Converting a pump for use in supercritical fluid chromatography

• US 6,561,767 B2
• Filed: 08/01/2001
• Issued: 05/13/2003
• Est. Priority Date: 08/01/2001
• Status: Expired due to Term

• Current Assignee: Thar Instruments, Inc. (Waters Corporation)
• Original Assignee: Berger Instruments, Inc. (Mettler-Toledo International Inc.)
• Inventors: Fogelman, Kimber D., Berger, Terry A., Bente, Paul F. III, Nickerson, Mark, Staats, L. Thompson III
• Primary Examiner(s): Freay, Charles G.
• Assistant Examiner(s): Solak, Timothy P.
• Application Number:
  US09/918,436
• Publication Number:
  US 20030026704A1
• Time in Patent Office: 650 Days
• Field of Search: 417/53, 417/313, 417/279, 73/190.2
• US Class Current: 417/53
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent
• CPC Class Codes: G01N 2030/326 pumps
• CPC Class Codes: G01N 30/02 Column chromatography
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence
• CPC Class Codes: G01N 30/36 in high pressure liquid systems

Abstract

A method for converting a pump for use in a flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid wherein the pump delivers a compressible fluid against a back-pressure regulator which in turn delivers a controllable flow rate downstream of the regulator without performing variable compressibility compensation adjustments on the pump. By using a pressurized source of compressible fluid combined with isocratic conditions, the delivery pressure from the pump is controlled at a rate higher than the downstream gradient with the back-pressure regulator, and an inexpensive pump may be used in place of specialized, expensive pumps and compressibility compensation systems for use in stems operating at or near supercritical fluid levels of compressible fluids. Significant capital and operating laboratory costs are saved through a simpler and cheaper system for accurately delivering compressible fluids into mobile phase flow streams.

Claims

1. A method for converting a pump for use in a combined flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid;

and a relatively incompressible liquid, comprising;

controlling pressure of a first flow stream containing a highly compressed gas, compressible liquid, or supercritical fluid, by maintaining an elevated pressure rate after said outlet of said pump but prior to joining a second flow stream of a relatively incompressible liquid;

pumping of said first flow stream consisting of a pure fluid resulting in delivery of a controllable flow rate of said first flow stream at a constant compressibility compensation without the need for dynamically compensating said pump for compressibility changes in said first flow stream.

2. The method of claim 1, wherein:

said maintenance of an elevated pressure rate after said outlet of said pump being accomplished by delivering said fluid first flow stream from said pump against a back pressure regulator valve installed in said first flow stream downstream of said pump and upstream to the joining of said first flow stream with said second fluid flow stream containing a relatively incompressible liquid.

3. The method of claim 2, further comprising the step of:

determining the mass flowrate of said first flow stream after said back-pressure regulator by calibration.

4. The method of claim 1, further comprising:

providing a fixed elevated back pressure against which said first fluid flow stream is pumped to provide a reproducible flow source to a supercritical fluid system.

5. The method of claim 1, wherein:

said pump rate is controllable with variable flow rates when pumping against said elevated pressure in said first fluid flow stream.

6. The method of claim 1, wherein:

said method is operated under approximate isocratic conditions.

7. A method for converting a pump for use in a combined flow stream containing a mixture of highly compressed gas, compressible liquid or supercritical fluid;

and a relatively incompressible liquid, comprising;

controlling inlet pressure to a pump of a first flow stream of a highly compressed gas, compressible liquid or supercritical fluid;

controlling temperature of said first flow stream;

pumping of said first flow stream, consisting of a pure fluid, against an elevated pressure rate resulting in delivery of a controllable flow rate of said first flow stream at a constant compressibility compensation without the need for dynamically compensating said pump for compressibility changes in said first flow stream.

8. The method of claim 7, wherein:

said pump is operated at variable flow rates when pumping against said elevated pressure in said first fluid flow stream.

9. The method of claim 7, further comprising:

providing a fixed elevated back pressure against which said first fluid flow stream is pumped to provide a reproducible flow source to a supercritical fluid system.

10. The method of claim 7, wherein:

said elevated pressure after said outlet of said pump is accomplished by delivering said first fluid flow stream from said pump against a back pressure regulator valve installed in said flow stream downstream of said pump and upstream from the joining of said first flow stream with said second fluid flow stream.

11. The method of claim 7, wherein:

said method is operated under approximate isocratic conditions.

12. The method of claim 7, further comprising the step of:

determining the flowrate of said first flow stream after said elevated pressure by calibration.