High efficiency packed column supercritical fluid chromatography

• US 5,340,476 A
• Filed: 06/17/1993
• Issued: 08/23/1994
• Est. Priority Date: 01/10/1992
• Status: Expired due to Fees

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Hewlett-Packard Company (HP Inc.)
• Inventors: Berger, Terry A., Wilson, William H.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US08/078,802
• Time in Patent Office: 432 Days
• Field of Search: 210/635, 210/656, 210/659, 210/198.2, 96/101, 96/104, 96/106, 95/82, 95/86
• US Class Current: 210/198.2
• 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: G01N 30/461 with serial coupling of separation columns

Abstract

A method and device are disclosed for performing supercritical fluid chromatography in packed columns of at least about 0.5 mm inside diameter. The column provides at least 50,000, preferably at least 100,000, theoretical plates with pressure drop across the column of at least 25 bar. The outlet pressure is controlled by the back pressure regulator. The column may comprise a plurality of individual columns in series. Separation is performed at a rate of at least 25 plates/min, preferably at least 100 plates/min.

Claims

1. A device for the separation of material by supercritical fluid chromatography which comprises a packed chromatographic column structure of a plurality of individual columns connected in series and packed with packing between about 0.5 micron and 50 microns in diameter, a mass flow control pump for introducing fluid into said column structure, the diameter of said columns being between about 0.5 millimeters and about 20 centimeters, said column structure having an inlet and an outlet and a column length therebetween sufficient to provide for about 100,000 to about 500,000 theoretical plates and a rate of separation of at least 100 plates per second, said device having a back pressure regulator at said outlet to control the outlet pressure and to maintain the pressure drop between said inlet to between about 50 bar and 400 bar and to maintain said fluid at said outlet near its critical point, the total length of said column structure being at least equal to two times the average packing diameter times the number of theoretical plates.

2. The device of claim 1 wherein the diameters of said separate columns are between about 1 millimeter and 10 centimeters and the number of said individual columns is from about 3 to about 20.

3. The device of claim 1 wherein the packing diameter is between about 1.5 microns to about 10 microns.