Low noise back pressure regulator for supercritical fluid chromatography

• US 8,419,936 B2
• Filed: 03/23/2010
• Issued: 04/16/2013
• Est. Priority Date: 03/23/2010
• Status: Active Grant

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Agilent Technologies, Inc.
• Inventors: Berger, Terry A., Colgate, Samuel, Casale, Michael
• Primary Examiner(s): Therkorn, Ernest G
• Application Number:
  US12/730,223
• Publication Number:
  US 20110233299A1
• Time in Patent Office: 1,120 Days
• Field of Search: 210/635, 210/656, 210/659, 210/137, 210/143, 210/198.2, 95/82, 961/01, 422/70, 436/161
• US Class Current: 210/198.2
• CPC Class Codes: B01D 15/10 characterised by constructional or operational features
• CPC Class Codes: B01D 15/163 Pressure or speed conditioning
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent
• 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: Y10T 137/7904 Reciprocating valves

Abstract

A drive mechanism for back pressure regulator used in liquid chromatography, supercritical fluid chromatography, or supercritical fluid extraction allows very fine automated control over a very wide range of pressures by combining a linear actuator compressing a spring, pushing a pin. The nozzle assembly of the regulator comprises a flow through chamber containing a diaphragm and a seat, in which the pin pushes the diaphragm against the seat, together with an upstream pressure sensor and electronic feedback control to the motor of the actuator. The BPR of the embodiments exhibits high pressure stability and extremely low pressure noise, even at moderate to high pressures. The exemplary BPR can be use at either constant pressure or to generate pressure programs where the pressure is varied versus time. Further, the nozzle assembly has a field-replaceable head, requiring no mechanical adjustment on replacement.

Claims

1. A system for chromatography, comprising:

a first pump for pumping a first relatively incompressible fluid flowstream;

a second pump for pumping a second relatively compressible solvent fluid flowstream;

mixing device that combines said first and second flowstreams;

an injection device that can introduce samples or solutions into any of said flowstreams;

a chromatography separation column, downstream of said mixing device and that can receive said combined flowstream;

a detector, for detecting a concentration of a constituent in one of said flowstreams;

a computer controller, directing certain operations of the system; and

a back pressure regulator, located downstream of said column, wherein said back pressure regulator includes a device comprising a nozzle insert with an outlet flow channel that can receive an outlet flow and an inlet flow channel that can receive an inlet flow, and further includes a seat, connected near an end of said insert, inset from said nozzle insert such that said seat can be in fluidic communication with said outlet flow channel.

2. The system of claim 1, wherein said outlet flow channel is located near to center axis of said nozzle insert, and

said inlet flow channel is located at a position offset from said outlet flow channel.

3. The system of claim 1, wherein the nozzle insert further comprises:

a heating element arranged near to said outlet channel such that heat from said heating element can be in thermal communication with said outlet flow channel.

4. The system of claim 1, further comprising:

a nozzle body at least partially receiving said nozzle insert and said seat; and

a diaphragm having a first surface positioned adjacent to said seat wherein said nozzle body constrains a circumferential edge of said diaphragm.

5. The system of claim 4, further comprising:

a shim element, positioned adjacent to a second surface of said diaphragm that is opposite to said first surface of said diaphragm that is adjacent to said seat.

6. The system of claim 4, further comprising:

a linear actuator that can apply a force to the second surface of said diaphragm directly or through said shim, wherein said force can cause the first surface of the diaphragm to seal against an orifice of said outlet flow channel.