Apparatus and method for supercritical fluid extraction or supercritical fluid chromatography

• US 6,149,814 A
• Filed: 05/07/1998
• Issued: 11/21/2000
• 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: Tehrani, Yoossef, Allington, Robert W., Jameson, Daniel Gene, Walters, Henry LeRoy
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US09/074,254
• Time in Patent Office: 929 Days
• Field of Search: 210/634, 210/635, 210/656, 210/659, 210/198.2, 210/511, 251/129.15, 251/331, 251/335.2, 422/256, 422/261, 422/285
• 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 2030/6008 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

A variable-orifice fluid restrictor for use with a supercritical extractor or chromatograph includes an inlet line for fluid at a pressure above its critical pressure, an extended tubular probe having an inner and an outer surface and a proximal and a distal end. The proximal end of the probe is disposed toward the inlet line. The distal end of the probe includes an adjustable orifice means adapted for metering the fluid and having first and second orifice members and an adjusting stem having first and second ends. The adjustable orifice means is adjacent to the outer surface of the probe and the orifice means is adjustable with the adjusting stem. The end of the adjusting stem is located at the distal end of the probe and is adapted for moving the first orifice member with respect to the second orifice member to control the adjustable orifice for varying the restriction of fluid passing through the adjustable orifice.

Claims

1. A method of supercritical fluid extracting, comprising the steps of:

extracting extract from a sample with an extractant;

adjusting the pressure in the extractor by adjusting a variable restrictor located at least partly within a collector; and

expanding the extract and extractant in the collector while avoiding plugging the variable orifice restrictor, wherein the extract directly is collected therein.

2. A method according to claim 1 further including the step of heating at least a portion of the restrictor.

3. A method in accordance with claim 2 wherein the step of heating the restrictor includes the step of applying heat to the restrictor from an external energy source.

4. A method in accordance with claim 2 wherein the step of heating the restrictor includes the step of controlling the flow of heat with a feedback system that controls the application of heat to the restrictor.

5. A method in accordance with claim 1 wherein the step of adjusting the pressure in the extractor comprises the step of adjusting the pressure in the extractor by adjusting a variable restrictor located at least partly within a collector wherein an adjustment means that extends outside of the collector is used to adjust the variable restrictor.