Apparatus and method for supercritical fluid extraction

• US 6,071,408 A
• Filed: 05/18/1998
• Issued: 06/06/2000
• 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: Davison, Dale A., Winter, Robin R., Jameson, Daniel Gene, Allington, Robert William, Tehrani, Yoossef, Clay, Dale
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US09/080,826
• Time in Patent Office: 750 Days
• Field of Search: 210/87, 210/90, 210/91, 210/97, 210/101, 210/137, 210/143, 210/198.2, 210/416.1, 210/511, 210/634, 210/656, 210/739, 210/741, 210/94, 417/2-5, 417/18, 417/43, 417/44.2, 417/53, 417/63, 417/286, 417/300, 422/69, 436/178, 95/19, 95/23, 95/82, 96/103, 96/105
• 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 provide performance particularly in handling supercritical extraction systems, a specially designed pump includes a cam-driven, single-plunger with a cam having a profile that enables the pumping system to avoid destructive reverse torque on the cam, gear train and drive motor after the cam passes top dead center. The fluid volume leaving the pump is determined by measuring only pressure or other parameters related to flow and movement of the plunger. Measurement of the fluid volume leaving the pump is useful for recording or indicating the flow rate while the pump is operating.

Claims

1. A supercritical fluid extraction apparatus comprising:

means for supercritical fluid extraction;

pump means for pumping supercritical fluid into said means for supercritical fluid extraction;

said pump means including a piston and a measuring means for measuring the pumped supercritical fluid by determining the pressure exerted by the fluid being pumped by said pump means and the movement of the piston and calculating fluid rate flow from piston movement and pressure exerted by the fluid being pumped.

2. Apparatus for supercritical fluid extraction in accordance with claim 1 in which said pump means includes a strain gauge means adapted to be positioned in contact with said supercritical fluid.

3. Apparatus in accordance with claim 1 in which said pump means includes means for measuring piston movement and said means for measuring piston movement includes an optical means mounted for movement in relation to the movement to said piston.

4. Apparatus in accordance with claim 1 in which:

said pump means includes a pressure sensor;

said means for measuring piston movement includes a pump means mounted for movement in relation to the movement of said piston;

said pressure sensing means and means for measuring movement, each including different means for generating electrical signals connected to a calculating means for determining the rate of flow of supercritical fluid.

5. Apparatus in accordance with claim 4 in which said pressure sensor is mounted within a pumphead.

6. Apparatus in accordance with claim 4 in which said measuring means includes means for measuring pressure;

said means for measuring pressure being mounted along a flow path of said supercritical fluid between said pumphead and said means for supercritical extraction.

7. Apparatus in accordance with claim 6 wherein said pump means includes

drive means for driving said piston;

means for determining volumetric flow rate;

feedback control means electrically connecting said drive means to said means for determining volumetric flow rate wherein said volumetric flow rate of said supercritical fluid is controlled by said feedback means.

8. Apparatus in accordance with claim 1 in which said pump means for pumping supercritical fluid includes:

first and second sources of respective first and second supercritical fluids supercritical fluid;

first and second pumps for pumping corresponding ones of said first and second fluids;

each of said first and second pumps having means for controlling the rate of pumping of said first and second pumps respectively;

feedback means being connected to said first and second means for controlling said first and second pumps;

feedback means including a controller wherein the rate of pumping of said first and second pumps is changed with respect to each other as the rate of flow of fluid changes so as to maintain a constant flow rate as the composition of said first and second fluids vary.

9. Apparatus in accordance with claim 8 in which:

said pump means includes a first valve means and a second valve means;

said feedback means includes a program means for controlling said first valve means and said second valve means;

said first valve means communicates with said first source of supercritical fluid;

said second valve means includes a means for communicating with said second source of supercritical fluid;

said first and second valve means each having an outlet means communicating with a mixer means;

said mixer means communicating with an outlet of said pump means, wherein said feedback controls gradients supplied to said outlet.

10. A method for supercritical fluid extraction comprising the steps of:

pumping supercritical fluid into means for supercritical fluid analysis;

measuring the pumped supercritical fluid by determining the pressure exerted by the fluid being pumped by a piston and movement of the piston and calculating fluid rate flow from the piston movement and the pressure exerted by the fluid being pumped.

11. A method for supercritical fluid extraction in accordance with claim 10 further comprising the step of measuring pressure with a strain gauge means wherein the strain gauge means is positioned in contact with said supercritical fluid.

12. A method in accordance with claim 11 further including the step of measuring piston movement by moving optical means mounted in relation to the movement of the piston.

13. A method in accordance with claim 11 comprising the steps of:

measuring piston movement by means which are moveable in relation to the movement of said piston;

determining rate of flow of supercritical fluid by generating electrical signals connected to a calculating means.

14. A method in accordance with claim 13 further including the steps of:

driving said piston;

electrically connecting drive means to means for determining volumetric flow rate by feedback means.

15. A method in accordance with claim 13 wherein the step of pumping includes the steps of:

controlling the rate of pumping of first and second pumps for pumping respective first and second supercritical fluids;

controlling said first and second pumps by connecting feedback means to said first and second pumps;

changing the rate of pumping of said first and second pumps with respect to each other as said rate of flow of fluid changes to maintain a constant flow rate as the composition of said first and second fluids varies.

16. A method in accordance with claim 13 wherein the step of pumping further includes using a first valve means and second valve means and comprises the steps of:

controlling said first valve means and said second valve means by feedback means including program means;

allowing said first valve means to communicate with a first source of said first supercritical fluid;

allowing said second valve means to communicate with a second source of said second supercritical fluid;

allowing said first and second valve means to communicate with a mixer means via respective outlet means;

allowing said mixer means to communicate with an outlet of said pump means, and the feedback controlling gradients supplied to said outlet.