Variable flow capillary gas chromatography method

• US 4,872,334 A
• Filed: 12/20/1988
• Issued: 10/10/1989
• Est. Priority Date: 05/09/1986
• Status: Expired due to Fees

• Current Assignee: The Dow Chemical Company (Dow, Inc.)
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Watanabe, Chuichi
• Primary Examiner(s): Williams, Hezron E.
• Application Number:
  US07/287,692
• Time in Patent Office: 294 Days
• Field of Search: 73/23.1, 422/89, 436/161
• US Class Current: 73/23.24
• CPC Class Codes: G01N 2030/385 by switching valves
• CPC Class Codes: G01N 30/16 Injection G01N30/24 takes precedence
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence

Abstract

A method for temperature programmed capillary column gas chromatography characterized in that carrier gas is flowed in an amount greater than that under normal separation conditions for a term starting from before injection of a sample or immediately after the injection and ending at any time point from immediately after a solvent in the sample commences to enter into a column to the solvent finishing passing through the column. The invention is also apparatus for the above method characterized in that the apparatus has two flow paths for carrier gas which, for example, join to one flow path before a sample injection device, and one of the flow paths has a valve which can rapidly stop or decrease the flow of the carrier gas in that flow path.

Claims

1. A method for temperature programmed capillary column gas chromatography, comprising the steps of:

flowing a carrier gas through a gas chromatography injection port with essentially all of the carrier gas subsequently flowing into a gas chromatography capillary column at a first flow rate and a first pressure;

heating the column to a first temperature;

introducing a sample through the injection port, the sample comprising a solvent and a component of interest;

reducing the flow rate of the carrier gas to a second flow rate at a time longer than immediately after beginning the step of introducing the sample, the second flow rate being a normal flow rate for the column; and

increasing the temperature of the column so that the component of interest emerges from the column.

2. The method of claim 1 wherein the first flow rate is more than about 1.5 times higher than the second flow rate.

3. The method of claim 1 wherein the first pressure is less than about 10 kilograms per square centimeter.

4. The method of claim 1 wherein the first temperature of the column is within 10 degrees centrigrade of the atmospheric pressure boiling point of the solvent of the sample.

5. The method of claim 1 further comprising the step of heating the injection port and the carrier gas therein to a temperature effective to vaporize a sample injected thereinto.

6. The method of claim 1 wherein the step of introducing a sample through the injection port consists essentially of introducing the sample through the injection port directly into the inlet of the column.

7. The method of claim 1 wherein the flow rate of the carrier gas is reduced at a time longer than 3 seconds after beginning the step of introducing the sample and shorter than the time after essentially all of the solvent has emerged from the column.