Apparatus and method for supercritical fluid extraction

• US 5,690,828 A
• Filed: 02/14/1996
• Issued: 11/25/1997
• 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: Liescheski, Phillip Bearnard III, Clay, Dale Lee, Jameson, Daniel Gene, Allington, Robert William, Winter, Robin Randall
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US08/601,250
• Time in Patent Office: 650 Days
• Field of Search: 210/86, 210/94, 210/149, 210/175, 210/177, 210/180, 210/198.2, 210/511, 210/634, 210/656, 210/741, 210/742, 210/774, 210/808, 210/232, 210/236, 210/237, 210/238, 210/97 , 210/744, 422/63, 422/64, 422/69, 422/70, 422/136, 422/109, 422/255, 422/256, 422/261, 422/285, 422/288, 96/101, 96/102, 96/105, 96/106, 436/161, 436/178
• US Class Current: 210/634
• 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 2030/6013 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: G21F 5/015 : for storing radioactive sources, e.g. source carriers for irradiation units; Radioisotope containers

Abstract

To supply supercritical fluid to an automatic supercritical fluid extractor and collect extract from the extractor, sample holding cartridges are lifted one by one in series by an elevator plug into a pressure chamber. An inlet at the top of the cartridge engages a pressure vessel inlet for the extractant so that extractant flows into the cartridge and into the space between the cartridge and inner walls of the pressure chamber. The outlets from the cartridge and pressure vessel communicate with the collector and exhaust through passageways in the plug. The plug has cleaning ports for cleaning seals and the outlet from the cartridge flows past the seals. The collector lifts vials into place and can precool the collection solvent, and later as part of the collection procedure, heat and pressurize the collector.

Claims

1. Apparatus for supercritical fluid extraction, comprising:

means for performing supercritical fluid extraction;

collection means for collecting analyte;

said collection means being in contact with said means for performing supercritical fluid extraction;

said collection means including means for storing a plurality of collection vials and for moving at least one collecting vial from said plurality of collection vials into position to receive analyte and means for controlling the temperature of the at least one collection vial;

said means for controlling the temperature including an aluminum block in contact with the at least one collection vial;

said aluminum block being pivotable and slidable with respect to the at least one collection vial; and

said block incorporating at least one of CO₂ cooling and electric heating means.

2. Apparatus according to claim 1 wherein said collection means incorporates means for controlling the pressure in said at least one collection vial to a pressure greater than atmospheric pressure.

3. Apparatus for supercritical fluid extraction according to claim 1 further including:

means for maintaining a predetermined solvent level in the at least one collection vial;

said means for maintaining the predetermined solvent level including a liquid level control system; and

optical sensing means for sensing the liquid level in the at least one collection vial.

4. Apparatus for supercritical fluid extraction according to claim 3 in which the means for maintaining includes:

collection solvent replenishment means;

means for sensing when collection solvent in the collection vial falls below a predetermined solvent level because of a loss of collection solvent due to evaporation; and

means responsive to said means for sensing for adding collection solvent.

5. Apparatus for supercritical fluid extraction according to claim 4 further including collection vial piercing means having means for controlling temperature and positive internal pressure for the at least one collection vial.

6. Apparatus according to claim 1 in which the collection means includes multiple collection vials, each of said multiple collection vials being partly filled with collection solvent wherein a restrictor may bubble solvent with entrained extractant into the collection solvent.

7. Apparatus according to claim 6 in which each of said plurality of collection vials has a slitted septum on its upper, open end to allow passage of an end of the restrictor into the at least one collection vial.

8. Apparatus in accordance with claim 7 in which said means for storing a plurality of collection vials and for moving at least one collection vial includes means for lifting comprising a collection vial lifter that is separate from the cartridge elevator.

9. Apparatus according to claim 8 wherein said means for controlling temperature is operable such that the at least one collection vial is precooled to a selected temperature before the extraction begins and then heat is added to maintain the precooled temperature.

10. Apparatus according to claim 9 wherein means for controlling pressure comprises a sealed collection means used with a regulator to maintain pressure;

and the at least one collection vial is pressurized sufficiently to reduce mist and vapors of collected analyte and collection solvent.

11. A method of supercritical fluid extraction, comprising the steps of:

performing supercritical fluid extraction;

the step of performing supercritical fluid extraction including the substeps of collecting analyte in an at least one collection vial of a plurality of collection vials stored in a collection means;

said at least one vial being pressurized to a pressure greater than atmospheric pressure;

moving the at least one collection vial into position to receive analyte; and

controlling the temperature of the at least one collection vial.

12. A method according to claim 11 in which the substep of collecting analyte comprises, for each said at least one vial, flowing solvent and extract into the at least one collection vial from the top of the vial through a restrictor below the surface of collection solvent while the interior of the vial is pressurized sufficiently to reduce bubble size and decrease the vaporization rate of collection solvent and extract.

13. A method according to claim 11 in which there is a predetermined collection solvent level in each of the at least one collection vial and the collection solvent level is replenished when it falls below a predetermined level.

14. A method according to claim 13 wherein the level of collection solvent is sensed and adjusted automatically.

15. A method according to claim 11 wherein the step of moving the at least one collection vial comprises moving the at least one collection vial while it is supported on its bottom surface and the substep of collecting analyte comprises, for each said at least one vial, inserting a tube through a septum at the top of the at least one collection vial to a level below the surface of collection solvent and flowing analyte and analyte solvent through the tube.