公开(公告)号：US4871453A

公开(公告)日：1989-10-03

申请号：US274753

申请日：1988-11-22

申请人： M. Lalith Kumar

发明人： M. Lalith Kumar

IPC分类号： G01N30/02 ,  G01N30/28

CPC分类号： G01N30/28 ,  G01N30/02

摘要： In one embodiment of the invention supercritical fluid chromatographic separation may be accomplished by apparatus which includes a column, an oven for maintaining the temperature of a sample in the oven, an injector for delivering a sample containing fluid to the column and a pump for delivering carrier fluid to the injector. A discharge outlet for receiving processed fluid from the column contains one or two restrictors and a nozzle for discharge of processed fluid. The pump also delivers fluid which is the carrier fluid not containing the sample to a position in the pressure control inlet so as to alter the linear velocity of the sample containing fluid through the column. A controller controls operation of the oven and pump. A valve and a transducer may be positioned in the line between the pump and the discharge outlet in order to permit adjustment of the pressure of the unprocessed carrier fluid being introduced into the discharge outlet by the controller. The method of this embodiment may employ equipment of this type to effect chromatographic separation at the desired flow rate.

公开(公告)号：US5372716A

公开(公告)日：1994-12-13

申请号：US929727

申请日：1992-08-13

申请人： Joseph M. Levy ,  Raymond K. Houck

发明人： Joseph M. Levy ,  Raymond K. Houck

IPC分类号： B01D11/02 ,  G01N1/34 ,  G01N7/04 ,  G01N30/02 ,  G01N30/06 ,  B01D15/08

CPC分类号： B01D11/0203 ,  G01N7/04 ,  G01N2001/4061 ,  G01N2030/025 ,  G01N2030/062 ,  G01N30/02

摘要： The present invention is a collection system for use with supercritical fluid extraction. The system comprises a device for collecting analyte from a fluid having the same. There is also a restrictor for controlling flow of analyte to the collecting device. The restrictor converts the fluid with analyte from a first pressure to a second pressure. The second pressure is less than the first pressure. The first pressure is a supercritical pressure. The restrictor is in fluidic communication with the collecting device. There is also a device for deabsorbing the analyte from the collecting device. The deabsorbing device is in fluidic communication with the collecting device. The collection system also includes a chromatograph for analyzing the analyte. The chromatograph is in fluidic communication with the collecting device to receive deabsorbed analyte. The chromatograph is remote from the collecting device. The chromatograph can be either a gas chromatograph or a liquid chromatograph. In one embodiment of the collection system, the deabsorbing device backflushes deabsorbing fluid through the collecting device into the chromatograph. That is, the flow of fluid during deabsorbing is in an opposite direction to the flow of fluid during collection. Alternatively, the deabsorbing device foreflushes the deabsorbing fluid through the collecting device into the chromatograph. That is, the flow of fluid during deabsorbing is the same direction as the flow of fluid during collection.

摘要翻译： 本发明是用于超临界流体萃取的收集系统。 该系统包括用于从具有该分析物的流体收集分析物的装置。 还存在用于控制分析物流向收集装置的限制器。 限流器将具有分析物的流体从第一压力转换为第二压力。 第二压力小于第一压力。 第一个压力是超临界压力。 限流器与收集装置流体连通。 还有一种用于从收集装置中吸收分析物的装置。 脱吸装置与收集装置流体连通。 收集系统还包括用于分析分析物的色谱仪。 色谱仪与收集装置流体连通，以接收去吸收的分析物。 色谱仪远离收集装置。 色谱仪可以是气相色谱仪或液相色谱仪。 在收集系统的一个实施例中，脱吸装置将吸收流体通过收集装置反冲洗成色谱仪。 也就是说，在吸收期间流体的流动与收集期间的流体流相反。 或者，脱吸装置通过收集装置将去吸收流体前驱到色谱仪中。 也就是说，吸收时的流体流动与收集期间的流体流动方向相同。

公开(公告)号：US5316262A

公开(公告)日：1994-05-31

申请号：US828729

申请日：1992-01-31

申请人： Douglas J. Koebler

发明人： Douglas J. Koebler

IPC分类号： F16K7/06 ,  G01M3/00

CPC分类号： F16K7/061 ,  G01M3/007 ,  Y10T137/0391 ,  Y10T137/2196

摘要： The present invention is an apparatus for restricting the flow of fluid. The apparatus defines a tubular member having a channel. The tubular member has a first portion in which the channel has a first cross sectional area. There is also a second portion for restricting the flow of fluid defined by a reproducible deformity in the channel such that the channel has a second cross sectional area which is smaller than the first cross sectional area of the first portion. The tubular member further defines a third portion having a third cross sectional area which is greater than the second cross sectional area of the second portion. All of the cross sectional dimensions of the second and third portions are disposed within a cylindrical envelope having a diameter equal to the diameter of the first portion and extending therefrom. The tubular member is comprised of a material having sufficient rigidity to maintain a preferred reproducible permanent deformity in the channel. Portion has an essentially constant outside diameter and wherein all cross sectional dimensions of the tubular member are less than or equal to the diameter of the first portion and all of the cross sectional dimensions of the second and third portions are disposed within a cylindrical envelope having a diameter equal to the diameter of the first portion and extending therefrom. Preferably, the deformity is defined by a spherical indentation and the tubular member is comprised of stainless steel. The present invention is also a method of forming a fluid restrictor comprising the steps of first placing a tubular member having a channel and a predetermined outside diameter into a fixed relationship with a deforming apparatus. Then, there is the step of deforming the tubular member in a reproducible manner such that a cross sectional area of the channel is decreased so flow of fluid through the channel is restricted a desired amount. The deforming step does not cause the tubular member to flare and all of the cross sectional dimensions of the second and third portions disposed within a cylindrical envelope having a diameter equal to the diameter of the first portion and extending therefrom. Preferably, the deforming step includes the step of forcing a shaping element of the deforming apparatus against the tubular member. Alternatively, the deforming apparatus can be used to adjust the magnitude of fluid restriction during operation of the fluid restrictor.

公开(公告)号：US5241998A

公开(公告)日：1993-09-07

申请号：US784768

申请日：1991-10-30

申请人： Mehdi Ashraf-Khorassani

发明人： Mehdi Ashraf-Khorassani

IPC分类号： G01N30/02 ,  G01N30/30 ,  G01N30/32 ,  G01N30/56

CPC分类号： G01N30/56 ,  G01N2030/3007 ,  G01N2030/565 ,  G01N30/02 ,  G01N30/32

摘要： The present invention is related to an apparatus for packing an analytical chromatography column having a first opening and a second opening with packing particles. The apparatus comprises means for providing solvent at a density essentially equal to the density of the packing particles. The providing means is in fluidic communication with the first opening of the column. The apparatus also comprises a first reservoir for containing the packing particles. The reservoir is in fluidic communication with the providing means such that solvent can mix with the particles in the first reservoir to form a slurry where the particles are suspended in the solvent and agglomeration of the packing particles is essentially absent when the slurry is introduced into the analytical chromatography column. There is also valve means in fluidic communication with the first reservoir and the first opening of the analytical column for controlling flow of the slurry of pressurized solvent and packing particles to the analytical column from the first reservoir. A fluid restrictor is fluidically connected to the second opening of the column for allowing the solvent to escape from the column while maintaining pressurization therein. The invention also relates to a method of packing an analytical column with packing particles. The method comprises the steps of pressurizing a first reservoir having packing particles disposed therein, with a solvent until the density of the solvent equals the density of the particles and forms a slurry where the particles are suspended in the solvent. Then, there is the step of fluidically connecting the first reservoir to an analytical column at essentially the same pressure as the first pressure such that the slurry flows into a chamber of the analytical column.

摘要翻译： 本发明涉及一种用于包装分析色谱柱的装置，其具有第一开口和具有填充颗粒的第二开口。 该装置包括以基本上等于包装颗粒的密度的密度提供溶剂的装置。 提供装置与柱的第一开口流体连通。 该设备还包括用于容纳填料颗粒的第一储存器。 储存器与提供装置流体连通，使得溶剂可以与第一储存器中的颗粒混合以形成浆料，其中颗粒悬浮在溶剂中，并且当浆料被引入到浆料中时，填充颗粒的聚集基本上不存在 分析色谱柱。 还存在与第一储存器和分析柱的第一开口流体连通的阀装置，用于控制加压溶剂和填充颗粒的浆料从第一储存器流到分析柱。 流体限流器流体连接到塔的第二开口，用于允许溶剂从塔中逸出，同时保持加压。 本发明还涉及一种用包装颗粒包装分析柱的方法。 该方法包括以下步骤：用溶剂对其中设置有填充颗粒的第一储存器加压，直到溶剂的密度等于颗粒的密度，并形成悬浮在溶剂中的浆料。 然后，存在以与第一压力基本相同的压力将第一储存器流体连接到分析柱的步骤，使得浆料流入分析柱的室。

公开(公告)号：US4814089A

公开(公告)日：1989-03-21

申请号：US157020

申请日：1988-02-17

申请人： M. Lalith Kumar

发明人： M. Lalith Kumar

IPC分类号： G01N30/02 ,  G01N30/28 ,  B01D15/08

CPC分类号： G01N30/28 ,  G01N30/02

摘要： In one embodiment of the invention supercritical fluid chromatographic separation may be accomplished by apparatus which includes a column, an oven for maintaining the temperature of a sample in the oven, an injector for delivering a sample containing fluid to the column and a pump for delivering carrier fluid to the injector. A discharge outlet for receiving processed fluid from the column contains one or two restrictors and a nozzle for discharge of processed fluid. The pump also delivers fluid which is the carrier fluid not containing the sample to a position in the pressure control inlet so as to alter the linear velocity of the sample containing fluid through the column. A controller controls operation of the oven and pump. A valve and a transducer may be positioned in the line between the pump and the discharge outlet in order to permit adjustment of the pressure of the unprocessed carrier fluid being introduced into the discharge outlet by the controller. The method of this embodiment may employ equipment of this type to effect chromatographic separation at the desired flow rate.

摘要翻译： 在本发明的一个实施方案中，超临界流体色谱分离可以通过以下装置实现，该装置包括柱，用于保持样品在烘箱中的温度的烘箱，用于将含有流体的样品输送到塔的注射器和用于输送载体的泵 流体到注射器。 用于从塔中接收加工流体的排出口包含一个或两个限流器和用于排出被处理流体的喷嘴。 泵还将不含样品的载体流体的流体输送到压力控制入口中的位置，以便改变通过柱的含有流体的样品的线速度。 控制器控制烤箱和泵的操作。 阀和换能器可以位于泵和排放出口之间的管线中，以便允许通过控制器调节被引入排放出口的未处理的载体流体的压力。 该实施方案的方法可以使用这种类型的设备以期望的流速进行色谱分离。

公开(公告)号：US5954954A

公开(公告)日：1999-09-21

申请号：US879336

申请日：1997-06-20

申请人： Raymond K. Houck ,  Douglas J. Koebler ,  Glen P. Williams ,  Joseph M. Levy ,  Victor G. Danielson

发明人： Raymond K. Houck ,  Douglas J. Koebler ,  Glen P. Williams ,  Joseph M. Levy ,  Victor G. Danielson

IPC分类号： B01D11/02 ,  B01D15/08 ,  G01N1/34 ,  G01N1/40 ,  G01N30/06 ,  G01N33/24

CPC分类号： G01N1/34 ,  B01D11/0203 ,  G01N2001/4061 ,  G01N2030/062 ,  G01N33/24

摘要： The present invention pertains to an apparatus for gathering analyte. The apparatus comprises a pumping mechanism for pumping solvent at supercritical pressure. The apparatus also comprises an extraction mechanism which receives a first sample and at least a second sample separate and distinct from the first sample and extract analyte from them essentially simultaneously. The extraction mechanism is connected to the pump mechanism to receive solvent at supercritical pressure for extracting the analyte from the samples. The apparatus additionally comprises a collection mechanism for collecting analyte from the solvent after the analyte has been extracted from the samples. The collection mechanism receives the supercritical solvent having the analyte extracted from the samples from the extraction mechanism. The present invention pertains to a method for extracting analyte. The method comprises the steps of pumping solvent at a supercritical pressure. Then there is the step of extracting analyte from N samples essentially simultaneously with the solvent at a supercritical pressure, where N is greater than or equal to two and is an integer. The N samples are separate and distinct from each other. Then there is the step of collecting the analyte of the N samples from the solvent.

摘要翻译： 本发明涉及用于收集分析物的装置。 该装置包括用于在超临界压力下泵送溶剂的泵送机构。 该装置还包括提取机构，其接收第一样品和至少第二样品，其与第一样品分离并且不同，并且基本上同时从其中提取分析物。 提取机构连接到泵机构以在超临界压力下接收溶剂以从样品中提取分析物。 该装置另外包括用于在从样品中提取分析物之后从溶剂收集分析物的收集机构。 收集机构接收来自提取机构的样品提取的分析物的超临界溶剂。 本发明涉及提取分析物的方法。 该方法包括以超临界压力泵送溶剂的步骤。 然后，在超临界压力下，基本上与溶剂同时从N个样品中提取分析物，其中N大于或等于2，并且为整数。 N个样本是分开的并且彼此不同。 然后是从溶剂中收集N个样品的分析物的步骤。

公开(公告)号：US5453198A

公开(公告)日：1995-09-26

申请号：US993295

申请日：1992-12-21

申请人： Mehdi Ashraf-Khorassani ,  Gregory Shogan ,  Raymond K. Houck

发明人： Mehdi Ashraf-Khorassani ,  Gregory Shogan ,  Raymond K. Houck

IPC分类号： B01D11/02 ,  G01N1/34 ,  G01N7/04 ,  G01N30/02 ,  G01N30/06 ,  B01D11/04

CPC分类号： G01N1/34 ,  B01D11/0203 ,  G01N7/04 ,  G01N2001/4061 ,  G01N2030/025 ,  G01N2030/062 ,  G01N30/02 ,  Y10T436/25875

摘要： An orifice which includes a housing having a low pressure side with a first bore hole and a second bore hole. The low pressure side has a first channel and a second channel in fluidic communication with the first bore hole and the second bore hole, respectively. The housing also has a high pressure side with a third bore hole. The orifice also includes an adapter which has a tip, a fourth bore hole and a third channel in fluidic communication therewith. The third channel has a constant diameter for maintaining an essentially constant pressure thereacross when pressure is applied thereto such that fluid flowing through the third channel does not solidify. The adapter is sealingly received by the third bore hole such that the third channel and the first channel align. Additionally, the housing includes an interface plate disposed in the housing between the third channel and the first channel. The plate sealingly receives the tip of the adapter and allows for flow to exist between the third channel and the first channel through a plate hole. A method for collecting analyte. The method includes the steps of providing analyte obtained from supercritical fluid extraction to a collection trap through a high pressure side of an orifice.

摘要翻译： 一种孔口，包括具有低压侧的壳体，其具有第一钻孔和第二钻孔。 低压侧分别具有与第一钻孔和第二钻孔流体连通的第一通道和第二通道。 壳体还具有具有第三钻孔的高压侧。 孔口还包括具有尖端，第四钻孔和与其流体连通的第三通道的适配器。 第三通道具有恒定的直径，用于在施加压力时保持基本恒定的压力，使得流过第三通道的流体不固化。 适配器被第三钻孔密封地接收，使得第三通道和第一通道对准。 此外，壳体包括设置在第三通道和第一通道之间的壳体中的接口板。 板密封地接收适配器的尖端，并允许流动通过板孔存在于第三通道和第一通道之间。 收集分析物的方法。 该方法包括以下步骤：通过孔的高压侧将从超临界流体萃取获得的分析物提供到收集阱。

公开(公告)号：US5379790A

公开(公告)日：1995-01-10

申请号：US848424

申请日：1992-03-06

申请人： Mark L. Bruce ,  Douglas J. Keebler

发明人： Mark L. Bruce ,  Douglas J. Keebler

IPC分类号： F16K7/06 ,  G01M3/00 ,  F16K7/04

CPC分类号： F16K7/061 ,  G01M3/007 ,  Y10T137/0318

摘要： The present invention pertains to an apparatus for restricting supercritical fluid. The apparatus comprises an elastic tube through which the supercritical fluid flows. The apparatus also comprises means for adjustably compressing the elastic tube. The comprising means is in contact with the tube. Preferably, there is also means for facilitating flow through the tube. The facilitating means is in communication with the tube in proximity to the compressing means. In a preferred embodiment, the adjustable compressing means includes a first member having a first opening through which the tube extends. The first opening has a threaded portion. There is also a second member having a second opening through which the tube extends. The second member has a threaded shaft for threadingly engaging with the threaded portion of the first opening. A compression structure is seated within the first opening in contact with the elastic tube such that as the threaded shaft is screwed within the threaded portion, the compression structure adjustably compresses the tube. Preferably, the first opening has a tapered portion upon which a tapered compression member of the compression structure is seated. In an alternative embodiment, the apparatus includes means to compress a second portion of the tube. If it is desired, the apparatus can be self-adjusting. In this embodiment, there is means for determining the magnitude of supercritical fluid restriction within the elastic tube. The determining means generates a signal. A motor is provided for automatically adjusting the compressing means according to the signal. Preferably, the determining means includes a flow sensor and supercritical fluid identification means. The present invention also pertains to a method of restricting supercritical fluid flow. The method comprises the steps of establishing supercritical fluid flow through an elastic tube, adjustably compressing the elastic tube such that a desired flow rate is maintained therein and applying energy to the supercritical fluid in the tube in proximity to where the tube is compressed. Preferably, there is the step of monitoring the magnitude of supercritical fluid restriction and the compressing step includes the step of automatically adjusting a first compression member against the tube according to the monitored supercritical fluid restriction. Preferably, the energy supplying step includes the step of heating the supercritical fluid in the tube.

公开(公告)号：US5205987A

公开(公告)日：1993-04-27

申请号：US662255

申请日：1991-02-28

申请人： Mehdi Ashraf-Khorassani ,  Gregory Shogan ,  Raymond K. Houck

发明人： Mehdi Ashraf-Khorassani ,  Gregory Shogan ,  Raymond K. Houck

IPC分类号： B01D11/02 ,  G01N1/34 ,  G01N7/04 ,  G01N30/02 ,  G01N30/06

CPC分类号： G01N1/34 ,  B01D11/0203 ,  G01N7/04 ,  G01N2001/4061 ,  G01N2030/025 ,  G01N2030/062 ,  G01N30/02 ,  Y10T436/25875

摘要： The present invention pertains to an off-line collection system for use with supercritical fluid extraction. The system is comprised of mechanism for collecting analyte associated with the supercritical fluid extraction. The system is additionally comprised of an orifice for controlling flow of analyte to the collecting mechanism. The orifice converts analyte at a high pressure to a lower pressure. The orifice has a high pressure side which receives said high pressure analyte, and a lower pressure side in fluidic communication with the high pressure side which receives said high pressure analyte after it has been converted to a lower pressure. The high pressure side is capable of transporting analyte thereacross without essentially any loss thereof to the low pressure side which is in fluidic communication with the collecting mechanism. The analyte experiences essentially constant pressure as it is transported across the high pressure side. The system is also comprised of mechanism for desorbing the analyte from the collection mechanism. The desorbing mechanism is in fluidic communication with the collecting mechanism. In a preferred embodiment, the system includes mechanism for purging the analyte. The purging mechanism is in fluidic communication with the collecting mechanism. Additionally, the collecting mechanism preferably includes a collection trap in which analyte is gathered, and mechanism for controlling the flow of analyte into the collection trap. The flow controlling mechanism is in fluidic communication with the collection trap and the purging mechanism. The flow control mechanism preferably includes an orifice.

摘要翻译： 本发明涉及一种用于超临界流体萃取的离线收集系统。 该系统由用于收集与超临界流体萃取物相关的分析物的机构组成。 该系统还包括用于控制分析物流到收集机构的孔口。 孔口将分析物在高压下转换成较低的压力。 孔口具有高压侧，其接收所述高压分析物，以及与高压侧流体连通的低压侧，其在将其转换成较低压力之后接收所述高压分析物。 高压侧能够将分析物在其上传输而基本上不会损失到与收集机构流体连通的低压侧。 分析物在高压侧运输时，基本上保持恒定的压力。 该系统还包括从收集机构解吸分析物的机理。 解吸机构与收集机构流体连通。 在优选实施例中，该系统包括用于清除分析物的机构。 清洗机构与收集机构流体连通。 此外，收集机构优选地包括其中收集分析物的收集阱，以及用于控制分析物流入收集阱的机构。 流量控制机构与收集阱和清洗机构流体连通。 流量控制机构优选地包括孔口。

公开(公告)号：US5866004A

公开(公告)日：1999-02-02

申请号：US524916

申请日：1995-09-08

申请人： Raymond K. Houck ,  Douglas J. Koebler ,  Glen P. Williams ,  Kenneth J. Kato ,  Robert D. Parks ,  Paul A. Bauer, Jr.

发明人： Raymond K. Houck ,  Douglas J. Koebler ,  Glen P. Williams ,  Kenneth J. Kato ,  Robert D. Parks ,  Paul A. Bauer, Jr.

IPC分类号： B01D11/02 ,  B01D15/08 ,  G01N1/34 ,  G01N1/40 ,  G01N30/06 ,  G01N33/24 ,  B01D11/00

CPC分类号： G01N1/34 ,  B01D11/0203 ,  G01N2001/4061 ,  G01N2030/062 ,  G01N33/24 ,  Y10T436/255

摘要： A supercritical fluid extraction (SFE) system. The SFE system includes a mechanism for providing supercritical fluid for extracting analyte from a sample. The SFE system also includes an extraction vessel and a mechanism for moving the extraction vessel into fluidic communication with the SFE system so that supercritical fluid can flow through the extraction vessel and extract analyte from the sample. Preferably, the SFE system is additionally comprised of a mechanism for holding a plurality of extraction vessels and an extraction chamber assembly. In this design, the moving mechanism selectively moves an extraction vessel from the holding mechanism into the extraction chamber in fluidic communication with the SFE system. Preferably, the SFE system further includes a computer for controlling the functions of the SFE system. The computer, for instance, could automatically and sequentially control the supercritical fluid extractions of the samples within the holding mechanism. The SFE system preferably includes a mechanism for collecting analyte from the fluid with analyte. The collecting mechanism is in fluid communication with extraction chamber assembly and preferably includes a restrictor for controlling the flow of fluid with analyte to the collecting mechanism. The restrictor converts the fluid with analyte from a first supercritical pressure to a second pressure which is less than the first supercritical pressure.

摘要翻译： 超临界流体萃取（SFE）系统。 SFE系统包括提供用于从样品中提取分析物的超临界流体的机制。 SFE系统还包括提取容器和用于将提取容器移动到与SFE系统流体连通的机构，使得超临界流体可以流过提取容器并从样品中提取分析物。 优选地，SFE系统还包括用于保持多个提取容器和提取室组件的机构。 在该设计中，移动机构选择性地将提取容器从保持机构移动到与SFE系统流体连通的提取室中。 优选地，SFE系统还包括用于控制SFE系统的功能的计算机。 例如，计算机可以自动和顺序地控制保持机构内的样品的超临界流体萃取。 SFE系统优选地包括用于从具有分析物的流体收集分析物的机构。 收集机构与提取室组件流体连通，并且优选地包括限制器，用于控制具有分析物的流体与收集机构的流动。 限流器将具有分析物的流体从第一超临界压力转换为小于第一超临界压力的第二压力。