Method for admitting and receiving samples in a gas chromatographic column

• US 5,846,293 A
• Filed: 05/06/1997
• Issued: 12/08/1998
• Est. Priority Date: 05/06/1996
• Status: Expired due to Term

• Current Assignee: University of Dayton
• Original Assignee: University of Dayton
• Inventors: Striebich, Richard C., Rubey, Wayne A.
• Primary Examiner(s): SPITZER, ROBERT H
• Application Number:
  US08/851,888
• Time in Patent Office: 581 Days
• Field of Search: 73/23.26, 73/23.27, 73/23.35, 95/82, 95/87, 95/89, 96/101-103
• US Class Current: 95/87
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/3015 temperature gradients along column
• CPC Class Codes: G01N 2030/3046 temperature control of column inlet
• CPC Class Codes: G01N 30/06 Preparation
• CPC Class Codes: G01N 30/30 of temperature
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence

Abstract

A method of admitting and receiving a sample into a gas chromatographic column is provided in which a step increase in pressure is performed in combination with the application of a negative axial thermal gradient to provide pre-separation of solutes in the sample within the inlet region of the column. The method includes the steps of introducing a sample into the column at a first pressure and temperature, rapidly raising the temperature to invoke a negative axial thermal gradient, and then substantially instantaneously increasing the pressure. The method causes the solutes in the sample to be partially separated into narrow zones within the inlet region, resulting in eventually achieving maximum resolution.

Claims

1. A method for admitting and receiving a sample into a gas chromatographic column

having an inlet region and an outlet region, wherein said sample travels in a direction from said inlet region to said outlet region, said method comprising:

admitting said sample into said inlet region of said column at a first temperature, said inlet region containing a carrier gas which is at a first pressure;

rapidly heating said inlet region of said column to a second temperature greater than said first temperature such that a negative axial thermal gradient is imposed along the length of said column;

substantially instantaneously increasing the gas pressure at said inlet region to a second pressure greater than said first pressure such that the velocity of said carrier gas is increased and solutes constituting said sample are pre-separated into narrow zones along the inlet region of said column.

2. The method of claim 1 in which said column comprises an open tubular column.

3. The method of claim 1 in which said first pressure is from about 1 to about 3 abs. atm and said second pressure is from about 6 to about 9 abs. atm.

4. The method of claim 1 in which said first temperature is about 20°

C. and said second temperature is from about 380°

C. to about 480°

C.

5. The method of claim 1 in which the velocity of said carrier gas is increased to about 5 m/s.

6. The method of claim 1 in which said inlet region is from about 20 cm to 2 meters in length.

7. The method of claim 1 further including the step of backflushing said inlet region of said column after said solutes constituting said sample are pre-separated by increasing the flow of gas in said inlet region in a backward direction such that non-volatile materials from said sample deposited in the inlet region are removed from said inlet region.

8. The method of claim 7 wherein the flow of gas in increased by increasing gas pressure in said inlet region.