Apparatus and method for supercritical fluid extraction or supercritical fluid chromatography

• US 5,601,707 A
• Filed: 07/12/1995
• Issued: 02/11/1997
• Est. Priority Date: 07/13/1990
• Status: Expired due to Term

• Current Assignee: Teledyne Isco, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Isco, Inc. (Teledyne Technologies Incorporated)
• Inventors: Jameson, Daniel G., Clay, Dale L., Allington, Robert W., Winter, Robin R.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US08/501,536
• Time in Patent Office: 580 Days
• Field of Search: 210/634, 210/635, 210/656, 210/659, 210/198.2, 210/511, 422/256, 422/257, 422/258, 422/259, 422/260
• US Class Current: 210/198.2
• CPC Class Codes: B01D 11/0203 with a supercritical fluid
• CPC Class Codes: B01D 11/0407 the supercritical fluid acting as solvent for the solute
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent
• CPC Class Codes: F04B 15/08 the liquids having low boiling points
• CPC Class Codes: F04B 2205/03 Pressure in the compression chamber
• CPC Class Codes: F04B 2205/05 Pressure after the pump outlet
• CPC Class Codes: F04B 2205/09 Flow through the pump
• CPC Class Codes: F04B 49/065 and making use of computers
• CPC Class Codes: F04B 9/042 the means being cams
• CPC Class Codes: F05B 2230/41 Hardening; Annealing
• CPC Class Codes: F05C 2201/0493 Tin
• CPC Class Codes: F05C 2253/12 Coating
• CPC Class Codes: F16K 15/1823 for ball check valves
• CPC Class Codes: G01F 1/34 by measuring pressure or differential pressure
• CPC Class Codes: G01N 1/34 Purifying; Cleaning processes or apparatus for extracting or separating nucleic acids from biological samples C12N15/1003
• CPC Class Codes: G01N 1/40 Concentrating samples
• CPC Class Codes: G01N 2001/4033 sample concentrated on a cold spot, e.g. condensation or distillation
• CPC Class Codes: G01N 2001/4061 Solvent extraction
• CPC Class Codes: G01N 2030/121 cooling; cold traps
• CPC Class Codes: G01N 2030/6008 capillary restrictors
• CPC Class Codes: G01N 2030/6013 : interfaces to detectors
• CPC Class Codes: G01N 2035/0441 : for samples
• 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
• CPC Class Codes: G01N 30/60 : Construction of the column
• CPC Class Codes: G01N 30/82 : Automatic means therefor
• CPC Class Codes: G21F 5/015 : for storing radioactive sources, e.g. source carriers for irradiation units; Radioisotope containers

Abstract

An apparatus for supercritical fluid extraction incorporates a removable extraction cartridge which in operation has insignificant pressure difference between its inside and outside walls. Because of the low pressure difference, the extraction cartridge need not have the strength to withstand significant pressure and can be made out of molded plastic for disposable use as well as stainless steel and/or machined plastic for reusability. The extraction cartridge can be removed and opened for sample access without the use of tools. The outside of the cartridge can be purged after it is installed in a heated high pressure vessel to remove contamination from its exterior. In one embodiment, the extractor includes a fraction collector for extractants, an automatic sample changer and an automatic cartridge transfer mechanism which provide completely automated extractions.

Claims

1. Apparatus comprising:

a plurality of sample containers;

at least some of said plurality of sample containers being adapted to hold a different one of a corresponding plurality of samples;

a first transport means;

said first transport means being adapted to carry said plurality of sample containers;

a second transport means;

programming means for causing said first transport means to move a selected sample container and sample to the location of said second transport means;

a supercritical extractor;

said programming means including means for causing said second transport means to move said selected container and sample from the said first transport means to a supercritical extraction means;

means for sealing the selected container at the place of extraction to resist the said extraction pressure;

means for heating sample container at the place of extraction; and

means for passing fluid at said supercritical condition through the said selected sample container and sample, thereby extracting an analyte from the sample.

2. The apparatus of claim 1 further including programming means for causing the second transport means to move the selected container out of the extraction means and back to the first transport means after the extracting of analyte.

3. The apparatus of claim 2 wherein the direction of motion of the said second transport means is vertical.

4. The apparatus of claim 3 wherein the direction of motion of the said first transport means is horizontal.

5. The apparatus of claim 2 wherein the direction of motion of the said first transport means is horizontal.

6. The apparatus of claim 2 in which another sample container and sample is selected from the said first transport after a previous sample has been extracted.

7. Apparatus according to claim 2 further including a fraction collector;

said fraction collector including means for receiving analyte from a sample and depositing the analyte in a corresponding one of a plurality of analyte receptacles.

8. Apparatus according to claim 7 including means for causing the analyte extracted from each of said plurality of samples to be collected in a corresponding one of said plurality of analyte receptacles.

9. The apparatus of claim 1 wherein the direction of motion of the said second transport means is vertical.

10. The apparatus of claim 9 wherein the direction of motion of the said first transport means is horizontal.

11. Apparatus according to claim 9 further including:

a fraction collector;

said fraction collector including means for receiving analyte from a sample and depositing the analyte in a corresponding one of a plurality of analyte receptacles.

12. Apparatus according to claim 11 including means for causing the analyte extracted from each of said plurality of samples to be collected in a corresponding one of said plurality of analyte receptacles.

13. The apparatus of claim 1 wherein the direction of motion of the said first transport means is horizontal.

14. The apparatus of claim 1 in which another sample container and sample is selected from the said first transport after a previous sample has been extracted.

15. Apparatus according to claim 1 further including a fraction collector;

said fraction collector including means for receiving analyte extracted from a sample and depositing the analyte in a corresponding one of a plurality of analyte receptacles.

16. Apparatus according to claim 15 including means for causing the analyte extracted from each of said plurality of samples to be collected in a corresponding one of said plurality of analyte receptacles.

17. Apparatus according to claim 15 further including a variable-orifice fluid restrictor and means for automatically adjusting the variable-orifice fluid restrictor to maintain pressure in the supercritical extractor during collection of the analyte.

18. Apparatus according to claim 17 wherein the variable-orifice fluid restrictor further includes motor control means for adjusting said outlet orifice means.

19. Apparatus according to claim 18 wherein the variable-orifice fluid restrictor further includes a biasing means, said motor control means being arranged to move said outlet orifice means in a first direction against pressure from said biasing means, wherein said biasing means moves the outlet orifice means in the opposite direction.

20. Apparatus according to claim 18 wherein the variable-orifice fluid restrictor further includes heating means for heating of said variable-orifice restrictor.

21. The apparatus of claim 1 further including:

locking means for retaining the selected sample container in the said place of extraction; and

,

said locking means disposed to resist the force produced by the said extraction pressure.

22. The apparatus of claim 21 wherein said locking means and said second transport means each are constructed to separately aid in retaining the selected sample container in said place of extraction.

23. Apparatus for automatic high-temperature high-pressure extraction processing of a sample with an extraction fluid comprising:

more than two samples each in individual sealable sample containers located in a first transport means;

said sample containers insertable and removable from the said first transport means;

said sample containers having a first flow port and a second flow port, and the said sample disposed between the said flow ports;

programming means for causing first transport means to move a selected one of the said more than two sample containers with its contained sample to a location corresponding to a place of extraction;

means for heating the said selected sample container and extraction fluid to a set temperature;

means for pressurizing said process of extraction within a pressure vessel means;

said selected sample container at the said place of extraction being sealed to the pressure of said pressurizing;

extraction fluid flow means producing an extraction fluid flow;

a first connecting means disposed to conduct fluid from the said extraction fluid flow means to the first flow port of the selected sample container;

said extraction fluid flow means forcing extraction fluid through said first fluid flow connecting means and through the first flow port of said selected sample container containing said sample wherein said extraction fluid contacting said sample at said heated and pressurized conditions produce an extract from the sample;

a plurality of collection containers located in a second transport means;

said programming means causing the selection of a collection container in the said second transport means in correspondence with the said selection of a sample container in the said first transport means;

said second fluid flow connecting means being disposed to conduct said extract from the said second flow port of the said selected sample container containing sample to the said selected collection container to receive said extract, wherein means are provided for forcing flow of extraction fluid with extract from the said selected sample container to the said selected collection container;

said selected collection container receiving extract from only one selected sample container; and

said second transport means moving the said selected sample container after the said container has received extract.

24. The apparatus of claim 23 wherein the means for heating includes means for setting set temperature to a temperature at least as high as 150 degrees Celsius.

25. The apparatus of claim 24 further including a third transport means for bringing the selected sample container and the heating means into proximity to cause the sample container to be heated to the said set temperature.

26. The apparatus of claim 23 further including:

an automatically controlled valve connected in line with the said second connecting means;

said programming means causing said valve to open at a first time permitting said flow of extract from the said selected sample container to the said selected collection vessel; and

,

said programming means causing the said valve to close at other times.

27. The apparatus of claim 26 further including a third transport means for bringing the selected sample container and the heating means into proximity to cause the sample container to be heated to the said set temperature.

28. The apparatus of claim 23 in which the said first and second transport means are rotary carousels each carrying sets of adjacent containers;

and

said carousels moving in step by step coordination with each other so that each collection container corresponds to a single particular sample container.

29. The apparatus of claim 28 in which each sample container corresponds to a single particular collection container.

30. The apparatus of claim 28 further including a third transport means for bringing the selected sample container and the heating means into proximity to cause the sample container to be heated to the said set temperature.

31. The apparatus of claim 23 further including a third transport means for bringing the selected sample container and the heating means into proximity to cause the sample container to be heated to the said set temperature.