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：US5133859A

公开(公告)日：1992-07-28

申请号：US487693

申请日：1990-03-02

申请人： Lenore R. Frank ,  Christopher M. Wurm ,  Paul C. Dryden ,  Steven J. Engel

发明人： Lenore R. Frank ,  Christopher M. Wurm ,  Paul C. Dryden ,  Steven J. Engel

IPC分类号： B01D11/00 ,  B01D11/02 ,  G01N1/10 ,  G01N30/02

CPC分类号： B01D11/0203 ,  G01N30/02 ,  Y10T436/255

摘要： Methods and apparatus for extracting sample components from complex matrices using supercritical carbon dioxide as the principal extracting solvent are disclosed. The present 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 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 setpoints. The flow rate is controlled and the system pressure regulated by the variable flow restriction. The present invention contemplates opening and closing the orifice in order to control the variable flow restriction, or closing the orifice until setpoint pressure is achieved and controlling the restriction of the orifice to maintain the setpoint pressure.The present invention also discloses apparatus for the extraction of components from a sample which include means for regulating the pressure and flowrate of a supercritical extraction solvent.

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：US5255205A

公开(公告)日：1993-10-19

申请号：US487658

申请日：1990-03-02

申请人： Christopher M. Wurm ,  Lenore R. Frank ,  Lee H. Altmayer

发明人： Christopher M. Wurm ,  Lenore R. Frank ,  Lee H. Altmayer

IPC分类号： B01D11/00 ,  B01D11/02 ,  G05D7/00 ,  G06F15/20

CPC分类号： B01D11/0203

摘要： Method and apparatus for regulating the passage of fluid through a chamber or other type of conduit. Fluid passage is terminated when the volume of fluid which has swept through a chamber equals a selected multiple of the chamber's internal volume, which multiple is known as swept chamber volumes.