Apparatus and method for supercritical fluid extraction

• US 6,241,890 B1
• Filed: 06/14/1999
• Issued: 06/05/2001
• 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: Clay, Dale Lee, Winter, Robin Randall, Liescheski, Philip Bernard III, Allington, Robert W., Jameson, Daniel Gene
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US09/332,710
• Time in Patent Office: 722 Days
• Field of Search: 210/175, 210/198.2, 210/511, 210/634, 210/656, 210/774, 422/63, 422/64, 422/70, 422/81, 738/630.1, 738/642.1, 738/642.3, 738/642.5, 738/648--86, 141/130, 141/329, 141/330
• 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 collect analyte from a supercritical fluid extractor, the collector lifts vials into place by a biasing means that guides the file up to the restrictor where it is sealed. The vial can be moved back down from the collecting mechanism even if frost forms on the vial while the restrictor means remains stationary. This vial is held in place by a guide that contains the seal for sealing the vial when it is raised in place.

Claims

1. Apparatus for collecting extract in a supercritical extraction system comprising:

means for moving sealed collection vials to and from a collection position;

penetrating means for penetrating a seal of said collection vials;

said penetrating means being positioned to penetrate the seal of a plurality of collection vials one at a time in series;

said penetrating means incorporating within it a restrictor capillary tube, wherein supercritical fluids with extract may enter the collection vial for collection.

2. Apparatus in accordance with claim 1 further including:

a plurality of sealed collection vials;

said restrictor capillary tube being adapted to penetrate a significant distance into the sealed collection vials;

said sealed collection vials including a liquid;

said means for penetrating being adapted to cause a port of the restrictor capillary tube to be at least partly immersed in the liquid, whereby a solvent and the extract are emitted into the liquid whereby a gas escapes as bubbles but the extract remains.

3. Apparatus in accordance with claim 2 in which the liquid is maintained at a temperature sufficient to condense the extract.

4. Apparatus in accordance with claim 2 in which the restrictor capillary tube is maintained at a temperature sufficient to prevent the condensing of excess extract in the restriction capillary tube.

5. A method of automatic fraction collecting of extract in a supercritical extraction system comprising the steps of:

moving a series of sealed collection vials to and from a collection position;

penetrating a corresponding seal of at least some of said series of collection vials one at a time with a restrictor, wherein supercritical fluids with extract may enter at least one of the collection vials for collection.

6. A method in accordance with claim 5 in which the step of penetrating the series of sealed collection vials includes the step of penetrating at least one seal a significant distance into the sealed collection vials with a restriction capillary tube wherein said at least one sealed collection vial is penetrated by the restriction capillary tube having a port of the restriction capillary tube sufficiently immersed in a liquid to permit a solvent and the extract to be emitted into the liquid whereby a gas escapes as bubbles but the extract remains.

7. A method in accordance with claim 6 wherein the restriction capillary tube is maintained at a temperature to prevent the condensing of excess extract in the restriction capillary tube.

8. A method in accordance with claim 5 wherein the liquid is maintained at a temperature sufficient to condense the extract.