Multi-chambered supercritical fluid extraction cartridge and processes using it

• US 6,296,769 B1
• Filed: 08/02/1999
• Issued: 10/02/2001
• 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: Walters, Henry, Clay, Dale, Messer, Dale, Allington, Robert W.
• Primary Examiner(s): Reifsnyder, David A.
• Application Number:
  US09/366,128
• Time in Patent Office: 792 Days
• Field of Search: 210/198.2, 210/137, 210/200, 210/206, 210/634, 210/637, 210/644, 210/656, 422/256, 220/200
• US Class Current: 210/637
• 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 method of supercritical fluid extraction comprising the steps of:

applying supercritical fluid to a first chamber of a sample cartridge while preventing flow to a second chamber;

after supercritical fluid has been applied to said first chamber of said cartridge, permitting said supercritical fluid from said first chamber to flow into a second chamber;

permitting at least a portion of the fluid from said second chamber to be collected.

2. A method in accordance with claim 1 in which the fluid is permitted to flow from said first chamber into said second chamber at a predetermined pressure differential between said first chamber and second chamber.

3. A method in accordance with claim 1 in which the step of applying supercritical fluid to said first chamber includes the step of applying supercritical fluid to a sample in said first chamber.

4. A method in accordance with claim 3 in which the step of permitting fluid to flow from said first chamber into said second chamber includes the step of permitting fluid to flow from said first chamber into said second chamber containing a separating material.

5. A method in accordance with claim 4 in which said fluid is applied to said first chamber at a predetermined pressure less than an operating pressure of said cartridge and released into said second chamber after pressure has equalized between said first chamber and a source of the predetermined pressure whereby the sample may be separated in said second chamber in a sufficiently short period of time to avoid plugging of the separating material in said second chamber.

6. A method in accordance with claim 5 in which said separating material and fluid are used for neutral oil and loss determination.

7. A method according to claim 1 wherein the flow of fluid to the second chamber is blocked by a membrane separating the first and second chambers.

8. A method according to claim 1 in which the flow of fluid to the second chamber is permitted by an increase in pressure in the first chamber beyond a predetermined design pressure.

9. A method according to claim 8 wherein the flow of fluid to the second chamber is blocked by a membrane separating the first and second chambers and the flow of fluid into the second chamber is permitted by causing the membrane to be ruptured by pressure.

10. A method according to claim 1 in wherein the fluid is permitted to flow when a pressure difference between the first and second chambers is at least 20 percent of the operating pressure of the cartridge.

11. A method according to claim 1 wherein extract is assayed after being collected from said second chamber.

12. A method according to claim 11 in which the first chamber includes a sample and the second chamber includes a separating medium.