Method and apparatus in gas chromatography for introducing a sample

• US 6,062,065 A
• Filed: 05/18/1998
• Issued: 05/16/2000
• Est. Priority Date: 06/23/1997
• Status: Expired due to Term

• Current Assignee: Osaka Pharmaceutical Association, Shimadzu Corporation
• Original Assignee: Osaka Pharmaceutical Company Limited, Shimadzu Corporation
• Inventors: Miyagawa, Haruhiko, Nakagawa, Katsuhiro, Sugimoto, Kiyoshi
• Primary Examiner(s): LARKIN, DANIEL SEAN
• Application Number:
  US09/080,818
• Time in Patent Office: 729 Days
• Field of Search: 73/23.35, 73/23.42, 96/101, 96/105
• US Class Current: 73/23.42
• CPC Class Codes: G01N 2030/122 cryogenic focusing
• CPC Class Codes: G01N 30/12 by evaporation

Abstract

A tubular insert with a small internal volume is disposed inside the vaporization chamber at the inlet of a capillary column of a gas chromatograph such that the sample with a solvent injected into the vaporization chamber is carried by a carrier gas through the insert into the column. The internal volume of the insert is such that the retention time of the carrier gas through the insert is less than 4 seconds. A heater is controlled to maintain the temperature inside the vaporization chamber within a specified range above the boiling point of the solvent as the sample is injected into the vaporization chamber, and this temperature is subsequently raised to a final temperature above the boiling points of the components to be analyzed. The carrier gas pressure is temporarily increased for better efficiency as the sample is injected.

Claims

1. A method of introducing into a capillary column of a gas chromatograph a sample, which contains target components to be analyzed and a solvent and is injected into a vaporization chamber at the inlet of said column, by causing a carrier gas to flow into said vaporization chamber and to carry said injected sample into said column, said method comprising the steps of:

temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected;

causing said carrier gas to introduce said sample through a tubular insert which is inserted into said vaporization chamber and has an internal volume so determined that the retention time of said carrier gas through said insert is less than 4 seconds; and

controlling the temperature inside said vaporization chamber to remain within a specified range above the boiling point of said solvent as said sample is injected into said vaporization chamber and thereafter raising the temperature inside said vaporization chamber.

2. The method of claim 1 wherein temperature inside said vaporization chamber is increased to a final temperature above the boiling points of said target components.

3. The method of claim 2 wherein said specified range is such that the temperature inside said vaporization chamber is higher than the boiling points of said target components.

4. The method of claim 3 wherein said specified range is 20°

C. to 30°

C.

5. The method of claim 3 further comprising the step of temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected.

6. The method of claim 2 further comprising the step of temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected.

7. The method of claim 1 wherein said specified range is such that the temperature inside said vaporization chamber is higher than the boiling points of said solvent.

8. The method of claim 7 wherein said specified range is 20°

C. to 30°

C.

9. The method of claim 7 further comprising the step of temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected.

10. An apparatus for supplying a carrier gas into a vaporization chamber at an inlet of a capillary column of a gas chromatograph for introducing into said column a sample which contains target components to be analyzed and a solvent and is injected into said vaporization chamber, said apparatus comprising:

a tubular insert disposed inside said vaporization chamber for causing said carrier gas and said sample to pass therethrough into said column, said insert having an internal volume such that the retention time of said carrier gas through said insert is less than 4 seconds;

a pressure control means for controlling the pressure of said carrier gas entering said vaporization chamber, said pressure control means temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected; and

a heater which is controlled to maintain the temperature inside said vaporization chamber within a specified range above the boiling point of said solvent as said sample is injected into said vaporization chamber and to thereafter raise the temperature inside said vaporization chamber.

11. The apparatus of claim 10 wherein said heater is controlled to raise the temperature inside said vaporization chamber to a final temperature above the boiling points of components in said sample to be analyzed.

12. The apparatus of claim 11 wherein said specified range is such that the temperature inside said vaporization chamber is higher than the boiling points of said target components.

13. The apparatus of claim 12 wherein said specified range is 20°

C. to 30°

C.

14. The apparatus of claim 12 further comprising a pressure control means for controlling the pressure of said carrier gas entering said vaporization chamber, said pressure control means temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected.

15. The apparatus of claim 11 further comprising a pressure control means for controlling the pressure of said carrier gas entering said vaporization chamber, said pressure control means temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected.

16. The apparatus of claim 10 wherein said specified range is such that the temperature inside said vaporization chamber is higher than the boiling points of said solvent.

17. The apparatus of claim 16 wherein said specified range is 20°

C. to 30°

C.

18. The apparatus of claim 16 further comprising a pressure control means for controlling the pressure of said carrier gas entering said vaporization chamber, said pressure control means temporarily increasing the pressure of said carrier gas flowing into said vaporization chamber as said sample is injected.