 94 % ethanol ( univar ) and 1 % orange oil fragrance ( citrus and allied ) was sprayed onto a polycarbonate lens which had a polysiloxane - based hardcoat . the solvent was allowed to evaporate ( 30 seconds ), and any visibly remaining coating or solvent was then gently wiped from the surface using a microfiber cloth ( hilco optiwipe ). water contact angle measurements were taken initially , and after abrading the surface with a microfiber cloth ( hilco optiwipe ) at 150 g / cm 2 ( table 1 ). | 8 |
in some embodiments , a two level authentication system in which the second level is optional based on customer preference and level of security is provided . an immobilizer transponder , passive keyless entry transponder , or remote keyless entry transmitter may be used to authenticate the holder of a token as a valid user for the system . in addition , an optional pin code may be used for enhanced authentication . keyboard entry of a pin number may be from radio preset selection buttons or other convenient buttons provided for this or other combined features . such token / pin authentication enables the appropriate function , features , content , and data for a valid user . fig1 is a block diagram of integrated system 10 of vehicle 12 . processor 14 provides an occupant of vehicle 12 with a common access point to various vehicle components and data . processor 14 receives input from wireless keyboard 16 , microphone 18 , and camera 20 . processor 14 also receives input via display screen 22 , e . g ., touchscreen , and displays various information via display screen 22 . processor 14 is also connected with the sound system for vehicle 12 . the sound system includes audio head unit 24 , amplifier 26 , and speakers 28 . the volume of speakers 28 may be remotely controlled with remote volume switch 30 . processor 14 receives signals via antenna 32 and transmits and receives wireless data via transceiver 34 . consumer port 36 , e . g ., usb port , permits an occupant to exchange information with vehicle 12 . gps sensor 38 , together with processor 14 , determines the current location of vehicle 12 . car area network 40 is connected with processor 14 , speed sensor 42 , ignition system 44 , and passive anti - theft system 46 . speed sensor 42 determines , in conventional fashion , the speed of vehicle 12 . in alternative embodiments , some or all of the elements connected directly with processor 14 may be connected with car area network 40 and thus communicate with processor 14 via car area network 40 . passive anti - theft system 46 prevents unauthorized use of vehicle 12 and processor 14 . as described below , passive anti - theft system 46 may prevent ignition system 44 from starting vehicle 12 and may also prevent the operation of processor 14 . keys 48 , 50 include embedded identifying information 49 , 51 respectively . passive anti - theft system 46 uses identifying information 49 , 51 to determine whether keys 48 , 50 are associated with vehicle 12 and to distinguish between keys 48 , 50 . if key 48 is inserted into key slot 52 , key slot 52 senses identifying information 49 . identifying information 49 includes a vehicle identifier , e . g ., “ z ”, that indicates key 48 is for use with vehicle 12 . this vehicle identifier , e . g ., “ z ”, is shared between keys 48 , 50 . that is , in this example , identifying information 51 of key 50 will also include the vehicle identifier “ z ”. on the basis of the vehicle identifier , passive anti - theft system 46 determines that key 48 , or key 50 , is for use with vehicle 12 . identifying information 49 also includes a driver identifier , e . g ., “ 4 ”, that indicates key 48 is different from key 50 . this driver identifier , e . g ., “ 4 ”, is not shared between keys 48 , 50 . that is , in this example , identifying information 51 of key 50 will include a different driver identifier , e . g ., “ 5 ”. on the basis of the driver identifier , passive anti - theft system 46 distinguishes between key 48 and key 50 and thus distinguishes between driver a who normally uses key 48 and driver b who normally uses key 50 . as described below , if processor 14 is informed as to which driver is to drive vehicle 12 , processor 14 can check to see if driver a or driver b has updated their respective configuration information and , if so , update system 10 with any updated configuration information . if key 48 is inserted into key slot 52 , passive anti - theft system 46 determines that key 48 is associated with a particular driver , e . g ., driver a , and may be used to start ignition system 44 . if , instead , key 50 is inserted in key slot 52 , passive anti - theft system 46 determines that key 50 is associated with a different particular driver , e . g ., driver b , and may be used to start ignition system 44 . if key 48 is inserted in key slot 52 , passive anti - theft system 46 enables processor 14 such that driver a will have use of processor 14 and access to data on processor 14 specific to driver a . if , instead , key 50 is inserted in key slot 52 , passive anti - theft system 46 enables processor 14 such that driver b will have use of processor 14 and access to data on processor 14 specific to driver b . identifying information 49 , 51 need not be embedded with keys 48 , 50 . in some embodiments , identifying information 49 , 51 may be provided by key fobs or other devices . in some embodiments , additional identifying information may be required prior to enabling ignition system 44 or processor 14 . for example , a driver may need to input an additional identifying code via touch display 22 . fig2 is an illustration of vehicle 12 , remote location 54 , and network 56 . during assembly , processor 14 ( fig1 ) is loaded with factory set configuration information 53 which determines , inter alia , the appearance and functionality of display screen 22 . configuration information 53 is uploaded and stored at remote location 54 via network 56 . in the example of fig2 , configuration information 53 specifies audio channels 1 , 2 , and 3 , a red background , and three ( 3 ) buttons for display 22 . configuration information 53 also includes a part number for a component of vehicle 12 , e . g ., hvac #: 35x71 . as described below , this component information may be used to verify that requested configuration information is directed to an authorized vehicle . fig3 is an illustration of update terminal 57 , remote location 54 , and network 56 . in the example of fig3 , driver a accesses remote location 54 via network 56 and submits updated configuration information 58 including audio channel , background , and number of button information for display 22 . remote location 54 checks to see whether updated configuration information 58 complies with policy 60 regarding the number of buttons for display 22 . in the example of fig3 , policy 60 permits a maximum of 5 buttons for display 22 . if updated configuration information 58 violates policy 60 , remote location 54 will modify updated configuration information 58 such that it complies with policy 60 . in the example of fig3 , updated configuration information specifies audio channels 3 , 5 , and 7 , a blue background , and twenty - five ( 25 ) buttons for display 22 . policy 60 , however , limits the number of buttons to five ( 5 ). remote location 54 will modify updated configuration information 58 such that it includes only five ( 5 ) buttons . modified configuration information 62 will be stored at remote location 54 and returned to driver a via network 56 . in alternative embodiments , remote location 54 may reject updated configuration information 58 if it does not comply with policy 60 . as such , remote location 54 is able to control the configuration information associated with processor 14 and display 22 . fig4 is an illustration of vehicle 12 , remote location 54 , and network 56 . upon the next authorized start - up of vehicle 12 by driver a , following the process described with respect to fig3 , processor 14 will communicate with remote location 54 , via wireless access point 34 ( fig1 ), through network 56 to determine whether factory installed configuration information 53 is to be updated . processor 14 will request from remote location 54 an indicator as to whether the configuration information has changed , and , if so , processor 14 will download modified configuration information 62 and configure processor 14 and display 22 based on modified configuration information 62 during the use of vehicle 12 by driver a . in the absence of any update to configuration information 53 by driver b , upon the next authorized start - up of vehicle 12 by driver b , processor 14 will reconfigure processor 14 and display 22 based on configuration information 53 during the use of vehicle 12 by driver b . in some embodiments , prior to the download of updated configuration information , remote location 54 may request the part number of a vehicle component , e . g ., hvac #: 35x71 , to confirm that the vehicle requesting the configuration information is authorized to do so . remote location 54 may compare the received vehicle component number and compare it to that stored and uploaded by the factory . if the numbers match , remote location 54 may allow the download of any updated configuration information to occur . if the numbers do not match , remote location 54 may deny the request to download any updated configuration information . in some embodiments , driver behavior may be used to determine whether to prevent access or disable some or all of the functionality of system 10 . for example , speed sensor 42 may indicate that the vehicle speed exceeds all legal limits , e . g ., 100 m . p . h ., suggesting unauthorized use of vehicle 12 . under such circumstances , passive anti - theft system may disable some or all of the functionality of processor 14 to protect information residing in processor 14 . it is contemplated that other techniques may be used to monitor driver behavior , e . g ., frequency of stop and start , intensity of breaking or acceleration , etc . fig5 is an perspective view of the dash panel of vehicle 12 and shows display 22 with modified configuration information 62 , e . g ., display unit 22 is shown with audio channels 3 , 5 , and 7 and five ( 5 ) buttons . while embodiments of the invention have been illustrated and described , it is not intended that these embodiments illustrate and describe all possible forms of the invention . rather , the words used in the specification are words of description rather than limitation , and it is understood that various changes may be made without departing from the spirit and scope of the invention . | 7 |
since many alternatives , modifications and variations can be made from the present invention , preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings . however , one should understand that it is not intended to be limiting , but embrace all modification , equivalents or substitutions included in the scope and technical field of the present invention . in the following description , well - known functions or constitutions will not be described in detail if they would obscure the invention in unnecessary detail . although terms like the first , the second , etc ., may be used for explaining diverse elements , the elements are not to be limited by the terms . the terms are used only for distinguishing one element from another . the terminology used in this application is used simply for explaining particular embodiments , and is not intended to limit the scope of the present invention in any way . as used throughout this disclosure , the singular forms include plural reference unless the context clearly indicates otherwise . also , it should be understood that the expression of “ comprise ” or “ include ” in this disclosure is to designate the existence of features , numbers , steps , operations , elements , parts or combinations thereof that are described in the specification , and does not eliminate beforehand the existence of one or more of other features , numbers , steps , operations , elements , parts , or combinations of thereof or the possibility of addition . hereinafter , preferred embodiments of the present invention will now be described with reference to the accompanying drawings . for a more complete understanding of the present invention and the advantages thereof , like reference numerals represent like parts even in different drawings . before getting into further details on the drawings , it is necessary to clarify that components described in this specification are divided by primary function each component is responsible for . that is , two or more components to be described below may be incorporated into one component , or one component may be differentiated into more than two by itemized function . in addition , any person skilled in the art may understand that each component may perform , besides its primary function , part or all of functions of another component additionally , and part of the primary function each component is responsible for may be carried out by another component . therefore , it is important to note whether all components that are explained throughout this specification exist or not should be interpreted in terms of function , and for this reason the configuration of components of mbs system in accordance with the present invention may differ from that of fig2 within the scope for achieving the foregoing objectives of the present invention . fig2 illustrates the structure of mbs system over mmr network using dynamic modification of the mcs level in accordance with one embodiment of the present invention . in the existing mbs system , amc scheme is employed only in the transmission between the bs and rs and the mcs level for the transmission between rs and mss is fixed . however , the mbs system according to the present invention introduces rs into the mobile wimax system based on ieee802 . 16e , continuously checks the channel condition using cqich , changes the mcs level for the transmission between the bs and rs if the mcs level is to be changed and changes the mcs level for the transmission between rs and ms based on the changed mcs level for the transmission between the bs and rs . accordingly , the mbs system according to the present invention guarantees the stable service quality . in the mbs system according to the present invention , rs is located and fixed at the location where it is possible to stably receive the mbs data with all mcs levels of the bs . the bs can select the optimum mcs level using amc scheme that guarantees the maximum throughput , depending on the channel conditions , and rs decides the mcs level for stable transmission of mbs data between rs and ms by dynamic modification of the mcs level according to the present invention . for this , it is required that mss are wirelessly connected to the bs through rs for mutual information exchange and mss can report the channel condition to the bs . as described above , the main purpose of introduction of the mbs system over mmr network using dynamic modification of the mcs level is to guarantee the successful data transmission to mss located even in the edge of the cell by solving problems caused by use of fixed mcs level . further , the mbs system over mmr network using dynamic modification of the mcs level according to the present invention provides high quality service by improving low data throughput of the existing mbs system and by maintaining stable data throughput during mbs data transmission . the dynamic modification of the mcs level according to the present invention is performed based on the calculation of spectrum efficiency and throughput and guarantees quality of service ( qos ) of the mbs system . fig3 is a flow chart for explaining a method for mbs over mmr network using dynamic modification of mcs level in accordance with one embodiment of the present invention . referring to fig3 , in step s 1 , the bs receives information on channel condition through cqich at a predetermined period . here , rs to which a ms get accessed may be placed outside the radio range of the bs . in accordance with this embodiment of the present invention , the rs forms mmr network . therefore , information on the channel condition of the rs can be sent to the bs through the information exchange with other rss connected through the mmr network . next , in step s 2 , the bs decides , based on the received information of the channel condition of the rs , whether the current mcs level should be updated . in detail , the information on the channel condition may include at least one of a group consisting of throughput values between the bs and the rs that is measured by the rs and / or spectrum efficiency values on the current channel . as such , the bs , based on the throughput values and / or the spectrum efficiency values extracted from the information on the channel condition , may decide to update the mcs level , if the extracted value is below a predetermined value . for instance , if the extracted throughput value is greater than a predetermined threshold throughput value ( for example , throughput values corresponding to other mcs levels which is not used currently ), the bs regards the channel condition between the bs and the rs as satisfactory . in this case , the bs does not update the mcs level and uses the existing mcs level . meanwhile , if the extracted throughput value is less than a predetermined threshold throughput value , the bs regards the channel condition between the bs and the rs unsatisfactory . in this case , the bs decides to update the mcs level for more efficient application of amc . if , in step s 2 , the bs decides not to update the mcs level ( no in s 2 ), in step s 7 , the bs transmits mbs data with the existing mcs level to the rs . however , if , in step s 2 , the bs decides to update the mcs level ( yes in s 2 ), the bs , in step s 3 , transmits test mbs data of plural mcs levels to the rs . for example , the bs can transmit test mbs data with a plurality of ( for example , six ) mcs levels to the rs . here , six mcs levels comprises : qpsk1 / 2 , qpsk3 / 4 , 16qam1 / 2 , 16qam3 / 4 , 64qam2 / 3 and 64qam3 / 4 . the rs reports to the bs channel condition ( i . e ., throughputs ) corresponding to each mcs level . the bs makes amc table with the mcs levels , throughputs corresponding to the mcs levels , and spectrum efficiencies corresponding to the mcs levels . among the mcs levels , the mcs level with the highest spectrum efficiency is selected as the most appropriate mcs level for the transmission between the bs and rs . in this regard , the most appropriate mcs level is decided by the bs &# 39 ; s transmission of the test mbs data to rs and the rs &# 39 ; s feedback and recorded in the amc table . next , in step s 4 , the mcs level recorded in the amc table can be changed and the amc table can thus be updated . in detail , the channel condition is periodically reported to the bs and the amc table is updated when newly measured spectrum efficiency is lower than spectrum efficiency corresponding to another mcs level which is not used currently . in order to decide the most appropriate mcs level under changed channel conditions , the bs sends test mbs data to rs , receives from the rs feedback information in response to the test mbs data with six different mcs levels and updates the amc table . in a process of updating the amc table , spectrum efficiencies corresponding to each mcs level are calculated . in step s 5 , spectrum efficiency of mobile station me is calculated through equation 3 to be explained later based on spectrum efficiency of rsi corresponding to the decided mcs level for transmission between the bs and rs and the throughput of the overall mbs system mbsthr . the mcs level corresponding to the calculated spectrum efficiency me is selected as the most appropriate mcs level for transmission between rs and ms and recorded in dmc table . the dmc table is updated as the amc table is updated . next , in step s 6 , the bs transmits an mcs control message including information on the updated mcs level in the dmc table to the rs . the mcs control message informs rs of the updated mcs level . in step s 7 , the bs transmits mbs data with the updated mcs levels through rs to mss . mss report each channel condition to the bs at the same time . however , it is not possible to transmit mbs data with various mcs levels appropriate for transmissions to every ms . accordingly , the mbs system according to the present invention is designed to guarantee the highest throughput in the transmission between the bs and rs and qos in the transmission between rs and mss . for example , if the mcs level of the bs is changed due to the changed condition of channel between the bs and rs , in order to maintain previous throughput , the mcs level of rs is dynamically changed according to the spectrum efficiency . through this mechanism , in the mbs such as live broadcast , hook - up , and vod whose qos should be guaranteed , better mbs data throughput is guaranteed and stable service is provided to mss . rs relays traffic and supports access of users and transmission of control and management message . the bs transmits the mbs data with the same throughput to all mss . referring to the network configuration illustrated in fig2 , the overall bandwidth ( ob ) of the mbs system according to the present invention can be expressed as equation 1 , where n denotes the number of rs , rbi denotes the bandwidth between the ( i − 1 ) th rs and the ( i ) th rs , and rb 0 denotes the bandwidth between the bs and the first rs . although mb denotes the bandwidth between ms and the rs or bs , a fixed bandwidth is used for the mb regardless of the number of ms since one spectrum bandwidth is shared in the mbs system . the spectrum efficiency refers to a maximum amount of data that can be transmitted over a given bandwidth in the wireless communication network , and it is measured in bit / s / hz . the current spectrum efficiency is calculated by transmitted data packets from the bs to the rs for the measurement of current channel condition . the bandwidth for relay station rbi and the bandwidth for mobile station mb in mbs can then be written as : rei denotes current spectrum efficiency of the ( i ) th rs , and me denotes current spectrum efficiency of the ms . using equation ( 2 ), the throughput value of overall mbs system can be written as : the spectrum efficiency of the overall rs in mobile n - hop relay network can be written as : in equation ( 4 ), re denotes the spectrum efficiency of the overall rs and rei denotes the current spectrum efficiency that is measured at the rs and is reported to the bs . this is used to decide the mcs level appropriate for transmission of mbs data from the rs . using equation ( 4 ), the relation between the mbs data throughput and the spectrum efficiency can be written as : equation ( 5 ) describes the relation between re and me for assuring qos when the mbs throughput value is constant . in the mbs system according to the present invention , the current spectrum efficiency of the rs and ms are used as factors for controlling the mbs throughput while ob value is fixed . generally , high spectrum efficiency achieved by high order mcs level allows high throughput . however , higher order mcs level does not always guarantee higher throughput . this is because the throughput is significantly affected by channel condition more than the mcs level . for high mbs throughput , therefore , high spectrum efficiency for the rs is needed in the current channel condition . for stable mbs throughput , it is preferable to decide the mcs level based on the relation between re and me . network simulator 2 version 2 . 29 is used to compare the performance of the mbs system according to the present invention and the performance of the existing mbs system , and the mobile wimax system based on ieee802 . 16e library and ieee802 . 16j is implemented for the simulation . further , the frs which is studied by ieee802 . 16j mmr project group is implemented . fig4 illustrates experimental environment for analyzing the performance of the mbs system according to the present invention and the performance of the existing mbs systems . fig4 illustrates mbs data transmission on downlink channel . fig4 ( a ) illustrates the existing mbs system with no rs , fig4 ( b ) illustrates the existing mbs system over mmr network employing the amc scheme only between the bs and rs , and fig4 ( c ) illustrates the mbs system over mmr network according to the present invention respectively employing the amc scheme between the bs and rs and the dmc scheme between rs and ms . the mcs level of the existing mbs system illustrated in fig4 ( a ) is qpsk1 / 2 which allows stable data delivery to the mss regardless of the location in the cell but has low throughput . although , in the existing mbs system illustrated in fig4 ( b ), higher throughput can be obtained by selectively using the mcs level due to the benefit of the expanded coverage through rs , the most stable mbs data throughput is guaranteed by employing the dmc scheme between rs and ms unlike the existing mbs systems illustrated in fig4 ( a ) and fig4 ( b ). fig5 illustrates throughputs of the mbs system according to the present invention , the existing mbs system with no rs and the existing mbs system over the mmr network as time moves . according to fig5 , it is noted that mbs data throughput of the mbs system according to the present invention is significantly improved comparing with the mbs data throughput of the existing mbs systems . the average throughputs of the mbs system according to the present invention , the existing mbs system with no rs and the existing mbs system over mmr network are 3 , 817 kbps , 889 kbps and 2 , 759 kbps . the throughput offered by the mbs system according to the present invention is about 3 times of the throughput of the existing mbs system with no rs and the throughput offered by the mbs system according to the present invention is improved about 38 % than the existing mbs system over mmr network . fig6 illustrates a graph comparing the transmission time of the mbs system according to the present invention , the existing mbs system with no rs and the existing mbs system over mmr network for different packet sizes up to 100 mb . fig6 illustrates that , when transmitting the mbs data whose size is bigger than 60 mb , the mbs system according to the present invention requires smaller transmission time than the existing mbs system over mmr network . further , it is illustrated that , the mbs system according to the present invention maintains constant level of transmission time regardless of the size of the mbs data while the transmission time of the existing mbs system with no rs increases as size of mbs data increases . fig6 illustrates that the mbs system according to the present invention offers higher throughput than that of the existing mbs systems . further , almost constant transmission time maintained by the mbs system according to the present invention means that the mbs system according to the present invention guarantees stable mbs data transmission . fig7 illustrates the impact of the number of mss on throughput of the mbs system according to the present invention , the existing mbs system with no rs and the existing mbs system over mmr network . it is illustrated that the impact of the number of the ms on throughput in each system is not so significant and throughput of the mbs system according to the present invention is higher and constant . the hardware devices described above can be configured as one or more software module to execute the operation of the present invention , and vice versa . while the invention has been shown and described with respect to the preferred embodiments , it will be understood by those skilled in the art that various changes and modification may be made without departing from the spirit and scope of the invention as defined in the following claims . | 7 |
in the following description , for purposes of explanation rather than limitation , specific details are set forth such as the particular architecture , interfaces , techniques , etc ., in order to provide a thorough understanding of the present invention . for purposes of simplicity and clarity , detailed descriptions of well - known devices , circuits , and methods are omitted so as not to obscure the description of the present invention with unnecessary detail . in order to facilitate an understanding of this invention , background information relating to the mpeg2 coding is briefly explained . as a person of average skill in the art will appreciate , in general , the mpeg2 coding is performed on an image by dividing the image into macro - blocks of 16 × 16 pixels , each with a separate quantizer scale value associated therewith . the macro - blocks are further divided into individual blocks of 8 × 8 pixels . each 8 × 8 pixel block is subjected to a discrete cosine transform ( dct ) to generate dct coefficients for each of the 64 frequency bands therein . the dct coefficients in an 8 × 8 pixel block are then divided by a corresponding coding parameter , i . e ., a quantization weight . the quantization weights for a given 8 × 8 pixel block are expressed in terms of an 8 × 8 quantization matrix . thereafter , additional calculations are affected on the dct coefficients to take into account , namely the quantizer scale value , among other things , and thereby complete the mpeg2 coding . in addition , as a person of average skill in the art will appreciate , a fundamental task in many statistical analyses is to characterize the location and variability of a data set . also , further characterization of the data includes skewness and kurtosis . skewness is a measure of symmetry , and a data set , or distribution , is considered symmetric if it looks the same to the left and right of the center point . kurtosis is a measure of whether the data are peaked or flat relative to a normal distribution . data sets with high kurtosis tend to have a distinct peak near the mean , then decline rapidly , and have heavy tails . data sets with low kurtosis tend to have a flat top near the mean rather than a sharp peak . fig1 illustrates a graphical representation of the increase in the peak of probability density functions corresponding to an increase in kurtosis ( k ). the kurtosis for a standard normal distribution is three . as described hereinafter with reference to fig2 - 7 , the present invention incorporates the above - mentioned statistical analysis and mpeg - coding techniques in evaluating the video quality of pictures without the need for gaining access to the source picture . [ 0024 ] fig2 is a simplified block diagram of the inventive sharpness metric detector 10 comprising a segment module 12 , an edge detector 14 , a k estimator 16 , and an adder 18 for estimating the quality of the picture that has been gathered from the dct coefficients without the need for gaining access to the source picture . as shown in fig2 the digital image data , after being converted from analog video data , is forwarded to the sharpness metric detector 10 , which may represent , i . e ., a microprocessor , a central processing unit , a computer , a circuit card , an application - specific integrated circuit ( asics ). referring to fig3 the edge detector 14 is configured to create the edge profile of each input video frame . fig3 shows the original and edge images , and examples of possible block assignments . all edges whose frequency values are greater than a predetermined threshold are detected . note that the edge pixel values at the center of the transition from high to low , or vice versa , indicates the center of the transition . mathematically , the center corresponds to the maximum of the gradient ( or first derivative of the transition values ) and the null point of the second derivative . detecting edges in a video frame is well known in the art that can be performed in a variety of ways . see for example , j . canny , a computational approach to edge detection , ieee transactions on pattern analysis and machine intelligence , vol . pami - 8 , no . 6 , november 1986 , the content of which is hereby incorporated by reference . this article provides a detector that is capable of detecting edges while excluding weak edges often associated with mpeg - blocking artifacts and low - level noise . meanwhile , the segment module 12 subjects the input digital - image data into 8 × 8 pixel blocks and assigns each edge pixel to an 8 × 8 block . the block assignment may be done centering the edge pixels on the block , but it must be done without assigning an edge pixel to more than one block . the simplest embodiment uses the mpeg grid , i . e . 8 × 8 size with origin at ( 0 , 0 ). then , the k estimator 16 subjects each 8 × 8 block containing an edge image to dct processing in order to generate dct coefficients for ac frequency bands on each block of the edge profile . thus , for a given 2 - d image region , i . e ., an 8 × 8 pixel block , the corresponding 2 - d coefficients , f ( u , v ), are obtained . f ( u , v ) is then normalized , after excluding f ( 0 , 0 ), to form the bivariate probability - density function ( pdf ), p ( u , v ). finally , the k estimator 16 computes the 2 - d kurtosis on each block having the edge frequency profile of image blocks centered at edge pixel locations , as described mathematically hereinafter . let d ( u , v ) be an 8 × 8 block dct coefficient matrix . the distribution of the coefficients , excluding d ( 0 , 0 ), can be normalized to form a legitimate bivariate probability - density function ( pdf ), p ( x , y ), as follows : as a person of average skill in the art will appreciate , the classical measure of the non - gaussianity of a random variable , i . e . x , is kurtosis . kurtosis is a measure of the departure of a probability distribution from the gaussian ( normal ) shape . as shown in fig1 the kurtosis measure is zero for a gaussian variable , and greater than zero for most non - gaussian random variables . note that there are non - gaussian random variables that have zero kurtosis , but they can be considered rare . for a given random variable x with the mean μ x , the kurtosis is defined by : wherein m 4 and m 2 represent the fourth and second central moments , respectively ; and , m k = e [( x − μ x ) k ]= σ ( x − μ x ) k p ( x ), ( 3 ) where e denotes the probability expectation or the mean value of a random variable . p ( x ) = ∑ y p ( x , y ) , ( 4 ) where e denotes the probability expectation or the mean value of a random variable . moreover , if x 1 and x 2 are two independent random variables , then kurtosis has the following linearity property : furthermore , let w be a p - dimensional random vector ( i . e . w =[ w 1 , w 2 , . . . w p ]) with finite moments up to the fourth moments , and μ and γ be the mean vector and covariance matrix of w , respectively . then , the p - dimensional kurtosis can be represented as : β 2 . p = e [( w − μ ) t γ − 1 ( w − μ )] 2 , ( 7 ) finally , using the above equation ( 7 ) and with p = 2 , a random vector w =[ x , y ] t is applied to the fourier transform of the entire image . this result can be represented as follows : β 2 , 2 =[ γ 4 , 0 + γ 0 , 4 + 2γ 2 , 2 + 4ρ ( ργ 2 , 2 − γ 1 , 3 − γ 3 , 1 )]/( 1 − ρ 2 ) 2 , ( 8 ) γ k , l = ∑ i = 0 n ∑ j = 0 m ( x i - μ x ) k ( y i - μ y ) l p ( x i , y i ) ( ∑ i = 0 n ( x i - μ x ) 2 p ( x i ) ) k / 2 ( ∑ j = 0 m ( y i - μ y ) 2 p ( y i ) ) l / 2 ( 9 ) σ xy 2 = e [( x − μ x )( y − μ y )] ( 10 ), and note that the 2 - d kurtosis is a sharpness indicator for the entire m × n image , or any region within . however , there is a very important difference found according to the present invention . while the 2 - d kurtosis of the overall image decreases when the image becomes sharper , the kurtosis of the 8 × 8 blocks increases with sharpness . this effect is the result of the local frequency distribution near the edges . thus , for a given 2 - d image region f ( x , y ), i . e . an 8 × 8 pixel block , where m , n = 0 , 1 , . . . 7 , the corresponding 2 - d dct coefficients f ( u , v ) can be obtained , where u and v are the spatial frequencies . f ( u , v ) is then normalized , after excluding f ( 0 , 0 ), to form the bi - variate probability - density function , p ( u , v ). referring to fig4 the kurtosis of each 8 × 8 dct block having an edge profile of image blocks centered at edge pixel locations is calculated according to equation ( 8 ). then , for each block of 8 × 8 pixels with the edge profile therein , the number of pixels that cross the edge frequency profile , w , is determined . thereafter , the value of 2 - d kurtosis , k , of 8 × 8 block is multiplied by the corresponding w . note that the value of 2 - d kurtosis on each block with the edge profile ( w × k ) indicates the local kurtosis of the edge frequency profile and therefore it represents a local measure of sharpness . as such , the average value can indicate the sharpness measure for the whole frame . accordingly , after computing 2 - d kurtosis according to equation ( 8 ) on each block with the edge profile , the adder 18 averages the kurtosis over all 8 × 8 blocks having the edge profile , by adding ( w × k ) for each block with the edge profile divided by the total number of blocks with the edge profiles . furthermore , the average can be determined per frame or image , or as a running average over a certain time window to obtain different levels of sharpness measurement , which varies depending on the application . [ 0042 ] fig5 is a flow diagram depicting the operation steps of evaluating video quality in accordance with the embodiment of the present invention . it should be noted that the processing and decision blocks can represent steps performed by functionally equivalent circuits , such as a digital signal - processor circuit or an application - specific integrated circuit ( asic ). the flow diagrams do not depict the syntax of any particular programming language . rather , the flow diagrams illustrate the functional information that a person of ordinary skill in the art requires to fabricate circuits or to generate computer software to perform the processing required of the particular apparatus . upon receiving the input video frame in step 110 , an edge image for each input video frame is created using the edge detector 14 of fig2 in step 120 . then , each edge pixel is assigned to an 8 × 8 block using the segment module 12 of fig2 in step 140 . the 8 × 8 dct , f ( u , v ), is performed in step 160 , and normalized to obtain the pdf , p ( u , v ), in step 180 . thereafter , the 2 - d kurtosis calculation is performed on each block of the edge - frequency profile using the k estimator 16 of fig2 in step 200 . if all edge pixels have been processed in step 202 , the kurtoses are averaged over all 8 × 8 blocks in step 204 using the adder 18 of fig2 . as is apparent from the foregoing , the present invention has an advantage in that the sharpness metric system 10 uses the kurtosis of small regions enclosing the image edges , thus taking into account frequency characteristics as well as local spatial information . the resulting sharpness metric is not content - dependent , and by focusing on local kurtosis in edge regions , the present invention can avoid noise . it should be noted that many video applications , such as the focus control of the video imager , video - processing algorithm development , real - time video quality monitoring / control , and real - time quality control of the networked video can benefit from the teachings of the present invention . as the metric have a simple and generic methodology , it may serve as a real - time quality observer with three advantages . it has 1 ) systematic and consistent sharpness quality control , 2 ) is very inexpensive to employ and feasible for many real - time applications without human intervention , and 3 ) saves the human quality observers from many boring tasks . for example , fig6 - 8 are simplified block diagrams whereto the embodiment of the present invention is applied . referring to fig6 the sharpness detector 10 may be coupled to any type of video - generating device , such as an unsupervised camera or other video equipment that is capable of generating video data based on a particular image . referring to fig7 the video storage 22 may be any conventional video - storage medium known in this art . referring to fig8 the sharpness - metric detector may be implemented in video - capture operations , such as detection , coding , transmission , enhancement , etc ., such that properly - selected monitoring and control points can be used to install sharpness - control loops of different scopes . while the preferred embodiments of the present invention have been illustrated and described , it will be understood by those skilled in the art that various changes and modifications may be made , and equivalents may be substituted for elements thereof without departing from the true scope of the present invention . in addition , many modifications may be made to adapt to a particular situation and the teaching of the present invention without departing from the central scope . therefore , it is intended that the present invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out the present invention , but that the present invention include all embodiments falling within the scope of the appended claims . | 7 |
in order that the nature of the present invention may be more clearly understood details are given in the following particularly preferred embodiments relating to the equipment , materials and how the techniques of the invention are administered and data analyzed . the embodiments are not to be taken as limiting the scope of the invention . ultrasound equipment can be sonos 5500 , hewlett - packard ( andover , mass .) or equivalent . for example an hdi - 5000 by atl ultrasound was also found to be suitable . albumin microbubbles containing a mixture of air and perfluorocarbon gas ( optison ®, mallinckrodt medical , inc . st louis , mo .). this is as applied to the human forearm . details on the forearm procedure can be found in published work which is herein incorporated by reference ( 27 - 29 ) and details for the use of contrast enhanced ultrasound / microbubbles in skeletal muscle are based on its use to study myocardial blood flow ( 30 , 31 ). a ) in response to a defined dose of insulin infused intra - arterially . typically , in response to low doses of insulin 0 . 01 to 0 . 05 mu / min / kg infused locally into the brachial artery , plasma insulin rises by 70 - 350 pm in blood perfusing forearm muscle with little or no effect on the systemic insulin , glucose , ffa , catecholamines or amino acid concentrations ( 29 ). as a result , the isolated effect of local insulin on total blood flow into the arm and glucose balance across the arm can be measured . in addition , capillary recruitment in the forearm flexor muscle can be measured using ceu . total forearm blood flow is measured on each subject by two techniques : capacitance plethysmography and brachial artery ultrasound . for the doppler flow measurements , an ultrasound system ( sonos 5500 , hewlett - packard , andover , mass .) with a linear - array transducer is used with a transmit frequency of 7 . 5 mhz to allow 2 - d imaging of the brachial artery in the long axis . brachial artery diameter is measured 2 cm proximal to the tip of the arterial catheter at peak systole using on - line video calipers . a pulsed - wave doppler sample blood volume is placed at the same location in the center of the vessel and the mean brachial artery blood velocity measured using on - line angle correction and analysis software . brachial artery blood flow is calculated from 2 - d doppler ultrasound data using the equation : q = vπ ·( d / 2 ) 2 to measure capillary recruitment with ceu , a suspension of albumin microbubbles is infused intravenously in the contra - lateral arm while 2d imaging of the deep flexor muscles of the test forearm is performed ( fig1 ). fig1 illustrates the experimental setup for measuring total forearm flow using doppler ultrasound and forearm capillary recruitment using ceu as well as making glucose balance measurements across the forearm . measurement is made in a trans - axial plane 5 cm distal to be antecubital fossa , using an ultrasound system ( sonos 5500 ) capable of harmonic imaging . intermittent imaging is performed with ultrasound transmitted at 1 . 8 mhz and received at 3 . 6 mhz . once the systemic microbubble concentration reaches steady - state ( 1 - 1 . 5 min ), intermittent imaging is begun , at pulse intervals ranging from 1 to 15 seconds , thus allowing progressively greater replenishment of the ultrasound beam elevation between destructive pulses . three images are acquired at each pulse interval . additional images are acquired with the same beam characteristics at a 30 hz sampling rate , at which there is replenishment of microbubbles only in vessels with very rapid flow , and these were used as background images . data are recorded digitally and analyzed using custom - designed software described elsewhere ( 32 ). averaged background frames ( acquired at a 30 hz frame rate ) are digitally subtracted from the averaged frames acquired at each pulsing interval . mean video intensity in the region of interest is measured from the background - subtracted images . pulsing interval vs . video intensity plots are generated and fitted to an exponential function : y = a ( 1 − e − βt ). where y is the video intensity at a pulsing interval t , a is the plateau video intensity representing microvascular blood volume , and β is the rate constant reflecting the rate of rise of video intensity ( and mean microbubble velocity , or microvascular flow velocity ) ( 32 , 33 ) ( fig2 ). fig2 illustrates in more detail how the microvascular blood volume or capillary volume and microvascular flow velocity are determined using ceu . fig2 a illustrates the successive filling of a capillary over time after all microbubbles in the capillary have been lysed by a high energy harmonic ultrasound pulse . as the delay time prior to signal detection increases ( t 0 through t5 ) the number of microbubbles and hence the videointensity increases . fig2 b plots this data for typical signals collected over forearm muscle . the tangent to the upward sloping hyperbolic function is a measure of the rate of microvessel filling ( mvfv ) while the asymptote that intercepts the y - axis is a measure of the maximal signal seen when the vessels are filled and is determined by the microvascular volume ( mvv ) i . e . capillary volume . in order to derive values for the mvfv and mvv , the time versus video intensity plots are fitted to the function : y = a ( 1 − e βt ), where y is the video intensity at time t , a is the plateau intensity which represents mvv , and β is the time constant of rise and reflects velocity . fig2 c is a typical experiment done before ( open circles ) and after ( filled circles ) infusing insulin ( 3 mu / min / kg ) to an anesthetized rat . the plateau videointensity ( a ) is clearly higher , with no change in the rate of microvascular filling ( β ). typical data for normal healthy subjects are shown in fig3 . shown here are the changes in microvascular blood volume ( fig3 a ) and microvascular flow velocity or β ( fig3 b ) in the insulin infused and contralateral human forearm of 7 subjects at basal and at 4 hrs of a 0 . 05 mu / min / kg brachial artery insulin infusion . * indicates p values significantly different from basal 0 . 05 . typical data for lean normal and obese subjects are compared in fig4 . in healthy humans high insulin concentrations increase muscle blood flow ( measured as total limb flow ). in states of insulin resistance , such as type 2 diabetes , obesity and hypertension , this vasoactive action of insulin is reported to be diminished . obesity is associated with resistance to insulin - mediated glucose disposal and diminished skeletal muscle capillary density by histology . whether physiologic insulin concentrations enhance muscle glucose metabolism by effects on muscle vasculature , and whether insulin &# 39 ; s vascular actions are blunted by insulin resistant states , such as obesity , is controversial . all previous studies of the vascular effects of insulin have relied on measurements of total blood flow . contrast ˜ enhanced ultrasound ( ceu ) combines ultrasound imaging with infusion of albumin - coated microbubbles and allows measurement of capillary blood volume in vivo in humans . combining ceu with an established forearm perfusion method , we compared the effects of physiologic levels of insulin on total blood flow , microvascular blood volume and flow velocity , and glucose uptake in lean and obese subjects . methods : subjects :— 11 lean healthy adults ( 23 . 8 ± 0 . 8 kg / m 2 bmi , 29 ± 2 years old ) and 6 obese healthy adults ( 34 . 6 ± 1 . 8 kg / m 2 bmi , 39 ± 3 years old ). ceu estimation of microvascular blood volume ( mbv ) and flow velocity ( mbv ) in forearm skeletal muscle measured by video intensity . catheter placement in brachial artery in one forearm for insulin infusion and deep retrograde antecubital vein for blood sampling . net glucose metabolism is measured over time by arterio - venous concentration difference multiplied by total blood flow . protocol : insulin was infused intra - arterially at a rate of 0 . 05 mu / min / kg for 4 hours . brachial artery and bilateral deep venous blood samples were obtained at baseline and post - insulin infusion for measurements of glucose , lactate , oxygen saturation and insulin levels . doppler u / s measured total blood flow . mbv and mbf were assessed using ceu . in lean individuals , physiologic hyperinsulinemia increases microvascular blood volume suggesting evidence of capillary recruitment in forearm skeletal muscle . this action of insulin can occur without significant changes in total blood flow . in insulin - resistant obese individuals , this action of insulin is absent . b ) in response to a standard meal which in healthy individuals raises the insulin levels 34 fold above the pre - meal level . leg glucose uptake increases at least four fold by 30 minutes after the meal ( 34 ), which consists of pizza ( 8 . 5 kcal / kg body weight , containing 75 g as carbohydrate , protein 37 g and fat 17 g ). other details are as above in a ). c ) in response to a defined amount of exercise . the forearm is exercised by contracting to 75 % maximum using a digital grip strength dynamometer ( takei scientific co ) 12 times each minute for 2 minutes , then 3 times each minute for the next 20 min . during the last 10 min , quadruplicate blood samples , total blood flow and ceu measurements are repeated as at basal in both forearms . this leads to a 3 - fold increase in forearm total blood flow . other details are as above in a ). typical data for a lean normal subject engaged in exercising the forearm are shown in fig5 and 6 . referring to fig5 , in healthy humans exercising the forearm increases muscle blood flow , measured as total brachial artery flow . the increase in flow is proportional to the level of exertion , being greatest at 80 % of maximum . capillary recruitment is evidenced by increased ceu signal shown in fig6 . referring to fig6 , in the same healthy humans as in fig5 , microvascular blood volume measured by ceu , increases maximally even at the lowest level of exertion that was tested ( 25 %). these data confirm that ceu detects changes in capillary recruitment consistent with the known physiology of exercise . comparing fig3 and 6 indicate that exercise and insulin have similar effects to increase capillary recruitment as measured by ceu , although the exercise effect is the greater . d ) in response to a drug intended and designed to act specifically by increasing skeletal muscle capillary blood flow . these will be taken by the normal oral route and intended to achieve the afore - mentioned effect on muscle capillary blood flow acutely ( within 20 - 60 minutes ). a number of responses were recorded on normal healthy male and female individuals at various ages . this provided a reference set of data which reflects a normal response to the defined dose of insulin and the defined exercise routine for each sex at each age . the male response could reasonably be expected to be larger than that of females at each age . however , the response would be expected to decline with age after about forty . individuals considered to have muscle insulin resistance showed reduced responses to the defined dose of insulin and the standard meal without change to the response to exercise . this group would include type 1 and 2 diabetics , hypertensives , and the obese (& gt ; 30 body mass index ). critical care patients would show markedly decreased responses to all three , defined insulin dose , standard meal , and defined exercise regimen . the efficacy of drugs intended to ameliorate skeletal muscle insulin resistance by specifically acting to increase capillary recruitment or by enhancing insulin &# 39 ; s action to do this , will increase the response determined by ceu to the defined insulin dose , the standard meal , but not to the exercise regimen . little or no effect is expected by these drugs in normal healthy individuals . any discussion of references , documents , acts , materials , devices , articles or the like which has been included in the present specification is solely for the purpose of providing a context for the present invention . it is not to be taken as an admission that any or all of these matters form part of the prior art base or were common general knowledge in the field relevant to the present invention as it existed in australia before the priority date of each claim of this application . any such references are herein incorporated in the application . it will be appreciated by persons skilled in the art that numerous variations and / or modifications may be made to the invention as shown in the specific embodiments without departing from the spirit or scope of the invention as broadly described . the present embodiments are , therefore , to be considered in all respects as illustrative and not restrictive . baron a d , laakso m , brechtel g , edelman s v : mechanism of insulin resistance in insulin dependent diabetes mellitus : a major role for reduced skeletal muscle blood flow . j . clin . endocrinol . metab . 73 : 637 - 643 , 1991 baron a d , steinberg h , brechtel g , johnson a : skeletal muscle blood flow independently modulates insulin - mediated glucose uptake . am j physiol 266 : e248 - e253 , 1994 baron a d : insulin and the vasculature - old actors , new roles . j investig . med . 44 : 406 - 412 , 1996 utriainen j , malmstrom r , makimattila s , yki - jarvinen h : methodological aspects , dose - response characteristics and causes of interindividual variation in insulin stimulation of limb blood flow in normal subjects . diabetologia 38 : 555 - 564 , 1995 laine h , yki - jarvinen h , kirvela o , tolvanen j , raitakari m , solin o , haaparanta m , knnuti j , nuutila p : insulin resistance of glucose uptake in skeletal muscle cannot be ameliorated by enhancing endo yki - jarvinen h , utriainen t : insulin - induced vasodilatation : physiology or pharmacology ? diabetologia 41 : 369 - 379 , 1998 scherrer u , randin d , vollenweider p , vollenweider l , nicod , p : nitric oxide release accounts for insulin &# 39 ; s vascular effects in humans . j . clin . invest . 94 : 2511 - 2515 , 1994 vollenweider l , tappy l , owlya r , jequier e , nicod p , scherrer u : insulin - induced sympathetic activation and vasodilation in skeletal muscle . diabetes 44 : 641 - 645 , 1995 natali a , bonadonna r , santoro d , galvan a , baldi s , frascerra s , palombo c , ghione s , ferrannini e . insulin resistance and vasodilation in essential hypertension . j clin invest 94 : 1570 - 1576 , 1994 sarabi m , lind l , millgard j , hanni a , hagg a , berne c , lithell h : local vasodilatation with metacholine , but not with nitroprusside , increases forearm glucose uptake . physiol res 48 : 291 - 295 , 1999 clark m g , colqhuoun e q , rattigan , s , dora k a , eldershaw t p d , hall j l & amp ; ye j . vascular and endocrine control of muscle metabolism . am . j . physiol . 268 : e797 - e812 , 1995 . clark m g , rattigan s , dora k a , newman j m b , steen j t , miller k a & amp ; vincent m a . vascular and metabolic regulation of muscle . in : physiology , stress and malnutrition ( kinney j m & amp ; tucker h , eds ). lippincott - raven : new york , pp . 325 - 346 , 1997 . baron a d & amp ; clark m g . role of blood flow in regulating glucose metabolism . ann . rev . nutr . 17 : 487 - 499 , 1997 . clark m g , rattigan s , dora k a , newman j m b & amp ; vincent m a . interaction between blood flow , metabolism and exercise . in : biochemistry of exercise x ( hargreaves m , ed .). human kinetics : champaign , pp . 3546 , 1998 . clark m g , newman j m b & amp ; clark a d h . microvascular regulation of muscle metabolism . in : nutrition in the icu : curr . opin . nutr . metab . care 1 : 205 - 210 , 1998 . clark m g , rattigan s , clerk l h , vincent m a , clark a d h , youd j m & amp ; newman j m b . nutritive and non - nutritive blood flow : rest and exercise . acta physiol . scand . 168 : 519 - 530 , 2000 . clark m g , clerk l h , newman j m b & amp ; rattigan s . interaction between metabolism and flow in tendon and muscle . scand . j . med . sci . sports , 10 : 338 - 345 , 2000 clark m g , barrett e j , wallis m g , vincent m a & amp ; rattigan s . the microvasculature in insulin resistance and type 2 diabetes . seminars in vascualr medicine . 2 : 21 - 31 , 2002 . rattigan s , dora k a , colquhoun e q & amp ; clark m g . serotonin - mediated acute insulin resistance in the perfused rat hindlimb but not in incubated muscle : a role for the vascular system . life sci . 53 : 1545 - 1555 , 1993 . rattigan s , appleby g j , miller k a , steen j t , dora k a , colquhoun e q & amp ; clark m g . serotonin inhibition of 1 - methylxanthine metabolism parallels its vasoconstrictor activity and inhibition of oxygen uptake in perfused rat hindlimb . acta physiol . scand . 161 : 161 - 169 , 1997 . jarasch e d , bruder g , heid h w : significance of xanthine oxidase in capillary endothelial cells . acta physiol . scand . suppl . 548 : 39 - 46 , 1986 youd j m , newman j m b , clark m g , appleby g j , rattigan s , tong a c y & amp ; vincent m a . increased metabolism of infused 1 - methylxanthine by working muscle . acta physiol . scand . 166 : 301 - 308 , 1999 . rattigan s , clark m g & amp ; barrett e j . haemodynamic actions of insulin in rat skeletal muscle : evidence for capillary recruitment . diabetes , 46 : 1381 - 1388 , 1997 . rattigan s , clark m g & amp ; barrett e j . acute vasoconstriction - induced insulin resistance in vivo in rat muscle . diabetes , 48 : 564 - 569 , 1999 . vincent m a , dawson d , clark a d h , lindner j , rattigan s , clark m g , kaul s , barrett e j . physiologic hyperinsulinemia rapidly recruits capillaries in rat skeletal muscle in vivo . diabetes submitted , 2000 coggins m p , fasy e , lindner j , jahn l , kaul s , barrett e j . physiologic hyperinsulinemia increases skeletal muscle microvascular blood volume in healthy humans ( abstract ). diabetes 48 : supplement : a220 , 1999 . barrett e , fryburg d , louard r , gelfand r , mcnulty p , young l . use of regional catherization methods to study the regulation of muscle protein metabolism . in : nair k , editor . protein metabolism in diabetes mellitus . great britain : smith - gordon ; 1992 . p 91 - 100 . fryburg d a , jahn l a , hill s a , oliveras d m , barrett e j . insulin and insulin - like growth factor - i enhance human skeletal muscle protein anabolism during hyperaminoacidemia by different mechanisms . journal of clinical investigation 96 : 1722 - 1729 , 1995 . louard r j , fryburg d a , gelfand r a , barrett e j . insulin sensitivity of protein and glucose metabolism in human forearm skeletal muscle . journal of clinical investigation 90 : 2348 - 2354 , 1992 . jayaweera a r , kaul s . quantifying myocardial blood flow with contrast echocardiography . american journal of cardiac imaging 7 ( 4 ): 317 - 35 , 1993 . wei k , jayaweera a r , firoozan s , linka a , skyba d m , kaul s . quantification of myocardial blood flow with ultrasound - induced destruction of microbubbles administered as a constant venous infusion . circulation 97 ( 5 ): 473 - 83 , 1998 wei k , skyba d m , firschke c , jayaweera a r , lindner j r , kaul s . interactions between microbubbles and ultrasound : in vitro and in vivo observations . journal of the american college of cardiology 29 ( 5 ): 1081 - 8 , 1997 . wei k , kaul s . recent advances in myocardial contrast echocardiography . current opinion in cardiology 12 ( 6 ): 539 - 46 , 1997 capaldo b , gastaldelli a , antoniello s , auletta m , pardo f , ciociaro d , guida r , ferrannini e , sacca l . ( 1999 ) splanchnic and leg substrate exchange after ingestion of a natural mixed meal in humans . diabetes 48 : 958 - 966 . | 0 |
the present system introduces a preferred mechanism for storing and dispensing items in a vending machine or automated retail store . it is preferably used in conjunction with an isolated and centralized robotic dispensing system that can support multiple inventory areas and technologies within those areas . the present system provides the capability to handle inventory of a wide range of form factors in size and shape , in a wide range of configurations . it also provides the ability to easily change the inventory configuration without any special tools quickly , efficiently and inexpensively . there is great value in having a flexible inventory storage and dispensing mechanism that is easily reconfigured in the field by hand and with a standardized set of inexpensive parts . some of the value adds include a wider range of products that can be accommodated without system redesign , decrease of development risks , decrease in costs associated with changes in merchandising and far fewer limits to merchandise / merchandising . in addition , the re - use of components to build and configure the inventory system lowers the amount of pieces that have to be manufactured , distributed and stored . inventory trays can be configured to fit merchandise of varying form factors and still use common pieces without any special tools or new parts saving cost and configuration time . inventory solutions can be updated and reconfigured to work with the central dispensing mechanism without significant customization of the dispensing mechanism , allowing for rapid accommodation of new types and amounts of merchandise for purchase or promotion . the flexibility in the inventory system also enables products to be oriented in the most efficient direction in order to increase the density of merchandise and optimize efficiency in the supply chain ( hypothetically decreasing the amount of stocking trips to the machine given greater capability to accommodate inventory units ). in addition , the flexibility of the inventory system permits items of greater popularity to be stocked at a greater density than less popular items . the importance of increasing the flexibility and field - based reconfigurability of the system by a layperson is that the technology is more capable of handling the quick changes that occur in retail merchandising within discretionary , or trend areas . in other words , the inventory system is able to change with retail dynamics and facilitate merchandising the most popular products without limitations imposed by existing inventory systems on the market today . the inventory system is flexible enough to accommodate a machine full of what has been designated by brand manufacturers as a “ product sample or sachet or trial size ” of a product . typically this unit will come in two form factors , a thin foil packaged sachet , or a vial mounted on a small piece of cardboard . other form factors could include small cylinders or boxes . the inventory system accommodates a wide universe of samples and full size products . the machine could also be reconfigured to accommodate all sample sizes , or all full sizes of the products ( as long as the full sizes met the size requirements ). in addition , due to the robust and flexible divider design and connection with the robotics system , items that are odd - sized will typically not necessitate secondary packaging . the system goes further than existing inventory offerings to accommodate odd , bulky , squishy , irregularly surfaced or weighted items without hypothetically requiring secondary packaging ( boxing ) of these items . for purposes of disclosure , the following co - pending u . s . utility applications , which are owned by the same assignee as in this case , are hereby incorporated by references , as if fully set forth herein : ( a ) pending u . s . utility application ser . no . 12 / 589 , 277 , entitled “ interactive and 3 - d multi - sensor touch selection interface for an automated retail store , vending machine , digital sign , or retail display ,” filed oct . 21 , 2009 , by coinventors mara segal , darrell mockus , and russell greenberg , that was based upon a prior pending u . s . provisional application , ser . no . 61 / 107 , 829 , filed oct . 23 , 2008 , and entitled “ interactive and 3 - d multi - sensor touch selection interface for an automated retail store , vending machine , digital sign , or retail display ”; ( b ) pending u . s . utility application ser . no . 12 / 589 , 164 , entitled “ vending machines with lighting interactivity and item - based lighting systems for retail display and automated retail stores ,” filed oct . 19 , 2009 by coinventors mara segal , darrell mockus , and russell greenberg , that was based upon a prior pending u . s . provisional application , ser . no . 61 / 106 , 952 , filed oct . 20 , 2008 , and entitled “ lighting interactivity and item - based lighting systems in retail display , automated retail stores and vending machines ,” by the same coinventors ; and , ( c ) pending u . s . utility application ser . no . 12 / 798 , 803 , entitled “ customer retention system and process in a vending unit , retail display or automated retail store ” filed apr . 12 , 2010 , by coinventors mara segal , darrell mockus , and russell greenberg , that was based upon a prior pending u . s . provisional application , ser . no . 61 / 168 , 838 filed apr . 13 , 2009 , and entitled “ customer retention system and automated retail store ( kiosk , vending unit , automated retail display and point - of - sale )”, by coinventors darrell scott mockus , mara segal and russell greenberg . ( d ) pending u . s . utility application ser . no . 12 / 806 , 862 , entitled “ modular vending with centralized robotic gantry ” filed aug . 23 , 2010 , by coinventors darrell mockus , mara segal , and russell greenberg , that was based upon a prior pending u . s . provisional application , ser . no . 61 / 237 , 604 filed aug . 27 , 2009 , and entitled “ system and method for dispensing items in an automated retail store or other self - service system ( including vending and self - service check - out or kiosk platforms )”: by co - inventors darrell scott mockus , mara segal and russell greenberg , and priority based on said application is claimed . with initial reference directed to fig1 a - 1i of the appended drawings , a inventory storage and dispensing module 100 is adapted to be integrated into a vending machine or automated retail store . a housing 101 contains a conveyor 102 that is driven by motor 103 . the motor 103 drives the conveyor 102 towards ramp 104 that facilitates the delivery of items stored on the conveyor 102 . fig1 b shows an isometric exploded view of the base inventory module . conveyor 102 is made up of a series of conveyor pieces 105 ( see fig1 d ) and divider pieces 106 ( see fig1 e ). the conveyor 102 slides on smooth rub strips 107 that reduce friction . these are mounted to conveyor support 108 that sits in housing 101 to provide support for conveyor 102 . the conveyor 102 is driven by motor 103 that is mounted in motor bracket 109 and connected directly to pulley 110 . this pulley connects to the drive pulley 111 via belt 112 . a shaft 113 goes through pulley 111 and drive gear 114 and rides on two press - fit bearings 123 . the wiring for the motor 103 and stop switch 122 is routed out the housing through grommet 115 through e clips 116 and 117 secured to the shaft 113 . the other end of the conveyor 102 rides on another gear 114 . an optional hook 118 that is part of the housing 101 that will insert into a slot on the tray shelf 171 ( see fig1 i ) to secure it . these hooks 118 can be added or removed during manufacturing . hole 125 provides an additional or alternative way to fasten the dispensing module 100 or lane to a tray . a screw such as a ia ″ is inserted through the hole into a threaded component on the tray 171 holding the dispensing module 100 in place . there is an additional hole ( not pictured ) towards the back of the dispensing module 100 that secures the other end of the dispensing module 100 . shaft 119 is inserted through the gear and rides on two press - ft bearings 124 pressed into housing 101 and secured by e clips 120 and 121 . stop switch 122 is mounted to housing 101 . fig1 c shows a side view of the base inventory dispensing module 100 . in this view , the flag post of part 106 ( fig1 e ) can be seen activating stop switch 122 which sends the signal that the conveyor has advanced enough to properly dispense a product down ramp 104 . fig1 d shows a number of detailed illustrations of conveyor piece 105 ( fig1 b ) from different angles . 105 a is an angled elevation of the conveyor piece . slots 130 exist at either side of the conveyor piece allowing the stop flag tabs 141 of the divider part 106 ( fig1 e ) to extend though the conveyor piece 105 . a slot 131 receives the divider connection tab 142 ( fig1 e ). male tab 132 and female tabs 133 allow conveyor pieces 105 to be strung together in any length . this flexibility allows the conveyor 102 to grow or contract to any size required . 105 b is a bottom elevation of the conveyor piece 105 . in this view , the alignment of the male connection tabs 132 can be seen in relation to the female connection tabs 133 . 105 c shows the side elevation of the conveyor piece 105 and the vertical alignment of male connection tabs 132 with female connection tabs 133 . 105 d shows a cross - sectional side view of the conveyor piece 105 . fig1 e shows a number of detailed illustrations of divider piece 106 ( fig1 b ) from different angles . the divider piece 106 fits into conveyor piece 105 ( fig1 d ) providing the ability to create a dividing separation at any distance in increments of the conveyor depth . this feature provides great flexibility in adjusting the conveyor 102 on - site in the field to accommodate different inventory . this process requires no tools and can be accomplished while the conveyor is installed in the machine . fork tabs 140 facilitate the handoff from the conveyor 102 to a receiving area . the fork tabs 140 pass through the ramp 104 ( fig1 a and 1b ) to provide a smooth item handoff . the motor stop flag tabs 141 fit through slots 130 ( fig1 d ) in the conveyor piece 105 . these tabs 141 activate the stop motor switch 122 ( fig1 c ) as they pass over the switch 122 . this signals the application that the conveyor 102 has dispensed one item and to stop rotating the motor 103 . connection tab 142 fits into slot 131 in the conveyor piece ( fig1 d ) securing the divider 106 to the conveyor piece 105 . the connection tab 142 includes two outwardly biased prongs each with a first ramped surface to introduce the tab 142 into the slot 130 and a second ramped surface to releasably retain the tab 142 in the slot 13 . the second ramped surface is preferably configured at a steeper angle to the longitude axis of the tab 142 than the first ramped surface . fig1 f shows an alternate configuration of the conveyor 102 illustrated in fig1 a through 1e . here , the majority of the same components are used to create a dispensing module 150 that can hold larger products . by using a different motor bracket 156 , axels 154 and 155 and housing 151 , the same inventory design can be adjusted to handle items of any size ( illustrated in fig1 g ). conveyors 102 fit inside a larger housing 151 . a wider forked ramp 152 helps guide dispensed products into a collection area . fig1 g shows an isometric exploded view of the dispensing module 150 in fig1 f . this figure illustrates the similar components used and the ones that are modified to fit the larger housing 151 . there is a larger mounting bracket 153 that supports the conveyor . a larger shaft 154 houses two gears 114 that drive the conveyors 102 . a larger shaft 155 holds the gears 114 that secure the other ends of the conveyors . a longer motor bracket 156 positions the motor 103 at the right position to drive the assembly . fig1 h shows another alternate configuration of the inventory assembly . a different housing 161 is used that contain two conveyors 102 that are side by side . a different fork ramp 162 is used that fits the housing . fig1 i shows several conveyor lanes , i . e ., dispensing modules 100 and 150 mounted on a shelf or inventory tray 171 in a support structure 170 . conveyor lanes 100 and 150 are shown affixed to an inventory tray 171 , which are affixed to c - channel upright side supports 172 . a rail support 173 spans the c - channel upright side support 172 and fits into holes 174 and notches 175 . ( rail support on other side not shown ). the rail supports 173 can be placed in any of the holes and notches so they shelves can adjust to any height without any tools . with additional reference directed to fig2 a and 2b , a vending machine constructed in accordance with the best mode of the present system has been generally designated by the reference numeral 200 ( fig2 a ). much of the hardware details are explained in the aforementioned pending applications that have been incorporated by reference herein . display module 210 can be attached with a hinge to an inventory area covered by control panel 211 , comprised of a rigid upright cabinet , or the module 210 can be mounted to a solid structure as a stand - alone retail display . the display module 210 forms a door hinged to an adjacent cabinet such as an inventory cabinet 212 a adjacent gantry 230 that is covered by control panel 211 . a variety of door configurations can be employed . for example , the display modules 210 can be smaller or larger , and they can be located on one or both sides of the control panel 211 . the display doors can have multiple square , oval , circular , diamond - shaped , rectangular or any other geometrically shaped windows . alternatively , the display area can have one large display window with shelves inside . a customizable , lighted logo area 201 ( fig2 a ) is disposed at the top of control panel 211 . touch screen display 202 is located below area 201 . panel 203 locates the machine payment system , coin acceptor machine or the like . additionally panel 203 can secure a receipt printer , keypad , headphone jack , fingerprint scanner or other access device . the product retrieval area 204 is disposed beneath the panel 203 in a conventional collection area compartment ( not shown ). a key lock 205 , which can be mechanical or electrical such as a punch - key lock , is disposed beneath the face of the display module 210 . one or more motion sensors 214 are disposed within smaller display tubes within the display module 210 interior . a plurality of generally circular product viewing areas 207 and a plurality of generally diamond shaped viewing areas 206 are defined upon the outer the face of the casing 208 that are aligned with internal display tubes behind the product viewing surface areas , though the shape of the viewing areas may alter with various merchandising concepts . however , the convention of framing merchandising offerings is consistent to enable intuitive interfacing whether a physical or virtual representation of the merchandise display . an exterior antenna 209 connects to a wireless modem inside the machine providing connectivity . inventory shelves 213 may be mounted in the inventory cabinet 212 . these inventory shelves 213 may contain any mechanism such as the dispensing modules 100 and 150 discussed above or other conveyors or spiral vending systems as long as they can push a product off the edge of the inventory tray . speakers 215 are mounted in the panel 211 . a camera 216 capable of capturing video and still images is also mounted in the panel 211 . the machine components are set on casters 217 with feet that can be retracted for moving or lowered to position a machine in a deployed location . fig2 b shows a standard configuration of the assembly . the robotized modular gantry 230 is shown connected to an inventory cabinet 212 a by bolting the upright c - channel structures 232 of the modular gantry 230 to upright c - channel beams 219 which are then affixed to the upright c - channel structures 220 of the inventory cabinet 212 a using additional bolts . power and controls are routed to the modular gantry 230 via a wiring harness ( not depicted ) located on the bottom of the modular gantry 230 . the cpu and power supplies ( detailed in fig4 and 5 ) are located in the bottom of the main inventory cabinet that is attached to a modular gantry 230 . a second inventory cabinet 2128 can also be attached to the other side of the robotized modular gantry 230 using the same method of bolting the upright supports of the inventory cabinets 220 and the upright supports 232 of the gantry 230 to a common upright c - channel support 219 . display modules 210 can be attached to the inventory cabinets via a piano hinge 218 running the full height of the door . the necessary electrical and control wiring connects via a wiring harness 221 located on the interior of the inventory cabinet near the hinge connection . these piano style hinges are located on the exterior corners of the inventory cabinets . they are covered with simple metal paneling if they are not in use . the control panel 211 is attached in a similar manner using a piano hinge 218 . the necessary electrical and control wiring connect to a wiring harness located in the interior of the control panel 211 ( wiring harness not depicted ). with primary reference directed to fig3 , a system consisting of a plurality of automated retail machines connected via a data connection to a centralized , backend operations center system has been designated by the reference numeral 300 . at least one automated retail machine 301 is deployed in a physical environment accessible by a consumer who can interact with the machine 301 directly . there can be any number of machines 301 , all connected to a single , remote logical operations center 330 via the internet 320 ( or a private network ). the operations center 330 can physically reside in a number of locations to meet redundancy and scaling requirements . the machine software is composed of a number of segments that all work in concert to provide an integrated system . logical area 302 provides the interface to deal with all of the machine &# 39 ; s peripherals such as sensors , keypads , printers and touch screen . area 303 handles the monitoring of the machine and the notifications the machine provides to administrative users when their attention is required . area 304 controls the reporting and logging on the machine . all events on the machine are logged and recorded so they can be analyzed later for marketing , sales and troubleshooting analysis . logical area 305 is responsible for handling the machine &# 39 ; s lighting controls . logical area 306 is the inventory management application . it allows administrative users on location to manage the inventory . this includes restocking the machine with replacement merchandise and changing the merchandise that is sold inside the machine . administrative users can set the location of stored merchandise and the quantity . logical area 307 is the retail store application . it is the primary area that consumers use to interface with the system . logical area 308 handles the controls required to physically dispense items that are purchased on the machine or physically dispense samples that are requested by a consumer . this area reads the data files that tell the machine how many and what types of inventory systems are connected to the machine . logical area 309 controls the inventory management system allowing authorized administrative users to configure and manage the physical inventory in the machine . area 310 controls the payment processing on the machine . it manages the communication from the machine to external systems that authorize and process payments made on the machine . area 311 is an administrative system that allows an authorized user to manage the content on the machine . this logical area handles the virtual administrative user interface described previously . the content can consist of text , images , video and any configuration files that determine the user &# 39 ; s interaction with the machine . the latter applications interface with the system through an application layer designated in fig3 by the reference numeral 312 . this application layer 312 handles the communication between all of these routines and the computer &# 39 ; s operating system 313 . layer 312 provides security and lower level messaging capabilities . it also provides stability in monitoring the processes , ensuring they are active and properly functioning . logical area 331 is the user database repository that resides in the operations center 330 . this repository is responsible for storing all of the registered user data that is described in the following figures . it is logically a single repository but physically can represent numerous hardware machines that run an integrated database . the campaign and promotions database and repository 332 stores all of the sales , promotions , specials , campaigns and deals that are executed on the system . both of these databases directly interface with the real - time management system 333 that handles real - time requests described in later figures . logical area 334 aggregates data across all of the databases and data repositories to perform inventory and sales reporting . the marketing management system 335 is used by administrative marketing personnel to manage the marketing messaging that occurs on the system ; messages are deployed either to machines or to any ecommerce or digital portals . logical area 336 monitors the deployed machines described in fig2 , and provides the tools to observe current status , troubleshoot errors and make remote fixes . logical area 337 represents the general user interface portion of the system . this area has web tools that allow users to manage their profiles and purchase products , items and services . the content repository database 338 contains all of the content displayed on the machines and in the web portal . logical area 339 is an aggregate of current and historical sales and usage databases comprised of the logs and reports produced by all of the machines in the field and the web portals . fig4 and 5 illustrate system wiring to interconnect with a computer 450 such as advantech &# 39 ; s computer engine with a 3 ghz cpu , 1 gb of ram memory , 320 gb 7200 rpm hard disk drive , twelve usb ports , at least one serial port , and an audio output and microphone input . the computer 450 ( fig4 ) communicates to the lighting system network controller via line 479 . through these connections , the lighting system is integrated to the rest of system . power is supplied through a plug 452 that powers an outlet 453 , which in turn powers a ups 454 such as triplite &# 39 ; s ups ( 900 w , 15 va ) ( part number smart1500lcd ) that conditions source power , which is applied to input 455 via line 456 . power is available to accessories through outlet 453 and ups 454 . computer 450 ( fig4 ) is interconnected with a conventional payment reader 458 via cabling 459 . a pin pad 485 such as sagem denmark int1315 - 4240 is connected to the cpu 450 via a usb cable . an optional web - accessing camera 461 such as a logitech webcam ( part number 961398 - 0403 ) connects to computer 450 via cabling 462 . audio is provided by transducers 464 such as happ controls four - inch speakers ( part number 49 - 0228 - 00r ) driven by audio amplifier 465 such a happ controls kiosk 2 - channel amplifier with enclosure ( part number 49 - 5140 - 100 ) with approximately 8 watts rms per channel at 10 % thd with an audio input though a 3 . 5 mm . stereo jack connected to computer 450 . a receipt printer 466 such as epson &# 39 ; s eu - t300 thermal printer connects to the computer 450 via cabling 467 . the printer is powered by a low voltage power supply such as epson &# 39 ; s 24 vdc power supply ( part number ps - 180 ). a remote connection with the computer 450 is enabled by a cellular link 470 such as multitech &# 39 ; s verizon cdma cellular modem ( part number mtcba - c - ip - n3 - nam ) powered by low voltage power supply 472 . the cellular link 470 is connected to an exterior antenna 209 . a touch enabled liquid crystal display 474 such as a ceronix 22 ″ widescreen ( 16 : 10 ) touch monitor for computer operation also connects to computer 450 . a bluetooth adapter 487 such as d - link &# 39 ; s dbt - 120 wireless bluetooth 2 . 0 usb adapter is attached to the cpu allowing it to send and receive bluetooth communication . a wireless router 488 such as cisco - linksys &# 39 ; wrt61 on simultaneous dual - n band wireless router is connected to the cpu to allow users to connect to the machine via a private network created by the router . digital connections are seen on the right of fig4 . gantry - y ( conveyor elevator ), stepper motor controller such as the arcus advanced motion driver + controller usb / rs485 ( part number arcus ace - sde ) connection is designated by the reference numerals 476 . connection 477 connects to the conveyor motor controller which can also be something similar to an arcus advanced motion driver + controller usb / rs485 ( part number arcus ace - sde ). dispenser control output is designated by the reference numeral 478 which operates the product collection wings motor on the gantry 230 . the led lighting control signals communicate through usb cabling to a dmx controller 479 that transmits digital lighting control signals in the rs - 485 protocol to the display tube lighting circuit board arrays . an enttec - brand , model dmx usb pro 512 i / f controller is suitable . cabling 480 leads to vending control . one or more inventory systems can be connected to the vending control depending on the configuration . dispenser door control is effectuated via cabling 481 . façade touch sensor inputs arrive through interconnection 482 . motion sensor inputs from a motion sensor such as digi &# 39 ; s watchport / d ( part number watchport / d 301 - 1146 - 01 ) are received through connection 483 . a usb connection connects the product weight sensor 484 such as sartorius ( part number ff03 vf3959 ) that is located in the collection area to determine the presence of a dispensed item . fig5 illustrates a detailed power distribution arrangement 500 . because of the various components needed , power has to be converted to different voltages and currents throughout the entire system . the system is wired so that it can run from standard 110 v . a . c . power used in north america . it can be converted to run from 220 v . a . c . for deployments where necessary . power from line - in 455 supplied through plug 452 ( fig4 ) powers a main junction box 453 with multiple outlets ( fig4 ) that powers ups 454 which conditions source power , and outputs to computer 450 line 456 . power is available to accessories through main junction box 453 and ground - fault current interrupt ac line - in 455 . an additional ac outlet strip 501 such as triplite &# 39 ; s six position power strip ( part number tlm606nc ) powers led lighting circuits 502 and a touch system 503 . power is first converted to 5 volts to run the lighting board logic using a converter 540 . another converter , 541 , converts the ac into 24 volt power to run the lights and touch system . an open frame power supply 505 ( fig5 ) provides 24 vdc , 6 . 3 a , at 150 watts . power supply 505 powers y - controller 506 such as the arcus advanced motion driver + controller usb / rs485 ( part number arcus ace - sde ), that connects to y axis stepper motor 507 . a suitable stepper 507 can be a moons - brand stepper motor ( part number moons p / n 24hs5403 - 01n ). power supply 505 also connects to a conveyor controller 508 , which can be an arcus - brand advanced motion driver + controller usb / rs485 ( part number arcus ace - sde ), that connects to a conveyor stepper 509 . a moons - brand stepper motor ( part number moons p / n 24hs5403 - 01n ) is suitable for stepper 509 . power supply 505 ( fig5 ) also powers dispenser controller 510 , dispenser door control 511 , and vending controller 512 . controller 510 powers collection wing motor 514 and door motor 515 . motors 514 and 515 can be canon - brand dc gear motors ( part number 05s026 - dg16 ). controller 512 operates conveyor motors 516 such as micro - drives dc gear motor ( part number m32p0264ysgt4 ). the logo space 201 ( fig2 ) is illuminated by lighting 518 ( fig5 ) powered by supply 505 . supply 505 also powers lcd touch screen block 520 ( fig5 ) such as a kristel 22 ″ widescreen ( 16 : 10 ) lcd touch monitor with usb connection for the touch panel . ups 454 ( fig5 ) also powers an ac outlet strip 522 that in turn powers a receipt printer power supply 523 such as epson &# 39 ; s 24 vdc power supply ( part number ps - 180 ) that energizes receipt printer 524 such as epson &# 39 ; s eu - t300 thermal printer , an audio power supply that powers audio amplifier 527 such a happ controls kiosk 2 - channel amplifier with enclosure ( part number 49 - 5140 - 100 ), and a low voltage cell modem power supply 530 that runs cellular modem 531 such as multitech &# 39 ; s verizon cdma cellular modem ( part number mtcba - c - ip - n3 - nam ). a proximity sensor 214 ( fig2 a ) such as a digi watchport / d part number 301 - 1146 - 01 is connected to the cpu 450 . 532 is a door sensor and actuator such as hamlin &# 39 ; s position and movement sensor ( part 59125 ) and actuator ( part 57125 ) which are connected to the cpu 450 . subroutine 600 ( fig6 ) illustrates the preferred method of initializing the machine and inventory and dispensing system at system runtime . the process begins at step 601 when the system application is launched . step 602 reads in and parses the lighting xml file 603 . the lighting file contains a sequence of lighting sequences to be performed for various user actions on the system such as selecting a product or category , adding to the virtual shopping bag and removing it from the shopping bag . these lighting sequences dictate both the onscreen coloring of products in the virtual display and the lighting of products in the physical display . these values are cached in local memory as an application variable . step 604 checks if there are any fatal errors . fatal errors are ones that prevent the system from allowing a user to complete a transaction . all errors are logged using the reporting and logging system 303 ( fig3 ). non - fatal errors are noted in the log file so they can be examined later to correct the issue . if the error is fatal , the process goes to step 605 where the user is notified of an error and given customer support information and an alert notification is sent out to the notification system 303 ( fig3 ). the system is placed in an idle state where the touch screen will display a message noting that the machine is currently not in service . the system will attempt to recover in step 606 by attempting to start the application process again and reinitialize the system . if there are no fatal errors , the process continues to step 607 that reads in and parses the planogram file 608 . the planogram file contains the product identification number , or item identification number , a product name and a boolean value if it is active or not for each display slot number . these values are cached in local memory as an application variable . step 609 checks if there are any fatal errors . if there are fatal errors , it routes to step 605 , otherwise the process continues at step 610 . step 610 reads in all of the inventory xml files . these files instruct the system on what inventory cabinets are attached to the machine and what inventory is in what inventory slots . each inventory slot is designated by the cabinet it is located in , the shelf it is on , the size of the inventory slot and the motors that drive the dispensing mechanism . using this information , the application can determine the shelf location ( height ). the xml file information is cached and then accessed during product dispensing to guide the robotic gantry elevator to the correct shelf height to collect a product . the dispensing motor information is used by the dispenser control to turn on the motor that dispenses the product until a mechanical switch is activated determining the product has been dispensed to the gantry elevator . because of the centralized layout of the robotic gantry , it does not matter which inventory system is connected or even what side from which the product is being dispensed . it only matters what shelf the product is on so the elevator can move to the correct height to collect the product . step 610 reads in all of the screen templates 611 that determine the layout of the visual selection interface . step 612 checks if there are any fatal errors . if there are fatal errors , it routes to step 605 , otherwise the process continues at step 613 . step 613 reads in all of the screen templates 611 that determine the layout of the user interface and all of the screen asset files 614 associated with the screen templates 611 . these asset files can be images or extended markup files that represent buttons , header banners graphics that fit into header areas , directions or instructions that are displayed in designated areas , image map files that determine which area on an image corresponds represents which area on the physical facade or images representing the physical façade . these assets are cached into local memory in the application . step 615 checks if there are any fatal errors . if there are fatal errors , it routes to step 605 , otherwise the process continues at step 616 . step 616 reads and parses the product catalog files 617 . the product catalog stores all of information , graphics , specifications , prices and rich media elements ( e . g . video , audio , etc .) for each item or product in the system . each element is organized according to its identification number . these elements can be stored in a database or organized in a file folder system . these items are cached in application memory . step 618 checks if there are any fatal errors . if there are fatal errors , it routes to step 605 , otherwise the process continues at step 619 . step 619 reads in all of the system audio files 620 and the file that the stores the actions with which each audio file is associated . audio files can be of any format , compressed or uncompressed such as wav , aiff , mpeg , etc . an xml file stores the name of the application event and the sound file name and location . step 621 checks if there are any fatal errors . if there are fatal errors , it routes to step 905 , otherwise the process continues at step 622 . step 622 does a system wide hardware check by communicating with the system peripherals and controllers 302 and 308 ( fig3 ). step 623 checks if there are any fatal errors . if there are fatal errors , it routes to step 605 , otherwise the process continues at step 624 . step 624 launches the application display on the touch screen interface . the system then waits for user input 625 . subroutine 700 ( fig7 ) illustrates the preferred runtime method the machine uses to dispense items to an end user during a user session . the process begins at step 701 after a user completed a transaction that purchases the merchandise about to be vended . this process assumes that a separate process has already checked that the inventory is available for vending and it has been paid for . the routine is passed a list of items to be dispensed . for items that have multiple quantities , each item is listed as a separate item . step 702 reads this list into the process memory . step 703 determines if the dispensing system is busy processing another request . if the dispensing system is busy for any reason , step 704 pings the resource until it is free and then directs the process to step 708 where the first ( or next ) item in the list is read . step 705 is a timer that monitors step 704 to determine if the wait for the resource times out to a preset time . if it does time out , the process is considered to have an error and it directs control to step 706 that sends out an alert using the notification system designated by 303 ( fig3 ). step 707 attempts the recovery of the system by running any preprogrammed diagnostics and self - repairing routines that check and restart power and communication links to the system . if the system cannot automatically recover , the machines goes into an idle state and a message is displayed on the main screen indicating the machine is currently out of service preventing users from using the system . if the system resources are free , step 708 reads the next item to be vended from the list and retrieves its associative information into memory . this information was originally loaded into the system as the inventory xml file 611 ( fig6 ) read into memory in step 610 . the item , or product id is used to retrieve this information . information associated with the identification number includes the item &# 39 ; s location in the inventory system ( shelf height and corresponding elevator position represented as the position the elevator needs to be in to properly collect the dispensed product ), the dispensing motors associated with vending the item from the inventory shelf and item details such as its name to prompt the user , and its weight and dimensions which are used in conjunction with the product weight sensor 484 ( fig6 ) to determine a successful vend . step 709 uses this information to move the elevator tray assembly of the gantry 230 to the correct shelf height for the current item being vended . the elevator height is determined by preset position values that tell the stepper motor where to position itself on the vertical aspect of the gantry . the stepper motor has an encoder that communicates with the controller to verify the position . this combination of hardware allows the software to set a height value and have the stepper motor and the stepper controller ensure the correct position is attained . if there is a detectable error with the elevator mechanics , an error message is generated and sent out by step 706 . step 707 will again try to recover if possible . if the elevator assembly reaches the correct height and position as designated by the product information record , the product collection wings are expanded to create an extended landing area that will catch products coming off the inventory trays 213 ( fig2 a ). if an error in this process is detected , an error message is generated and step 706 will send out an alert . otherwise , if the elevator is in position and the production collection wings are extended , step 711 will use the information retrieved in the product record to activate the motor ( s ) associated with that item of inventory . a mechanical switch is used to indicate that the motor has revolved enough times to properly dispense the product or item off the shelf at which point it falls on to the product collection wings and into the conveyor . errors are again detected if present and routed to the notification system in step 706 . step 712 retracts the product collection wings so the elevator can freely move up and down in the dispensing assembly . this step also assists in positioning the product on the conveyor where it can be delivered to the user later in the process . any detected errors in this step are routed to step 706 . if there are no errors , step 713 moved the elevator gantry to the user collection area . the movement of the elevator mechanically opens up the product collection area by activating levers that open the top and back of the area . if no errors are detected , step 714 notes which control activated the dispensing process . this is only relevant when the machine is configured for dual sided vending ( see fig9 and 11 ). step 715 then spins the conveyor in the direction of the user that initiated the dispensing process . if no errors were detected , step 716 repositions the elevator that reverses the mechanical operation that opened the back of the collection area and closed it sealing off the internal components of the machine from the user . if no errors were detected , step 717 turns on the lights in the collection area 204 ( fig2 ) and opens the exterior collection area door . step 718 prompts the user on the screen 202 ( fig2 a ) to collect their product . step 719 monitors signals from the product weight sensor 484 ( fig4 ) and records the weight and matches it against the product weight information stored in the inventory xml file 611 ( fig6 ). this sensor could also be a motion or light curtain sensor . if the item was not removed for a preset amount of time , the user is prompted again to collect their item in step 718 . if user does not collect their product after a set number of attempts , an error is generated . if the sensor determines the user has removed their item , the process continues to step 720 where the exterior door is closed and the product collection area lights are turned off . the system again monitors for any mechanical errors in this process ( line to step 706 not shown ). step 721 determines if there are any additional items in the list of items to be vended . if there are additional items to be vended , the process routes back to step 703 where it begins again for the next item . if there are no more items to be vended , the process ends at step 722 . with reference directed to fig8 , an alternative vending machine 800 constructed in accordance with the best mode of the present system incorporates a variant on the display module designated as 210 in fig2 a . in this version the display module has a plurality of generally square product viewing areas 801 that present an alternative display , different from the diamond and circle display windows designated at 206 and 207 respectively in fig2 a . with reference directed to fig9 , an alternative 900 ( fig9 ) shows an alternative configuration of the machine where it has been outfitted to dispense merchandise out of both the front and back of the machine . this machine has display modules 210 affixed to both sides of the inventory cabinet 212 . it also has a vertical control panel 211 affixed to both sides of the central robotic gantry 230 . this configuration allows the unit to serve two people at the same time . with reference directed to fig1 , alternative machine 1000 represents a similar configuration but with only one inventory cabinet 212 and display module 210 . these are once again attached to the common centralized robotic dispensing gantry 230 . in this configuration a simple metal plate 1001 ( not shown ) cut the size of the dispensing system tower is affixed to the side where the inventory cabinet was attached in fig8 using the same bolts to secure the system . with reference directed to fig1 , another configuration of a vending machine 1100 utilizes the centralized robotic dispensing gantry 230 with one inventory cabinet and two display modules 210 and two vertical control panels 211 . as in fig9 , this configuration allows for two users to simultaneously interact with the machine while using only one robotic dispensing mechanism and sharing a common inventory cabinet . it will be understood that certain features and subcombinations are of utility and may be employed without reference to other features and subcombinations . this is contemplated by and is within the scope of the claims . as many possible embodiments may be made of the present system without departing from the scope thereof , it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense . | 6 |
many therapeutic drugs have undesirable properties that may become pharmacological , pharmaceutical , or pharmacokinetic barriers in clinical drug applications . among the various approaches to minimize the undesirable drug properties while retaining the desirable therapeutic activity , a chemical approach using drug derivatization offers perhaps the highest flexibility and has been demonstrated as an important means of improving drug efficacy . the prodrug approach , a chemical approach using reversible derivatives , can be useful in the optimization of the clinical application of a drug . the prodrug approach gained attention as a technique for improving drug therapy in the early 1970s . numerous prodrugs have been designed and developed since then to overcome pharmaceutical and pharmacokinetic barriers in clinical drug application , such as low oral drug absorption , lack of site specificity , chemical instability , toxicity , and poor patient acceptance ( bad taste , odor , pain at injection site , etc .) ( stella v ., pro - drugs : an overview and definition . in : higuchi t ., stella v ., eds . prodrugs as novel drug delivery systems . acs symposium series . washington , d . c . : american chemical society ; 1975 : 1 - 115 ). as used herein , the term “ prodrug ” refers to an agent rendered less active by a chemical or biological moiety , which metabolizes into or undergoes in vivo hydrolysis to form a drug or an active ingredient thereof . the term “ prodrug ” can be used interchangeably with terms such as “ proagent ”, “ latentiated drugs ,” “ bioreversible derivatives ,” and “ congeners ” ( harper n j . drug latentiation . prog drug res . 1962 ; 4 : 221 - 294 ; roche eb . design of biopharmaceutical properties through prodrugs and analogs . washington , d . c . : american pharmaceutical association ; 1977 ; sinkula a a , yalkowsky s h . rationale for design of biologically reversible drug derivatives : prodrugs . j pharm sci . 1975 ; 64 : 181 - 210 ). usually , the use of the term implies a covalent link between a drug and a chemical moiety , though some authors also use it to characterize some forms of salts of the active drug molecule . although there is no strict universal definition for a prodrug itself , and the definition may vary from author to author , generally prodrugs can be defined as pharmacologically inert chemical derivatives that can be converted in vivo , enzymatically or nonenzymatically , to the active drug molecules to exert a therapeutic effect ( sinkula a a , yalkowsky s h . rationale for design of biologically reversible drug derivatives : prodrugs . j pharm sci . 1975 ; 64 : 181 - 210 ; stella v j , charman w n , naringrekar v h . prodrugs . do they have advantages in clinical practice ? drugs . 29 : 455 - 473 ( 1985 )). in one embodiment , the prodrug described herein includes a drug and heparin that form a linkage that can be enzymatically or hydrolytically cleaved under in vivo conditions . in some embodiments , the linkage can be an ester group , a schiff base , or an acetal or hemi - acetal . in another embodiment , the prodrug described herein can include a drug , a polymer and heparin . heparin is conjugated or linked to the polymer by a physical or chemical linkage . the drug can link or be attached to the heparin or the polymer . in some embodiments , the linkage between heparin and the polymer can be , for example , ionic bonding , hydrogen bonding , or a chemical bonding such as an ester group , a schiff base , or an acetal or hemi - acetal . the linkage between the drug and the polymer can be , for example , an ester group , a schiff base , or an acetal or hemi - acetal , and the linkage between the drug and heparin can be , for example , an ester group , a schiff base , or an acetal or hemi - acetal . the term “ heparin ” refers to a heparin molecule , a heparin fragment such as pentasaccharide , a heparin derivative or a heparin complex . heparin derivatives can be any functional or structural variation of heparin . representative variations include alkali metal or alkaline - earth metal salts of heparin , such as sodium heparin ( e . g ., hepsal or pularin ), potassium heparin ( e . g ., clarin ), lithium heparin , calcium heparin ( e . g ., calciparine ), magnesium heparin ( e . g ., cutheparine ), low molecular weight heparin ( e . g ., ardeparin sodium ) with a molecular weight of from about 4 , 000 to about 5 , 000 daltons and high affinity heparin ( see , e . g ., scully , et al ., biochem . j . 262 : 651 - 658 ( 1989 )). other examples include heparin sulfate , heparinoids , heparin based compounds and heparin having a hydrophobic counter - ion such as tridodecylmethylammonium and benzalkonium . heparin contains both carboxyl groups and hydroxyl groups ( fig1 ). carboxyl groups can form an ester linkage by reacting with hydroxyl reactive groups on a drug ( see scheme 1 , below ). alternatively , the hydroxyl groups on heparin can also form an ester linkage by reacting with carboxyl groups on a drug ( see scheme 2 , below ). in some other embodiments , the prodrug described herein can be formed of a functionalized heparin and a drug molecule . for example , heparin - cho can react with an amine group on a drug or vice versa to form a schiff - base - type prodrug ( see scheme 3 , below ). heparin - cho can also react with hydroxyl groups on a drug or vice versa to form acetal or hemi - acetal type prodrugs ( see scheme 4 , below ). heparin is a highly negatively charged molecule very soluble in water . it has some solubility in formamide , but is practically insoluble in other organic solvents . this lack of solubility in organic solvents limits its use in certain applications . the conventional method of improving the solubility of heparin in organic solvents can be achieved by complexing heparin with a positive charged organic moiety such as a quaternary ammonium salt , e . g . tridodecylmethylammoniumchloride and benzalkonium chloride . some exemplary , useful hydrophobic quaternary ammonium compounds and methods of forming complexes of these compounds with heparin are described in u . s . pat . nos . 4 , 654 , 327 , 4 , 871 , 357 and 5 , 047 , 020 . heparin contains many reactive groups such as carboxyl , amine , and hydroxyl groups in its molecular structure . partially oxidized heparin contains terminal aldehyde groups . prior to or subsequent to forming the prodrug described above , in some embodiments , heparin can be physically or chemically ( e . g . covalently ) attached to hydrophilic and hydrophobic polymers by chemical reactions between the functional groups on heparin and the polymer . heparin can also be copolymerized with other monomer ( s ) to form a polymer containing heparin . in some other embodiments , attachment of heparin can be accomplished by chemically ( e . g . covalently ) or physically coupling heparin onto a polymer - coated surface . physical coupling includes , for example , ionic interaction or hydrogen bonding . as used herein , the term “ hydrophobic ” refers to an attribute of a material that defines the degree of water affinity of the molecules of the material . hydrophobicity and hydrophilicity are relative terms . generally , hydrophobicity and hydrophilicity of a polymer can be gauged using the hildebrand solubility parameter δ . the term “ hildebrand solubility parameter ” refers to a parameter indicating the cohesive energy density of a substance . the δ parameter is determined as follows : if a blend of hydrophobic and hydrophilic polymer ( s ) is used , whichever polymer in the blend has a lower δ value compared to the δ value of the other polymer in the blend is designated as a hydrophobic polymer , and the polymer with a higher δ value is designated as a hydrophilic polymer . if more than two polymers are used in the blend , then each can be ranked in order of its δ value . in some embodiments , the defining boundary between hydrophobic and hydrophilic can be set at 10 . 5 , ( cal / cm 3 ) 1 / 2 . any biocompatible polymer can be used to modify the hydrophilicity of heparin . representative hydrophobic polymers include , but are not limited to , poly ( ester amide ), polystyrene - polyisobutylene - polystyrene block copolymer ( sis ), polystyrene , polyisobutylene , polycaprolactone ( pcl ), poly ( l - lactide ), poly ( d , l - lactide ), poly ( lactides ), polylactic acid ( pla ), poly ( lactide - co - glycolide ), poly ( glycolide ), polyalkylene , polyfluoroalkylene , polyhydroxyalkanoate , poly ( 3 - hydroxybutyrate ), poly ( 4 - hydroxybutyrate ), poly ( 3 - hydroxyvalerate ), poly ( 3 - hydroxybutyrate - co - 3 - hydroxyvalerate ), poly ( 3 - hydroxyhexanoate ), poly ( 4 - hyroxyhexanoate ), mid - chain polyhydroxyalkanoate , poly ( trimethylene carbonate ), poly ( ortho ester ), polyphosphazenes , poly ( phosphoester ), poly ( tyrosine derived arylates ), poly ( tyrosine derived carbonates ), polydimethyloxanone ( pdms ), polyvinylidene fluoride ( pvdf ), polyhexafluoropropylene ( hfp ), polydimethylsiloxane , poly ( vinylidene fluoride - co - hexafluoropropylene ) ( pvdf - hfp ), poly ( vinylidene fluoride - co - chlorotrifluoroethylene ) ( pvdf - ctfe ), poly ( methacrylates ) such as poly ( butyl methacrylate ) ( pb ma ) or poly ( methyl methacrylate ) ( pmma ), poly ( vinyl acetate ), poly ( ethylene - co - vinyl acetate ), poly ( ethylene - co - vinyl alcohol ), poly ( ester urethanes ), poly ( ether - urethanes ), poly ( carbonate - urethanes ), poly ( silicone - urethanes ), poly ( urea - urethanes ) or a combination thereof . methods of derivatizing heparin with hydrophobic materials or polymers are described in , for example , u . s . pat . nos . 4 , 331 , 697 ; 5 , 069 , 899 ; 5 , 236 , 570 ; 5 , 270 , 046 ; 5 , 453 , 171 ; 5 , 741 , 881 ; 5 , 770 , 563 ; 5 , 855 , 618 ; 6 , 589 , 943 and 6 , 630 , 580 . any hydrophobic counter ion can be used to modify the hydrophilicity of heparin . for example , hydrophobic quaternary ammonium compounds have been commonly used to form complexes with heparin that are soluble in organic solvents . some exemplary useful hydrophobic quaternary ammonium compounds and methods of forming complexes of these compounds with heparin are described in u . s . pat . nos . 4 , 654 , 327 , 4 , 871 , 357 and 5 , 047 , 020 . in some other embodiments , a hydrophilic polymer and / or a non - fouling polymer can be used to modify the hydrophilicity of heparin . non - fouling or anti - fouling is defined as preventing , delaying or reducing the amount of formation of protein build - up caused by the body &# 39 ; s reaction to foreign material . representative hydrophilic polymers include , but are not limited to , polymers and co - polymers of peg acrylate ( pega ), peg methacrylate , 2 - methacryloyloxyethylphosphorylcholine ( mpc ) and n - vinyl pyrrolidone ( vp ), carboxylic acid bearing monomers such as methacrylic acid ( ma ), acrylic acid ( aa ), hydroxyl bearing monomers such as hema , hydroxypropyl methacrylate ( hpma ), hydroxypropylmethacrylamide , and 3 - trimethylsilylpropyl methacrylate ( tmspma ), poly ( ethylene glycol ) ( peg ), poly ( propylene glycol ), sis - peg , polystyrene - peg , polyisobutylene - peg , pcl - peg , pla - peg , pmma - peg , pdms - peg , pvdf - peg , pluronic ™ surfactants ( polypropylene oxide - co - polyethylene glycol ), poly ( tetramethylene glycol ), poly ( l - lysine - ethylene glycol ) ( pll - g - peg ), poly ( l - g - lysine - hyaluronic acid ) ( pll - g - ha ), poly ( l - lysine - g - phosphoryl choline ) ( pll - g - pc ), poly ( l - lysine - g - vinylpyrrolidone ) ( pll - g - pvp ), poly ( ethylimine - g - ethylene glycol ) ( pei - g - peg ), poly ( ethylimine - g - hyaluronic acid ) ( pei - g - ha ), poly ( ethylimine - g - phosphoryl choline ) ( pei - g - pc ), and poly ( ethylimine - g - vinylpyrrolidone ) ( pei - g - pvp ), pll - co - ha , pll - co - pc , pll - co - pvp , pei - co - peg , pei - co - ha , pei - co - pc , and pei - co - pvp , hydroxy functional poly ( vinyl pyrrolidone ), polyalkylene oxide , dextran , dextrin , sodium hyaluronate , hyaluronic acid , elastin , chitosan , acrylic sulfate , acrylic sulfonate , acrylic sulfamate , methacrylic sulfate , methacrylic sulfonate , methacrylic sulfamate and combination thereof . the non - fouling polymer can be , for example , poly ( ethylene glycol ), poly ( alkylene oxide ), hydroxyethylmethacrylate ( hema ) polymer and copolymers , poly ( n - propylmethacrylamide ), sulfonated polystyrene , hyaluronic acid , poly ( vinyl alcohol ), poly ( n - vinyl - 2 - pyrrolidone ), sulfonated dextran , phosphoryl choline , choline , or combinations thereof . the heparin can be readily attached to a polymer or polymeric surface by forming a schiff base between an amino group and an aldehyde group that heparin and the polymer may have , by forming an amide group between an amine group on a polymer and the carboxyl group on heparin via nhs ( n - hydroxysuccinimide ) activation ( see , e . g ., staros , et al ., anal . biochem . 156 : 220 - 222 ( 1986 )), edc ( 1 - ethyl - 3 -( 3 - dimethylaminopropyl ) carbodiimide hydrochloride ) activation ( see , e . g ., j . m . tedder , a . nechvatal , a . w . murray , et al . amino - acids and proteins . in : basic organic chemistry . london : john wiley & amp ; sons , chapter 6 , pp . 305 - 342 ( 1972 ); d . sehgal , i . k . vijay , anal . biochem . 218 : 87 ( 1994 )) or aziridine chemistry . some representative methods of attaching heparin to a polymer or polymeric surface are described in u . s . application ser . no . 10 / 857 , 141 , filed on may 27 , 2004 , the teachings of which are incorporated herein by reference . in a further embodiment , heparin can be derivatized with an unsaturated group such as acrylate , e . g ., methacrylate , or vinyl alcohol using the chemistry described above . the heparin functionalized with an unsaturated group can be used in a free radical polymerization to graft or crosslink to a substrate or another formulation component such as a polymer . the drug can be any agent which is biologically active and capable of forming an ester bond with the carboxyl group or hydroxyl group of the heparin molecule or capable of forming a schiff base or acetal or hemi - acetal with heparin functionalized to have an aldehyde group . in the alternative , the drug can have an aldehyde so as to react with the amino group of heparin - nh 2 to form a schiff base prodrug or an aldehyde or keto group so as to react with the hydroxyl group or groups on heparin to acetal or hemi - acetal prodrug . most drugs have one of hydroxyl , carboxyl , amino , keto or aldehyde groups and thus can form the prodrugs described herein . the drug can be , for example , a therapeutic , prophylactic , or diagnostic agent . as used herein , the drug includes a bioactive moiety , derivative , or metabolite of the drug . examples of suitable therapeutic and prophylactic agents capable of forming the prodrugs described herein include synthetic inorganic and organic compounds , proteins and peptides , polysaccharides and other sugars , lipids , and dna and rna nucleic acid sequences having therapeutic , prophylactic or diagnostic activities . nucleic acid sequences include genes , antisense molecules which bind to complementary dna to inhibit transcription , and ribozymes . other examples of drugs include antibodies , receptor ligands , and enzymes , adhesion peptides , oligosaccharides , blood clotting factors , inhibitors or clot dissolving agents such as streptokinase and tissue plasminogen activator , antigens for immunization , hormones and growth factors , oligonucleotides such as antisense oligonucleotides and ribozymes and retroviral vectors for use in gene therapy , in one embodiment , the drug can be a drug for inhibiting the activity of vascular smooth muscle cells . more specifically , the drug can be aimed at inhibiting abnormal or inappropriate migration and / or proliferation of smooth muscle cells for the inhibition of restenosis . the drug can also include any substance capable of exerting a therapeutic or prophylactic effect in the practice of the present invention . for example , the drug can be a prohealing drug that imparts a benign neointimal response characterized by controlled proliferation of smooth muscle cells and controlled deposition of extracellular matrix with complete luminal coverage by phenotypically functional ( similar to uninjured , healthy intima ) and morphologically normal ( similar to uninjured , healthy intima ) endothelial cells . the drug can also fall under the genus of antineoplastic , cytostatic or anti - proliferative , anti - inflammatory , antiplatelet , anticoagulant , antifibrin , antithrombin , antimitotic , antibiotic , antiallergic and antioxidant substances . examples of such antineoplastics and / or antimitotics include paclitaxel ( e . g . taxol ® by bristol - myers squibb co ., stamford , conn . ), docetaxel ( e . g . taxotere ®, from aventis s . a ., frankfurt , germany ) methotrexate , azathioprine , vincristine , vinblastine , fluorouracil , doxorubicin hydrochloride ( e . g . adriamycin ® from pharmacia & amp ; upjohn , peapack n . j . ), and mitomycin ( e . g . mutamycin ® from bristol - myers squibb co ., stamford , conn .). examples of such antiplatelets , anticoagulants , antifibrin , and antithrombins include heparinoids , hirudin , argatroban , forskolin , vapiprost , prostacyclin and prostacyclin analogues , dextran , d - phe - pro - arg - chloromethylketone ( synthetic antithrombin ), dipyridamole , glycoprotein iib / iiia platelet membrane receptor antagonist , antibody , recombinant hirudin , and thrombin inhibitors such as angiomax ä ( biogen , inc ., cambridge , mass .). examples of cytostatic or antiproliferative agents include angiopeptin , angiotensin converting enzyme inhibitors such as captopril ( e . g . capoten ® and capozide ® from bristol - myers squibb co ., stamford , conn . ), cilazapril or lisinopril ( e . g . prinivil ® and prinzide ® from merck & amp ; co ., inc ., whitehouse station , n . j . ), actinomycin d , or derivatives and analogs thereof ( manufactured by sigma - aldrich 1001 west saint paul avenue , milwaukee , wis . 53233 ; or cosmegen available from merck ). synonyms of actinomycin d include dactinomycin , actinomycin iv , actinomycin i 1 , actinomycin x 1 , and actinomycin c 1 . other drugs include calcium channel blockers ( such as nifedipine ), colchicine , fibroblast growth factor ( fgf ) antagonists , fish oil ( omega 3 - fatty acid ), histamine antagonists , lovastatin ( an inhibitor of hmg - coa reductase , a cholesterol lowering drug , brand name mevacor from merck & amp ; co ., inc ., whitehouse station , n . j . ), monoclonal antibodies ( such as those specific for platelet - derived growth factor ( pdgf ) receptors ), nitroprusside , phosphodiesterase inhibitors , prostaglandin inhibitors , suramin , serotonin blockers , steroids , thioprotease inhibitors , triazolopyrimidine ( a pdgf antagonist ), and nitric oxide . an example of an antiallergic agent is permirolast potassium . other therapeutic substances or agents which may be appropriate include alpha - interferon , genetically engineered epithelial cells , antibodies such as cd - 34 antibody , abciximab ( reopro ), and progenitor cell capturing antibody , prohealing drugs that promotes controlled proliferation of muscle cells with a normal and physiologically benign composition and synthesis products , enzymes , anti - inflammatory agents , antivirals , anticancer drugs , anticoagulant agents , free radical scavengers , estradiol , steroidal anti - inflammatory agents , non - steroidal anti - inflammatory , antibiotics , nitric oxide donors , super oxide dismutases , super oxide dismutases mimics , 4 - amino - 2 , 2 , 6 , 6 - tetramethylpiperidine - 1 - oxyl ( 4 - amino - tempo ), tacrolimus , dexamethasone , rapamycin , rapamycin derivatives , 40 - o -( 2 - hydroxy ) ethyl - rapamycin ( everolimus ), 40 - o -( 3 - hydroxy ) propyl - rapamycin , 40 - o -[ 2 -( 2 - hydroxy ) ethoxy ] ethyl - rapamycin , 40 - o - tetrazole - rapamycin , abt - 578 , clobetasol , cytostatic agents , aspirin , and a combination thereof . the foregoing substances are listed by way of example and are not meant to be limiting . other active agents which are currently available or that may be developed in the future are equally applicable . the dosage or concentration of the drug required to produce a favorable therapeutic effect should be less than the level at which the drug produces toxic effects and greater than the level at which non - therapeutic results are obtained . the dosage or concentration of the drug can depend upon factors such as the particular circumstances of the patient , the nature of the trauma , the nature of the therapy desired , the time over which the ingredient administered resides at the vascular site , and , if other active agents are employed , the nature and type of the substance or combination of substances . therapeutic effective dosages can be determined empirically , for example by infusing vessels from suitable animal model systems and using immunohistochemical , fluorescent or electron microscopy methods to detect the agent and its effects , or by conducting suitable in vitro studies . standard pharmacological test procedures to determine dosages are understood by one of ordinary skill in the art . the carboxylic acid group of the heparin molecule can form an ester bond with a drug molecule via an established procedure in the art of organic synthesis ( see , for example , larock , comprehensive organic transformations : a guide to functional group preparations , john wiley & amp ; sons , inc ., copyright 1999 ). generally , the prodrug described herein can be prepared according to scheme 1 , as described below . in scheme 1 , r represents a drug molecule or a derivative thereof . heparin represents a heparin molecule or a moiety or derivative thereof . x represents a leaving group attached to the drug molecule . for example , x can be oh , a halo group , mesylate or tosyl group , and any other groups capable of leaving the drug molecule in forming the drug / heparin ester bond . alternatively , the prodrug can be made via a hydroxyl group in the heparin molecule and a carboxylic acid , as shown in scheme 2 . in scheme 2 , r represents a drug molecule or a derivative thereof . heparin represents a heparin molecule or a moiety or derivative thereof . x represents a leaving group attached to the carboxyl group of the drug molecule . for example , x can be h , a halo group , a carboxylate , mesylate or tosyl group , or any other group capable of leaving the drug molecule in forming the drug / heparin ester bond . in some other embodiments , the prodrug described herein can be formed via an imine schiff base by heparin - cho with an amine - containing drug ( scheme 3 ) or vice versa ( scheme 4 ). as shown in scheme 3 , the aldehyde group of heparin - cho can react with the amine group of an amine - containing drug to form an imine schiff base , which is hydrolytically unstable and can release the amine - containing drug under in vivo conditions . scheme 4 shows an alternative strategy for forming the prodrug by the reaction of the amino group of heparin - nh 2 with a keto group on the drug molecule to form an imine schiff base linkage . in still some other embodiments , the prodrug described herein can be formed via an acetal or hemi - acetal by heparin - cho with a hydroxyl group or hydroxyl groups on a drug ( scheme 5 ) or vice versa ( scheme 6 ). the acetal or hemi - acetal can undergo hydrolysis under in vivo conditions to release the drug . as shown in scheme 5 , the aldehyde group of heparin - cho can react with the hydroxyl group or groups on a drug to form a prodrug with an acetal linkage or hemi - acetal linkage ( scheme 5 ). alternatively , the hydroxyl group or groups can react with an aldehyde or keto group on a drug to form a prodrug with an acetal linkage or hemi - acetal linkage ( scheme 6 ). in one embodiment , the hydroxyl group on the c40 position of everolimus can react with the carboxyl group on heparin to form an ester bond so as to form an everolimus / heparin prodrug . in another embodiment , a drug can form a prodrug with heparin attached to a polymer such as poly ( l - lysine - g - ethylene glycol ) ( pll - peg ), which can be pll - g - peg or pll - co - peg . in this embodiment , the amino group in the pll - peg can react with a carboxyl group in heparin to form an amide bond via edc activation and / or nhs activation , as described above . alternatively , the amino group in the pll - peg can react with heparin - cho to form a schiff base . a drug such as paclitaxel , docetaxel , or everolimus can then be attached or linked to the heparin via one of the functionalities , such as an amino group , an aldehyde group , a carboxyl group or a hydroxyl group to form a prodrug as per the above description . in addition to heparin , the point of attachment for the drug can also be the pll backbone via nh 2 groups on pll or peg via a terminal hydroxyl group , an amino group or an aldehyde group of peg . using the same strategy , in some other embodiments , prodrugs can be formed by a drug and a polymer such as poly ( l - lysine - hyaluronic acid ) ( pll - ha ), poly ( l - lysine - phosphoryl choline ) ( pll - pc ), poly ( l - lysine - vinylpyrrolidone ) ( pll - pvp ), poly ( ethylimine - ethylene glycol ) ( pei - peg ), poly ( ethylimine - hyaluronic acid ) ( pei - ha ), poly ( ethylimine - phosphoryl choline ) ( pei - pc ), and poly ( ethylimine - vinylpyrrolidone ) ( pei - pvp ). these pll or pei based copolymers can be graft or block copolymers , e . g ., pll - g - peg , pll - g - ha , pll - g - pc , pll - g - pvp , pei - g - peg , pei - g - ha , pei - g - pc , pei - g - pvp , pll - co - ha , pll - co - pc , pll - co - pvp , pei - co - peg , pei - co - ha , pei - co - pc , and pei - co - pvp . note , in still some other embodiments , the primary amine — nh 2 groups in pll or pei can be converted to nh 3 + ions on the polymer under an acidic ph to bind or link with heparin . the prodrug can be used to form a coating on an implantable device . the prodrug can also be attached to a polymer via the heparin molecule to form a polymer bearing the prodrug defined herein , which can then be coated onto an implantable device . alternatively , the prodrug can be attached or grafted onto a polymeric coating on an implantable device . the prodrug provided herein can be used alone to form a coating on a medical device . the prodrug can also be used in combination with a polymeric material . the prodrug can be blended with a polymeric coating material or deposited as a coating on top of a polymeric coating which itself may optionally include a drug . the polymeric material can be any biocompatible polymer such as a hydrophobic polymer , a hydrophilic polymer , a non - fouling polymer , or a combination thereof . the polymeric material can be biodegradable , bioerodable , bioabsorable or biodurable . in one embodiment , the coating material is a hydrophobic polymer . representative hydrophobic polymers include , but are not limited to , polystyrene - polyisobutylene - polystyrene block copolymer ( sis ), polystyrene , polyisobutylene , polycaprolactone ( pcl ), poly ( l - lactide ), poly ( d , l - lactide ), poly ( lactides ), polylactic acid ( pla ), poly ( lactide - co - glycolide ), poly ( glycolide ), polyalkylene , polyfluoroalkylene , polyhydroxyalkanoate , poly ( 3 - hydroxybutyrate ), poly ( 4 - hydroxybutyrate ), poly ( 3 - hydroxyvalerate ), poly ( 3 - hydroxybutyrate - co - 3 - hydroxyvalerate ), poly ( 3 - hydroxyhexanoate ), poly ( 4 - hyroxyhexanoate ), mid - chain polyhydroxyalkanoate , poly ( trimethylene carbonate ), poly ( ortho ester ), polyphosphazenes , poly ( phosphoester ), poly ( tyrosine derived arylates ), poly ( tyrosine derived carbonates ), polydimethyloxanone ( pdms ), polyvinylidene fluoride ( pvdf ), polyhexafluoropropylene ( hfp ), polydimethylsiloxane , poly ( vinylidene fluoride - co - hexafluoropropylene ) ( pvdf - hfp ), poly ( vinylidene fluoride - co - chlorotrifluoroethylene ) ( pvdf - ctfe ), poly ( butyl methacrylate ), poly ( methyl methacrylate ), poly ( methacrylates ), poly ( vinyl acetate ), poly ( ethylene - co - vinyl acetate ), poly ( ethylene - co - vinyl alcohol ), poly ( ester urethanes ), poly ( ether - urethanes ), poly ( carbonate - urethanes ), poly ( silicone - urethanes ), poly ( 2 - hydroxyethyl methacrylate ), poly ( urea - urethanes ) and a combination thereof . in one embodiment , the coating material is a hydrophilic polymer , such as those previously described . in some embodiments , hydrophilic polymers include , but are not limited to , polymers and co - polymers of peg acrylate ( pega ), peg methacrylate , 2 - methacryloyloxyethylphosphorylcholine ( mpc ) and n - vinyl pyrrolidone ( vp ), carboxylic acid bearing monomers such as methacrylic acid ( ma ), acrylic acid ( aa ), hydroxyl bearing monomers such as hema , hydroxypropyl methacrylate ( hpma ), hydroxypropylmethacrylamide , and 3 - trimethylsilylpropyl methacrylate ( tmspma ), poly ( ethylene glycol ) ( peg ), poly ( propylene glycol ), sis - peg , polystyrene - peg , polyisobutylene - peg , pcl - peg , pla - peg , pmma - peg , pdms - peg , pvdf - peg , pluronic ™ surfactants ( polypropylene oxide - co - polyethylene glycol ), poly ( tetramethylene glycol ), hydroxy functional poly ( vinyl pyrrolidone ), polyalkylene oxide , dextran , dextrin , sodium hyaluronate , hyaluronic acid , elastin , chitosan , acrylic sulfate , acrylic sulfonate , acrylic sulfamate , methacrylic sulfate , methacrylic sulfonate , methacrylic sulfamate or combination thereof . in another embodiment , the coating material is a non - fouling polymer such as , for example , poly ( ethylene glycol ), poly ( alkylene oxide ), hydroxyethylmethacrylate ( hema ) polymer and copolymers , poly ( n - propylmethacrylamide ), sulfonated polystyrene , hyaluronic acid ( ha ), poly ( vinyl alcohol ), poly ( n - vinyl - 2 - pyrrolidone ), sulfonated dextran , phospholipids such as phosphoryl choline ( pc ) and choline , or combinations thereof . as used herein , an implantable device may be any suitable medical substrate that can be implanted in a human or veterinary patient . examples of such implantable devices include self - expandable stents , balloon - expandable stents , stent - grafts , grafts ( e . g ., aortic grafts ), artificial heart valves , cerebrospinal fluid shunts , pacemaker electrodes , and endocardial leads ( e . g ., fineline and endotak , available from guidant corporation , santa clara , calif .). the underlying structure of the device can be of virtually any design . the device can be made of a metallic material or an alloy such as , but not limited to , cobalt chromium alloy ( elgiloy ), stainless steel ( 316l ), high nitrogen stainless steel , e . g ., biodur 108 , cobalt chrome alloy l - 605 , “ mp35n ,” “ mp20n ,” elastinite ( nitinol ), tantalum , nickel - titanium alloy , platinum - iridium alloy , gold , magnesium , or combinations thereof . “ mp35n ” and “ mp20n ” are trade names for alloys of cobalt , nickel , chromium and molybdenum available from standard press steel co ., jenkintown , pa . “ mp35n ” consists of 35 % cobalt , 35 % nickel , 20 % chromium , and 10 % molybdenum . “ mp20n ” consists of 50 % cobalt , 20 % nickel , 20 % chromium , and 10 % molybdenum . devices made from bioabsorbable or biostable polymers could also be used with the embodiments of the present invention . in accordance with embodiments of the invention , a coating of the various described embodiments can be formed on an implantable device or prosthesis , e . g ., a stent . for coatings including one or more active agents , the agent will retain on the medical device such as a stent during delivery and expansion of the device , and be released at a desired rate and for a predetermined duration of time at the site of implantation . preferably , the medical device is a stent . a stent having the above - described coating is useful for a variety of medical procedures , including , by way of example , treatment of obstructions caused by tumors in bile ducts , esophagus , trachea / bronchi and other biological passageways . a stent having the above - described coating is particularly useful for treating occluded regions of blood vessels caused by abnormal or inappropriate migration and proliferation of smooth muscle cells , thrombosis , and restenosis . stents may be placed in a wide array of blood vessels , both arteries and veins . representative examples of sites include the iliac , renal , and coronary arteries . for implantation of a stent , an angiogram is first performed to determine the appropriate positioning for stent therapy . an angiogram is typically accomplished by injecting a radiopaque contrasting agent through a catheter inserted into an artery or vein as an x - ray is taken . a guidewire is then advanced through the lesion or proposed site of treatment . over the guidewire is passed a delivery catheter which allows a stent in its collapsed configuration to be inserted into the passageway . the delivery catheter is inserted either percutaneously or by surgery into the femoral artery , brachial artery , femoral vein , or brachial vein , and advanced into the appropriate blood vessel by steering the catheter through the vascular system under fluoroscopic guidance . a stent having the above - described coating may then be expanded at the desired area of treatment . a post - insertion angiogram may also be utilized to confirm appropriate positioning . while particular embodiments of the present invention have been shown and described , it will be obvious to those skilled in the art that changes and modifications can be made without departing from this invention in its broader aspects . therefore , the appended claims are to encompass within their scope all such changes and modifications as fall within the true spirit and scope of this invention . | 0 |
the fuser device , according to this invention , is shown in fig1 and is generally designated by the numeral 10 . the fuser device 10 , to be utilized in any well known electrostatographic reproduction apparatus ( not shown ), basically includes a fusing roller 12 selectively rotated at a predetermined speed , an external heater assembly 14 , and a pressure nip - forming backup film and support structure assembly 26 . the fuser device 10 may be controlled by reproduction apparatus intelligence in any well known manner . for example , the fuser process set - points ( fuser nip width , fuser temperature , and energy requirements ) for various types of receiver media may be stored as lookup tables in a media catalog for a machine control unit . the receiver media can include heavy stock cover material , interior page print material , insert material , transparency material , or any other desired media to carry text or image information . a typical machine control unit includes a microprocessor and memory or microcomputer . it stores and operates a program that controls operation of the reproduction apparatus ( including the fuser device ) in accordance with programmed steps and machine inputs , such as temperature of the fuser roller . temperature data is supplied , for example , by a thermocouple or any other suitable thermal sensor in a manner well known to those skilled in the art . as a sheet of a specific media bye is requested , a data signal to the machine control unit ( or alternatively , directly to an independent control for the fuser device ) that is representative of the image contents and the type of media sheet to be fixed in the fuser device . the machine control unit sets the fuser conditions ( temperature ; dwell time ) from the media catalog as a function of the data provided . the machine control unit directs the heating nip width control according to the power requirements of the fuser roller per the information provided from media catalog . the machine control unit also directs the fuser roller nip width controller to adjust the fuser nip per the information provided from media catalog . the fuser roller 12 of the fuser device 10 includes , for example , an aluminum core 7 , a relatively thick elastomeric base - cushion 16 ( 5 to 10 mils thick depending on the process speed ), and a thin top release coating layer 22 ( 1 to 2 mils thick ). the external heater assembly 14 includes an endless metal film 18 . the film 18 is internally heated by a low mass heating element 20 , such as for example , a metal resistance trace embedded in a ceramic substrate operating on a the joule heating principle such that heat transfer is purely diffusive . thus heat generated in the heating element 20 is transferred to the film 18 by thermal diffusion . the film 18 is urged into selective pressure relation with the polymer release layer 22 of the fusing roller 12 by the heating element 20 to form a heating nip 20 ′. the heating film 18 then transfers heat to the external surface of the fusing roller 12 in the heating nip 20 ′ by thermal diffusion . such heat is then transferred , by thermal diffusion , to image - wise toner powder particles carried by a receiver media sheet ( for example sheet r ) transported to the fuser device 10 in any well known manner ( not shown ). the image - wise toner powder particles on a receiver media sheet r and the sheet are pressed between the release layer 22 of the fusing roller 12 and the pressure film assembly 26 in a fusing nip 24 as the fuser roller 12 is rotated , in any well known controlled manner in the direction of arrow a ( see fig3 ). the amount of energy transferred to the toner powder and receiver media sheet is dependent on the resident ( dwell ) time of the receiver media sheet in the fusing nip 24 . using a pressure film assembly 26 to create an extended fusing nip 24 ( as compared with a pressure roller such as well known in the art ) provides a long resident time required for high quality surface finishes on receiver media where medium to high gloss is desired . the pressure film assembly 26 includes an endless pressure film belt 28 . an entrance roller 30 about which the pressure film belt 28 is wrapped establishes an entrance guide for transporting a toner powder bearing receiver media sheet r into the fusing nip 24 . a pressure applicator 32 is provided within the pressure film belt endless path for applying a preselected pressure to urge the pressure film belt 28 into operative contact with the fusing roller 12 . an exit roller 34 within the pressure film belt endless path supports the pressure film belt 28 to apply contact pressure of the pressure film belt to the fusing roller 12 , and further creates a mechanical release feature at an exit of the fusing nip 24 . a tracking structure 36 , also located within the path of the pressure film belt 28 , about which the pressure film belt 28 is wrapped , serves to guide the pressure film belt 28 in the desired path relative to the fusing roller 12 . with such pressure film assembly 26 , a toner powder bearing receiver media sheet r is guided through the fusing nip 24 at a desired pressure and with a desired dwell time in the fusing nip . externally heating the surface of the fusing roller 12 with the external heater 14 is the fastest way to bring the surface temperature of the fusing roller 12 up to a required fusing temperature . using a thick fuser roller elastomer cover 16 enables attaining a large fusing nip 24 . the larger the fusing nip , the longer the fusing dwell time for achieving a high level of gloss . externally heating the fusing roller 12 , with a thick elastomeric cover 16 greatly reduces the time constant to heat the fusing surface ( as opposed to internally heating the fuser roller ). for example , see table 1 in which an internally heated fuser roller with a 5 mm red silicone elastomeric cover and a 6 . 35 mm thick aluminum 6061 - t6 core structure is compared to a similarly constructed fuser roller externally heated with a 50 micron thick nickel film belt . table 1 shows the mathematical relationship for the thermal time constant based on conductive heat transfer ( thermal diffusion ). the first layer is heated by the appropriate heating element , the second layer is heated by contact conduction from the first layer . with the externally heated roller case , only one layer ( the heating film 18 ) is provided . the total time constant is shown in the last row of the table . the externally heated fuser roller has a thermal time constant that is than a millisecond , whereas the internally heated fusing roller has a time constant of approximately 85 seconds . the smaller time constant of the externally heated fuser roller is significant , and would result in substantially faster heating times , faster cooling times , less environmental heating ( waste heat ), and more constant temperature control response . the above described time constant is not the only heating factor . the dwell time in the fuser nip 24 is also a significant factor . the dwell time in the fuser nip 24 is a function of the speed of rotation of the fusing roller 12 and the fusing nip width 11 . the longer the fusing nip width , at a given fusing roller surface velocity results in longer dwell times . fig3 shows the temperature points around the surface of the fusing roller 12 . t 0 to t 1 is the fusing nip , t 1 to t 2 is the cooling span , and t 2 to t 3 is the heating nip . to optimize the change in temperature from t 2 to t 3 , the longest possible dwell time and the highest possible heating film 18 temperature should be used . maximizing the nip width is accomplished by shaping the tracking structure 18 ′ for the heating film 18 and the heating element 20 so as to be at least substantially flat or concave , and pressing the heating element 20 , through the heating belt 18 , against the fusing roller 12 with sufficient force ( pressure ). as discussed above , the width of the fuser nip 24 and the rotational speed of the fusing roller 12 define the fusing dwell time . further , the pressure profile in the fuser nip 24 ( see fig5 ) defines the contact thermal conductance , in addition to the mechanical work necessary to cause the toner powder particles to sinter together for fixing to the receiver media sheet and flow for gloss level control . to maximize the fusing dwell time , the pressure film belt 28 is supported in the endless travel path by the entrance roller 30 , the pressure applicator 32 , the exit roller 34 , and the tracking structure 36 . the exit roller 34 forces the exiting receiver media sheet r off the fuser roller 12 with the pressure film belt 28 , a mechanical release process well known in the art . to accomplish this end , the exit roller 34 needs to be smaller in diameter , or posses a stiffer elastomeric cover than the fuser roller 12 to provide the proper fusing nip exit geometry for good consistent release of the receiver media sheet from the fuser roller 12 . if the release is not consistent the gloss level will vary due to an inconsistent point of release from the fusing roller 12 , which causes a variability in dwell time . utilizing the described pressure film assembly 26 enables the fusing nip width to be extended by adjusting , and controlling , the contact length ( and area ) of the pressure film belt 28 and the fuser roller 12 . the contact length adjustment is provided by positioning the exit roller 34 and the entrance roller 30 with respect to each other and the fuser roller 12 . optimizing the pressure in the fusing nip 24 , by maximizing the pressure throughout the nip while maintaining good sheet handling characteristics , will maximize the thermal contact conductance between the surface of the fuser roller 12 and the receiver media sheet and the image - wise toner powder particles on the receiver media sheet . fig2 shows a general relationship between thermal conductance and thermal response time , in this instance to reach 100 degrees c . as the thermal conductance increases , the thermal response time decreases . to have a faster response time , the thermal conductance should be maximized knowing that the thermal conductance increases with increasing pressure in the fusing nip . for pressure application in the fusing nip 24 , four elements are used to back up the pressure film belt 28 : the entrance roller 30 , the pressure applicator 32 , the exit roller 34 , and a tracking structure 36 . the tracking structure 36 supports the pressure film belt 28 between the exit roller 34 and the entrance roller 30 . it can also be used to control tension in the pressure film belt 28 in any well known manner . having these pressure inducing parts creates three pressure pulses through the fusing nip 24 ( see fig4 ). while a continuous pressure throughout the fusing nip would be optimum , it is not practical . therefore , minimizing the loss in pressure between the components is done to optimize the pressure profile in the fusing nip . fig4 shows each of the three mentioned pressure parts through the fusing nip 24 with their respective applied forces : entrance roller load f er , pressure applicator load f pa , and the exit roller load f rr . fig5 shows a pressure profile for the fusing nip of this configuration . fig6 shows the same pressure profile while indicating the ideal ( optimum ) pressure profile . the minimum pressure between each part is equal to the pressure applied by the pressure film belt 28 . the amount of pressure that the pressure film belt 28 applies is proportional to the tension in the pressure film belt established by the elements used to back up the pressure film belt . the shape , stiffness , and load f pa of the pressure applicator 32 determines the pressure profile for a given fuser roller configuration . the pressure applicator 32 of this embodiment is made of metal and acts as a rigid member . the shape is curved to approximately match the outer curvature of the fuser roller 12 in the compressed ( loaded ) state . the width w of the pressure applicator 32 is as close as possible to the width of the entrance roller 30 and the exit roller 34 , without contact . in an alternate embodiment shown in fig7 , the pressure applicator , designated by the numeral 40 , is made of an elastomeric material , such as silicone rubber . the geometrical shape of the elastomeric pressure applicator 40 is configured to provide the broadest pressure profile result . fig8 shows the temperature points around the fuser roller for the fuser device of fig7 . the invention has been described in detail with particular reference to certain preferred embodiment thereof , but it will be understood that variations and modifications can be effected within the spirit and scope of the invention . | 6 |
in fig1 an induction heating workcell 10 includes tools or dies 20 and 22 mounted within an upper 24 and a lower 26 strongback . the strongbacks are each threaded onto four threaded column supports or jackscrews 28 or they float free on the columns and are fixed with nuts . we can turn the jackscrews to move one strongback relative to the other . the strongbacks 24 and 26 provide a rigid , flat backing surface for the upper and lower dies 20 and 22 to prevent the dies from bending and cracking during manufacturing operations . preferably , the strongbacks hold the dies to a surface tolerance of ± 0 . 003 inches per square foot of the forming surface . such tolerances are desirable to achieve proper part tolerances . the strongbacks may be steel , aluminum , or any other material capable of handling the loads present during forming or consolidation , but we prefer materials that are non - magnetic to avoid any distortion to the magnetic field that our induction coils produce . in some circumstances , the dies may be strong enough themselves that strongbacks are unnecessary . the strongbacks transfer pressure input through the columns evenly to the dies . the dies 20 and 22 are usually ceramic and are reinforced with a plurality of fiberglass rods 32 that are held with bolts 74 and that extend both longitudinally and transversely in a grid through each die . each die usually is framed with phenolic reinforcement 72 as well to maintain a compressive load on the die . each die may be attached to its strongback by any suitable fastening device such as bolting or clamping . in the preferred embodiment , both dies are mounted on support plates 76 which are held in place on the respective strongbacks through the use of clamping bars 77 . the clamping bars 77 extend around the periphery of the support plates 76 and are bolted to the respective strongbacks through the use of fasteners ( not shown ). the dies should not be susceptible to inductive heating so that heating is localized in the retort . we prefer a ceramic that has a low coefficient of thermal expansion , good thermal shock resistance , and relatively high compression strength , such as a castable fused silica ceramic . we embed portions of an induction coil 35 in the dies . in the illustrated embodiment , we use four separate induction segments , but the number can vary . each segment is formed from a straight tubing section 36 that extends along the length of each die and a flexible coil connector 38 that joins the straight tubing sections 36 in the upper die 20 to the corresponding straight tubing section in the lower die 22 . connectors 40 located at the ends of the induction coil 35 connect the induction coil 35 to an external power source or coil driver 50 and to a coolant source . cavities 42 and 44 in the respective dies can hold tool inserts 46 and 48 . the upper tool insert 46 in some applications has a contoured forming surface 58 that has a shape corresponding to the desired shape of the outer mold line surface of the completed composite . the lower tool insert usually determines the inner mold line . the tool inserts also should not be susceptible to inductive heating , preferably being formed of a castable ceramic . in some cases , both the dies and the tool inserts can be made from a matrix resin rather than from a ceramic . using a resin , however , limits use of the tooling to low temperature operations , such as forming or consolidating certain organic matrix composites . we prefer cast ceramic tooling which provides the greatest flexibility and versatility for the induction heating workcell . the forming surfaces can be an integral part of the dies . each die surrounds and supports the respective tool insert and holds the straight sections 36 of the induction coil in proper position in relationship to the tool insert 46 or 48 . in the preferred embodiment , the interior 70 of the dies is formed of a castable phenolic or ceramic and the exterior sides from precast composite phenolic resin blocks 72 . in some applications , we prefer to reinforce the phenolic or ceramic with chopped fibers or non - woven or woven reinforcing mats . fig2 shows a retort 60 between the tool inserts 46 and 48 . the retort 60 includes an organic matrix composite panel or metal workpiece sandwiched with susceptor facesheets . the retort is heated to the operating temperature by energizing the coil 35 . in the case of a composite panel , when the panel reaches the bonding temperature where the adhesive melts or the theromplastic resin flows , we can apply gas pressure to the outer surfaces of the retort by pressure sources 52 and 54 to form the workpiece in regions remote from the bondline . pressure source 52 applies pressure to the upper surface of the retort 60 through a conduit 62 that passes through the upper die 20 and upper tool insert 46 , while pressure source 54 applies a pressure to the lower surface of the retort 60 through a conduit 64 that passes through the lower die 22 and lower tool insert 48 . the pressure applied to the retort 60 is maintained until the retort has formed to the contour of the forming surface 58 and the matrix resin has consolidated . the pressure sources 52 and 54 generally apply a differential pressure to the retort 60 . pin holes ( not shown ) in the tool inserts vent gas trapped between the retort 60 and the forming surface 58 as the retort deforms . such pin holes can be coupled to a flow meter to monitor the progress of the deformation . when the bonding is complete , the induction coil 35 is de - energized and the pressure relieved . the tool inserts and dies are separated . we remove the formed retort 60 from the press and recover the composite part from between the susceptor facesheets . an alternating oscillating electrical current in the induction coil 35 produces a time varying magnetic field that heats the susceptor sheets of the retort via eddy current heating . the frequency at which the coil driver 50 drives the coils 35 depends upon the nature of the retort 60 . we power the coil with up to about 400 kw at frequencies of between about 3 - 10 khz . current penetration of copper at 3 khz is approximately 0 . 06 inches ( 1 . 5 mm ), while penetration at 10 khz is approximately 0 . 03 inches ( 0 . 75 mm ). the shape of the coil has a significant effect upon the magnetic field uniformity . field uniformity usually is important because temperature uniformity induced in the retort is directly related to the uniformity of the magnetic field . uniform heating insures that different portions of the workpiece will reach the operating temperature at approximately the same time . solenoid type induction coils like those we illustrate provide a uniform magnetic field , and are preferred . greater field uniformity is produced in a retort that is located symmetrically along the centerline of the surrounding coil . those of ordinary skill can establish series / parallel induction coil combinations , variable turn spacing , and distances between the part and the induction coil by standard electrical calculations to achieve the desired heating from whatever coil configuration is used . the tool inserts and dies are usually substantially thermally insulating and trap and contain heat within the retort . since the dies and tool inserts are not inductively heated and act as insulators to maintain heat within the retort , the present invention requires far less energy to achieve the desired operating temperature than conventional autoclave or resistive hot press methods where the metal tooling is a massive heat sink . bonding operations using our workcell are faster than prior art operations because we do not heat the large thermal mass of either the dies or tool inserts . the retort is heated , the tool is not . thus , the necessary processing temperature is achieved more rapidly . in addition , the highly conductive materials in the retort provide rapid heat transfer to the workpiece . when the driver 50 is de - energized , the dies and the retort cool rapidly to a temperature at which we can remove the retort from the workcell , saving time and energy over conventional systems . coolant flowing through the coil tubes functions as an active heat exchanger to transfer heat out of the workpiece , retort , and dies . in addition , the thermal cycle is not as limited by the heating and cooling cycle of the equipment and tools so we can tailor the thermal cycle better to the process for which we are using the induction heating workcell . in a bonding or bonding - and - forming process for organic ( resin ) matrix composites , a composite panel assembly is laid - up from individual prefabricated composite sheets . the composite panel assembly includes a thermoplastic sheet that functions as a bonding agent between the prefabricated parts . the assembly is placed between a first sheet 100 and second sheet 102 of a susceptor ( usually aluminum , an aluminum alloy , or a &# 34 ; smart &# 34 ; susceptor ) to form a retort . as shown in fig4 & amp ; 5 , the susceptor sheets are sealed around their periphery with a crimp and seal ring 110 formed into the susceptor sheets . a first pressure zone 117 between the susceptors 100 and 102 surrounds the composite panel . in fig4 the susceptor sheets 100 and 102 contact the dies , without leaving additional pressure zones between the outer susceptors and the dies , as we described with reference to fig2 . when additional pressure zones are used , these zones receive pressurized forming gas through a system of conduits fabricated in the dies as described in u . s . pat . nos . 4 , 708 , 008 ; 5 , 129 , 249 ; or 5 , 309 , 747 or in u . s . patent application ser . no . 08 / 138 , 282 , which we incorporate by reference . if the retort incorporates the necessary pressure zones to allow forming , the dies can be porous . such dies do not need to carry or contain high pressure gases . they are lighter , are easier to make , and are less expensive . forming gas is introduced to pressure zone 118 between the two prefabricated composite panels 200 , such as carbon - fiber reinforced peek thermoplastic sheets , through suitable pressure lines to deliver pressurized inert gas which forms the panel in its &# 34 ; bead &# 34 ; region simultaneously with bonding in the regions to the immediate left and right of pressure zone 118 and the &# 34 ; bead &# 34 ; region , as shown in fig5 . where we intend to form bonds between the panels 200 and 202 , we sandwich a thermoplastic film 204 ( generally ultem ). such a film should melt at a lower temperature than the thermoplastic in the panels 200 and 202 so that bonding can occur without delaminating the panels . fig5 shows an optional silicone rubber pressure pads 206 between the lower die and the lower susceptor sheet 102 . we use these pads 206 to provide an even pressure across the entire bondline to correct for imperfections in the retort or dies that world otherwise leave isolated high spots . fig5 also shows shim plates 208 between the lower susceptor sheet 102 and the panel 202 in the bondline region to provide relief in gap 10 between the lower panel 202 and the lower susceptor sheet in the &# 34 ; bead &# 34 ; zone remote from the bondlines . while we have described that the part can be formed and bonded simultaneously , the operations can be done sequentially with forming preceding bonding . sequential processing is simpler but slower . we energize the coils with a time varying electrical field to produce a time varying magnetic field to heat the susceptors inductively to the bonding temperature of the composite panel . heat is transferred by conduction and / or radiation from the susceptors into the composite panel , so it , too , reaches bonding temperature . the shims transfer heat faster to the bondline so the ultem film bonding agent melts before the remote &# 34 ; bead &# 34 ; regions heat to their delaminating temperature . after completing bonding , we de - energize the induction coils and cool the retort and tool inserts to freeze the bonding agent ( e . g ., the adhesive , thermoplastic , or braze alloy ) in the joint . then we remove the retort from the tool inserts . although there is some heat transfer between the retort and the tool inserts , it is insufficient to heat the tool inserts or dies significantly because the dies are such good thermal insulators . therefore , the retort can quickly be pulled from the press . when the retort cools sufficiently , we remove the edge strips and recover the completed part . often the edge strips and the susceptor sheets are reusable . in one example of composite bonding in accordance with the present invention , we bonded two composite panels each comprising 48 layers of thermoplastic peek . im6 prepreg 3 / 8 inch thick . two aluminum sheets having a thickness of 1 / 16 inch were placed around the composite panel and aluminum shims were positioned in the bondline region between the lower susceptor and lower peek panel as shown in fig5 . we used a pressure pad as previously described and placed the retort in the tool inserts and inductively heated the assembly to a temperature of 550 ° f . in 15 minutes we maintained the retort at 550 ° f . for two minutes and then cooled it for 15 minutes . when we reached the bonding temperature of 550 ° f ., we applied a constant pressure of about 100 psi within pressure zone 117 until the part was cool . these times and pressures are representative only and would differ depending upon the composite material used and the thickness and complexity of the bonded part . the present invention is applicable to all types of organic matrix composites including both thermosetting and the thermoplastic composites such as epoxies , bismaleimides , polyimides , peek , pek , pekk , pes , or the like . if the materials have high solvent concentrations or the resins emit volatiles when they cure , we need to &# 34 ; bag &# 34 ; the workpiece to permit egress of these volatiles . therefore , we prefer using resins with low volatiles that are true thermoplastics , like peek . we can bond metals in a comparable process that we will describe in greater detail in section 4 . fig6 illustrates the bonding of thermoset facesheets 300 and 302 to a honeycomb core 304 using an adhesive film 306 in a cobond operation . the thermoset sheets and core are contained within two &# 34 ; 6061 &# 34 ; aluminum alloy susceptor sheets with silicone or shinitzu rubber overlay 308 configured to provide a lay - up of substantially constant thickness despite changes in the part configuration . fig6 shows a three susceptor sheet retort with two sheets 310 and 312 defining a pressure zone in which we can inject argon gas 314 to increase the bonding pressure . bonding pressure is transferred through the susceptor 310 to the rubber overlay 308 and into the upper thermoset sheet 300 when the temperature activates adhesive , typically around 375 ° f . for adhesives used with epoxy thermosets . the third susceptor sheet 316 underlies the facesheet 302 . the bonding time is about 1 hour with heat - up and cool - down taking about 15 min . each for a total cycle time of 90 mins . the surface of an aircraft wing skin must be maintained to a close tolerance to achieve an efficient aerodynamic surface . the tolerances of the inner mold line surface of the wing skin must also be maintained at a close tolerance at least in a buildup area where the wing skin will be joined to a spar to ensure that the wing skin and spar can be precisely joined . it is not critical , however , to control the inner mold line surface in areas where the wing skin is not attached to other structures . the composite panel has additional plies to define the buildup areas . the additional reinforce the composite panel in these areas which is necessary where a spar will be attached , and provide a convenient way to match the skin and spar to produce the desired outer wing configuration even if the spars are imprecise in their dimensions . we can fabricate built up areas at the faying surfaces to provide the precision fit , in which case we can eliminate shims . for brazing metal we prefer to use copper susceptor sheets about 0 . 032 - 0 . 062 inches thick , stainless steel , or a cobalt alloy &# 34 ; smart &# 34 ; susceptors as described in u . s . pat . no . 5 , 728 , 309 entitled : &# 34 ; method for achieving thermal uniformity in induction processing of organic matrix composites or metals ,&# 34 ; which we incorporate by reference . sometimes , the part itself can be the susceptor . copper is a good susceptor and allows higher processing temperatures than aluminum or aluminum alloys . copper also is an excellent susceptor material because it provides excellent heat transfer . copper &# 39 ; s excellent heat transfer properties help to ensure improved thermal uniformity . when processing metals , especially when using a copper retort at high temperatures , we typically use an inert atmosphere within the interior pressure zones to protect the copper and the parts being produced ( i . e . the workpiece ) against oxidation . that is , the inert gas purge protects the workpiece ( and the copper retort materials ) from oxygen damage . the susceptor can be a laminate of aluminum and copper . aluminum outer sheets efficiently convert the magnetic energy to heat . the underlying copper sheets transfer the heat well from the aluminum skin to the metal or resin workpiece . brazing of metals is essentially the same process as that described for the bonding of organic matrix composites , so we will not repeat it here . we substitute a braze alloy for the thermoplastic film or thermoset adhesive , and form braze joints between the metal sheets at selected locations . we can combine brazing with forming or with other operations as described in u . s . pat . no . 5 , 705 , 294 . as shown in fig7 the present invention also contemplates adhering two metal parts together using a hot melt , organic matrix resin thermoplastic or thermoset adhesive . in fig7 complementary machined aluminum missile fin halves 400 and 402 are bonded together with a thermoset adhesive 404 in the induction heating workcell . the adhesive is applied to the prepared surfaces that abut . in the process illustrated , we heat the parts directly with the induction coil 36 that surrounds the parts . this adhesive bonding process uses less expensive tooling than alternative processes , accomplishes the bonding in short thermal cycles , and is faster and cheaper than batch mode autoclave bonding operations . the process is just one more operation that one workcell can accomplish , thereby showing the versatility and agility of this flexible manufacturing workcell . while we have described preferred embodiments , those skilled in the art will readily recognize alterations , variations , and modifications which might be made without departing from the inventive concept . therefore , interpret the claims liberally with the support of the full range of equivalents known to those of ordinary skill based upon this description . the examples are given to illustrate the invention and not intended to limit it . accordingly , limit the claims only as necessary in view of the pertinent prior art . | 1 |
wherein r1 represents an optionally substituted 5 - 6 membered aromatic hetero ring containing nitrogen atom , except a non - substituted 2 - pyridyl ; r2 represents a hydrogen , a carbamoyl , a mono or di c1 - 5 alkyl carbamoyl , a thiocarbamoyl , a mono or di c1 - 5 alkylthiocarbamoyl , a sulfamoyl , a mono or di c1 - 5 alkylsulfamoyl , an optionally substituted c1 - 5 alkyl , an optionally substituted c2 - 5 alkenyl , an optionally substituted c2 - 5 alkynyl , an optionally substituted c3 - 8 cycloalkyl , an optionally substituted c3 - 8 cycloalkenyl , an optionally substituted aryl or - y - r5 ; r5 represents a hydrogen , an optionally substituted c1 - 5 alkyl , an optionally substituted c2 - 5 alkenyl , an optionally substituted c2 - 5 alkynyl , an optionally substituted c3 - 8 cycloalkenyl or an optionally substituted aryl ; r3 represents a hydrogen , an optionally substituted c1 - 5 alkyl , an optionally substituted c2 - 5 alkenyl , an optionally substituted c2 - 5 alkynyl , an optionally substituted c3 - 8 cycloalkyl or an optionally substituted c3 - 8 cycloalkenyl ; the present invention provides a method of protecting a crop by combatting eggs of insects susceptible to damage the said crop whereby an effective amount of a compound of formula ( i ), or a salt thereof , is applied at a locus where there are eggs or where eggs are expected to be present or where eggs are expected to be going to be present . according to the invention it has also been found ovicidal compositions which comprise an effective amount of a compound of formula ( i ) or a salt thereof . the present invention provides a method of protecting a crop by combatting eggs of insects susceptible to damage the said crop whereby an effective amount of an ovicidal composition as already defined is applied at a locus where there are eggs or where eggs are expected to be present or where eggs are expected to be going to be present . another feature of the present invention is that an ovicidal composition is applied at a locus where a crop is growing , especially a plantation crop , more especially cotton . the method of the invention is particularly appropriate to kill or control the following insects at the egg stage : tobacco budworm ( heliothis virescens ), mexican bean beetle ( epilachna varivestis ), colorado potato beetle ( leptinotarsa decemlineata ). the method of the invention is especially advantageous to kill tobacco budworms , at the egg stage , which are resistant to pyrethroids . the method of the invention is particularly appropriate to protect cotton crop from tobacco budworm or pyrethroid resistant tobacco budworm , beans and soybean from mexican bean beetle , potato crop from colorado potato beetle . preferred active ingredients which may be used in the invention are those wherein : the preparation of compounds of formula ( i ), or a salt thereof , may be made according to any process described in patent application wo 91 / 04965 , or other process according to the knowledge of a man skilled in the art of chemical synthesis . the disclosure of wo 91 - 4075 is in toto incorporated herein by reference . by the term &# 34 ; eggs &# 34 ; as used in this specification , it is to be understood eggs which are in their simple state laid upon the soil or on the plant or eggs which are inside pregnant insect . most of the eggs which are to be killed according to the present invention are eggs upon leaves , so that the method whereby an active ingredient of formula ( i ), or a salt thereof , is applied is also a treatment of leaves of crops . the invention enables compounds of formula ( i ), or salts thereof , to combat insects , especially the tobacco budworm , at the egg stage before they reach the damaging later stages . thus , compounds of formula ( i ), or salts thereof , are applied to the locus to be treated before substantial infestation with tobacco budworm larvae occurs . for instance , on cotton plants , an ovicidal composition comprising a compound of formula ( i ), or a salt thereof , should be applied to eggs before applying it to the larval stage , preferably 4 to 7 days before one would first apply such a composition to the larval stage of tobacco budworm . the ovicidal compositions of the invention may be applied once , or more than once . thus , for some crops one may apply the ovicidal compositions periodically through the insects season . usually ovicidal compositions according to the invention are applied to the crop area at a rate of 0 . 04 to 2 kg / ha of active ingriedent , preferably 0 . 1 to 1 kg / ha . ovicidal compositions according to the invention may be applied in a manner which is safe for the crop . the ovicidal concentrated compositions according to the invention may be in the form of a solid , e . g . dusts or granules or wettable powders , or , preferably , in the form of a liquid , such as an emulsifiable concentrate or a true solution . the concentrated compositions are the compositions which are commercialized or transported or stored . for application to plant they are normally diluted in water and applied in such a diluted form . the diluted form are part of the invention as well as the concentrated forms . the concentrated ovicidal compositions of the inventions contain generally from 0 . 001 to 90 % of active ingredient of formula ( i ), or a salt thereof . a concentrate may contain from 5 to 90 % of active ingredient . parts and percentages in this specification are by weight unless otherwise indicated . the ovicidal compositions may also contain all kind of compatible surface active agent and / or carrier . the agriculturally acceptable carrier may be solid or liquid . the composition may further contain a fertilizer . the compounds of formula ( i ), or a salt thereof , may be used in sequence or admixture , particularly admixtures with another pesticide e . g . an insecticide , acaricide or fungicide . ( 6 - cl pyrid 3 - yl )- ch2 - n ( ch3 )- c ( ch3 )═ n - cn was dispersed in a mixture of acetone / surfactant / dimethylformamide and then diluted in water . strips of cheese cloth which contained about 30 to 40 one day old eggs of tobacco budworm were used . they were eggs of tobacco budworm non resistant to pyrethroids . the aqueous dispersion of active ingredient was sprayed upon the eggs . the application condition were such that a 1000 ppm concentration corresponds to an application rate of 188 g / ha on the crop . the observation of the obtained results was made three days after spraying . the dead eggs are brown and do not hatch ( they normally hatch about 3 to 4 days after being laid down ). a lethal dose killing 90 % of the eggs was found at 1000 ppm . a lethal dose killing 50 % of the eggs was found at 230 ppm . example 1 was repeated , except that eggs of pyrethroids resistant tobacco budworm were used . a lethal dose killing 64 % of the eggs was found at 250 ppm ( 6 - cl pyrid 3 - yl )- ch2 - n ( ch3 )- c ( ch3 )═ n - cn was dispersed in a mixture of acetone / surfactant / dimethylformamide and then diluted in water . strips of bean plant leaves bearing about 65 one day old eggs of mexican bean beetle were used . the aqueous dispersion of active ingredient was sprayed upon the eggs , the application condition were such that a 1000 ppm concentration corresponds to an application rate of 188 g / ha on the crop . the observation of the obtained results was made three days after spraying , the dead eggs are brown and do not hatch ( they normally hatch about 7 days after being laid down ). a lethal dose killing 100 % of the eggs was found at 250 ppm . ( 6 - cl pyrid 3 - yl )- ch2 - n ( ch3 )- c ( ch3 )═ n - cn was dispersed in a mixture of acetone / surfactant / dimethylformamide and then diluted in water . strips of egg plant leaves bearing about 20 one day old eggs of colorado potato beetle were used . eggs of beetles resistant as well as non resistant to pyrethroids were used . the aqueous dispersion of active ingredient was sprayed upon the eggs . the application condition were such that a 1000 ppm concentration corresponds to an application rate of 188 g / ha on the crop . the observation of the obtained results was made three days after spraying . the dead eggs are brown and do not hatch ( they normally hatch about 5 days after being laid down ). a lethal dose killing 100 % of the eggs of both type of beetles was found at 250 ppm . | 0 |
fig1 shows a schematic sectional side view of a basic multi - layer thermistor structure according to an example embodiment of the present invention . the thermistor structure is formed on a substrate 10 and comprises a first metallic layer 12 , a layer of particulate silicon 14 printed onto the first metallic layer 14 , and a second metallic layer 16 deposited onto the layer of particulate silicon 14 . as indicated above , the substrate 10 can take many forms , but will typically comprise a flexible sheet , which may , for example , be composed of a solid film such as a metal foil or polymer sheet ; a fibrous material such as paper and felted materials ; or a woven fabric . these examples are provided merely for illustrative purposes and are not intended to be limiting . the metallic layers and the particulate silicon layer are preferably deposited by printing as defined above . in the embodiment of fig1 , the substrate 10 is either non - conducting or , if conducting , does not serve as an electrical contact to the thermistor structure . in this embodiment , the first and second metallic layers 12 and 16 serve as conducting electrodes or contacts , to which respective wires or other conductors 18 and 20 can be connected . several example embodiments of thermistors produced by the methods of the invention are described below with reference to fig2 to 8 . the first embodiment , as shown in fig2 , is a bottom - contact two - terminal thermistor . this embodiment includes two elongate conducting contacts 22 and 24 formed on a substrate 26 , which extend side by side and which may be arranged in a pattern such as a spiral to cover a relatively large area . the contacts are connected or bridged by a layer 28 of printed particulate silicon having an elongate spiral shape and which partially overlies the respective contacts , the whole structure being supported by the substrate . electrical connections can be made to the contacts 22 and 24 as required . instead of the illustrated squared - off spiral shape , the contacts and the bridging layer of particulate silicon may follow another parallel meander or curved spiral path . the thermistor structure may cover a relatively large area , to allow the average temperature of a large and possibly irregularly shaped area of the substrate 26 ( or an object to which the substrate 26 is attached ) to be monitored . a similar top contact device may be fabricated by simply reversing the deposition sequence , with the layer of particulate silicon being printed first and the contacts being deposited over it . in an alternative approach , the silicon strip may form a continuous layer deposited on or underneath the contact strips . fig3 is an illustration of an interdigitated two terminal thermistor consisting of two interdigitated electrical contacts 30 and 32 , which are connected or bridged by a layer 34 of printed particulate silicon . the contacts 30 and 32 each have a plurality of elongate strips or fingers 36 and 38 which extend parallel and adjacent to one another to define a serpentine gap over which a layer of silicon ink is printed to form the layer 34 and to connect the two sets of electrodes . the number and length of the contacts or electrodes and their fingers may be varied to cover any desired area . the thermistor is printed on a substrate 40 . this silicon layer 34 may be structured to follow the gaps between the electrodes as shown , or may form a continuous layer . the device may be either a bottom - contact or top - contact device , depending on the order of deposition of the materials as described above . fig4 shows an embodiment in which the electrical path of the thermistor is in the radial direction of a circular structure having an inner electrical contact 42 and a concentric ring - shaped outer contact or electrode 44 . the contacts are connected by an annular layer of printed particulate silicon 46 . the thermistor is printed on a substrate 48 fig5 shows a similar embodiment to that of fig4 , in which the two contacts comprise a solid inner circle 50 and a concentric outer ring 52 deposited in a coaxial geometry . a printed particulate silicon layer 54 forms a second concentric ring , bridging the two contacts . however , in the device of fig5 the inner electrode contact 50 is extended radially outwardly to a first electrical contact pad through a gap in the outer contact 52 . the outer contact is also extended outwardly to a second electrical contact pad 58 . the structure is printed on a substrate 60 . the concentric ring defined by the printed silicon layer 54 , which bridges the annular gap between the two contacts , may be either complete or broken ( as illustrated ). the example embodiments of fig4 and 5 , which may be fabricated as either top - contact or bottom - contact devices , are specifically adapted to printing processes . the radial electrical path of these thermistor structures ensures that the resistance measured is averaged over all directions relative to the printing direction , thus eliminating the effect of any lateral anisotropy in the deposition process . for higher accuracy , thermistor devices adapted for use in the well known four point resistance measurement technique may be desirable . this may be achieved by a device having four coplanar electrodes as indicated in fig6 . this device has two finely structured inner electrodes 62 and 64 between which the potential difference is determined and two additional electrodes 66 and 68 through which a current is supplied . all four electrodes are connected by an over - printed layer 70 of printed particulate silicon . the device is formed on a substrate 72 . each of the inner electrodes 62 and 64 has an enlarged contact pad at each end thereof . the two inner electrodes 62 and 64 are used to measure the potential difference in the particulate silicon layer , and may be very finely printed . the outer electrodes 66 and 68 are used to supply an excitation current and may be relatively large compared to the inner electrodes . in the simplest variation of this geometry , as illustrated , the silicon layer 70 is simply printed as a thick strip bridging the four electrodes in a central area of the device . an alternative to the four point resistance method is to use any of the well - known van der pauw geometries , such as the circular design shown in fig7 or the “ greek cross ” geometry shown in fig8 . in the printed thermistor device of fig7 , four equispaced wedge - shaped electrical contacts 74 , 76 , 78 and 80 are provided , connected by a layer 82 of printed particulate silicon having a solid circular shape . the device is printed on a substrate 84 . the four contacts are arranged symmetrically in a circular pattern with a space in the centre of the pattern which is filled by the layer of printed silicon . to obtain the highest accuracy , this latter layer should have a circular form and be centrally located . however , this is not essential , and adequate devices can be produced by printing a continuous layer of silicon onto or underneath the electrodes . in the device of fig8 , four electrodes 86 , 88 , 90 and 92 are deposited symmetrically on a substrate 94 . a layer 96 of particulate silicon is deposited in a central region of the device between the contacts . the layer 96 has a greek cross geometry , with the tips of the arms of the cross partially overlying the respective electrodes and defining two perpendicular silicon paths between the electrodes . further well known variations of the van der pauw geometry which can be defined by thermistors of the invention include structures which combine the geometrical features of these two basic forms , such as a clover leaf or maltese cross . a novel method of determining the temperature dependent resistance , made possible by the use of printing to fabricate the devices , is to extend the principles of the van der pauw technique by having the same symmetrical electrode structure forming top and bottom contacts . any of the two - contact designs presented above can be used to determine the resistance through the bulk of the silicon layer in an analogous method to the standard four - point van der pauw technique . similarly , four - electrode configurations applied as both top and bottom contacts will give an even higher accuracy and stability of the resistance measurement . furthermore , any of the above designs , or similar arrangements of electrodes , can be arranged in an array over a large area on the substrate to form a pixellated sensor which will allow the temperature distribution over a given area to be mapped . in a first example a negative temperature coefficient thermistor was produced according to the design shown in fig6 . four silver electrodes or contacts were deposited on 80 g / m 2 wood - free paper sheet substrate by screen - printing using du pont 5000 silver conductor . the separation between any two adjacent electrodes was 2 mm . after allowing the silver ink to dry for approximately one day under ambient conditions , silicon ink was drop - cast to form a connection between all four electrodes of the device . the silicon nanoparticles used in the ink were milled from a boron doped p - type silicon wafer , according to the method disclosed in wo 2009 / 125370 . these particles were mixed with a commercially available acrylic screen - printing base in a ratio of 95 % silicon by weight , and the consistency of the ink was adjusted by thinning with propylene glycol . the completed device was cut out from the larger sheet of paper to form a small flexible device of size approximately 15 mm by 10 mm . in preliminary tests , the room temperature current / voltage characteristics were determined by both four - point and two - point techniques . for testing its temperature response , this device was fixed with adhesive tape to the outside of a glass beaker of diameter 65 mm , such that the paper substrate was between the printed thermistor device and the glass , and so that the axis of the device followed the circumference of the glass . to calibrate the temperature dependence of the resistance , the beaker was filled with iced water and heated on an electric hotplate , while the temperature of the water was measured with a digital thermometer . for convenience the resistance was simply measured with a digital multimeter . fig9 shows the resistance temperature response of the thermistor on an arrhenius scale . in the temperature range indicated , the device exhibits a logarithmic temperature coefficient , commonly referred to as a beta value , of 2 210 ± 30k . in a second example a negative temperature coefficient thermistor was produced , also according to the design shown in fig5 . silver contacts were deposited on a substrate comprising a sheet of 80 g / m 2 wood - free paper by screen - printing using du pont 5000 silver conductor . the diameter of the inner electrode was 5 mm , and the separation between the two electrodes was 0 . 5 mm . after allowing the silver ink to dry for approximately one day under ambient conditions , a silicon layer was screen - printed over the gap between the electrodes , using silicon nanoparticles milled from 2503 grade metallurgical silicon according to the method disclosed in wo 2009 / 125370 . these nanoparticles were mixed with a commercially available acrylic screen - printing base in a ratio of 88 % silicon by weight , and the consistency of the ink was adjusted by thinning with propylene glycol . the completed device was cut out from the larger sheet of paper to form a small flexible device of size approximately 20 mm by 15 mm . silver wires were soldered to the contact pads to form secure permanent connections . current / voltage characteristics were measured for the device , in the temperature range 50k to 350k , using a lake shore 7700 hall measurement system , and associated cryostat , under zero magnetic field conditions . the resistance / temperature characteristics shown as an example in fig1 were determined from the slope of the voltage / current characteristics at low excitation current . over an extended temperature range , there are at least two arrhenius coefficients , of typically 1 000k at liquid nitrogen temperatures and 2 000k around room temperature . further studies of similar devices indicate a third beta value of approximately 10 000k which is apparent at temperatures above 350k . the combination of these different beta values in different ranges allows the printed silicon thermistors to be applied over a wide range of temperatures . fig1 is a photograph of a negative temperature coefficient thermistor according to the design shown in fig3 . in this case the silicon is printed as a solid block over the interdigitated silver contacts , but only the area of silicon deposited between the contacts contributes to the temperature dependent resistance . for a low resistance , the length to width aspect ratio of the silicon semiconductor should be low , ideally less than 1 / 1 000 . in this example , the silver contacts comprise 25 individual electrodes , with 24 gaps between adjacent electrodes , each gap having a length of 16 mm and the width of each gap ( the separation between adjacent electrodes ) of 0 . 25 mm . in contrast to the device of example 2 , which is a high resistance device and has a length to width aspect ratio of approximately 1 / 30 ( given by the ratio of the transverse gap between the conductors to the circumference of a circle defining the gap between the conductors in fig5 ), the design of the present example has an aspect ratio of 1 / 1 600 , and a correspondingly lower resistance for the same silicon layer thickness . the silver contacts were deposited by screen printing on 160 gsm paper board substrates using du pont 5000 silver conductor . after allowing the silver ink to dry for approximately one day under ambient conditions , a silicon layer was screen - printed over the gap between the electrodes , using silicon nanoparticles milled from 2503 grade metallurgical silicon according to the method disclosed in wo 2009 / 125370 . these nanoparticles were mixed with a commercially available acrylic screen - printing base in a ratio of 80 % silicon by weight , and the consistency of the ink was adjusted by thinning with propylene glycol . the final thermistor was then packaged as a discrete component according to the method disclosed in south african provisional patent specification 2010 / 06533 , with the silver contacts being allowed to protrude from the plastic lamination . tests of many such devices were conducted in a box oven , over a temperature range from 20 ° c . to 60 ° c ., yielding a consistent beta value of 2 000 k with a statistical variation of ± 100 k . typical resistances , depending on the thickness of the silicon layer , are 100 kω . detailed analysis of the conductance from low temperature measurements using a lake shore 7700 system , over an extended temperature range from 15 k to 350 k , showed three characteristic beta values of approximately 20 k , 650 k and 1 900 k . fig1 is a photograph of variation of the interdigitated thermistor described in example 3 , according to the basic design of fig3 , which is extended over a larger area , and which takes its form as a graphic design . as an example a full size human handprint was chosen as the design , but any other abstract or pictorial design could have been selected without restriction . a plurality of silver tracks , with their common connections forming the outline of the hand , are screen printed , using du pont 5000 silver conductor on various colours of 180 gsm paper board , to form the interdigitated electrodes . the gaps between the electrodes are adjusted to fit the shape of the design , and range from 0 . 5 mm to 1 mm . silicon ink , comprising 80 % by weight of nanoparticles milled from 2503 grade silicon according to the method disclosed in wo 2009 / 125370 , is printed in different positions to form both the graphic design and a set of thermistors connected in parallel . equally the whole area of the hand could have been printed in silicon , but this was not done to allow an illustration of the principles of construction and operation of the thermistor . after printing , the thermistor was packaged as a discrete component according to the method disclosed in south african provisional patent specification 2010 / 06533 , with the silver contacts being allowed to protrude from the plastic lamination . typical resistances for this design , depending on the thickness of the silicon layer , are between 20 and 40 kω , and the beta value is consistent at 2 000 ± 100 k . | 7 |
as shown in fig1 , vehicle 10 has a passenger airbag restraint , 48 , and a driver &# 39 ; s airbag restraint , 50 , mounted adjacent steering wheel 52 . a fire suppression system includes controller 66 which is mounted upon floor pan 68 of vehicle 10 , and reservoirs 18 which are mounted under floor pan 68 in the so - called kick - up area adjoining the rear axle of vehicle 10 . those skilled in the art will appreciate in view of this disclosure that additional passenger restraint devices , such as seat belt pretensioners and side airbags , may be installed in a vehicle and controlled at least in part by , or in conjunction with , controller 66 . fig1 shows not only reservoirs 18 but also a portion of right and left side fire suppression conduits 28 , as well as fixed geometry nozzles 30 and variable geometry nozzles 36 . as seen in fig1 , variable geometry nozzles 36 project downwardly to allow fire suppression agent to be expelled from reservoirs 18 and placed at a low angle to the ground surface the vehicle is operating upon . this mode of operation is possible because variable geometry nozzles 36 are , as shown in fig2 , telescopingly extensible . this telescoping feature , which is shown in greater detail in fig8 , is produced by a sliding spray head , 40 , which is slidingly engaged with conduit 28 such that gas pressure within conduit 28 forces spray head 40 downwardly into its extended position , causing fire suppression agent 22 to be discharged through a number of holes 42 formed in spray head 40 . as shown in fig2 , at least two variable geometry nozzles 36 may be employed with single reservoir 18 , along with at least two fixed nozzles 30 which are spray bars each having a number of orifices 34 . while in their normally closed state , variable geometry nozzles 36 are liquid - tight by virtue of seals 46 , which are interposed between an end of each of spray heads 40 and the corresponding ends of conduits 28 . in a preferred embodiment , seals 46 comprise elastomeric boots attached to an outer surface of conduit 28 . seals 46 are simply sheared by the deploying spray head 40 when the present system is discharged . fixed nozzles 30 are also rendered liquid - tight by covers 44 , which are simply blown off when the present system is discharged . the sealing of nozzles 30 and 36 is important , because this prevents the ingress of road splash , which could block the system in sub - freezing weather or cause corrosion or blockage due to mud or other foreign matter . additional details of reservoir 18 are shown in fig7 . tank 90 contains approximately 1 . 5 l of fire suppression agent 22 , and a propellant 92 . propellant 92 includes two squibs ( not shown ) which are activated simultaneously by controller 66 via lines 91 so as to release a large amount of gas , forcing fire suppressant agent 22 from tank 90 and into distribution system 26 , including conduit 28 and the various fixed and variable geometry nozzles . a preferred propellant , marketed by primex aerospace company as model fs01 - 40 , is a mixture including aminotetrazole , strontium nitrate , and magnesium carbonate . this is described in u . s . pat . no . 6 , 702 , 033 , which is hereby incorporated by reference into this specification . those skilled in the art will appreciate in view of this disclosure that other types of propellants could be used in the present system , such as compressed gas canisters and other types of pyrotechnic and chemical devices capable of creating a gas pressure force in a vanishingly small amount of time . moreover , fire suppressant agent 22 , which preferably includes a water - based solution with hydrocarbon surfactants , fluorosurfactants , and organic and inorganic salts sold under the trade name lvs wet chemical agent ® by ansul incorporated , could comprise other types of agents such as powders or other liquids , or yet other agents known to those skilled in the art and suggested by this disclosure . if two reservoirs 18 are employed with a vehicle , as is shown in fig1 , all four squibs will be deployed simultaneously . fig4 shows manually activatable switch 54 for use with the present system . as shown in fig1 , switch 54 may be advantageously located on the headliner of vehicle 10 between the sun visors , or at any other convenient position . to use this switch 54 , hinged clear cover 56 is first opened by pressing on cover 56 . thereafter , the fire suppression system may be triggered by manually pressing pushbutton 58 . if the vehicle occupants are not disposed to release cover 56 , the system may be triggered by merely sharply depressing cover 56 , thereby closing contacts ( not shown ) contained within platform 60 . because the present system is intended for use when the vehicle has received a severe impact , controller 66 , which is shown in fig3 , contains a redundant power reserve or supply , which allows operation of the fire suppression system for about nine seconds , even if controller 66 becomes isolated from the vehicle &# 39 ; s electrical power supply . wiring harness 80 , as shown in fig5 , is armored , and has a para - aramid fiber inner sheath , 82 , of about 2 mm in thickness , which helps to shield the conductors within harness 80 from abrasion and cutting during a vehicle impact event . this para - aramid fiber is sold under the trade name kevlar ® by the dupont company . this armoring helps to assure that communication between controller 66 and reservoirs 18 remains in effect during an impact event . post - impact communications are further aided by redundancy in the control system . specifically , four independent sets of primary conductors , 79 a - d , extend from controller 66 to reservoirs 18 protected by sheath 82 . moreover , an h - conductor , shown at 81 in fig5 , extends between reservoirs 18 . thus , if one or both of the primary conductors 79 a - b , or 79 c - d , extending to one of reservoirs 18 should become severed , h - conductor 81 will be available to carry the initiation signal from the undamaged lines to both of reservoirs 18 . as noted above , an important feature of the present invention resides in the fact that the control parameters include not only vehicle impact , as measured by an accelerometer such as that shown at 70 in fig9 , but also vehicle speed , as measured by means of speed sensors 74 , also shown in fig9 . speed sensors 74 may advantageously be existing sensors used with an anti - lock braking system or vehicle stability system . alternatively , speed sensors 74 could comprise a global positioning sensor or a radar or optically based ground - sensing system . accelerometer 70 , as noted above , could be used with a conventional occupant restraint airbag system , thereby maximizing use of existing systems within the vehicle . advantageously , accelerometer 70 may be an amalgam of two or more accelerometers having differing sensing ranges . such arrangements are known to those skilled in the art and suggested by this disclosure . at least a portion of the various sensors could either be integrated in controller 66 or distributed about vehicle 10 . fig6 shows a sequence which is used according to one aspect of the present invention for activating a release of fire suppressant agent . beginning at block 100 , controller 66 performs various diagnostics on the present system , which are similar to the diagnostics currently employed with supplemental restraint systems . for example , various sensor values and system resistances will be evaluated on a continuous basis . controller 66 periodically moves to block 102 , wherein the control algorithm will be shifted from a standby mode to an awake mode in the event that a vehicle acceleration , or , in other words , an impact , having a magnitude in excess of a relatively low threshold is sensed by accelerometer 70 . also , at block 102 a backup timer will be started . if the algorithm is awakened at block 102 , controller 66 disables manually activatable switch 54 at block 104 for a predetermined amount of time , say 150 milliseconds . this serves to prevent switch 54 from inadvertently causing an out - of - sequence release of fire suppression agent . note that at block 104 , a decision has not yet been made to deploy fire suppression agent 22 as a result of a significant impact . at block 106 , controller 66 uses output from accelerometer 70 to determine whether there has been an impact upon vehicle 10 having a severity is in excess of a predetermined threshold impact value . such an impact may be termed a significant , or “ trigger ”, impact . if an impact is less severe than a trigger impact , the answer at block 106 is “ no ”, and controller 66 will move to block 105 , wherein an inquiry is made regarding the continuing nature of the impact event . if the event has ended , the routine moves to block 100 and continues with the diagnostics . if the event is proceeding , the answer at block 105 is “ yes ”, and the routine loops to block 106 . if a significant impact is sensed by the sensor system including accelerometer 70 and controller 66 , the answer at block 106 will be “ yes .” if such is the case , controller 66 moves to block 108 wherein the status of a backup timer is checked . this timer was started at block 102 . once the timer within controller 66 has counted up to a predetermined , calibratable time on the order of , for example , 5 - 6 seconds , controller 66 will cause propellant 92 to initiate delivery of fire suppressant agent 22 , provided the agent was not released earlier . propellant 92 is activated by firing an electrical squib so as to initiate combustion of a pyrotechnic charge . alternatively , a squib may be used to pierce , or otherwise breach , a pressure vessel . those skilled in the art will appreciate in view of this disclosure that several additional means are available for generating the gas required to expel fire suppressant agent 22 from tank 90 . such detail is beyond the scope of this invention . an important redundancy is supplied by having two squibs located within each of tanks 90 . all four squibs are energized simultaneously . the velocity of the vehicle 10 is measured at block 110 using speed sensors 74 , and compared with a low velocity threshold . in essence , controller 66 processes the signals from the various wheel speed sensors 74 by entering the greatest absolute value of the several wheel speeds into a register . this register contains both a weighted count of the number of samples below a threshold and a count of the number of samples above the threshold . when the register value crosses a threshold value , the answer at block 110 becomes “ yes ”. in general , the present inventors have determined that it is desirable to deploy fire suppression agent 22 prior to the vehicle coming to a stop . for example , fire suppression agent 22 could be dispersed when the vehicle slows below about 15 kph . at block 112 , controller 66 enters a measured vehicle acceleration value into a second register . thereafter , once the acceleration register value decays below a predetermined low g threshold , the answer becomes “ yes ” at block 112 , and the routine moves to block 114 and releases fire suppressant agent 22 . in essence , a sensor fusion method combines all available sensor information to verify that the vehicle is approaching a halt . the routine ends at block 116 . because the present fire suppression system uses all of the available fire suppression agent 22 in a single deployment , the system cannot be redeployed without replacing at least reservoirs 18 . fig6 does not include the activation of occupant restraints 48 and 50 , it being understood that known control sequences , having much different timing constraints , may be employed for this purpose . in point of contrast , the low velocity threshold allows the present system to deliver the fire suppression agent while the vehicle is still moving , albeit at a very low velocity . this prevents the rear wheels of the vehicle from shadowing , or blocking dispersion of fire suppressant agent 22 . also , in many cases , a vehicular fire may not become well - established until the vehicle comes to a halt . fig1 and 11 illustrate an additional nozzle embodiment according to another aspect of the present invention . rather than having a stamped and welded construction , nozzle 232 is porous . the porous material may be either ceramic , or sintered metal , or other types of porous materials known to those skilled in the art and suggested by this disclosure . the material may be cast , or pressed , or extruded , or formed by any other suitable method . fig1 shows nozzle body 236 in its stowed position , and fig1 shows nozzle body 236 in its telescopically deployed position , which results from the buildup of fluid pressure within feeder conduit 28 . while in the stowed position of fig1 , nozzle body 236 is retained within feeder conduit 28 by frangible sealing disc 252 , which functions as a stowage seal by sealing against annular surface 258 formed in the end of feeder conduit 28 . frangible sealing disc 252 is maintained in contact with annular surface 258 by means of external seal retainer 260 , which is attached to the outer end of feeder conduit 28 . frangible sealing disc 252 serves not only to prevent the ingress of contamination into feeder conduit 28 when nozzle body 236 is in its stowed position , but also prevents the escape of fire suppression agent from the closed , or bulkhead end , 244 of nozzle body 236 . this feature may be used to tune or adjust the distribution of fire suppression agent from nozzle 232 . when nozzle body 236 is projecting telescopically from feeder conduit 28 , integral stop abutment and fluid seal 248 cooperates with internal stop abutment 256 formed at the end of conduit 28 to both seal the joint between nozzle body 236 and feeder conduit 28 , and to prevent nozzle body 236 from separating from feeder conduit 28 in response to the fluid pressure of the flowing fire suppressant agent . fig1 , 13 , and 14 illustrate another aspect of the present invention . a quick connect coupler attaches the fire suppressant feeder conduit to the suppressant reservoir . this facilitates assembly of the present fire suppression system in the underbody environment of a vehicle , thereby reducing assembly cost , while helping to assure integrity of the fire suppression system . reservoir 18 is equipped with a spud , 200 , having external threads , 204 . threads 204 are interrupted . the importance of this feature will be explained below . feeder conduit 28 has an annular retention flange , 208 , which abuts collar 216 when feeder conduit 28 is attached to reservoir 18 . a section of a fully assembled joint consisting of feeder conduit 28 , spud 200 , collar 216 , and o - ring seal 212 is shown fully assembled in fig1 . threads 220 , which are formed internally on collar 216 , cooperate with threads 204 formed on spud 200 to lock the various components together . o - ring seal is compressed between bore 202 of spud 200 and an outer surface of conduit 28 , so as to provide a leak - tight seal between spud 200 and conduit 28 . the joint of fig1 is made up by inserting conduit 28 into spud bore 202 until retention flange 208 abuts spud 200 . then , collar 216 is brought into contact with spud 200 and collar 216 is rotated to lock threads 204 and 220 . because each of threads 204 and 220 are interrupted — i . e ., they do not circumscribe the bases to which they are attached , collar 216 may be fully driven and seated upon spud 200 with less than one full revolution . this greatly facilitates assembly of the present system under a vehicle body . fig1 illustrates an anti - rotation feature provided by axially displaceable pints 224 . when collar 216 has been fully rotated upon spud 200 , pins 224 will be extended by compression springs ( one spring , 228 being shown ). once pins 224 have extended , rotation of collar 216 in a direction permitting detachment of collar 216 from spud 200 will be prevented because each of pins 224 will abut one of threads 204 formed on spud 200 . fig1 a and 15 b illustrate a fire suppressant reservoir , 264 , formed as a composite characterized by a pressure vessel having an outer wall , 268 , combined with a sealing liner , 272 . outer wall 268 may be formed from metal or fiber reinforced resin , or other metallic or nonmetallic materials or composites known to those skilled in the art and suggested by this disclosure . liner 272 is said to be a dynamic reservoir seal because liner 272 is sufficiently extrudable in response to fluid pressure produced by the propellant device that liner 272 will extrude or squeeze directly into discontinuities caused by the high operating pressure of the present fire suppression system . this extrusion will seal outer wall 268 , preventing an excessive loss of the fire suppressant agent . in fig1 b , portion 280 of liner 272 is shown as having extruded through discontinuity 276 . as shown in fig1 b , portion 280 is in sealing engagement with outer wall 268 . sealing liner 272 may be formed from plastics or metals , elastomers , composites , or yet other materials known to those skilled in the art and suggested by this disclosure . in any event liner 272 is selected to provide the pressure - driven extrusion characteristic needed to seal outer wall 268 if a high pressure leak develops in reservoir 18 . fig1 shows a second type of propellant useful for practicing the present invention . compressed gas cylinder 284 is pre - charged with a high pressure gas , such as nitrogen . valve 288 , which is operatively connected with controller 66 , is opened when needed to permit gas to flow from cylinder 284 and through high pressure conduit 292 , thereby initiating discharge of the fire suppressant agent from reservoir 18 . as but one alternative to the arrangement shown in fig1 , gas cylinder 284 could be located within reservoir 18 in the manner shown in fig1 a and 15 b , albeit at the expense of volume for the fire suppressant agent . the present compressed gas propellant provides a supply - chain advantage , inasmuch as non - pyrotechnic propellants are subject to less stringent shipping restrictions than are pyrotechnic devices . fig1 illustrates a system for connecting high pressure conduit 292 with reservoir 18 . a dome , 298 is provided in an upper surface of reservoir 18 . dome 298 has a port , 296 , through which conduit 292 extends into the interior of reservoir 18 . as conduit 292 is inserted , it displaces valve disc 308 and spring 312 . conduit 292 is retained within port 296 by means of retainer 300 , which passes through holes ( not shown ) formed dome 298 . once conduit 292 has been installed , high pressure gas may flow into reservoir 18 through a series of exit orifices 304 formed in conduit 292 . according to another aspect of the present invention , a fire suppressant agent used with this system may be either a single component , generally an aqueous - based preparation , or a binary system in which a primary component is carried within a first , or primary , reservoir , and a secondary component , such as potassium carbonate , is carried within a secondary reservoir accessible to the fire suppression system &# 39 ; s feeder conduits . passage of the primary component through a feeder conduit will cause the secondary component to be released such that the primary component and the secondary component will be combined before being discharged from the distribution nozzles . in essence , the purpose of the secondary component delivery system is to place the secondary component into a stream of primary component flowing within the present distribution system . if the secondary delivery system is housed within feeder conduit 28 , the need for an additional discrete reservoir for the secondary component may be avoided . fig1 a - 18 d illustrate several embodiments of secondary reservoirs . fig1 a shows a secondary reservoir defined by venturi tube 316 , which establishes an annular - shaped storage chamber , 320 within feeder conduit 28 . a number orifices , 324 are formed at the throat , 322 , of venturi tube 316 , such that primary component flowing through venturi tube 316 will cause secondary component 318 to be drawn through orifices 324 and aspirated into the flowing primary component stream . in the embodiment of fig1 a , secondary component 318 could be in either a liquid or a powder state . fig1 b illustrates a secondary reservoir having a generally cylindrical housing , 328 , which is filled with secondary component 318 in either a powder or gelatinous state . as with the embodiment of fig1 a , housing 328 is located within feeder conduit 28 . pressure - responsive piston 332 is displaced by the pressure of the flowing primary component , and , as piston 332 moves down the bore of cylindrical housing 328 , secondary component 318 will be expelled through discharge orifices 336 . fig1 c illustrates a secondary reservoir having a generally cylindrical housing , 340 , enclosing a quantity of secondary component 318 , preferably in either a gelatinous or powdered state . when the primary component is flowing through feeder conduit 28 , turbine 346 , as well as shaft 352 and shredder blade 356 , will rotate in the manner of a windmill . as a result , shredder blade 356 will cooperate with shredder plate 360 to pulverize secondary component 318 , which is forced through shredder plate 360 by piston 344 and compression spring 348 . fig1 d illustrates a sacrificial secondary reservoir having a hollow cylindrical plug or lining , 364 made from solid secondary component , such as potassium carbonate . lining 364 has a number of integral internal splines , 368 . lining 364 is formulated and processed so that flowing primary component will cause lining 364 to be eroded and entrained in the flowing primary component . with a composite fire suppressant reservoir , it is generally not possible to weld the initiator conductor conduit extending from an upper portion of the reservoir to a lower portion of the reservoir , to the reservoir itself . however , with the axially compliant conduit illustrated in fig1 , this problem is avoided , while permitting the initiator conductor to be protected against damage . conduit 384 is inserted into reservoir 18 after the pressure vessel shell , in this case , the outer wall of reservoir 18 , has been fabricated . this process begins with insertion of conduit 384 into the interior of reservoir 18 through assembly port 378 . installation of conduit 384 continues with placement of the conduit &# 39 ; s upper end , 384 a , into an upper conduit port formed in wall 18 a . then , axial compliance section 388 is compressed sufficiently to allow lower end 384 b of conduit 384 to be inserted to a lower conduit port located in lower wall 18 b . conduit 384 is then permitted to expand axially . then , an initiator conductor or wire , 380 may be inserted into conduit 384 . finally , propellant device 372 , which is attached to base 382 , may be mounted within port 378 . conduit 384 has an upset section , 396 , adjacent to each of its upper and lower ends , 384 a and 384 b , and these upset sections 396 lock into bonding flanges 392 , which are adhesively sealed to reservoir walls 18 a and 18 b . fig2 a - 20 c illustrate a method for assembling a composite fire suppression agent reservoir having a closure plug either made from a different material than the outer wall of the reservoir , or from a material which is not thermally weldable to the outer wall . fig2 a shows a preform having outer wall 400 , and inner reinforcement 404 . closure plug 406 has a circumferential groove , 406 a , which allows tension band 410 purchase to bind outer wall 400 and inner reinforcement 404 to closure plug 406 . plug 406 may be solvent welded , or bonded with various adhesives known to those skilled in the art , to outer wall 400 and inner reinforcement 404 . the embodiment of fig2 a - 20 c is especially useful for practicing a variant of the present invention in which an external propellant is employed . on the other hand , the embodiment of fig2 shows a combined structure in which closure plug 412 is also employed as a base for internally located propellant 372 . as before , plug 412 may be attached to the composite wall of reservoir 18 both mechanically by means of tension band 410 and / or by chemical bonding or friction welding . fig2 - 25 b show a reservoir construction based upon a composite wall , 424 , which may be formed from fiber or metal reinforced resin , or other composites known to those skilled in the art and suggested by this disclosure . the reservoir shown in fig2 , which is ideally constructed of composite material 424 , employs at least one double concave section to promote the adaptability of the reservoir for installation into spaces having irregular geometry . accordingly , reservoir 416 is shown with double concave section 420 , which is generally bowl - shaped . fig2 shows a first concavity , following the curve of arrow “ a ,” and fig2 a shows a second concavity following the curve of arrow “ b .” of course , both concavities originate at the outside of reservoir 416 . section 420 is reinforced by metallic doubler 428 , which may be insert molded to the interior surface of double concave section 420 . fig2 a illustrates an embodiment in which mold 426 has a groove , 427 , which forms an integral rib , 432 , on an outer portion of double concave section 420 during the process of molding reservoir 416 . fig2 b illustrates a similar embodiment in which rib 432 is formed on an inner surface of section 420 . in the interest of clarity , mold 426 is not shown in fig2 b , or fig2 a and 25 b . in the embodiments of fig2 a and 25 b , preformed ribs are insert molded to double concave section 420 . more specifically , in fig2 a , rib 436 is shown as having been insert molded to an outer portion of section 420 , and in fig2 b , rib 436 is shown as having been molded or bonded to an inner surface of section 420 . those skilled in the art will appreciate in view of this disclosure that insert molding may be accomplished by fabricating a preform , in this case ribs 436 , which are placed into the mold 426 prior to injecting and curing the resin . ribs 436 may be fabricated from either fiber - reinforced resin , or other metallic or non - metallic materials or composites known to those skilled in the art and suggested by this disclosure . although the present invention has been described in connection with particular embodiments thereof , it is to be understood that various modifications , alterations , and adaptations may be made by those skilled in the art without departing from the spirit and scope of the invention set forth in the following claims . | 0 |
looking at fig5 and 6 there is presented a representation of a top plan view and a side elevational view of an exemplary plano - plano molded lens 60 having an optical surface 62 that is free of defects . fig7 and 9 all depict exemplary plano - plano molded lenses 64 , 66 , and 68 all molded from an eco - glass such as stih - 53 ( ohara corporation , rancho santa margarita , calif .) using the prior art method of molding . each lens 64 , 66 , 68 molded from an eco - glass has a respective optical surface 70 , 72 , 74 that has defects therein which appear as bubbles 76 . it is theorized that during the molding process , there are changes in the structure that release oxygen from the glass in the form of oxygen gas or oxygen ions which then react with other materials in the proximity of the glass preform - mold tool interface and create gaseous compounds ( such as co & amp ; co 2 ) with enough pressure to form bubbles on the surface of the glass preform when carbon is present at the interface . phase equilibria studies suggest that sio 2 — tio 2 glasses with titania greater than 7 - mol % may be metastable . titanium oxide rich zones precipitate in the form of phase - separated regions where the titanium is tetrahedrally and octahedrally coordinated with oxygen . this behavior is not surprising in the light of the phase diagram shown in fig1 . turning next to fig1 there is shown a cross - sectional schematic of an apparatus 80 used to practice the method of the present invention . the apparatus 80 of the present invention includes an upper mold fixture 82 and the lower mold fixture 84 . the upper mold fixture 82 has mounted therein an upper mold half or tool 86 . upper mold tool 86 is depicted as having a molding surface 88 that is piano . however , molding surface 88 may have other surface figures or shapes such as concave ( see fig1 ) or convex ( see fig4 ). lower mold fixture 84 has mounted therein a lower mold half or tool 90 . lower mold tool 90 is depicted as having an exemplary molding surface 92 that is piano . however , molding surface 92 , like molding surface 88 may also have other surface figures or shapes . both mold surfaces 88 , 92 are metal ion implanted . mounting of upper mold half or tool 86 within upper mold fixture 82 is accomplished with support member 94 residing in bore 96 . similarly , mounting of lower mold half or tool 90 within lower mold fixture 84 is accomplished with support member 98 residing in bore 100 . a mold or lens cavity is formed between upper mold half or tool 86 and lower mold half or tool 90 when upper mold fixture 82 and / or lower mold fixture 84 are moved to a closed or molding position ( see fig1 ). this relative movement may be accomplished by moving upper mold fixture 82 toward lower mold fixture 84 , or by moving lower mold fixture 84 toward upper mold fixture 82 , or by moving both upper mold fixture 82 and lower mold fixture 84 toward each other . surrounding upper and lower mold fixtures 82 , 84 is a heating apparatus , preferably an induction - heating coil ( not shown ). in operation , a preform 102 , such as stih53 titania glass ( ohara corporation ) is placed on mold surface 92 , and through actuation of induction heating coil , the temperature of the upper and lower mold fixtures 82 , 84 , mold tools 86 , 90 , and preform 102 is raised to at least the glass transition temperature of the preform 102 . then the perform 102 is pressed between the upper and lower mold fixtures 82 , 84 causing the preform 102 to deform and flow generally radially outwardly in the mold cavity . as the preform 102 flows radially outwardly , it substantially fills the mold cavity . compression is performed to a positive stop at which point the upper and lower mold fixtures 82 , 84 , mold tools 86 , 90 , and preform 102 are allowed to cool to below the glass transition temperature of the preform glass material , and preferably to below the annealing point of such glass . in such manner , an eco - glass lens 60 ( see fig5 ) free of surface defects is formed . the molded lens can then be removed from the molding apparatus . it should be understood that upper and lower mold fixtures 82 , 84 are not necessarily directly heated by induction . rather , upper and lower mold fixtures 82 , 84 preferably reside in a mold body ( not shown ) fabricated from a conductive material such as graphite or molybdenum . the mold body is heated by the induction field and the upper and lower mold fixtures 82 , 84 are heated indirectly by conduction and radiant heat transfer . an exemplary mold tool 104 having a concave mold surface 106 is shown in fig1 . the mold surface 106 ( see fig1 ) has a metal ion implanted subsurface layer 108 , with a metal such as titanium to a depth ranging from 0 to 200 å . mold tool 104 is preferably formed from silicon carbide . however , mold tool 104 may be fabricated from other materials including glasslike or vitreous carbon , tungsten carbide , refractory metals and their oxides , carbides or nitrides ( e . g . w , mo , rh , ir ), silicon nitride , glass , such as yas - 6 ( mo - sci corporation , rolla , mo . ), fused silica , and a mixture of silicon . lenses molded from eco - glasses using the method of the present invention are free from surface figure distortion that can be caused by the formation of bubbles at the interface between the mold surfaces and the glass preform during the molding operation . experiments were conducted where stih53 titania glasses ( ohara corporation ) were molded with titanium ion implanted mold tools 86 , 90 . after suitable heating time , the mold fixtures 82 , 84 were brought together compressing each glass preform 102 into a final molded shape . the viscosity of the preform 102 was less than 10 10 p during the compression step . as the glass perform 102 was compressed between the mold tools 86 , 90 , the glass flowed generally radially outwardly and across the surface of the mold tools 86 , 90 thereby substantially filling the lens cavity expelling nitrogen therefrom . in conducting this experiment , a force of 75 lbf . was applied to successfully mold optical elements ( lenses ). the viscosity , molding force , compression rate , lens mold geometry , location of the lens cavities relative to the initial location of the perform , and the sag of the lens mold will affect the propensity for void formation by stagnation , that is , the trapping of gas in the mold cavity . typically , with mold glass lenses a release coating is applied to the mold surfaces , the preform , or both . the release coating is traditionally some variant of a hard carbon coating . however , there is an inherent propensity for carbon to react with any oxygen present and generate bubbles at the glass - mold interface , which could be trapped regardless of the inhibition created by the titanium ions implanted in the substrate . therefore , alternate release coatings should be considered when necessary . it is preferred to place the release agent or coating on the mold surface rather than on the preform because the preform surface is remapped during the pressing operation . when the molding process is performed correctly , the curvature of the preform will always be greater than the curvature of the mold surface . in this way , the finished lens will always have a greater surface area than the surface area of the preform from which it was made . it is also possible to coat both the preform and the tool with a release coating other than carbon . the heater described is an induction - type heater . heating could also be performed using other types of heaters such as , for example , radiant heaters , resistance heaters , infrared heaters , halogen heaters , etc . it is important to understand that the material choices for mold tools 86 , 90 , ion implantation species , and release coating ( if any ) are made in relation to the particular eco - glass from which preform 102 is made . the ion species is chosen according to the kinetics and thermodynamics of the mold - glass interface interactions . one key to successful molding is choosing an ion implantation process that prevents the formation of a gaseous substance trapped between the mold - glass interface in the molding operation . for example , an alternate embodiment to the present invention could use a tungsten carbide mold tool implanted with zirconium , hafnium ( e . g . group 4 elements from the chemical periodic table ) or other reducing element . reducing substances or elements are those substances or elements that , under certain environmental conditions , will react with oxygen thereby causing adjacent substances of interest to reduce their oxidation state , in some cases to their neutral or ground state . in thermodynamics , the formation of a compound by means of a solid - gas reaction can be described by equation 1 and can be plotted as shown in fig1 . δ g ° = rt ln ( p o 2 ) 1 2 ( 1 ) where δg ° is the gibb &# 39 ; s free energy of formation for any substance , r is the gas constant , t is temperature in degrees kelvin and p o2 is the partial pressure of oxygen at equilibrium . by plotting several curves , one can choose an element such as ti or zr , which have much larger negative free energies than si or c , which will allow for the formation of the solid oxides of ti and zr rather than co 2 . however , there are limitations on the use of equation 1 and it can only be used as a starting point for the selection of a candidate ion implantation species because equation 1 and the ellingham diagram are only true when the reactions have reached equilibrium and the elements are pure . once you introduce alloys and solutions , such as those existing in the glass preform 102 and the mold tools 82 , 84 , the partial pressures of oxygen needed for a given reaction will be lower than the ones obtained by equation 1 . it is also necessary that the ion species form a solid oxide , soluble in the glass of interest to prevent the formation of a gas . finally , if the materials chosen have met the conditions for solid - solution equilibrium at the interface , they must not create disturbances in the other physical and chemical properties of the glass of interest for preform 102 . turning to fig1 there is depicted a basic schematic of an ion implantation system . in general an ion implantation system comprises an ion source 110 , which in a preferred embodiment of the present invention would be a titanium source . when a voltage is applied , an ion beam is generated and is accelerated and extracted through an extraction mechanism 112 and then filtered in an ion analyzing mechanism 114 dedicated to filtering the desired mass of the ion beam . the ion beam then passes through a second ion analyzing mechanism 116 that filters for the desired energy of the ion beam . the ion beam finally passes through a scanning station 117 that directs the beam to the substrate 118 , which in the case of the present invention is a mold tool surface for molding of glass optical elements . an exemplary ion implantation system that is suitable for use in the practice of the method of the present invention is the eaton nova 10 - 160 high current ion implanter as sold by eaton semiconductor of beverly , mass . the resulting ion implantation profile for a given substrate is typically presented in atoms or ions / cm 3 versus depth in the substrate as seen in fig1 . these profiles can be estimated by using equations 2 and 3 to calculate the mean projected range , r p , and the straggle , δr p . the mean projected range is a measure of the average penetration depth of the ions , and is defined as : r p = ( ∑ i x i ) n eq . 2 where n is the number of ions , and x i is the perpendicular distance from the surface to the end of each ion track . straggling is a measure of the width of the distribution and is given by : δ r p = ( ∑ i x i - r p ) n eq . 3 the objective of modeling efforts with regard to ion implantation is to predict the distribution of implanted ions for a given combination of ion species , ion energy and target species . to accomplish this task requires a detailed knowledge of how the ions lose energy during collisions . several plano silicon carbide tools were implanted with titanium ions and energy ranging from 85 kev to 175 kev . in the experiments performed , the samples were implanted with a constant titanium dose of 1 × 10 15 ions / cm 3 ( 10 ions / nm 2 ). initially there were concerns about the migration of the titanium ions from its original depth when subjected to high temperature molding conditions needed . annealing experiments were performed and the migration of the peak ion concentration r p with respect to depth was found to be insignificant . actual measurements of the ion concentration with respect to depth were made on plano mold tools to verify the ion implantation profiles and to assess the effect of using the carbon coating . secondary ion mass spectrometry , sims , was used to obtain the ion implantation profile shown in fig1 . the plot in fig1 is shown with concentration in ions / nm 3 instead of the traditional atoms / cm 3 because it is easier to understand the physical implication of the concentration of 1 titanium ion / nm 3 more than 1 × 10 21 titanium ions / cm 3 . further , it can be seen that the experiments performed show how the peak concentration r p ( in reference to equation 2 ) becomes shallower with an increase in the thickness of the carbon coating . [ 0048 ] fig1 and 20 show an exemplary mold tool 120 after the mold surface 122 has coated with an attenuating layer 124 of carbon . fig2 and 22 show the exemplary mold tool 120 after the mold surface 122 has been ion implanted with titanium ions through the attenuating layer 124 of carbon . the implanted region 126 extends to a depth of about 1500 å , depending on the thickness of the carbon coating 124 . following ion implantation , the carbon coating 124 is burned off the mold tool 120 yield the structure previously described with reference to fig1 and 14 . carbon readily oxidizes or burns forming carbon dioxide when subjected to air at temperatures greater than 300 ° c . the remaining mold tool 120 is left with a high titanium ion concentration near the mold surface 122 without any changes in the surface geometry required for molding glass lenses . from the foregoing it will be seen that this invention is one well adapted to attain all of the ends and objects herein above set forth together with other advantages which are apparent and which are inherent to the process . it will be understood that certain features and sub combinations are of utility and may be employed with reference to other features and sub combinations . this is contemplated by and is within the scope of the claims . as many possible embodiments may be made of the invention without departing from the scope thereof , it is to be understood that all matter herein set forth and shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense . parts list 10 upper mold half 12 lower mold half 14 spherical glass preform 16 concave mold surface 18 concave mold surface 20 upper mold half 22 plano mold surface 24 lower mold half 26 concave mold surface 28 spherical preform 30 upper mold half 32 convex mold surface 34 lower mold half 36 concave mold surface 38 plano convex preform 42 upper mold half 44 convex mold surface 46 lower mold half 48 convex mold surface 50 plano plano preform 60 plano plano molded lense 62 optical surface 64 plano plano molded lenses 66 plano plano molded lenses 68 plano plano molded lenses 70 optical surface 72 optical surface 74 optical surface 76 bubble 80 apparatus 82 upper mold fixture 84 lower mold fixture 86 upper mold tool 88 mold surface 90 lower mold half or tool 92 molding surface 94 support member 96 bore 98 support member 100 bore 102 preform 104 mold tool 106 concave mold surface 108 metal ion implanted subsurface layer 110 ion source 112 extraction mechanism 114 ion analyzing mechanism 116 second ion analyzing mechanism 117 scanning station 118 substrate 120 exemplary mold tool 122 mold surface 124 attenuating layer of carbon 126 implanted region | 2 |
fig1 a reveals a schematic view of a device for producing and / or applying an essentially two - dimensional composite 3 formed of at least two areal regions 1 , 2 in predeterminable composite width 4 , predeterminable composite height 5 and / or predeterminable composite length 6 . the areal regions 1 , 2 each form a layer 1 , 2 of the composite 3 . the device includes an applicator appliance 7 which comprises an applicator die 8 . a transporting appliance 9 is disposed underneath the applicator die 8 , which is formed as a coextrusion die . the transporting appliance 9 is formed as a transportation belt 10 which has a transport area 11 on the topside of the belt 10 . owing to the transporting appliance 9 , the transport area 11 can move in transport direction y under the spatially fixedly disposed coextrusion die 8 . the falling curtain 12 coming out of the coextrusion die 8 in a virtually vertical direction z can be applied to the transporting appliance 9 in the region of transport area 11 . the composite 3 can preferably be applied to a substrate 13 which lies on the transport area 11 and is conveyable in transport direction y using the transporting appliance 9 . the transportation belt 10 as per fig1 a can be formed as a cooling belt which comprises a cooling appliance 28 . as a result , the generally hot , viscid or molten coextrudate 14 exiting from the coextrusion die 8 is cooled on the transporting appliance 9 , causing the composite 3 to at least partially harden and / or change its viscosity . the device as per fig1 a makes it possible to adjust the layer width 15 and / or the layer length 16 and / or the layer height 17 of at least one of the layers 1 , 2 / areal regions 1 , 2 of the composite 3 portionally . this is effected by varying the coextrusion parameters within the coextrusion die 8 . a side view of an applicator appliance 7 having a coextrusion wide - slot die 8 is discernible from fig1 b . especially the areal region width 15 and the areal region length 16 of at least one areal region ( 1 and / or 2 ) of the composite 3 can be varied according to the particular requirements by means of the applicator appliance 7 of fig1 a and 1b . for this , at least one extrudate is conveyed by a plurality of conveying appliances / metering pumps disposed on a ( pump ) block 40 in those coextrusion chambers ( 19 a to 19 f ) which are involved in the application of composite 3 to the substrate 13 . the pump block 40 is shown by fig1 b to be driven by one or more drives 41 . circulation modules 43 upstream of the coextrusion chambers can be switched via fluidic switch elements such as , for instance , valves such that an extrudate can circulate in the applicator appliance 7 and / or the conveying appliance 22 . circulating the normally heated extrudate stops the lines and channels from gumming up and ensures that the extrudate is always conveyable . channels and line are schematically indicated in fig1 b by broken lines . switching one of the circulation modules 43 , each of which is assigned to a coextrusion chamber ( 19 a to 19 f ) such that the extrudate ( s ) circulate means that the circulating extrudate is not conveyed into the coextrusion chamber . the extrudate is conveyed back into the pumps and circulates in the applicator appliance 7 . the application of the circulating extrudate is thus interrupted in the region of the assigned coextrusion chamber . accordingly , application interruption for variation of areal region width 15 and / or of areal region length 16 is effected by fluidic cooperation of pump block 40 with the circulation modules 43 or , to be more precise , by switching the fluidic switch element in individual or two or more circulation modules 43 in accordance with the particular requirements . when a circulation module 43 is switched such that the extrudate does not circulate but is conveyed to the outlet 24 of applicator appliance 7 , application of the extrudate takes place in the region of the coextrusion chamber fluidically assigned to circulation module 43 . fig2 shows a schematic plan view of a device for producing and / or applying an essentially two - dimensional composite 3 formed of at least two layers 1 , 2 in predeterminable composite width 4 , predeterminable composite height 5 and / or predeterminable composite length 6 . it is also apparent in fig2 that the coextrusion die 8 used for application is formed as a wide - slot die whose die - slot length determines virtually the maximum composite width 4 . the transport direction y therein is defined by the transporting appliance 9 , the transport direction y being essentially parallel to the composite length 6 and essentially perpendicular to the composite width 4 and / or to the composite height 5 . the device of fig2 makes it possible to adjust the composite width 4 , the composite length 6 and / or the composite height 5 . this is accomplished because the coextrusion die 8 comprises a coextrusion channel 18 having a plurality of coextrusion chambers 19 a to 19 f . each and every one of the coextrusion chambers 19 a to 19 f has a first inlet 20 for the first extrudate 21 , which forms the first layer 1 , and a second inlet 20 ′ for the second extrudate 21 ′, which forms the second layer 2 . every one of the inlets 20 , 20 ′ of every one of the coextrusion chambers 19 a to 19 f is shown by fig2 to be fluidically assigned a conveying device 22 . the fluidic assignment of the conveying appliances 22 to each and every inlet 20 , 20 ′ of each and every chamber 19 a to 19 f renders the layered structure parameters of the entire applied material 3 adjustable in a varied manner . for instance , by specifically controlling individual conveying appliances 22 it is possible to control the feed of the first and / or optionally of the second extrudate 21 , 21 ′ in a time - dependent manner , generating in effect an applied material which portionally has different areal region / areal region parameters . areal region parameters include the areal region thickness ( layer height 17 ) as well as the areal region width 15 and the areal region length 16 . fig2 by way of example depicts a composite structure comprising the formation , at irregular intervals relative to the composite width 4 and the composite length 6 , of portions 37 having a first and a second layer 1 , 2 and also portions having just one first layer 1 . fig3 shows a schematic depiction of an applicator die 8 in vertical section . the applicator die 8 depicted therein can be provided in a device according to fig1 a , 1 b or 2 , for example . it accordingly serves to generate and / or apply a two - dimensional multilayered material 3 formed of a coextrudate 14 , preferably on a transport area 11 of a transporting appliance 9 or on a substrate 13 . the applied material is shown in fig3 to be formed of a first extrudate 21 and of a second extrudate 21 ′. the first extrudate 21 forms the first areal region / first layer 1 of composite material 3 while the second extrudate 21 ′ forms the second areal region / layer 2 . the applicator die 8 of fig3 comprises a first inlet 20 for the first extrudate 21 and a second inlet 20 ′ for the second extrudate 21 ′. every one of the inlets 20 , 20 ′ is in communication with a channel or line 23 . an extrudate pressure between about 10 and about 100 bar can prevail in the lines 23 and / or in the die 8 . the temperature of the extrudates 21 , 21 ′ can be greater than 60 ° c . more particularly , the extrudates 21 , 21 ′ can have temperatures between about 100 ° c . and about 220 ° c . an outlet 24 for the coextrudate 14 is provided on the underside of coextrusion die 8 . a heater 25 is disposed in the region of the outlet 24 to render the outlet 24 and thus also the coextrudate 14 leaving the outlet 24 heatable . the coextrusion wide - slot die 8 of fig3 can be used to alter the application width of the material leaving the outlet 24 . the application width is not more than the maximum application width which is essentially defined by the width of the outlet 24 . the material is applied portionally in fig3 , so the portions of the applied material have strip - shaped interruptions 27 . the coextrusion die 8 of fig3 comprises a plurality of conveying appliances 22 for conveying the extrudates 21 , 21 ′, which are each in fluidic communication with the first inlet 20 and the second inlet 20 ′. the conveying appliances 22 can be for example disposed in a block ( not depicted in fig3 ), in which case each and every conveying appliance may comprise a ( metering ) pump . the ( pump ) block may comprise a conjoint drive 41 which drives each and every metering pump of the conveying appliance 22 . the drive may comprise one or more motors . the first inlet 20 and the second inlet 20 ′ are shown by fig3 to empty into a coextrusion channel 18 which — as depicted in fig2 — can be subdivided into a plurality of coextrusion chambers 19 a to 19 f . fig3 shows that every one of the conveying appliances 22 which is in fluidic communication with the inlets 20 , 20 ′ comprises a pump 29 , a switch element formed as a valve 30 and a fluidic return line 31 which bypasses the pump 29 and is switchable by the valve 30 . if no extrudate 21 , 21 ′ is to be conveyed into the inlet 20 , 20 ′, the valve 30 is switched such that the extrudate 21 , 21 ′ conveyed by the pump 29 is returned , via the return line 31 , into the feed line 32 connected to the pump 29 . this accordingly short - circuits the conveyance of extrudate 21 , 21 ′ to ensure that both the conveyance velocity and the feed pressure of the circulating extrudate remain essentially constant . if the conveyance of the extrudate is to be continued , the valve 30 is switched such that the extrudate 21 , 21 ′ is conveyed into the inlet 20 , 20 ′ via the line 23 connected thereto . the valve 30 and the return line 31 can be constituent parts of a circulation module ( 43 ). each and every conveying appliance 22 can be assigned a separate circulation module 43 . the circulation module 43 is capable of effectuating an interruption to the application of the extrudate ( 21 or 21 ′), alternatively the extrudates ( 21 and 21 ′), without the operation of one or all pumps 29 of the conveying appliances 22 having to be interrupted . this is particularly advantageous when the pumps 29 of the conveying appliance 22 are actuated by a conjoint drive 41 . the conjoint drive 41 is in sustained operation and the interruption or ( temporary ) deactivation of the application of the extrudates 21 , 21 ′ is effected by controlling one or more switch elements 30 in one or more circulation modules 43 so that the extrudate 21 , 21 ′ ( the extrudates 21 and / or 21 ′) are not conveyed through the outlet 24 from the applicator die 8 , but circulate within the applicator appliance 7 . by switching the extrudate ( 21 , 21 ′) between through - flow and circulation it is possible to alter , for example , the application width , the application length and / or further application parameters . control appliances 33 are provided according to fig3 to render each and every conveying appliance 22 controllable . the conveying appliances 22 can thereby be switched and / or controlled portionally so the applied material will have one , two or no layers 1 , 2 as required . because every one of the conveying appliances 22 is separately and preferably mutually independently controllable , especially open and closed loop controllable , the layer width 15 , the layer length 16 and / or the layer height 17 of one or more layers 1 , 2 of the applied material are alterable . to stabilize the flow behavior of the extrudates 21 , 21 ′, every one of the inlets 20 , 20 ′ or , alternatively , only one inlet ( 20 or 20 ′) can be assigned a preferably electric heating device 34 . a detailed view of an alternative design of a coextrusion die 8 as per fig3 can be seen in fig4 . coextrusion die 8 is shown therein to comprise a coextrusion channel 18 into which the first and second inlets 20 , 20 ′ empty and to which the outlet 24 of the coextrusion die 8 is connected . according to fig4 , the second inlet 20 ′ empties into the coextrusion channel 18 such that the second extrudate 21 ′ is disposable at an extrudate surface 35 formed by the first extrudate 21 . it is accordingly possible to drive the second extrudate 21 ′ against the extrudate surface 35 , formed in the coextrusion channel 18 , of the first extrudate 21 . this is particularly advantageous when the layer 1 formed by the first extrudate 21 is distinctly thicker than the layer 2 , formed by the second extrudate 21 ′. as a result of the thicker first layer 1 , formed by the first extrudate 21 , being conveyed through the coextrusion channel 18 at a conveyance velocity and as a result of the second , thinner layer 2 , formed of the second extrudate 21 ′, being driven against the first layer 1 , the second layer 2 will attach to the first layer 1 so that the second layer 2 is endowed with the conveyance velocity of the first layer 1 . fig4 reveals a dividing wall 36 which extends at least regionally into the coextrusion channel 18 of the coextrusion die 8 . the dividing wall 36 can augment the flow properties of the extrudates 21 , 21 ′ in that premature commixing of the extrudates 21 , 21 ′ in the region of the adjacent inlets 20 , 20 ′ is avoided . fig5 shows a two - dimensional composite 3 obtained using a device as per fig1 a and 2 or , more precisely , using a coextrusion die 8 as per fig3 and 4 . it can be seen in fig5 that the composite 3 consists of a first areal region 1 and of a second areal region 2 disposed on the first areal region 1 , the first areal region 1 being formed of a first extrudate 21 and the second areal region 2 being formed of a second extrudate 21 ′. the two areal regions 1 , 2 are in layer - type disposition . the second layer 2 is a function layer and the first layer 1 is an effect layer , which augments the effect of the function layer . the function layer may be an adhesive layer . this adhesive layer may be durably adhesive or only after some reactivation , for example with a solvent such as , for instance , water , with a heated roll or with an infrared radiator ( ir radiator ). the effect layer 1 may optionally have adhesive properties . the effect layer 1 may additionally have a volume - filling or an acoustically and / or mechanically damping property . the effect layer 1 may also have a flameproofing property or a barrier property . if the effect layer 1 has adhesive properties , it can augment the adhesive properties of the adhesive / function layer 2 . more particularly , the adherence of the second layer 2 to an adherend material but also to the first layer 1 and / or the adherence of the first layer 1 to a substrate 13 or any desired surface can be augmented as a result . fig6 shows a vertical section through a composite of fig5 . it can be seen in fig6 that the second layer 1 , which forms an adhesive layer , is thinner than the first layer 1 , which forms an effect or filling layer . that is , the layer height 17 ′ of the second layer 2 is less than the layer height 17 of the first layer 1 . for example , the second layer 2 can have a layer height 17 ′ in a range between about 1 μm and about 10 μm , preferably about 3 μm the first layer 1 can for example have a layer height 17 in a range between about 5 μm and about 5 mm , preferably about 15 μm . both layers 1 , 2 can be formed of a hot - melt adhesive , in which case the thinner , second layer 2 is formed of a high - value adhesive and the thicker , first layer 1 is formed of a lower - value adhesive , the adhesive properties of which are less effective than those of the thinner , second layer 2 . the thicker , first layer 1 can work as an effect layer 1 to serve the purpose of smoothing out unevennesses 38 on the adherend surface in that the volume of the first , thicker layer 1 fills out the surface unevennesses 38 . this filling function of the first , thicker ( effect ) layer 1 contributes to the higher - value , thinner second layer 2 having better , i . e ., more effective , adherence on the adherend surface . the function layer depicted as per fig6 can be formed of an eva , for example , and the effect layer disposed thereunder can be formed of a uv - acrylate . the method which the present invention provides of coextruding and then applying the extrudates with or without cooling or hardening is a straightforward way to produce the composite of these materials . fig7 shows a composite 3 where there is a sequence of layers formed of different materials . more particularly , the different layers 1 , 2 in fig7 are formed of different adhesives . the upper , thinner adhesive layer 2 has an weakening 27 , which is marked by a portional reduction in layer height 17 . the adhesive is less efficient at the weakening , i . e ., the composite has worse adherence there . a composite 3 disposed on a substrate 13 is shown in fig8 . the second layer 2 is disposed on the first layer 1 and the first layer 1 is directly disposed on the substrate 13 . the substrate 13 can be formed for example of a foil or of a paper , for example a silicone paper . fig9 shows a schematic plan view of a composite 3 . it can be seen that the first areal region 1 extends across the full length 6 and across the full width 4 of composite 3 . the second areal region 2 is portionally disposed on the first areal region 1 such that strip - shaped interruptions 26 are disposed in each case between the portions 37 of the second areal region 2 in both the longitudinal direction y and in the transverse direction x . where there are interruptions 26 , the composite 3 has no or less adhesive properties relative to the adhesive properties of the portions 37 of the second areal region 2 disposed on the first areal region 1 . fig1 shows a schematic section through a four - ply composite 3 in the vertical direction ( i . e ., in the z - direction ). the effect layer 1 ( first areal region ) and the function layer 2 ( second areal region ) have been applied to a substrate 13 , formed of a polymeric foil for example , such that the effect layer 1 is disposed on the substrate 13 and the function layer 2 is disposed on the effect layer 1 . the effect layer 1 may comprise for example an inorganic adhesive which is firmly adherent to the substrate 13 . in order for a third areal region 39 to be adherently disposable on the function layer 2 , the function layer 2 can comprise an organic adhesive , in which case the third areal region 39 can be formed in a layer - type manner of a fibrous material in particular . the result is a configuration wherein the first and second areal regions 1 , 2 are disposed between the substrate 13 and the third areal region 39 . the configuration of the composite as per fig1 is useful , for example , for ( glass fiber ) wallpapers . said composite can be created by conveying the substrate 13 in a transport direction y while the areal regions 1 and 2 are applied to the substrate 13 by an above - described coextrusion process . all the while , the third areal region is applied to the substrate 13 , for example via a roll or an alternative feeding appliance , at a point which , relative to the transport direction y , is downstream of the point where the coextrudate is applied . the four plies 13 , 1 , 2 and 39 can thereby be applied on top of each other in one operation in that , in particular , the third areal region 39 is applied in - line , i . e ., during the production of the plies 13 , 1 and 2 . | 8 |
the objective of this invention is to provide a process for producing a mixture of 2 , 4 - fdca and 2 , 5 - fdca by subjecting furoic acid salts to a disproportionation reaction ( see fig1 ), catalyzed by metal salts , comprising the steps of : a ) oxidizing furfural compounds in the presence of catalysts and alkaline solution in order to obtain biobased furoic acid salts ; b ) heating the furoic acid salts under stirring in the presence of a metal based catalyst and cooling the reaction mixture until room temperature ; c ) collecting the furan obtained in item ( b ) in order to obtain the mixture of 2 , 4 fdca and 2 , 5 - fdca ; d ) optionally , filter off the black insoluble material of the reaction mixture obtained in item ( c ) and acidifying the reaction mixture in order to collect the 2 , 5 - fdca ; e ) optionally , subjecting the mixture obtained in item 1 ( c ), to an extraction or other separation method in order to purify 2 , 4 - fdca . the furfural oxidation of the first step is made in the presence of au / tio 2 catalyst . the au / tio2 is optimized for this reaction . furfural , au / tio2 and naoh in water was charged into the reactor and pressurized with oxygen ( 3 × 10 5 pa of o 2 ) and stirred at 600 rpm and at 50 ° c . for 3 - 5 h . the furoic acid product is further converted to a furoic acid salt , which can be potassium , sodium , cesium and preferably potassium . other renewable sources can be used to produce the furoates . the furoic acid salt and a metal salt catalyst are then heated under stirring for an interval ranging from 1 h to 5 . 5 h , preferably 5 h . the temperature of the system ranges from 220 ° c . to 280 ° c ., preferably 260 ° c . ( salt bath temperature not the internal temperature .) the catalyst is chosen from transition metal salts , alkaline earth metal salts , preferably fecl 2 , cdl 2 , zn ( otf ) 2 or zncl 2 . when the fecl 2 catalyst is used , the reactive mixture is placed under a slight flow of n 2 . among the wide range of catalysts used , zncl 2 ( 20 mole %) was found to be active ( best ) and the results obtained are comparable or more even better than the cdl 2 catalyst which has been screened as the best catalyst by andrisano for the disproportionation reaction of k - furoate . the reaction was stopped after the specified time and cooled down to room temperature in 2 h . the furan is collected via a dean - stark trap and a co 2 - aceton - ice bath . after cooling , water is added and the black insoluble material is filtered off and upon acidification the 2 , 5 - fdca was collected . 12 n hcl is used to acidify the reaction mixture until reaches ph 1 . 2 , 5 - fdca is precipitated out immediately from the reaction mixture . nmr analysis shows that there is a high degree of k - furoate conversion which allows to precise the amount of 2 , 4 - fdca in the product mixture . the use of the process described herein allows 2 , 4 - fdca yields of at least 7 wt %, preferably at least 15 to 20 wt %, more preferably 32 wt % at least ( the remaining fraction of the products is basically 2 , 5 - fdca ). furthermore , the present invention presents the following advantages : production of 2 , 4 - fdca from furoates derived from cheap and renewable stock feed , e . g . furfural production of 2 , 4 - fdca through a simple 2 - step process which produces no harmful , toxic or undesirable byproducts ( the main byproduct furan has actually highly interesting applications ) the use of an iron catalyst , cheaper than the usual metals catalysts and environmentally more benign . the diacid obtained with the present invention may be useful to produce chemical compounds which can be useful monomers to the polymer industry and other industries such as solvents , lubricants or plasticizers industry . furthermore , these 2 , 4 - fdca based compounds can be used to produce polyesters . the following examples illustrate the present invention , however not limiting the scope of the invention furfural ( 3 . 00 grammes , 31 . 22 mmol ) was dissolved in 40 ml water . one equivalent ( 31 . 75 mmol ; 1 . 02 eq ) of base ( naoh ) and 0 . 012 grammes of au / tio2 catalyst ( ex - strem - autek ; 1 . 2 wt % au , au particle size 2 - 3 nm ) were added to the furfural solution in water . the 100 ml reaction vessel ( büchi glasuster picoclave ) was closed and overhead stirring was applied . oxygen pressure ( 303974 , 99 pa of o 2 ) was applied to the reaction mixture . the reaction mixture was put at 50 ° c . after one hour reaction the pressure has dropped to approximately one atmosphere and the reaction vessel was repressurised to 303974 , 99 pa of o 2 and subsequently stirred overnight . after overnight stirring the reaction was stopped and the catalyst was filtered off . the solvent ( water ) was removed by a rotary evaporator and applying vacuum . the yield of sodium furoate was 94 . 9 %. the use of gold catalysts in the above reaction often is a little bit more selective than other metal based catalysts such as pt or pd and under the circumstances used in the reaction , the combination of a heterogeneous catalyst that acts under the same basic conditions required for the subsequent disproportionation reaction is advantageous . h nmr analysis ( see fig2 ) showed the three protons for furoate in equal ratio , without any other signal besides the nmr solvent , confirming that the furfural had been converted completely and selectively into sodium furoate . in the absence of base no reaction is occurring . this reaction demonstrates the efficiency in obtaining furoate salts from furfural , that can serve as input for the subsequent disproportionation reaction . 6 . 00 grams of k - furoate ( 39 . 95 mmol ) and 2 . 20 grams of cdl 2 ( 6 . 01 mmoles ) were grinded together well and charged into a 3 - necked flat flange reaction vessel . the mixture was then heated in a salt bath at 265 □ c with stirring using a mechanical overhead stirrer under continuous ( very slow ) flow of nitrogen . during the course of reaction , the furan formed was collected via a dean - stark trap and an co 2 / acetone ice bath (− 78 ° c . ), yielding furan of 1 , 35 grams ( 95 % of the theoretical amount ). after 4 hours , the reaction was stopped and allowed to cool down at room temperature for 1 h . thus obtained black hard solid substance was dissolved in water ( 50 ml ). a residual amount of water insoluble black material was filtered off and the deep yellow colour filtrate was acidified using 12 n hcl ( until ph : 1 ). 2 , 5 - fdca was precipitated and filtered off . 60 . 9 % of the theoretical amount of 2 , 5 - fdca was isolated . nmr analysis of the reaction mixture after filtering off the insoluble black material showed that the k - furoate had been converted over 90 % and that there is a mixture being present of 2 , 4 - fdca and 2 , 5 - fdca , in a ratio of 0 . 32 : 0 . 68 . based upon this and the 60 . 9 % of 2 , 5 - fdca isolated , it can be calculated that the k - furoate has been disproportionated into a mixture of furandicarboxylic acids in 89 % of the theoretical yield . process for production of a mixture of 2 , 4 - fdca followed by 2 , 5 - fdca isolation 5 . 3 grams of k - furoate ( 35 . 4 mmoles ) and 0 . 97 grams ( 7 . 65 mmoles ) of fecl 2 catalyst were grinded together well and charged into a 3 - necked flat flange reaction vessel . the mixture was then heated in a salt bath at 250 □ c with stirring using a mechanical overhead stirrer under continuous ( very slow ) flow of nitrogen . during the course of reaction , the furan formed was collected via a dean - stark trap and an co2 - aceton - ice bath (− 78 ° c .). after 5 . 5 hours , the reaction was stopped and allowed to cool down at room temperature for 1 h . thus obtained black hard solid substances were dissolved in water ( 45 ml ). a residual amount of water insoluble black material was filtered off and the deep yellow colour residue was acidified using 12 n hcl ( until ph : 1 ). 2 , 5 fda was precipitated and filtered off . 60 . 9 % of the theoretical amount of 2 , 5 fda was isolated . nmr analysis of the reaction mixture after filtering off the insoluble black material showed that the k - furoate had been disproportionated over 81 % and that there is a mixture being present of 2 , 4 - fdca and 2 , 5 - fdca , in a ratio of 0 . 21 : 0 . 79 . based upon this and the 60 . 9 % of 2 , 5 - fdca isolated , it can be calculated that the k - furoate has been disproportionated into a mixture of furandicarboxylic acids in 75 % of the theoretical yield . the reaction crude mixture ( 2 , 4 - fdca , 2 , 5 - fdca , 2 - furoic acid and cdl 2 ) was subjected to soxhlet extraction using acetone for 8 h . after cooling to room temperature , acetone insoluble white crystalline powder was analyzed by nmr which showed no proton signals . the acetone soluble part was recovered and the solvent was evaporated under reduced pressure in the rotatory evaporator . nmr analysis showed the presence of 2 , 4 - fdca , 2 , 5 - fdca and 2 - furoic acid in the crude mixture . the mixture was then stirred vigorously with chloroform for 10 min at room temperature and filtered . this process was repeated until 2 - furoic acid was completely removed from the mixture . the product was then dried in a vacuum oven at 40 ° c . for 12 h . as the solubility difference of 2 , 4 - fdca was comparatively high in acetone at room temperature , the same technique ( adapted with chloroform previously ) was repeated with acetone to separate the 2 , 4 - fdca from 2 , 5 - fdca . thus acetone soluble part was separated , combined together and evaporated under reduced pressure in a rotatory evaporator yielded 2 , 4 - fdca , which was not 100 % qualitative , but not less than 85 % purity ( from nmr - see fig3 ) and the investigation is in progress to find the more precise way to get 100 % pure compound of 2 , 4 - fdca . 1 . 0 g of crude reaction mixture ( mainly consisting of 2 , 4 - fdca , 2 , 5 - fdca , 2 - furoic acid and a trace amount of 3 , 4 - fdca ) was refluxed in methanolic hcl ( 1 . 2 m ) ( 10 ml ) at 75 ° c . for 3 h . after completion of the reaction , the solvent was evaporated in a rotatory evaporator under reduced pressure . the resulting yellow viscous oil was dissolved in ethyl acetate and washed with water ( 15 ml × 2 ), dried over magnesium sulfate , filtered and the solvent evaporated . highly purified 2 , 4 - furan dicarboxylic acid methyl ester and 2 , 5 - furan dicarboxylic methyl ester were obtained by using column chromatography separation using 6 % ethyl acetate and petroleum ether as eluents . the esters were further recrystallized from methanol . although the foregoing has been described in some detail by way of illustration for purposes of clarity of understanding , it will be apparent that various changes and modifications may be practiced within the scope of the appended claims . | 2 |
hereinafter , exemplary implementations will be described with reference to the accompanying drawings . however , variations and modifications may be made without departing from the basic concepts described herein . in an image forming apparatus , the image forming apparatus can control power of the image forming apparatus . in a conventional image forming apparatus , when the image forming apparatus shifts the power mode from the energy saving mode to the normal mode , the image forming apparatus controls power - on and power - off of image forming devices included in the image forming apparatus based on the stored status of an application . however , even if the state of the application is the same , the same devices are not always used . thus , in the conventional image forming apparatus , if a device that is not used exists , power is wasted . in an image forming apparatus according to aspects of this disclosure , the image forming apparatus is able to reduce power consumption . fig1 is a block diagram of an exemplary hardware configuration of the image forming apparatus 1 . as illustrated in fig1 , the image forming apparatus 1 includes a controller 10 and an engine 60 , which are mutually connected to each other by a peripheral component interface ( pci ) bus . the controller 10 controls a main process of the image forming apparatus 1 , a drawing process , a communication process , and an input process . the engine 60 includes , for example , a printer engine , a plotter , a scanner , and a fax unit . further , the engine 60 further includes an image processing part which performs error diffusion or gamma conversion . the controller 10 includes a central processing unit ( cpu ) 11 , a northbridge ( nb ) 13 , a system memory ( mem - p ) 12 , a southbridge ( sb ) 14 , a local memory ( mem - c ) 17 , an application specific integrated circuit ( asic ) 16 , and a hard disk drive ( hdd ) 18 . the nb 13 is connected the asic 16 via an accelerated graphics port ( agp ) bus 15 . further , the nb 13 is a bridge to connect the cpu 11 , the mem - p 12 , the sb 14 , and the agp 15 . further , the nb 13 includes a memory controller to control input and output to the mem - p 12 , and further includes pci master and an agp target . the mem - p 12 includes a read only memory ( rom ) 12 a and a random access memory ( ram ) 12 b . the rom 12 a is a read only memory to store programs and data . the ram 12 b is able to read and write , and is used as an expanding memory to expand the programs and the data , and as a drawing memory . the sb 14 is a bridge to connect the nb 13 , a pci device , and a peripheral device . the sb 14 is connected to the nb 13 via a pci bus . the pci bus is able to connect to a network interface . the asic 16 is an integrated circuit that processes an image . the asic 16 is a bridge to connect the agp 15 , the pci bus , the hdd 18 , and the mem - c 17 . further , the asic 16 includes a pci target , an agp master , an arbiter , a memory controller for controlling the mem - c 17 , a plurality of direct memory access controllers ( dmac ), and a pci unit for sending data to the engine 60 via the pci bus . the asic 16 is connected to a facsimile control unit ( fcu ) 30 , an universal serial bus ( usb ) 40 , and an ieee 1394 interface 50 . the mem - c 17 is a local memory to be used as buffer . the hdd 18 is a storage device to store image data , program , font data , and a form . the agp 15 is a bus interface to speed up a process of graphics . fig1 is a diagram illustrating a functional configuration of the image forming apparatus 1 . as illustrated in fig1 , the image forming apparatus 1 includes an energy saving processing unit 100 , a display unit 20 , a scanner 31 , a plotter 32 , and a peripheral device 33 . in response to input by a user , the image forming apparatus 1 shifts an operation status from normal status to energy saving status . the normal status is a status in which the image forming apparatus 1 provides power to all hardware units . the energy saving status is a status in which the image forming apparatus 1 stops power to some of the hardware units . power consumption in the energy saving status is less than power consumption in the normal status . the energy saving processing unit 100 controls the supplying of power to each hardware unit . the energy saving processing unit 100 includes a receiving unit 101 , a display information storing unit 102 , a display processing unit 103 , a power status storing unit 104 , a power status determining unit 105 , a power control unit 106 , a driver control unit 107 , an operating time measuring unit 108 , and an operating time storing unit 109 . the receiving unit 101 receives input of information from a user . the information includes , for example , a display instruction to display on the display unit 20 , a screen to be displayed by an application , or an execution instruction to execute a function . the display information storing unit 102 stores display information to be displayed on the display unit 20 by an application to be executed on the image forming apparatus 1 . the display processing unit 103 , in response to receiving a display instruction by a user , extracts display information corresponding to the display instruction among the display information stored by the display information storing unit 102 . further , the display processing unit 103 displays a screen on the display unit 20 based on the extracted display information . the power status storing unit 104 stores power status information to determine a power status of each device . the power status information will be described below . fig2 is a table indicating the power status information . as illustrated in fig2 , the power status storing unit 104 stores a display screen to be displayed on the display unit 20 and a corresponding power status of each device . herein , the display screen is a display screen displayed on the display unit 20 by an application . when one application displays a plurality of display screens , the power status storing unit 104 stores each of the plurality of display screens . the power status is information indicating power to be supplied to each device . during execution of an application , the display processing unit 103 displays a display screen on the display unit 20 based on the application . further , the receiving unit 101 is able to receive from a user , on the display screen , an execution instruction to execute a function . that is to say , even while an application is executed , it is possible to execute a different function , and it is possible to use different devices . in this description , the power status storing unit 104 stores display screens and the power status of devices corresponding with them . in detail , the power status storing unit 104 stores , corresponding to every display screen of application , a power - on status of a device or a power - off status of a device . for example , the power status storing unit 104 stores statuses , which are scanner on , plotter on , and peripheral device on , corresponding to screen 1 of a copy application . in another example , the power status storing unit 104 stores statuses , which are scanner on , plotter on , and peripheral device off , corresponding to screen 2 of the copy application . in this way , the power status storing unit 104 is able to store the power status of devices for every screen of an application . return to the fig1 , the power status determining unit 105 determines the power status of a device based on a display screen displayed on the display unit 20 and information stored by the power status storing unit or the operation time storing unit 109 . the power control unit 106 controls , based on the power status determined by the power status determining unit 105 , power supplying to the scanner 31 , the plotter 32 , and the peripheral device 33 . when the receiving unit 101 receives an execution instruction while a display screen is displayed by the display processing unit 103 , the driver control unit 107 determines a driver to execute a function based on the execution instruction . further , the driver control unit 107 controls the determined driver to execute a process of the function . the operating time measuring unit 108 measures an operating time of the driver . the operation time storing unit 109 stores the measured operation time corresponding to the display screen that is displayed on the display unit 20 . as illustrated in fig3 , the operation time storing unit 109 stores , in association with one another , a display screen displayed on the display unit 20 , operation time of each device , and operation time of all devices . the operation time of each device is the operation time that is measured during display of the display screen on the display unit 20 . the operation time of all devices is the total time of the operation time of each device . a detailed process of controlling of power supply to each device will be described below with reference with a flowchart . fig4 and fig5 are a flowchart illustrating a procedure for controlling of power supply of the image forming apparatus . as illustrated in fig4 , the receiving unit 101 receives a display instruction input from a user ( step s 100 ). next , in response to receiving the display instruction , the display processing unit 103 displays a display screen on the display unit 20 based on the display instruction ( step s 101 ). next , in response to displaying the display screen on the display unit 20 , the power status determining unit 105 determines whether the displayed display screen is stored in the power status storing unit 104 or not ( step s 102 ). next , when the power status determining unit 105 determines that the displayed display screen is stored in the power status storing unit 104 ( step s 102 : yes ), the power status determining unit 105 determines the power status of each device associated with the displayed display screen ( step s 103 ). next , the power control unit 106 controls power supplying to each device based on the determined power status ( step s 104 ). as shown in fig2 , when screen 1 of copy application is displayed , the power control unit 106 supplies power to the scanner 31 , the plotter 32 , and the peripheral 33 . thus , for the image forming apparatus 1 described herein , even while the same application is executed , the image forming apparatus 1 is able to variably control power supplying to each device . thus , the image forming apparatus 1 is able to save power by not supplying power to a device that will not be used during display of the display screen . next , when the power status determining unit 105 determines that the displayed display screen is not stored in the power status storing unit 104 ( step s 102 : no ), the power status determining unit 105 determines whether the displayed display screen is stored in the operating time storing unit 109 or not ( step s 110 ). next , when the power status determining unit 105 determines that the displayed display screen is stored in the operation time storing unit 109 ( step s 110 : yes ), the power status determining unit 105 extracts the operation time of each device and the operation time of all devices , which are associated with the displayed display screen . further , the power status determining unit 105 calculates an operating rate of the operation time of each device to the operation time of all devices ( step s 111 ). next , the power status determining unit 105 compares the calculated operating time to a predetermined threshold ( step s 112 ). next , the power status determining unit 105 determines the power status of each device based on a result of comparison ( step s 113 ). in detail , when the calculated power operating time of a device is more than the predetermined threshold , the power status determining unit 105 determines that power status of the device indicates power on . further , when the calculated power operating time of a device is less than the predetermined threshold , the power status determining unit 105 determines that power status of the device indicates power off . in fig3 , for screen 6 of the fax application , the operation rate of the scanner 31 is 20 percent , the operation rate of the plotter 32 is 80 percent , and operation rate of the peripheral device is 0 percent . further , when the predetermined threshold is 30 percent , power status of the plotter 32 is determined as power on , and power statuses of the scanner 31 and peripheral device 33 are both determined as power off . thus , the result of the determination is that only the plotter 32 will be provided power . next , when the power status determining unit 105 determines that the displayed display screen is not stored in the operation time storing unit 109 ( step s 110 : no ), the procedure goes to s 120 of fig5 . as illustrated in fig5 , when the power status determining unit 105 determines that the displayed display screen is not stored in the operation time storing unit 109 ( step s 110 : no ), the driver control unit 107 supplies power to all devices . in detail , the driver control unit 107 supplies power to the scanner 31 , the plotter 32 , and the peripheral device 33 . next , in response to receiving an execution instruction by the receiving unit 101 ( step s 121 : yes ), the driver control unit 107 determines a driver to execute function based on the execution instruction , and controls each driver to execute the function . next , the operation time measuring unit 108 starts measuring an operation time of each device ( step s 122 ). next , when the process of each device is finished ( step s 123 : yes ), the operation time measuring unit 108 stores the operating time in the operating time storing unit 109 associated with a display screen that is displayed when the execution instruction is received ( step s 124 ). further , when the operating time storing unit 109 has already stored an operation time , the operating time storing unit 109 stores the measured operation time in addition to the stored operation time . in this way , when an application that is not stored in the power status storing unit 104 is executed , the image forming apparatus 1 is able to determine a power status by executing from the process of s 111 to the process of s 104 . for example , an application that is not stored in the power status storing unit 104 includes an added new application like sdk ( software development kit ) application . thus , when the new application is added in this image forming apparatus 1 , the image forming apparatus 1 is able to control power without prior information of the new application . descriptions of configurations below having reference numerals that are the same as those in the above description are omitted unless there is a special necessity . the image forming apparatus 1 is able to control power supplied to each device based on information from a user . fig6 is a diagram illustrating a functional configuration of the image forming apparatus 2 . as illustrated in fig6 , the image forming apparatus 2 includes the energy saving processing unit 110 , the display unit 20 , the scanner 31 , the plotter 32 , and the peripheral device 33 . the energy saving processing unit 110 includes the input unit 101 , the display information 102 , the display processing unit 103 , the power control unit 106 , the driver control unit 107 , a power state determining unit 112 , a power state storing unit 111 , an operating time measuring unit 113 , an operating time storing unit 114 , and an update unit 115 . the power state storing unit 111 stores power status information of each device corresponding to each user . the power status information will be described below . fig7 is a table indicating the power status information . as illustrated in fig7 , the power state storing unit 111 stores , associated with each display screen , a user id for identifying a user , and power status of each device . further , the user id includes a shared id that does not identify a user . returning to the fig6 , when the receiving unit 101 receives a display instruction together with a user id , the power state determining unit 112 determines the power status of each device by referring the power state storing unit 111 or the operating time storing unit 114 . the operating time measuring unit 113 measures an operation time of a device . further , the operating time measuring unit 113 stores the measured operation time in the operation time storing unit 114 corresponding to a display screen that is displayed on the display unit 20 . fig8 is a table indicating operation time . as illustrated in fig8 , the operation time storing unit 114 stores an operation time of scanner , an operation time of plotter , an operation time of peripheral device , and an operating time of all devices corresponding to a display screen . in fig6 , an update unit 115 updates power status stored in the power state storing unit 111 by referring to the operation time storing unit 114 . fig9 is a flowchart illustrating a procedure for the controlling of power supply of the image forming apparatus 2 . as illustrated in fig9 , the receiving unit 101 receives a display instruction and user id , which are input from a user ( step s 200 ). next , in response to receiving the display instruction and the user id , the display processing unit 103 displays a display screen on the display unit 20 based on the display instruction ( step s 201 ). next , in response to displaying the display screen on the display unit 20 , the power status determining unit 112 determines whether the displayed display screen is stored in association with the received user id in the power state storing unit 111 or not ( step s 202 ). next , when the power status determining unit 112 determines that the displayed display screen is stored in association with the received user id in the power state storing unit 111 ( step s 202 : yes ), the power status determining unit 112 determines the power state of each device associated with the displayed display screen and the received user id ( step s 203 ). next , the power control unit 106 controls power supplying to each device based on the determined power status ( step s 204 ). next , in response to receiving an execution instruction and a user id by the receiving unit 101 ( step s 211 : yes ), the driver control unit 107 determines a driver to execute a function based on the execution instruction , and controls each driver to execute the function . here , when the receiving unit 101 does not receive any execution instruction ( step s 211 : no ), the power control process is finished . next , the operation time measuring unit 113 starts measuring an operation time of each device ( step s 212 ). next , when the process of each driver is finished ( step s 213 : yes ), the operation time measuring unit 113 stores the operating time in the operating time storing unit 114 in association with user id and a display screen that is displayed when the execution instruction is received ( step s 214 ). further , when the operating time storing unit 114 has already stored an operation time , the operating time storing unit 114 stores the measured operation time in addition to the stored operation time . next , the update unit 115 updates the power status stored in the power state storing unit 111 based on the operation time stored in the operation time storing unit 114 ( step s 215 ). in detail , the update unit 115 measures an operating rate of each device based on the operation time of each device and the operating time of all devices . further , when the measured operating rate is more than a predetermined threshold , the update unit 115 updates the power status of a device associated with the user id and the displayed display screen to the status of power on . further , when the measured operating rate is less than the predetermined threshold , the update unit 115 updates the power status of a device associated with user id and the displayed display screen to the status of power off . here , when the power status determining unit 112 determines that the displayed display screen is not stored in association with the received user id in the power state storing unit 111 ( step s 202 : no ), the power control process goes to step s 110 of fig4 . the descriptions provided herein are only exemplary , and variations and modifications may be made without departing from the concepts discussed herein . | 6 |
fig1 depicts a three - layer fire - resistant slab composite ( 1 ). it is provided with the core layer ( 3 ) that essentially corresponds in its composition with fig3 . the core layer ( 3 ) is provided with the outer layers ( 2 , 2 ′) on both sides , which essentially correspond with fig2 . the outer layers ( 2 , 2 ′) are each provided with the reinforcement layer ( 5 ). fig2 shows the outer layers ( 2 , 2 ′) enlarged in a section along line a — a in fig1 . they are comprised of layers ( 4 , 4 ′), which consist of glued expanded ( blown ) vermiculite . the reinforcement layer ( 5 ) is provided between these layers ( 4 and 4 ′). in fig3 the core layer ( 3 ) is depicted enlarged in a section along line b — b in fig1 . in that figure , the vermiculite particles with a smaller grain size are referred to by reference number 6 , while the vermiculite particles with a larger grain size are indicated by reference number 7 . the inorganic , fiber - containing fillers or perlite ( 8 ) are provided between the said vermiculite particles . the invention will now be explained in greater detail by means of an example . the three - layer slab ( 1 ) in accordance with the invention is manufactured , for example , by feeding the vermiculite , of the various origins and various grain sizes indicated by reference numbers 4 , 5 and 6 , to an oven . the heat - treating temperature is 800 to 850 degrees celsius , depending upon which type of vermiculite is present and the grain size of the vermiculite particles . the volume of the vermiculite particles is increased by an eight - to ten - fold value relative to their original size . impurities are removed before the vermiculite particles are fed or supplied to the mixing equipment . in the mixing equipment , the vermiculite particles are glued with binders . the binders used are , for instance , urea - formaldehyde resins , silicates ( water glass ), and phosphates , as well as their mixtures . the binders are used in the form of a solution ; the binder content is in the range of 40 to 70 [%]. thus the binder content in the outer layers ( 2 , 2 ′) is in a range from 15 to 30 %, and in the core layer ( 3 ) it ranges from 15 to 30 %. after glueing , the binder content in the outer layer ( 2 , 2 ′) is approximately 20 %. the binder content in the core layer is also about 20 %. the outer layers ( 2 , 2 ′) are , for instance , produced as follows : a cake of the glued vermiculite particles ( 4 ) is poured on a conveyor belt and the reinforcement layer ( 5 ) is manually deposited on this heap . this reinforcing layer ( 5 ) may be , for instance , a mat or a network of carbon , glass , or metal fibers of varying thickness and web structure . next , this poured cake is fed to a discontinuously operating press and is compressed at a temperature of 160 ° celsius and a compacting pressure of 150 to 200 n / cm 2 . with the set - up according to fig2 a semi - finished product is produced . on one hand , it can be employed as a final product or it is further used for the manufacture of the slab composite , for instance , in accordance with fig1 . in order to produce the core layer ( 3 ), glued vermiculite particles ( 6 , 7 ) of various grain sizes are mixed with inorganic , fiber - containing fillers in a mixer . the grain size of the smaller vermiculite particles ( 6 ) is in the range from 0 . 350 to 3 mm . the grain size of the larger vermiculite particles ranges from 1 to 2 . 5 mm . as inorganic , fiber - containing fillers ( 8 ), rock wool or perlite can be mixed in , for instance . in the finished slab , they serve as sound -, cold -, and heat - insulators . in order to further enhance sound insulation , a metal foil ( 9 , 9 ′) can be provided on both sides of the core layer ( 3 ), the thickness of which is in a range of 0 . 075 mm to 0 . 15 mm . from this mixture , a poured cake is likewise produced , which is transferred to a discontinuous press in which it is processed into a semi - finished product at a temperature of 130 ° celsius and a compacting pressure of 150 to 200 n / cm 2 . this semi - finished product can now be employed for the following purposes : as a semi - finished product in a slab composite in accordance with fig1 . the slab composite ( 1 ) in accordance with the invention is now manufactured from the semi - finished products ( 2 , 2 ′) with which the outer layers are formed , and from the semi - finished product ( 3 ) that forms the core layer . in this process , a pressed stack is formed in such a way that the outer layers ( 2 , 2 ′) enclose the core layer ( 3 ) on both sides . this pressed stack is compressed inside a press in the cold - press process . the improved product characteristics of the slab composite ( 1 ) in accordance with the invention will now be compared to a three - layer slab composite named negor ®, which is generally known to the art , and which consists exclusively of inorganic materials . it can be seen from the table that the binder content of the slab composite in accordance with the invention is substantially less than that of the slab with the brand name negor ®, which has already been known to the art and which consists of purely inorganic expanded materials . nevertheless , surprisingly , the mechanical properties can be retained , and this is the case because of the reinforcement layer ( 5 ). by virtue of this reinforcement layer , the weight of the slab composite is also lower than that of the negor ® slab , which results in advantages in terms of construction technology . moreover , the value of the flexural strength is higher , so that the slab composite ( 1 ) in accordance with the invention can be molded more easily than the negor ® slab . owing to these improved technical parameters , the slab composite in accordance with the invention can be employed for the interior construction of ships and buildings in an easily manageable manner , while international fire - protection standards are met as well . | 1 |
referring to fig5 , the tensioner 110 of the present invention is operatively engaged with a closed loop power transmission system of an internal combustion engine . the power transmission system contains a driving sprocket 102 and at least one driven sprocket 104 , 104 ′. power from the engine &# 39 ; s drive shaft is transmitted from the driving sprocket 102 to the driven sprockets by means of a chain 100 or drive belt . most commonly used with internal combustion engines are chain drives . proper tension must be applied to the chain 100 at all times in order to prevent the jumping of the sprocket teeth by the chain during slackening of any portion of the chain during operation or as a result of increasing wear of the components over time . the tensioner 110 includes a tensioning arm 112 that is operatively engaged with the outer surface of one of the strands of chain between the driving sprocket 102 and one of the driven sprockets 104 . the second tensioning arm 112 ′ of tensioner 110 is operatively engaged with the outer surface of the other strand of chain between the driving sprocket 102 and a second driven sprocket 104 ′. it should be understood that the tensioner 110 of the present invention is also capable of being used in a closed loop power transmission system that has only one driving and one driven sprocket . each tensioning arm , 112 and 112 ′, may be pivotally secured to the face of the engine housing ( not shown ) by pivot mounting means 106 and 106 ′ at respective first ends 107 and 107 ′ of each tensioning arm 112 and 112 ′, as shown in fig5 . the pivot mounting means 106 and 106 ′ allow their respective tensioning arms 112 and 112 ′ to pivot in response to changes in the tension of the chain 100 . alternative pivot mounting points may also be used , such as pivot mounting means 106 a and 106 a ′, which may be located substantially at a mid - point along the longitudinal length of each of the respective tensioning arms 112 and 112 ′. the mounting of tensioning arms 112 and 112 ′ need not be symmetrical in that tensioning arm 112 may be pivot mounted to the engine housing at 106 while tensioning arm 112 ′ may be pivot mounted at 106 a ′. alternatively , tensioning arm 112 ′ may be pivot mounted at 106 ′ while tensioning arm 112 is pivot mounted at 106 a . also , tensioning arms 112 and 112 ′ may concurrently be pivot mounted at 106 a and 106 a ′, respectively . an alternative embodiment of tensioner 110 includes having one of the tensioning arms 112 or 112 ′ securely mounted to the engine housing so that it cannot pivot in response to changing chain tension conditions . for example , tensioning arm 112 may be securely mounted to the engine housing at both locations 106 and 106 a . the other tensioning arm 112 ′ is allowed to pivot about a single pivot mount 106 ′ in response to changing chain tension conditions . each tensioning arm 112 and 112 ′ contains an elongated rectangular shaped chain wear face 105 and 105 ′, respectively , that is semi - rigidly mounted along the length of each tensioning arm facing the strand of chain 100 with which it is operably engaged . each chain wear face 105 and 105 ′ terminates in hooked ends that wrap around the ends of the tensioning arm on which it is installed . each chain wear face 105 or 105 ′ is the contact surface with the strand of chain with which its corresponding tensioning arm is engaged . each chain wear face 105 and 105 ′ has a first end 105 a and 105 a ′, respectively , and a second end 105 b and 105 b ′, respectively . each first end 105 a and 105 a ′ is joined to its corresponding second end 105 b and 105 b ′ by a middle portion that acts as the chain sliding face 105 c and 105 c ′. this is best shown in fig9 . each chain sliding face 105 c and 105 c ′ is in sliding contact with a different strand of chain 100 . each first end lo 5 a and lo 5 a ′ and each second end 105 b and 105 b ′ of its respective chain wear face 105 and 105 ′ are curved underneath and around towards the center of the corresponding wear face . each chain wear face 105 and 105 ′ is longer than its corresponding tensioning arm 112 and 112 ′ such that each curved first end 105 a and 105 a ′ receives the respective first end 107 and 107 ′ of the corresponding tensioning arm 112 and 112 ′ and each curved second end 105 b and 105 b ′ receives the respective second end 109 and 109 ′ of the corresponding tensioning arm 112 and 112 ′, thereby loosely securing each chain wear face 105 and 105 ′ to its corresponding tensioning arm 112 and 112 ′. the chain wear faces 105 and 105 ′ are preferably made of a material that is semi - flexible at engine operating temperatures , in order to allow them to bow out to conform to the changing tension conditions of the chain 100 . optionally , additional biasing means may be provided by one or more blade springs 114 located between the tensioning arm and the rear surface of each of the chain wear faces 105 and 105 ′. a gap clearance exists between each of the first ends 105 a and 105 a ′ of the chain wears faces 105 and 105 ′ and the first ends 107 and 107 ′ of tensioning arms 112 and 112 ′. as well , a gap clearance exists between the second ends 105 b and 105 b ′ of the chain wear faces 105 and 105 ′ and the second ends 109 and 109 ′ of tensioning arms 112 and 112 ′. as at least one blade spring 114 biases each of the chain guide elements 105 and 105 ′ out and away from its respective tensioning arm , the . combined gap clearances between the ends of tensioning arms 112 and 112 ′ and the ends of the chain wear faces 105 and 105 ′ is gradually eliminated until the chain wear faces 105 and 105 ′ can not bow out any further . at this point , the tensioning arms 112 and 112 ′ alone cannot provide further chain tensioning . the second ends 109 and 109 ′ of each of their respective tensioning arms 112 and 112 ′, are connected to each other by an adjusting arm 130 . referring . to fig6 , the second end 109 of tensioning arm 112 is secured to first ends 138 and 138 ′, respectively , of a first pair of elongated straps 134 and 134 ′ by pivot joint 132 . the second end 109 ′ of tensioning arm 112 ′ is secured to first ends 140 and 140 ′, respectively , of a second pair of elongated straps 136 , 136 ′, by pivot joint 132 ′. elongated straps 134 , 134 ′, 136 and 136 ′ may be made of any rigid material , such as , for example , steel , aluminum , alloys thereof , or non - deformable synthetic resinous composite materials . referring to fig7 , the second ends 142 and 142 ′, of their respective first pair of elongated straps 134 and 134 ′ each terminate into a substantially 180 ° hook shape . the second ends 150 and 150 ′ of their respective second pair of elongated straps 136 and . 136 ′ also each terminate into a substantially 180 ° hook shape . second end 150 is slidably engaged through a longitudinal slot 146 in elongated strap 134 and second end 150 ′ is slidably engaged through a longitudinal slot 146 ′ in elongated strap 134 ′. second ends 142 and 142 ′ create a seat to secure a first end of coil spring 160 ( fig6 ). a second end of coil spring 160 is secured by the seat created by second ends 150 and 150 ′. the resting state of coil spring 160 is longer than its length when installed in the adjusting arm 130 in order to provide a force to bias the respective second ends 142 and 142 ′ away from second ends 150 and 150 ′. the elongating force of coil spring 160 urges the first pair of elongated straps 134 and 134 ′ to overlap with the second pair of elongated straps 136 and 136 ′, when required , in response to increasing slack or wear conditions exhibited by the chain 100 . referring to fig8 , various elements of the adjusting arm 130 are removed to better show certain features of ratcheting means 155 . located on the inner surface 137 and in proximity to the second end 150 of elongated strap 136 is an inner rack of teeth 170 . although not shown in this figure , the mirror image elongated strap 136 ′ also contains the same elements as does elongated strap 136 . specifically , on the inner surface 137 ′ and in proximity to the second end 150 ′ of elongated strap 136 ′ is a rack of teeth 170 ′. located on the outer surface 135 ′ and in proximity to the second end 142 ′ of elongated strap 134 ′ is an outer rack of teeth 172 ′. also not shown in this figure , the mirror image elongated strap 134 contains similar elements as are present on elongated strap 134 ′, that is , on the outer surface 135 and in proximity to the second end 142 of elongated strap 134 is an outer rack of teeth 172 . when the adjusting arm 130 is fully assembled , the inner rack of teeth 170 of elongated strap 136 mesh with the outer rack of teeth 172 of elongated strap 134 and the inner rack of teeth 170 ′ of elongated strap 136 ′ mesh with the outer rack of teeth 172 ′ of elongated strap 134 ′. the teeth are designed to index in only one direction in response to the force of the coil spring 160 urging the second ends 142 and 142 ′ of the first pair of elongated straps 134 and 134 ′ away from the second ends 150 and 150 ′ of the second pair of elongated straps 13 and 136 ′. consequently , the distance between the tensioning arms 112 and 112 ′ will decrease in response to an increase in slack or excessive wear conditions exhibited by chain 100 . as the distance between the tensioning arms 112 and 112 ′ decreases , a relatively constant tensioning force on chain 100 is maintained . in order to insure that the inner racks of teeth 170 and 170 ′ remain securely engaged with their corresponding outer racks of teeth 172 and 172 ′, the coil spring seating surfaces of the second ends 150 and 150 ′ are angled toward the central axis of the adjusting arm 130 . concurrently , the coil spring seating surfaces of the second ends 142 and 142 ′ are angled outward away from the central axis of the adjusting arm . when the compressed coil spring 160 is seated between second ends 142 and 142 ′ and second ends 150 and 150 ′, its natural tendency to return to its elongated resting state generates a force on both the angled portions of second ends 142 and 142 ′ and the angled portions of second ends 150 and 150 ′ to insure that the corresponding enmeshed racks of teeth do not jump out of engagement with each other until desired in response to changing chain tension conditions . the tensioning arms 112 and 112 ′ may only employ wear faces 105 or 105 ′ to provide tensioning in the direction of a slack or worn chain . in conjunction with the ratcheting means 155 , the minimal force applied by the wear faces alone may be sufficient enough to tension certain chain drive transmission systems . this embodiment may provide the desired tension for certain power transmission systems . however , other drive transmission systems may have different tension requirements . fig9 shows a cross section of tensioning arm 112 in which an alternate embodiment is shown . a blade spring 114 is added within a recess in the body of the tensioning arm 112 to provide additional force for urging the wear face 105 into forcible sliding contact with the chain 100 . similar embodiments would include more than one blade spring , either stacked on top of one another in a single recess or placed in separate recesses along the length of the tensioning arm 112 . it should be understood that tensioning arm 112 ′ may also incorporate at least one blade spring , if desired . the design parameters of each specific chain drive system may necessitate a tensioner 110 in which both tensioning arms 112 and 112 ′ contain blade springs , or one in which only one of the tensioning arms would contain blade springs . also , neither one of the tensioning arms 112 or 112 ′ might contain a blade spring . backlash is the backward or untensioned travel of a tensioning device . the combination of the amount of force provided by the wear faces 105 and 105 ′ and the indexing movement of the ratcheting means 155 of the invention controls the amount of backlash that occurs in the operation of a closed loop chain driven power transmission system . the gap created between the body of the tensioning arms 112 and 112 ′ and the under side of their respective wear faces 105 and 105 ′ is limited by the amount of gap clearance , previously discussed , between the ends of the wear faces 105 and 105 ′ and the corresponding ends of the tensioning arms 112 and 112 ′. the total amount of the combined gap from both tensioning arms defines the backlash in the power transmission system . backlash determines the timing variation in the driven sprocket ( s ) and must be kept to a minimum . when slack in the chain cannot be absorbed because the maximum gap between the wear faces 105 and 105 ′ and their corresponding tensioning arms 112 and 112 ′ has been reached , the coil spring 160 of the ratchet means 155 provides the required force to index the meshed racks of teeth by at least one tooth and in only one direction . the indexing of the teeth increases the overlap between the pairs of elongated straps of the adjusting arm 130 , and biases the second ends 109 and 109 ′ of the corresponding tensioning arms 112 and 112 ′ toward each other . the reduced distance between the second ends of the tensioning arms 112 and 112 ′ reestablishes forceful contact of the wear faces 105 and 105 ′ with their respective strands of chain 100 . the unidirectional movement of the teeth prevents the adjusting arm 130 from returning to its previous elongated state which would result in an inability to tension the chain due to the loss of or a reduction in forceful contact between the wear faces 105 and 105 ′ and their corresponding strands of chain . accordingly , it is to be understood that the embodiments of the invention herein described are merely illustrative of the application of the principles of the invention . reference herein to details of the illustrated embodiments is not intended to limit the scope of the claims , which themselves recite those features regarded as essential to the invention . | 5 |
reference is first made to fig1 which shows one heated nozzle 10 of a multi - cavity hydraulically actuated valve gated injection molding system seated in a steel cavity plate 12 with a cavity 14 extending between the cavity plate 12 and a movable mold platen 16 . a manifold 18 positioned by locating ring 20 extends between the heated nozzle 10 and cavity plate 12 and a back plate 22 . the heated nozzle 10 is formed generally of a corrosion and abrasion resistant metal such as steel , but has an electric heating element 24 cast into an inner portion 26 formed of a highly thermally conductive metal such as copper to more rapidly disperse the heat to the steel . the heated nozzle 10 has a central bore 28 which receives an elongated valve pin 30 having a driven end 32 and a tip end 34 . the driven end 32 of the valve pin 30 is engaged by hydraulically driven actuating mechanism which is seated in the back plate 22 and reciprocates the valve pin longitudinally between the open position shown and a closed position in which the tip end 34 is seated in a gate 36 leading to the cavity 14 . the actuating mechanism includes a piston 38 which reciprocates in a cylinder 40 seated in a bore in the back plate 22 . the cylinder 40 is secured in position by bolts 42 extending through a flanged portion 44 . the cylinder is sealed by a cap 46 which is screwed into the cylinder 40 and tightened by a forked wrench ( not shown ) which has pins that fit into the small holes 48 in the top of the cap 46 . the valve pin 30 extends through a hole in the piston 38 and is secured to it by a plug 50 which is tightened against the driven end 32 of the piston by inserting a hexagonal wrench ( not shown ) into a socket 52 . the piston 38 has an o - ring 54 which provides a seal between it and the cylinder , and a high temperature seal is provided around the neck 56 of the piston 38 by a v - shaped flexible ring 58 which is held in position by an expansion washer 60 seated in a groove . an abutment sleeve 62 is located between the piston 38 and the cap 46 so that the extent of travel of the piston 38 and the valve pin 30 in the open position can be adjusted by changing the height of the abutment sleeve 62 . as described in more detail in the applicant &# 39 ; s u . s . patent application ser . no . 485 , 024 filed apr . 14 , 1983 entitled &# 34 ; hydraulically actuated injection molding system with alternate hydraulic connections &# 34 ;, the piston is driven according to a predetermined cycle by the application of pressurized hydraulic fluid through ducts 64 , 66 leading to the cylinder 40 on opposite sides of the piston 38 . a melt passage 68 branches out from a recessed inlet 70 through the manifold 18 and extends around the valve pin 30 through the bore 28 in the heated nozzle 10 to the gate 36 . the melt passage 68 joins the bore 28 in a stainless steel bushing seal 72 which is seated in the nozzle 10 . as described in the applicant &# 39 ; s u . s . pat . no . 4 , 026 , 518 which issued may 31 , 1977 , the bushing seal prevents leakage of the pressurized melt along the reciprocating valve pin 30 . the cavity plate 12 and back plate 22 are cooled in a conventional manner by cooling channels 74 . as described above , the nozzle 10 is heated by the insulated electrical element 24 which is cast into it and receives power through terminals 76 ( only one shown ) to maintain the melt flowing through the melt passage 68 within the necessary temperature range . the heated nozzle 10 is seated in the cavity plate 12 on an insulation bushing 78 which provides an insulative air space 80 between the hot nozzle and the cool cavity plate . similarly , the locating ring 20 separates the hot manifold 18 from the cool cavity plate to ensure the insulative air space 80 continues between them . as may be seen , a second insulative air space 82 extends between the cool back plate 22 and the hot manifold 18 . as mentioned above , in the past , the gate to the cavity has extended through the cavity plate itself and the air space 80 between the heated nozzle 10 and the cavity plate 12 has been bridged by a cylindrical titanium nozzle seal extending around the gate . as may be seen , according to the present invention , the heated nozzle 10 has a cylindrical shaped nose portion 84 through which the gate 36 extends to the cavity 14 . the nose portion 84 is securely seated in a cylindrical opening 86 through the cavity plate 12 and has a forward face 88 which , at working temperature , is in alignment with the face 90 of the cavity plate 12 which partially defines the cavity 14 . in addition to sealing off the air space 80 from the pressurized melt , this arrangment has the advantage for critical temperature materials such as polyester and also very high and sharp melting point materials that a more uniform temperature is provided right into the cavity . in other words , improved heat transfer is provided to the gate area and it is not necessary to overheat the melt in the area of the heating element 24 to avoid too low a temperature adjacent the cavity . as compared with the great majority of polymers which have a gradual softening curve , there is a variety of heat and shear sensitive polymers with high and sharp melting points where it is desirable to have a gate temperature that is somewhat below the melting point of the polymer , without the temperature of the melt at any other point in the system rising to more than about 20 ° c . above its melting point . for these mostly crystalline polymers , a simple means of adjusting gate temperature without separate heating means is important . in addition , as will now be described with particular reference to fig2 this structure enables the nozzle manufacturer to supply a single size of nozzle which may be readily adapted by the customer &# 39 ; s moldmaker to the necessary gate size for a particular application . fig2 shows the nose portion 84 and the valve pin tip end 34 as they are supplied by the manufacturer prior to installation . the moldmaker then machines the nose portion to a particular length corresponding to one of the dotted lines shown in fig2 which provides the gate with a selected minimum size at the forward face 88 due to the fact that the gate 36 is tapered in the area . the manufacturer provides the moldmaker with a chart showing the nozzle length to which the nose portion must be machined to provide minimum gate diameters of say 1 . 5 mm , 2 . 0 mm , 2 . 5 mm or 3 . 0 mm . of course , the tip end 34 of the valve pin 30 must similarly be machined to a selected length to correspond to the minimum gate diameter as indicated by the dotted lines in fig2 . the tip end 34 of the valve pin 30 is tapered to match the taper of the gate 36 to provide a tight seal in the closed position . as will be appreciated , both of these are formed by the manufacturer and the gate is normally lapped to provide a good match . thus , the moldmaker has the much easier task of providing cylindrical opening 86 through the cavity plate rather than forming a tapered gate of a particular size to match a particular valve pin . in use , the moldmaker machines the nose portions 84 of the nozzles and the tip ends 34 of the valve pins 30 to provide gates of a particular size , and the system is assembled as shown in fig1 . the cylindrical opening 86 in the cavity plate 12 is made to receive the nose portion 84 of the nozzle 10 when it is cool so that it expands to provide a tight press fit when the nozzle is heated to operating temperature . the amount of heat in the gate area may also be increased by the moldmaker reducing the length of contact h between the cooled cavity plate 12 and the nose portion 84 of the heated nozzle 10 . this will depend upon the material to be molded ; for instance h might be about 2 mm for nylon and about 4 mm for pvc or abs . it is , of course , necessary that the insulation bushing 78 be machined to provide for substantial alignment of the forward face 88 of the nose portion 84 with the adjacent cavity face 90 of the cavity plate after heat expansion at operating temperature . similarly , the height of the locating ring 20 is adjusted to accurately position the manifold 18 against the nozzle 10 . electrical power is then applied to the terminals 76 of the heating element 24 to heat the nozzle 10 up to operating temperature . pressurized melt from the molding machine is then introduced into the melt passage 68 and controlled hydraulic pressure is applied to the actuating mechanism according to a predetermined cycle in a conventional manner . after sufficient melt has been injected to fill the cavity 14 and the high injection pressure held for a short period to pack , the hydraulic pressure is applied to reciprocate the valve pin 30 and piston 38 to the closed position in which the valve pin tip end 34 is seated in the gate 36 . the melt pressure is then reduced and the position held for a cooling period before the mold is opened for ejection . after the mold is closed again , hydraulic pressure is applied to reciprocate the valve pin 30 to the open position and the high injection pressure is reapplied . the forward face 88 of the nose portion 84 and the adjacent face 90 of the cavity plate 12 form one side of the cavity 14 , and therefore it is important that the fit between them be tight to provide the desired temperature in the gate , minimize the witness line on the product , as well as , of course , to avoid leakage . reference is now made to fig3 which shows an alternate embodiment of the invnetion in which the nose portion 84 of the heated nozzle 10 has a somewhat different configuration . in this embodiment , the nose portion 84 is undercut to provide it with a cylindrical shaped head portion 92 extending from a reduced diameter neck portion 94 to the forward face 88 . this extends the air space 80 down around the reduced neck portion 94 and reduces heat loss to the cavity plate 12 and also enhance heat transfer to the gate area . thus , this undercut configuration may be used in addition to or instead of increasing height h for materials where less heat is required or can be tolerated at the forward face 88 . otherwise , the structure and operation of this embodiment of the invention is the same as that described above , and the description need not be repeated . although the description of this invention has been given with respect to particular embodiments , it is not to be construed in a limiting sense . variations and modifications will occur to those skilled in the art . for instance , different types of nozzles and / or actuating mechanisms could be used within the scope of the invention . for a definition of the invention , reference is made to the attached claims . | 8 |
fig1 shows a perspective view of a gripper 1 , which is used as a discharge gripper or as holding pliers , is centrally mounted to a base frame of a wire - bending machine and mainly serves to fix the received workpieces during processing . in contrast thereto , fig2 shows , again in perspective view , a gripper 1 serving as an auxiliary gripper and being mounted to the base frame 2 of a bending machine , but also being movable relative to said frame . such movable auxiliary grippers stabilize the workpieces during bending and fetch new workpieces from the magazine or a conveyor belt . each of the two grippers 1 comprises a gripper arm 3 , which is pivotable about a pivoting axis x and has a respective gripping apparatus 8 mounted thereon . at its freely protruding end , the gripper arm 3 carries a guiding body 4 adjoined by a housing 5 which is supported within the guiding body 4 so as to be displaceable and moveable relative to said guiding body . the assembly consisting of the guiding body 4 and of the housing 5 ( including their built - in elements ) constitutes the actual gripping apparatus 8 . on the housing 5 , there are provided , respectively articulated in a pivotable manner via an axis of rotation 7 , two gripping jaws 6 which protrude from said housing and can be pivoted with respect to each other , namely between open and closed states . whereas the representation of fig1 shows a position in which the housing 5 contacts the guiding body 4 , i . e . is in its retracted position in which the gripping jaws 6 are opened , the representation according to fig2 shows the housing 5 in its position extended out of the guiding body 4 , in which position the two gripping jaws 6 assume their closed clamping position . as fig1 and 2 further show , the guiding body 4 is securely mounted to the respective gripper arm 3 by suitable fasteners ( preferably screws , for example ) not shown in detail . fig3 shows a clearly enlarged perspective view of a gripper 1 , which corresponds to the embodiment of fig1 ; however , the constructive design fully applies also to a different embodiment , such as that which is shown in fig1 . however , unlike shown in fig1 , fig3 shows the housing 5 , which carries the clamping jaws 6 , in the end position in which the housing 5 is extended away from the guiding body 4 . fig4 shows ( in a non - enlarged representation ) a central longitudinal section through the assembly of fig3 . the gripping apparatus 8 is mounted , as shown in fig1 and 2 , to the protruding end of the gripper arm 3 of an auxiliary gripper , of holding pliers or of a discharge gripper by suitable fasteners , which were already mentioned above and are not shown in detail in the figures . the guiding body 4 is fitted directly onto the gripper arm 3 , and two guiding rods 9 are supported in the guiding body 4 , as is apparent from fig3 and in particular fig4 , so that they are displaceable in a direction which is parallel to the central longitudinal axis m of the gripper arm 3 and of the guiding body 4 . further , a rod 10 , which is also displaceable in the direction of the central longitudinal axis m , is supported in the guiding body 4 , such that the central longitudinal axis of this rod 10 coincides with the central longitudinal axis m of the gripping apparatus 8 . the guiding rods 9 are respectively introduced , at their upper ends facing the housing 5 , into corresponding receiving recesses 11 of the housing 5 , were they are connected to the bottom region 20 of the housing 5 in a suitable manner , which connection is illustrated only very schematically in fig3 to 7 . mounted to the lower ends of the guiding rod 9 are resiliently flexible plastic pins or plastic rings 12 , respectively , which have an external diameter that is greater than the through hole provided for each guiding rod 9 in the guiding body 4 , so that , when moving the housing 5 in a direction away from the guiding body 4 , the plastic pins 12 , upon reaching the maximum desired extension position ( cf . fig3 and 4 ), respectively abut against the end surface of the guiding body 4 facing them or against an intermediate plate 19 covering said surface , respectively , which thus forms a stop for the plastic pins 12 and terminates the extension movement of the guiding rod 9 . the actuating rod 10 passes through the guiding body 4 and enters the interior space of the gripper arm 3 behind said guiding body 4 , where the actuating rod 10 can be moved by a pneumatic cylinder in the direction of the central axis min one place ( not shown in the figures ). to the upper end of the rod 10 , there is mounted a control element in the form of a cam body 13 , whose cam contour ( control surface ) has a cross section , as shown in fig4 to 7 , whose width is symmetrical to the central axis m and continuously decreases in the direction of said central axis m , with the specific cam shape being selected such that a desired course of the opening and closing movement of the gripping jaws 6 is achieved during their rotation about the axes of rotation 7 at a predetermined amount of the retracting movement of the cam body 13 between rollers 14 which are attached to the lower end region of each of the gripping jaws 6 . the respective axis of rotation 7 of a gripping jaw 6 is located in a central region of the latter between its two ends , with the respective lever arm being suitably selected according to the desired clumping forces and the forces of pressure of the cam body 13 . as fig4 to 7 further show , the gripping jaws 6 have attached to them , between their rotary axes 7 and the rollers 14 , a biasing tension spring 15 , which extends into a special recess 16 of a gripping jaw 6 with both of its end regions and is mounted to said gripping jaw 6 there by its end . the spring 15 is biased in the tension direction such that a tension bias is exerted upon the gripping jaws 6 at all times and in any position of the two gripping jaws 6 , i . e . also in their fully opened position ( cf . fig7 ). in this manner , there is always a spring bias acting on the gripping jaws 6 towards their opened position ( cf . fig6 and 7 ). a compression spring 17 is also provided between the guiding body 4 and the housing 5 , said compression spring 17 extending around the rod 10 in the central region of the gripping apparatus 8 and always building up a pressure bias in a direction towards the extended position of the housing 5 in any position of the two parts 4 and 5 relative to each other . this compression spring 17 is supported at its upper end on the lower surface of the housing 5 , whereas its other axial side extends into an annular receiving space 18 , which is provided in the central region of the guiding part 4 , around the rod 10 , as shown in fig4 to 7 . the axial length of the annular receiving space 18 is dimensioned such that , in the state of the housing 5 in which it is fully extended as far as the guiding body 4 , the compression spring 17 is seated entirely inside the annular receiving space 18 , as shown in fig7 . the bias of the compression spring 17 is selected such that the latter exerts a bias in the extension direction even in the extended condition of the housing 5 as shown in fig3 and 4 . detailed reference will now be made to the different working positions of the gripping apparatus 8 shown in fig4 to 7 : fig4 shows the closed position of the gripping jaws 6 , between which a workpiece ( not shown ) is securely fixed . the rod 10 is fully extended and , thus , the cam body 13 is retracted between the rollers 14 , while pushing them outwardly . the housing 5 is urged into its extended position by the compression spring 17 , in which extended position the guiding rod 9 with its plastic pins 12 is in contact with the lower surface of an intermediate plate 19 arranged between the gripper arm 3 and the guiding part 4 as a stop . fig5 shows a position in which the housing 5 is still fully extended , while the rod 10 comprising the cam body 13 has been retracted somewhat , to such an extent that the two gripping jaws 6 are no longer in their fully closed position , which is still present in fig6 , but now open a very small gap a , which is smaller , however , than the diameter of the workpiece ( e . g . a wire ) received between the gripping jaws 6 . in this position , the gripping jaws 6 , and , thus , the gripping apparatus 8 can be moved along the received workpiece in the longitudinal direction of the latter , or the workpiece can be displaced in the gripping apparatus 8 , relative to the latter . however , it is then not possible to remove the workpiece from the gripping apparatus 8 . fig6 shows an opened position of the gripping apparatus 8 . in this case , the rod 10 has been lowered so far that the lower surface of the cam body 13 contacts the top surface of the bottom 20 of the housing 5 , in which position the gripping jaws 6 are fully opened . the workpiece can now be taken out upwardly from the gripping apparatus 8 , in which case pivoting of the gripping apparatus 8 about the pivoting axis x is not possible without first removing the workpiece . finally , fig7 shows the fully lowered and opened position of the gripping apparatus 8 . the rod 10 is fully lowered and , in doing so , has pulled the housing 5 downwards against the action of the compression spring 19 also to such an extent that the housing 5 is in contact with the upper surface of the guiding body 4 . in doing so , the guiding rods 9 have also been lowered and the resilient parts 12 ( plastic pins ) are now no longer supported on the intermediate plate 19 at the lower surface of the guiding body 4 , as shown in fig7 . thus , the workpiece can be taken out of the gripping apparatus 8 without any vertical movement , i . e . the gripping apparatus can pivot away without colliding with the workpiece . | 1 |
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