Supercritical fluid extraction coupled to analytical chromatography system

• US 5,372,716 A
• Filed: 08/13/1992
• Issued: 12/13/1994
• Est. Priority Date: 02/28/1991
• Status: Expired due to Fees

• Current Assignee: Teledyne Isco, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Suprex Corp (Teledyne Technologies Incorporated)
• Inventors: Houck, Raymond K., Levy, Joseph M.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US07/929,727
• Time in Patent Office: 852 Days
• Field of Search: 210/634, 210/635, 210/656, 210/659, 210/198.2, 422/70, 422/285
• 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 2001/4061 Solvent extraction
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/062 extracting sample from raw material
• CPC Class Codes: G01N 30/02 Column chromatography
• CPC Class Codes: G01N 7/04 by absorption or adsorption alone

Abstract

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.

Claims

1. A collection system for use with supercritical fluid extraction comprising:

a device for collecting analyte from a fluid;

a restrictor for controlling flow of fluid with analyte to the collecting device, said restrictor converting fluid with analyte from a first pressure to a second pressure, said second pressure less than said first pressure, said first pressure being a supercritical pressure, said restrictor in fluidic communication with said collecting device;

a device for deabsorbing the analyte from the collecting device, said deabsorbing device in fluidic communication with said collecting device;

a chromatograph for analyzing the analyte, said chromatograph in fluidic communication with said collecting device to receive deabsorbed analyte, said chromatograph remote from said collecting device; and

an alternative loop for fluidically connecting the deabsorbing means to the chromatograph remotely from the device for collecting analyte such that the chromatograph can analyze a first sample while the collecting device simultaneously collects a second sample.

2. A system as described in claim 1 wherein the collecting device has a first end and a second end, said restrictor fluidically connected to the collecting device through the first end, said deabsorbing device in fluidic communication with the collecting device through the first end such that a deabsorbing fluid of the deabsorbing device flows from said first end to said second end.

3. A system as described in claim 2 wherein the chromatograph is in fluidic communication with the collecting device through the second end of the collecting device.

4. A system as described in claim 3 wherein the chromatograph includes a gas chromatograph.

5. A system as described in claim 3 wherein the chromatograph includes a liquid chromatograph.

6. A system as described in claim 1 wherein the collecting device has a first end and a second end, said restrictor fluidically connected to the connecting device through the first end, said deabsorbing device in fluidic communication with the collecting device through the second end such that a deabsorbing fluid of the deabsorbing device flows from said second end to said first end of said collecting device.

7. A system as described in claim 6 wherein the chromatograph is in fluidic communication with the collecting device through the first end of the collecting device.

8. A system as described in claim 7 wherein the chromatograph includes a gas chromatograph.

9. A system as described in claim 6 wherein the chromatograph includes a liquid chromatograph.

10. A system as described in claim 1 wherein said collecting device includes a collection trap in which analyte is gathered.

11. A system as described in claim 10 wherein the collecting device includes a device for cryogenically cooling the collection trap to at least -180°

C. and a device for heating the collection trap to at least 275°

C. at a rate up to 1000°

C./min., said cooling device and said heating device in thermal communication with said collection trap.

12. A system as described in claim 11 wherein the deabsorbing device includes N reservoirs, where N is an integer ≧

1, said liquid reservoirs holding deabsorbing fluid that deabsorbs analyte gathered in the collection trap and transports it to the chromatograph;

said deabsorbing device also including a device for pumping the liquid in the reservoir to the collection trap, said pumping device in fluidic communication with said reservoir and said collection trap.

13. A system as described in claim 12 wherein said heating device includes a resistance coil disposed about the collection trap to inductively or resistively heat the trap.

14. A system as described in claim 13 wherein said cooling device includes a device for supplying liquid CO₂ about the collection trap to cryogenically cool the trap.

15. A system as described in claim 14 wherein the pumping device includes a pump in fluidic communication with the liquid reservoir.

16. A system as described in claim 15 wherein the collection trap includes absorbing beads disposed therein to increase the surface area upon which the analyte can be gathered.

17. A system as described in claim 16 wherein fluidic communications are obtained by steel tubing, and the collection trap is made of stainless steel.

18. A collection system as described in claim 1 wherein the deabsorbing device includes a liquid pump in fluidic communication with the collecting device and the chromatograph to provide fluid to the collecting device to deabsorb analyte in the collecting device and to provide fluid to the chromatograph to analyze the analyte.