Multi-chambered supercritical fluid extraction cartridge

• US 5,932,095 A
• Filed: 03/01/1996
• Issued: 08/03/1999
• Est. Priority Date: 07/13/1990
• Status: Expired due to Fees

• Current Assignee: Teledyne Isco, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Isco, Inc. (Teledyne Technologies Incorporated)
• Inventors: Allington, Robert W., Walters, Henry, Clay, Dale, Messer, Dale
• Primary Examiner(s): Reifsnyder, David A.
• Application Number:
  US08/609,345
• Time in Patent Office: 1,250 Days
• Field of Search: 210/198.2, 210/511, 210/634, 210/137, 210/205, 210/206, 210/233, 210/637, 422/68.1, 422/69, 422/70, 422/81, 422/83, 422/88, 422/101, 422/100, 422/102, 422/103, 422/104, 422/256, 436/54
• US Class Current: 210/206
• 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 2030/009 Extraction
• 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 30/6034 : joining multiple columns
• CPC Class Codes: G01N 30/6069 : with compartments or bed substructure
• CPC Class Codes: G01N 30/6091 : Cartridges
• CPC Class Codes: G21F 5/015 : for storing radioactive sources, e.g. source carriers for irradiation units; Radioisotope containers

Abstract

A multiple chamber sample holding cartridge is used with a supercritical fluid extractor that causes membranes dividing the cartridge into chambers to rupture upon the pressurization of the sample cartridge, thereby allowing the intermixing of materials contained in the chambers. The neutral oil and loss determination of soybean and other oilseed oils by supercritical fluid extraction is efficient with this two-chambered sample cartridge.

Claims

1. A cartridge adapted for use in a supercritical fluid extraction system that operates at a predetermined pressure, comprising:

at least one seal means for sealing against the flow of fluids;

at least a first and second chamber divided by the at least one seal means;

the flow of fluids causing a pressure difference between said at least first and second chambers;

said at least one seal means having a strength sufficient to resist release of the seal between said at least first and second chambers when the pressure difference between said at least first and second chambers is at a pressure in a range of less than 20 percent of said predetermined pressure between said at least first and second chambers; and

said strength being insufficient to resist release of said seal at said predetermined pressure.

2. A cartridge in accordance with claim 1 wherein said seal means dividing the at least one first and second chambers is a fluid tight seal which can be released by pressurization of the sample cartridge during supercritical fluid extraction.

3. A cartridge in accordance with claim 1 in which the combined volume of the chambers is between 0.2 and 2000 cubic centimeters.

4. A cartridge in accordance with claim 1 in which one of said chambers includes a sample and the other includes a separation medium. cotton seed, soy bean, peanut, lin seed, coconut and sunflower seed.

5. A cartridge adapted for use in a supercritical fluid extraction system that operates at a predetermined pressure, comprising:

at least one seal means for sealing against the flow of fluids;

at least a first and second chamber divided by the at least one seal means;

the flow of fluids causing a pressure difference between said at least first and second chambers;

said at least one seal means having a strength sufficient to resist release of the seal between said at least first and second chambers when the pressure difference between said at least first and second chambers is at a pressure in a range of less than 20 percent of said predetermined pressure between said at least first and second chambers;

said strength being insufficient to resist release of said seal at said predetermined pressure;

a first housing section;

a second housing section;

means for separating said first and second housing sections; and

said first and second housing sections being separable sufficiently close to said seal means to permit cleaning of said seal means prior to used without lose of function.

6. A cartridge in accordance with claim 5 in which said means for separating said first and second housing sections permit the separation of said first and second housing sections without the use of tools.

7. A cartridge in accordance with claim 6 in which said means for separating said first and second housing sections permits separation of said first and second housing sections with a torque of less than 35 inch pounds.

8. A cartridge adapted for use in a supercritical fluid extraction system that operates at a predetermined pressure, comprising:

at least one seal means for sealing against the flow of fluids;

at least a first and second chamber divided by the at least one seal means;

the flow of fluids causing a pressure difference between said at least first and second chambers;

said at least one seal means having a strength sufficient to resist release of the seal between said at least first and second chambers when the pressure difference between said at least first and second chambers is at a pressure in a range of less than 20 percent of said predetermined pressure between said at least first and second chambers;

said strength being insufficient to resist release of said seal at said predetermined pressure; and

at least a third chamber separated by at least a second sealing means.

9. A cartridge in accordance with claim 8 in which the first seal means is a first membrane and the second seal means is a second membrane wherein the first and second membranes release at substantially the same pressure.

10. A cartridge in accordance with claim 8 in which the first and second seal means release at different pressures.

11. Apparatus in accordance with claim 10 further including at least one separation medium wherein said at least one separation medium is alumina.

12. Apparatus in accordance with claim 11 further including at lease one sample wherein said at least one sample is a selected one of oil seed, cotton seed, soy bean, peanut, lin seed, coconut and sunflower seed.

13. A supercriticial fluid extraction system, comprising:

a source of supercritical fluid;

a pressure chamber;

said pressure chamber having at least one inlet and at least one outlet means;

cartridge means adapted to be mounted within said pressure chamber;

said at least one inlet and said outlet means being arranged such as to permit supercritical fluid under pressure to flow inside said cartridge means mounted within said pressure means and outside the cartridge whereby said cartridge has equal pressure on both sides;

said cartridge means including at least one seal means for sealing against the flow fluids;

at least a first and second chamber separated by said at least one seal means.

14. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 13 in which the cartridge means includes:

the flow of supercritical fluid causing a pressure difference between said at least first and second chambers;

said at least one seal means having a strength sufficient to resist release of the seal between said at least first and second chambers when the pressure difference between said at least first and second chambers is at a pressure in a range of less than 20 percent of said predetermined pressure between said at least first and second chambers; and

said strength being insufficient to resist release of said seal at said predetermined pressure.

15. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 14 wherein said seal means dividing the first and second chambers is a fluid tight seal which can be released by pressurization of the sample cartridge during supercritical fluid extraction.

16. A supercritical fluid extraction system that operates at a predetermined pressure according to claim claim 14 in which the combined volume of the chambers is between 0.2 and 2000 cubic centimeters.

17. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 14 in which one of said chambers includes a sample and the other includes a separation medium.

18. A supercritical fluid extraction system that operates at a predetermined pressure, comprising:

a source of supercritical fluid;

a pressure chamber;

said pressure chamber having at least one inlet and at least one outlet means;

cartridge means adapted to be mounted within said pressure chamber;

said at least one inlet and one outlet means being arranged such as to permit supercritical fluid to flow inside said cartridge means mounted within said pressure chamber and outside said cartridge means mounted whereby the cartridge means has equal pressure on both sides;

the cartridge means including;

a first housing section;

a second housing section;

means for separating said first and second housing sections; and

said first and second housing sections and means for separation said first and second housing sections including corresponding ones of at least a first and second chamber separated by at least one seal means for sealing against the flow of fluids;

the flow of fluids causing a pressure difference between said at least first and second chambers;

said at least one seal means having a strength sufficient to resist release of the seal between said at least first and second chambers when the pressure difference between said at least first and second chambers is at a pressure in a range of less than 20 percent of said predetermined pressure between said at least first and second chambers;

said strength being insufficient to resist release of said seal at said predetermined pressure; and

said first and second housing sections being separable sufficiently close to said seal means to permit cleaning of said seal means prior to used without lose of function.

19. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 18 in which said means for separating said first and second housing sections permit the separation of said first and second housing sections without the use of tools.

20. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 19 in which said means for separating said first and second housing sections permits separation of said first and second housing sections with a torque of less than 35 inch pounds.

21. A supercritical fluid extraction system that operates at a predetermined pressure, comprising:

a source of supercritical fluid;

a pressure chamber;

said pressure chamber having at least one inlet and at least one outlet means;

cartridge means adapted to be mounted within said pressure chamber;

said at least one inlet and one outlet means being arranged such as to permit supercritical fluid under pressure to flow inside said cartridge means mounted within said pressure chamber and outside the cartridge means whereby said cartridge means has equal pressure on both sides;

said cartridge means including at least a first and second chamber divided by at least one seal means for sealing against the flow of fluids where said cartridge means has at least a first and second chamber separated by said seal means;

the flow of fluids causing a pressure difference between said at least first and second chambers;

said at least one seal means having a strength sufficient to resist release of the seal between said at least first and second chambers when the pressure difference between said at least first and second chambers is at a pressure in a range of less than 20 percent of said predetermined pressure between said at least first and second chambers;

said strength being insufficient to resist release of said seal at said predetermined pressure; and

said cartridge including at least a third chamber separated by at least a second sealing means.

22. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 21 in which said one seal means incudes a first membrane and said second seal means includes a second membrane wherein each of the at least first membrane and second membrane release at substantially the same pressure.

23. A supercritical fluid extraction system that operates at a predetermined pressure according to claim 22 in which the seal means release at different pressures.

24. Apparatus in accordance with claim 23 in which said separation medium is alumina.

25. Apparatus in accordance with claim 24 further including at least one sample, said at least one sample is a selected one of oil seed, cotton seed, soy bean, peanut, lin seed, coconut and sunflower seed.