Apparatus and method for supercritical fluid extraction

• US 5,653,885 A
• Filed: 12/27/1995
• Issued: 08/05/1997
• 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: Jameson, Daniel Gene, Allington, Robert William, Macomber, Robert Joseph
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US08/579,644
• Time in Patent Office: 587 Days
• Field of Search: 95/14, 95/82, 95/87, 96/105, 210/85, 210/149, 210/175, 210/180, 210/198.2, 210/511, 210/541, 210/634, 210/635, 210/656, 210/659, 210/742, 210/774, 210/808, 422/69, 422/255, 422/256, 422/261, 422/285, 422/288, 422/289
• 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 2201/0209 Duration of piston stroke
• 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 53/08 Cooling; Heating; Preventing freezing
• CPC Class Codes: F04B 53/143 Sealing provided on the piston
• 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 avoid deposits on the restrictor that channels extractant into a collector, a heated capillary tube pressure release restrictor, has a thermally insulated outlet end in a collecting trap substantially colder than the capillary tube. The restrictor is heated between the insulation and the capillary tube by Joulean heating. The solvent in the trap is at a pressure of 5 to 200 psi above atmospheric pressure. The thermal resistance of the insulation is selected to reduce the heat added to the extractant to a minimum and yet cause the temperature of the extractant to be in a range within which it is sufficiently hot so it does not freeze when added to the collection solvent but not so hot as to reduce partitioning of the extract and extractant before the extractant leaves the collection solvent. It has a thermal conductivity no greater than 60 BTU'"'"'s per hour, per square foot, per inch for a one degree Fahrenheit difference.

Claims

1. A supercritical fluid extraction system, comprising:

means for performing supercritical fluid extraction;

a capillary tube;

said means for performing supercritical fluid extraction including a temperature control system;

said temperature control system includes a directly heated, at least partly metal, capillary tube pressure release restrictor on said capillary tube; and

a temperature sensing means for sensing the temperature in a vicinity of the capillary tube sufficiently close to measure the temperature of the capillary tube and fluid therewithin.

2. A supercritical fluid extraction system, comprising:

a capillary tube;

means for performing supercritical fluid extraction;

said means for performing supercritical fluid extraction including a temperature control system;

said temperature control system includes a directly heated, at least partly metal, capillary tube pressure release restrictor on said capillary tube; and

a temperature sensing means for sensing the temperature in a vicinity that includes the capillary tube;

said metal part of the at least partly metal capillary tube pressure release restrictor possesses a temperature coefficient of resistance, the temperature sensing means being operative for sensing said temperature coefficient.

3. A supercritical fluid extraction system, comprising:

a capillary tube;

means for performing supercritical fluid extraction;

said means for performing supercritical fluid extraction including a temperature control system;

said temperature control system includes a directly heated, at least partly metal, capillary tube pressure release restrictor on said capillary tube; and

a temperature sensing means for sensing the temperature in a vicinity that includes the capillary tube;

said metal part of the at least partly metal capillary tube pressure release restrictor possesses a temperature coefficient of resistance, the temperature sensing means being operative for sensing said temperature coefficient;

a return path for current;

said return path being in the form of an outer metal tube surrounding the capillary tube pressure release restrictor and sealingly connected to provide an electrical connection to the outlet end of the at least partly metal capillary tube pressure release restrictor;

said outer metal tube extending outside a collecting trap; and

the outer metal tube being thermally insulated from the at least partly metal capillary tube pressure release restrictor, except at a location of the electrical connection.

4. The apparatus of claim 3 wherein the collecting trap is a solvent trap.

5. A method of supercritical fluid extracting comprising the steps of:

extracting extract from a sample with an extractant;

collecting the extract in a collector having a pressure control on it in a collecting trap, wherein the pressure of collecting is controllable; and

controlling the flow of heat between said extractant and the collecting trap to prevent freezing of extractant before partition of extract and extractant from collection solvent and bubbling away of extract with extractant.

6. A method in accordance with claim 5 wherein the step of controlling the flow of heat includes the step of applying heat to a capillary tube from an external energy source.

7. A method of supercritical fluid extracting comprising the steps of:

extracting extract from a sample with an extractant;

collecting the extract in a collector having a pressure control on it, wherein the pressure of collecting is controllable; and

controlling the flow of heat between said extractant and a collecting trap to prevent freezing of extractant before partition and bubbling away of extract with extractant;

the step of controlling the flow of heat includes the steps of applying heat to a capillary tube from an external energy source and controlling the flow of heat with a feedback means for controlling the application of heat to the capillary tube.

8. A method in accordance with claim 7 wherein the step of controlling the flow of heat includes the steps of:

applying heat to a pressure release restrictor;

said pressure release restrictor comprising a thermally insulated, metal capillary tube restrictor;

said thermally insulated metal capillary tube restrictor being between an insulation layer and a surface of the capillary tube, wherein a surface of the insulation layer on the capillary tube restrictor forms a substantially coaxial cylindrical surface about the capillary tube restrictor.