公开(公告)号：US5094741A

公开(公告)日：1992-03-10

申请号：US525964

申请日：1990-05-18

申请人： Lenore R. Frank ,  Christoper M. Wurm ,  Paul C. Dryden ,  Steven J. Engel ,  Mark A. Nickerson ,  Ernest Zerenner

发明人： Lenore R. Frank ,  Christoper M. Wurm ,  Paul C. Dryden ,  Steven J. Engel ,  Mark A. Nickerson ,  Ernest Zerenner

IPC分类号： G01N1/00 ,  B01D11/02 ,  G01N30/02 ,  G01N30/28 ,  G01N30/32

CPC分类号： B01D11/0203 ,  G01N30/28 ,  G01N2030/324 ,  G01N30/02 ,  G01N30/32

摘要： Methods and apparatus for extracting sample components from complex matrices using supercritical fluid as the principal extracting solvent are disclosed. The invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using fluid flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time set points. Flow rate is controlled and system pressure regulated by the variable flow restriction. The invention contemplates opening and closing an orifice in order to control the variable flow restriction, or closing the orifice until set point pressure is achieved and controlling the restriction of the orifice to maintain the set point pressure. The present invention also discloses apparatus for the extraction of components from a sample which include means for regulating the pressure and flow rate of a supercritical extraction solvent.

摘要翻译： 公开了使用超临界流体作为主要提取溶剂从复杂基质中提取样品组分的方法和装置。 本发明利用超临界流体的溶剂功率可以通过密度参数，改性剂浓度和温度来逐步设定的事实。 因此，公开了使用具有可变和可控流量限制的流体流动系统从样品中提取组分的方法和装置。 本发明的方法包括将样品插入样品容器部分，输入温度，压力，流速和提取时间设定点的步骤。 流量控制，系统压力由可变流量限制调节。 本发明设想打开和关闭孔口以便控制可变流量限制，或者关闭孔口，直到实现设定点压力并且控制孔口的限制以保持设定点压力。 本发明还公开了一种用于从样品中提取组分的装置，其包括用于调节超临界萃取溶剂的压力和流速的装置。

公开(公告)号：US5322626A

公开(公告)日：1994-06-21

申请号：US13899

申请日：1993-02-05

申请人： Lenore R. Frank ,  Christopher M. Wurm ,  Paul C. Dryden ,  Steven J. Engel ,  Mark A. Nickerson ,  Ernest H. Zerenner

发明人： Lenore R. Frank ,  Christopher M. Wurm ,  Paul C. Dryden ,  Steven J. Engel ,  Mark A. Nickerson ,  Ernest H. Zerenner

IPC分类号： B01D11/02 ,  G01N30/02 ,  G01N30/28 ,  G01N30/32 ,  B01D15/08

CPC分类号： B01D11/0203 ,  G01N30/28 ,  G01N2030/324 ,  G01N30/02 ,  G01N30/32

摘要： Methods and apparatus for extracting sample components from complex matrices using supercritical fluid as the principal extracting solvent are disclosed. The invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using fluid flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time set points. Flow rate is controlled and system pressure regulated by the variable flow restriction. The output stream from the extraction is then expanded through a nozzle and into a trap. In certain embodiments, the trap is filled with chemically active packing material. In other embodiments, a fractionation zone and other analytical instruments are coupled to the apparatus of the present invention. Methods and apparatus for rinsing the extraction instrument and for diluting the extraction fluid are also disclosed. Methods for operating a supercritical fluid extraction systems comprising a pressure and thermal control systems which are programmable to regulate the system to maintain such values within the design specifications during the extraction process.

摘要翻译： 公开了使用超临界流体作为主要提取溶剂从复杂基质中提取样品组分的方法和装置。 本发明利用超临界流体的溶剂功率可以通过密度参数，改性剂浓度和温度来逐步设定的事实。 因此，公开了使用具有可变和可控流量限制的流体流动系统从样品中提取组分的方法和装置。 本发明的方法包括将样品插入样品容器部分，输入温度，压力，流速和提取时间设定点的步骤。 流量控制，系统压力由可变流量限制调节。 然后将来自提取的输出流通过喷嘴扩展并进入陷阱。 在某些实施方案中，捕集器填充有化学活性填料。 在其他实施例中，分馏区和其它分析仪器耦合到本发明的装置。 还公开了用于冲洗提取仪器和稀释萃取流体的方法和装置。 用于操作超临界流体提取系统的方法包括压力和热控制系统，其可编程以调节系统以在提取过程期间将该值保持在设计规范内。

公开(公告)号：US5240603A

公开(公告)日：1993-08-31

申请号：US804155

申请日：1991-12-06

申请人： Lenore R. Frank ,  Christopher M. Wurm ,  Paul C. Dryden ,  Steven J. Engel ,  Mark A. Nickerson ,  Ernest H. Zerenner

发明人： Lenore R. Frank ,  Christopher M. Wurm ,  Paul C. Dryden ,  Steven J. Engel ,  Mark A. Nickerson ,  Ernest H. Zerenner

IPC分类号： B01D11/00 ,  B01D11/02 ,  G01N30/00 ,  G01N30/02 ,  G01N30/28 ,  G01N30/32 ,  G01N31/00

CPC分类号： G01N30/28 ,  B01D11/0203 ,  G01N2030/324 ,  G01N30/02 ,  G01N30/32

摘要： Methods and apparatus for extracting sample components from complex matrices using supercritical fluid as the principal extracting solvent are disclosed. The invention takes advantage of the fact that the solvent power of a supercritical fluid is stepwise settable by the parameters of density, modifier concentration, and temperature. Accordingly, methods and apparatus for extracting a component from a sample using fluid flow system having a variable and controllable flow restriction are disclosed. The methods of the present invention comprise the steps of inserting the sample into the sample container section, inputting temperature, pressure, flow rate and extraction time set points. Flow rate is controlled and system pressure regulated by the variable flow restriction. The output stream from the extraction is then expanded through a nozzle and into a trap. In certain embodiments, the trap is filled with chemically active packing material. In other embodiments, a fractionation zone and other analytical instruments are coupled to the apparatus of the present invention. Methods and apparatus for rinsing the extraction instrument and for diluting the extraction fluid are also disclosed. Methods for operating a supercritical fluid extraction systems comprising a pressure and thermal control systems which are programmable to regulate the system to maintain such values within the design specifications during the extraction process are also disclosed.

摘要翻译： 公开了使用超临界流体作为主要提取溶剂从复杂基质中提取样品组分的方法和装置。 本发明利用超临界流体的溶剂功率可以通过密度参数，改性剂浓度和温度来逐步设定的事实。 因此，公开了使用具有可变和可控流量限制的流体流动系统从样品中提取组分的方法和装置。 本发明的方法包括将样品插入样品容器部分，输入温度，压力，流速和提取时间设定点的步骤。 流量控制，系统压力由可变流量限制调节。 然后将来自提取的输出流通过喷嘴扩展并进入陷阱。 在某些实施方案中，捕集器填充有化学活性填料。 在其他实施例中，分馏区和其它分析仪器耦合到本发明的装置。 还公开了用于冲洗提取仪器和稀释萃取流体的方法和装置。 还公开了用于操作超临界流体提取系统的方法，其包括压力和热控制系统，其可编程以调节系统以在提取过程期间将该值保持在设计规范内。

公开(公告)号：US5827944A

公开(公告)日：1998-10-27

申请号：US602673

申请日：1996-02-16

申请人： Mark A. Nickerson

发明人： Mark A. Nickerson

IPC分类号： G01N1/34 ,  C12Q1/68

CPC分类号： G01N1/405

摘要： A method and apparatus for sample screening and sample preparation within a vessel sealed with a cap, the vessel having at least a portion of the inside surface coated with a stationary phase having an affinity for analytes of interest. A sample possibly containing such analytes is introduced into the vessel whereby the analytes of interest migrate out of the sample and into the stationary phase for detection by a screening device and for desorption.

摘要翻译： 一种在用盖密封的容器内的样品筛选和样品制备的方法和装置，所述容器具有内表面的至少一部分涂覆有对感兴趣的分析物具有亲和力的固定相。 将可能含有这些分析物的样品引入容器中，由此感兴趣的分析物从样品中迁移到固定相中，以便通过筛选装置进行检测和解吸。

公开(公告)号：US5151178A

公开(公告)日：1992-09-29

申请号：US659244

申请日：1991-02-22

申请人： Mark A. Nickerson ,  John S. Poole ,  Lenore G. R. Frank

发明人： Mark A. Nickerson ,  John S. Poole ,  Lenore G. R. Frank

IPC分类号： G01N30/02 ,  G01N30/08 ,  G01N30/20

CPC分类号： G01N30/08 ,  G01N30/20 ,  G01N2030/085 ,  G01N30/02

摘要： A solenoid driven valve is disclosed which is adaptable for controlling the introduction of a high pressure fluid into a fluid trapping assembly having an absorption column topped with an annular orifice expansion nozzle. The valve has an inlet port to introduce high pressure fluid, an axially moving solenoid driven pin which engages means to restrict fluid flow into said column. A diaphragm is located within the valve to direct fluid into the column and which separates the fluid in a region of high pressure from ambient pressures.

摘要翻译： 公开了一种电磁驱动阀，其适用于控制将高压流体引入具有顶部具有环形孔膨胀喷嘴的吸收塔的流体捕获组件。 阀具有用于引入高压流体的入口端口，轴向移动的电磁驱动销，其接合限制流入所述塔的流体的装置。 隔膜位于阀门内以将流体引导到塔中，并将流体在高压区域与环境压力分离。

公开(公告)号：US5716525A

公开(公告)日：1998-02-10

申请号：US624334

申请日：1996-04-03

申请人： Mark A. Nickerson

发明人： Mark A. Nickerson

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

CPC分类号： B01D11/0203 ,  B01D11/0407 ,  G01N30/02

摘要： Methods and apparatus for extracting an analyte from a sample using a field-portable extraction instrument. The preferred embodiment of the extraction instrument includes an extraction fluid source, a sample container, a valve element, a nozzle, and a collection trap vessel. The methods of the present invention include the steps of inserting the sample into the sample container, attaching the sample container to the instrument, and providing a quantity of pressurized extraction fluid from the pressurized extraction fluid source into the sample container to initiate the extraction process. Extraction is facilitated by directing the extraction fluid into the sample at a rapid flow rate such that the sample and extraction fluid are vigorously mixed and a sample/solvent mixture is created. The valve element is then operated to isolate the extraction fluid source and to fully close the sample container. As an optional step, heat may be applied to the closed sample container to create conditions for effecting supercritical fluid extraction. The valve element is then operated to direct a fluid/constituent mixture from the sample container section to the collection trap vessel. The analyte of interest that is present in the fluid/constituent mixture is thereby trapped.

公开(公告)号：US5142875A

公开(公告)日：1992-09-01

申请号：US662687

申请日：1991-03-01

申请人： Michael S. James ,  Meliss A. Powell ,  Mark A. Nickerson ,  Louis T. Staats, III

发明人： Michael S. James ,  Meliss A. Powell ,  Mark A. Nickerson ,  Louis T. Staats, III

IPC分类号： F04B53/08 ,  F17C13/02

CPC分类号： F17C13/026 ,  F04B53/08 ,  F17C2221/013 ,  F17C2223/0115 ,  F17C2223/0153 ,  F17C2223/033 ,  F17C2227/015 ,  F17C2227/0353 ,  F17C2227/0395 ,  F17C2250/0439 ,  F17C2250/0631

摘要： A method and apparatus for accurately regulating the compressibility of a compressible fluid in a pumping system utilizing a single zone of controlled cooling. Cryogenic cooling is employed for cooling a pump head and a thermally integrated heat exchanger such that a single source of cryogenic fluid can be applied to the heat exchanger to increase the bulk modulus of the compressible fluid just prior to and during the pumping process.

摘要翻译： 一种用于在利用受控冷却的单个区域的泵送系统中精确地调节可压缩流体的压缩性的方法和装置。 低温冷却用于冷却泵头和热集成热交换器，使得单个低温流体源可以施加到热交换器，以在泵送过程之前和期间增加可压缩流体的体积弹性模量。

公开(公告)号：US06423120B1

公开(公告)日：2002-07-23

申请号：US09617215

申请日：2000-07-17

申请人： Mark A. Nickerson ,  Clayton E. Law ,  Rich White

发明人： Mark A. Nickerson ,  Clayton E. Law ,  Rich White

IPC分类号： B01D1508

CPC分类号： G01N30/30 ,  G01N2001/2229 ,  G01N2030/3007 ,  G01N2030/3046 ,  G01N2030/3061

摘要： A preferred sample introduction apparatus includes a wall that defines a channel, with the channel being configured to receive a sample and being adapted to engage in fluid communication with the separation column of a chromatographic apparatus. Preferably, a coating of semi-conductive material is arranged adjacent to at least a portion of the wall. Additionally, a heater controller is provided which electro-magnetically communicates with the coating. So configured, the coating, in response to receiving energy from the heater controller, increases in temperature, thereby increasing a temperature of the sample.

摘要翻译： 优选的样品引入装置包括限定通道的壁，其中通道被配置为接收样品并适于与色谱仪的分离柱进行流体连通。 优选地，半导电材料的涂层被布置成与壁的至少一部分相邻。 另外，提供了与涂层电磁连通的加热器控制器。 如此配置，涂层响应于从加热器控制器的接收能量而增加温度，从而增加样品的温度。

公开(公告)号：US5178767A

公开(公告)日：1993-01-12

申请号：US660447

申请日：1991-02-22

申请人： Mark A. Nickerson ,  John S. Poole ,  Lenore G. R. Frank

发明人： Mark A. Nickerson ,  John S. Poole ,  Lenore G. R. Frank

IPC分类号： G01N30/02 ,  G01N30/08 ,  G01N30/20

CPC分类号： G01N30/08 ,  G01N30/20 ,  G01N2030/085 ,  G01N30/02

摘要： A solenoid driven valve is disclosed which is adaptable for controlling the introduction of a high pressure fluid into a fluid trapping assembly having an absorption column topped with an annular orifice expansion nozzle. The valve has an inlet port to introduce high pressure fluid, an axially moving solenoid driven pin which engages means to restrict fluid flow into said column. A diaphragm is located within the valve to direct fluid into the column and which separates the fluid in a region of high pressure from ambient pressures.

摘要翻译： 公开了一种电磁驱动阀，其适用于控制将高压流体引入具有顶部具有环形孔膨胀喷嘴的吸收塔的流体捕获组件。 阀具有用于引入高压流体的入口端口，轴向移动的电磁驱动销，其接合限制流入所述塔的流体的装置。 隔膜位于阀门内以将流体引导到塔中，并将流体在高压区域与环境压力分离。

公开(公告)号：US5009778A

公开(公告)日：1991-04-23

申请号：US403024

申请日：1989-08-31

申请人： Mark A. Nickerson ,  John S. Poole ,  Lenore G. R. Frank

发明人： Mark A. Nickerson ,  John S. Poole ,  Lenore G. R. Frank

IPC分类号： G01N30/02 ,  G01N30/08 ,  G01N30/20

CPC分类号： G01N30/08 ,  G01N30/20 ,  G01N2030/085 ,  G01N30/02

摘要： A solenoid driven valve is disclosed which is adaptable for controlling the introduction of a high pressure fluid into a fluid trapping assembly having an absorption column topped with an annular orifice expansion nozzle. The valve has an inlet port to introduce high pressure fluid, an axially moving solenoid driven pin which engages means to restrict fluid flow into said column. A diaphragm is located within the valve to direct fluid into the column and which separates the fluid in a region of high pressure from ambient pressures.

摘要翻译： 公开了一种电磁驱动阀，其适用于控制将高压流体引入具有顶部具有环形孔膨胀喷嘴的吸收塔的流体捕获组件。 阀具有用于引入高压流体的入口端口，轴向移动的电磁驱动销，其接合限制流入所述塔的流体的装置。 隔膜位于阀门内以将流体引导到塔中，并将流体在高压区域与环境压力分离。