Decoupled flow and pressure setpoints in an extraction instrument using compressible fluids

• US 5,240,603 A
• Filed: 12/06/1991
• Issued: 08/31/1993
• Est. Priority Date: 03/02/1990
• Status: Expired due to Fees

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Hewlett-Packard Company (HP Inc.)
• Inventors: Zerenner, Ernest H., Nickerson, Mark A., Dryden, Paul C., Engel, Steven J., Frank, Lenore R., Wurm, Christopher M.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US07/804,155
• Time in Patent Office: 634 Days
• Field of Search: 202/169, 202/170, 203/49, 210/634, 210/635, 210/656, 210/659, 210/198.2, 210/137, 210/143, 55/386, 422/255, 422/256
• US Class Current: 210/198.2
• CPC Class Codes: B01D 11/0203 with a supercritical fluid
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent
• CPC Class Codes: G01N 2030/324 speed, flow rate
• CPC Class Codes: G01N 30/02 Column chromatography
• CPC Class Codes: G01N 30/28 Control of physical parameters of the fluid carrier
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence

Abstract

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.

Claims

1. Apparatus for the extraction of components from a sample comprising:

a pump for pumping a supercritical fluid comprising a pump motor and a pump motor speed control;

means for regulating the pressure of the output of said pump to a setpoint pressure;

a flow system for connecting a flow of supercritical fluid from the pump to an extraction section for retaining a sample;

an expansion nozzle connected to the extraction section and having an orifice of a variable predetermined opening size thereby achieving a degree of decoupling flow and pressure; and

a static trap subassembly connected directly to the expansion nozzle,

whereby the pressure drop across said nozzle permits the recovery of dissolved material precipitating from the expanding fluid.

2. The apparatus of claim 1 further comprising means for directing rinse solvent through the trap subassembly to dissolve precipitated components and move the precipitated components to a fraction collection destination.

3. The apparatus of claim 2, wherein said trap is filled with porous granular material.

4. The apparatus of claim 3, wherein said porous material is inert.

5. The apparatus of claim 3, wherein said porous material is chemically active.

6. The apparatus of claim 3, wherein said porous material comprises an adsorbent.

7. The apparatus of claim 6, further comprising means for sampling the fluid solution leaving the extraction chamber prior to the recovery of solutes in the nozzle and the trap.

8. The apparatus of claim 6, further comprising a fractionation bed means for retaining chemically active packing material to provide fractionation of the mixture of the solution leaving the extraction chamber.

9. The apparatus of claim 8, wherein the fractionation bed comprises an inlet that is selectively connected to one of the stream of fluid exiting the extraction section, or a stream of solvent fluid by a multiple port valve means having at least one position that permits the fractionation bed to be isolated from the stream of fluid.

10. The apparatus of claim 8, wherein the fractionation bed further comprises valve means and thermal control means connected to said extraction section and said nozzle.

11. The apparatus of claim 6, further comprising an analytical instrument connected to the stream of fluid exiting the extraction section prior to expansion in the nozzle.

12. The apparatus of claim 11, wherein said analytical instrument is a chromatograph.

13. The apparatus of claim 1, further comprising means for directing rinse solvent through the trap subassembly to dissolve precipitated components and move the precipitated components and additional means for connecting the precipitated components rinsed from the trap to the analytical instrument for further manipulation and subsequent analysis.

14. The apparatus of claim 1, wherein the expansion nozzle having an orifice of a predetermined opening size comprises a plurality of expansion nozzles each of the ones of the plurality having a different degree of restriction.

15. The apparatus of claim 14, wherein each of the plurality of expansion nozzles is adapted to be manually interchangeable.

16. The apparatus of claim 15, wherein at least two of the plurality of expansion nozzles are selectively connected to the flow of pressurized fluid by a two position valve.

17. The apparatus of claim 14, wherein the plurality of expansion nozzles are selectively connected to the flow of pressurized fluid by a multiple position valve.

18. Apparatus for the extraction of components from a sample comprising:

one or more sources of extraction solvent fluid;

one or more extraction solvent fluid input ports;

a high pressure pump connected to the input ports;

a pressure transducer to measure the pressure of the fluid delivered by the high pressure pump;

an extraction chamber flow system connected to the high pressure pump comprising an extraction chamber for retaining the sample in the flow stream of the fluid and a sample input module for containing the sample in the extraction chamber;

a bypass flow system connected to the high pressure pump which routes fluid flow around said extraction chamber section;

means for merging the bypass flow system and extraction chamber flow system together to create a merged flow stream;

sample collection means for separating the extracting solvent fluid from components extracted from said sample connected to the merged flow stream, comprising at least one variable expansion nozzle connected directly to a static trap subassembly;

a flow transducer; and

at least one sample collection vessel,

whereby pressurized liquid flows through the sample under independently predetermined and controlled conditions of flow rate and pressure, and whereby the pressurized fluid dissolves one or more selected components from the sample, said components being collected by the sample collection vessel.