Gas chromatograph-mass spectrometer

Patent metadata

Field	Value
Publication number	US-10126276-B2
Application number	US-201315021959-A
Country	US
Kind code	B2
Filing date	Sep 25, 2013
Priority date	Sep 25, 2013
Publication date	Nov 13, 2018
Grant date	Nov 13, 2018

Abstract

A column protection gas supply channel (4) is connected to a channel (17) for carrier gas present between a sample vaporization chamber (12) and an MS section (2). During a standby, a column (11) may be protected on the downstream side of a merging section (16) of the column protection gas supply channel (4) and the channel (17) for carrier gas by supplying column protection gas through the column protection gas supply channel (4). At this time, there is remaining carrier gas in the channel (17) for carrier gas on the upstream side of the merging section (16). Accordingly, when carrier gas is then supplied at a time of start of an analysis, a certain amount of carrier gas is already present inside the channel (17). Therefore, the time required to completely replace the column protection gas in the channel (17) by the carrier gas is reduced, and the standby time until the start of the analysis may be reduced.

First claim

The invention claimed is:

1. A gas chromatograph-mass spectrometer comprising:
a sample vaporization chamber for vaporizing a sample;
a column to which carrier gas containing a sample component is introduced from the sample vaporization chamber;
a mass spectrometry section for performing mass spectrometry by ionizing, inside a vacuum chamber, a sample component separated by the column;
a channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section, the channel comprising the column;
a column protection gas supply channel connected to the channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section, the column protection gas supply channel being for supplying column protection gas for protecting the column and the channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section; and
a gas flow rate adjustment section implemented by a computer and configured to adjust a flow rate of gas in such a way that, during an analysis, the carrier gas containing a sample component flows into the mass spectrometry section and the column protection gas does not flow into the mass spectrometry section, and during a standby, the column protection gas flows into the mass spectrometry section and the carrier gas does not flow into the mass spectrometry section,
wherein the gas flow rate adjustment section adjusts the flow rate of gas in such a way that, during the standby, the pressure, at a merging section of the column protection gas supply channel to the column, of the column protection gas acting on the side of the sample vaporization chamber and the supply pressure of the carrier gas from the sample vaporization chamber become equal,
wherein during the standby the column is supplied with the column protection gas on a side of the column downstream from the merging section, and is supplied with the carrier gas on a side of the column upstream from the merging section,
wherein the column protection gas is a gas different from the carrier gas, and
wherein the gas flow rate adjustment section adjusts the flow rate of gas in such a way that the carrier gas is present in the column on the upstream side of the merging section while the column protection gas is supplied, and a certain amount of the carrier gas is already present inside the channel for carrier gas when the carrier gas is supplied at the time of a start of a next analysis.

2. The gas chromatograph-mass spectrometer according to claim 1 , wherein the column protection gas supply channel is connected to the channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section on a downstream side of the column.

3. The gas chromatograph-mass spectrometer according to claim 1 , further comprising a notification processing section implemented by a computer and configured to issue, in a case where the flow rate of the carrier gas has reached or exceeded a predetermined value during the standby, a notification to an effect.

4. The gas chromatograph-mass spectrometer according to claim 1 , further comprising:
a column oven for heating the column; and
a column temperature adjustment section implemented by a computer and configured to heat the column by the column oven during the analysis, and to reduce a temperature of the column during the standby compared to the temperature at a time of the analysis.

5. The gas chromatograph-mass spectrometer according to claim 1 , wherein the gas flow rate adjustment section is configured to cause an analysis to automatically start, by causing the carrier gas containing a sample component to flow into the mass spectrometry section, and after completion of the analysis, to cause a shift to a standby state to automatically take place, by causing the column protection gas to flow into the mass spectrometry section.

6. The gas chromatograph-mass spectrometer according to claim 1 , wherein the column protection gas is nitrogen gas (N 2 ), and the carrier gas is helium gas (He).

7. The gas chromatograph-mass spectrometer according to claim 1 , wherein a downstream end of the column is connected to the mass spectrometry section.

8. A method for reducing the time from a standby time to a start time of an analysis for a gas chromatograph mass spectrometer, the gas chromatograph mass spectrometer comprising: a sample vaporization chamber for vaporizing a sample; a column to which carrier gas containing a sample component is introduced from the sample vaporization chamber; a mass spectrometry section for performing mass spectrometry by ionizing, inside a vacuum chamber, a sample component separated by the column; a channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section, the channel comprising the column; and a column protection gas supply channel connected to the channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section, the column protection gas supply channel being for supplying column protection gas for protecting the column and the channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section; the method comprising:
adjusting a flow rate of gas in such a way that during an analysis, the carrier gas containing a sample component flows into the mass spectrometry section and the column protection gas does not flow into the mass spectrometry section, and during a standby, the column protection gas flows into the mass spectrometry section and the carrier gas does not flow into the mass spectrometry section,
wherein the flow rate of gas is adjusted in such a way that, during the standby, the pressure, at a merging section of the column protection gas supply channel to the column, of the column protection gas acting on the side of the sample vaporization chamber and the supply pressure of the carrier gas from the sample vaporization chamber become equal,
wherein during the standby the column is supplied with the column protection gas on a side of the column downstream from the merging section, and is supplied with the carrier gas on a side of the column upstream from the merging section,
wherein the column protection gas is a gas different from the carrier gas, and
wherein the flow rate of gas is adjusted in such a way that the carrier gas is present in the column on the upstream side of the merging section while the column protection gas is supplied, and a certain amount of the carrier gas is already present inside the channel for carrier gas when the carrier gas is supplied at the time of a start of a next analysis.

9. The method according to claim 8 , wherein the column protection gas supply channel of the gas chromatograph mass spectrometer is connected to the channel for carrier gas present between the sample vaporization chamber and the mass spectrometry section on a downstream side of the column.

10. The method according to claim 8 ,
wherein the method further comprises:
issuing, in a case where the flow rate of the carrier gas has reached or exceeded a predetermined value during the standby, a notification to an effect.

11. The method according to claim 8 , wherein the gas chromatograph mass spectrometer further comprises:
a column oven for heating the column; and
a column temperature adjustment section;
wherein the method further comprises:
using the column oven to heat the column during analysis; and
using the column oven to reduce a temperature of the column during the standby compared to the temperature at a time of the analysis.

12. The method according to claim 8 , wherein the meth

Assignees

• Shimadzu Corp

Inventors

• Takakura Masato
• Kawana Syuichi

Classifications

• G01N2030/324

  speed, flow rate · CPC title

• G01N2030/3084

  ovens · CPC title

• G01N30/30

  of temperature · CPC title

• G01N30/7206 Primary

  interfaced to gas chromatograph (interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04) · CPC title

• G01N30/32 Primary

  of pressure or speed (G01N30/36 takes precedence) · CPC title