Mass spectrometer and mass analyzing method for efficiently ionizing a sample with less carry-over

Patent metadata

Field	Value
Publication number	US-9543135-B2
Application number	US-201213562435-A
Country	US
Kind code	B2
Filing date	Jul 31, 2012
Priority date	Aug 26, 2011
Publication date	Jan 10, 2017
Grant date	Jan 10, 2017

Abstract

A mass spectrometer for efficiently ionizing a sample with less carry-over. The ratio of the amount of sample gas to that of a whole headspace gas is increased by decreasing the pressure inside of a sample vessel in which the sample is sealed thereby efficiently ionizing the sample.

First claim

What is claimed is:

1. A mass spectrometer comprising:
a sample vessel in which a water solution containing sample molecules is sealed, where at least some of sample is vaporized;
an ionization housing connected to the sample vessel by a first pipeline having a pulse valve connected thereto and to the ionization housing, and having a discharge ionization source of taking in a gas containing vaporized sample molecules and water molecules which are present in the sample vessel and ionizing the sample molecules by ion molecule reaction, the pressure being lower than the pressure inside of the sample vessel, the pulse valve configured to discontinuously introduce the gas into the ionization housing;
a vacuum chamber connected to the ionization housing, said vacuum chamber having a pump coupled thereto, said pump configured to maintain a pressure of the vacuum chamber at 0.1 Pa or lower, and said vacuum chamber having a mass analyzer for analyzing the ionized sample by m/z; and
means for decreasing the pressure inside of the sample vessel,
wherein the means for decreasing the pressure inside of the sample vessel is connected to a second pipeline in which the other side of the second pipeline is connected to the sample vessel or the first pipeline.

2. The mass spectrometer according to claim 1 ,
wherein the means for decreasing the pressure inside of the sample vessel decreases the pressure inside the sample vessel to 50,000 Pa or lower.

3. The mass spectrometer according to claim 1 ,
wherein the means for decreasing the pressure inside of the sample vessel decreases the pressure inside the sample vessel to 30,000 Pa or lower.

4. The mass spectrometer according to claim 1 ,
wherein the means for decreasing the pressure inside of the sample vessel decreases the pressure inside the sample vessel to 10,000 Pa or lower.

5. The mass spectrometer according to claim 1 , comprising means for heating the sample vessel.

6. The mass spectrometer according to claim 1 ,
wherein an on-off mechanism for controlling the introduction of the sample gas is interposed between the sample vessel and the vacuum chamber.

7. The mass spectrometer according to claim 1 ,
wherein the ionization source comprises paired electrodes disposed while putting a portion of the ionization housing formed of a dielectric substance therebetween and a power source, in which a discharge plasma is generated by dielectric barrier discharge generated by the application of a voltage on the electrode pair to thereby generating ions.

8. The mass spectrometer according to claim 1 ,
wherein the ionization source comprises paired electrodes disposed inside the ionization housing and a power source, in which discharge plasma is generated by glow discharge generated by the application of a voltage to the electrode pair, thereby generating ions.

9. A mass analyzing method using a sample vessel in which a water solution containing sample molecules is sealed, where at least some of sample is vaporized;
an ionization housing connected to the sample vessel by a first pipeline having a pulse valve connected thereto and to the ionization housing, and having a discharge ionization source for ionizing the sample molecules by ion molecule reaction, and
a vacuum chamber connected to the ionization housing said vacuum chamber having a first pump coupled thereto, said first pump being configured to maintain a pressure of the vacuum chamber at 0.1 Pa or lower, and said vacuum chamber having a mass analyzer for analyzing the ionized sample by m/z and a second pump connected to a second pipeline in which the other side of the second pipeline is connected to the sample vessel or the first pipeline, the method comprising:
decreasing pressure inside of the vacuum chamber;
decreasing the pressure inside of the sample vessel using the second pump;
taking in, discontinuously, a gas containing vaporized sample molecules and water molecules which are present in the sample vessel to the ionization housing via the pulse valve and ionizing the sample molecules; and
analyzing the ionized sample in the mass analyzer.

10. The mass analyzing method according to claim 9 , comprising:
using the pulse valve for controlling the introduction of the sample interposed between the sample vessel and the vacuum chamber, decreasing the pressure inside of the vacuum chamber in a state where the pulse valve is closed; and
decreasing the pressure inside of the sample vessel by switching the pulse valve from a closed state to an open state.

11. A mass spectrometer comprising:
a sample vessel in which a solid or liquid sample is sealed, where at least some of sample is vaporized;
an ionization housing coupled to the sample vessel and having an ionization source of taking in, discontinuously, a gas containing vaporized sample molecules which is present in the sample vessel via a pulse valve coupled to the sample vessel and to the ionization housing and ionizing the same, the pressure being lower than the pressure inside of the sample vessel;
a vacuum chamber coupled to the ionization housing said vacuum chamber having a first pump coupled thereto, said first pump configured to maintain a pressure of the vacuum chamber at 0.1 Pa or lower, and said vacuum chamber having a mass analyzer for analyzing the ionized sample by m/z; and
a second pump for decreasing the pressure inside of the sample vessel,
wherein the second pump is coupled to one side of a pipeline in which another side of the pipeline is coupled to the sample vessel.

Assignees

• Kumano Shun
• Sugiyama Masuyuki
• Hashimoto Yuichiro
• Hasegawa Hideki
• Yamada Masuyoshi
• Nishimura Kazushige
• Morokuma Hidetoshi
• Hitachi High Tech Corp

Inventors

• Kumano Shun
• Sugiyama Masuyuki
• Hashimoto Yuichiro
• Hasegawa Hideki
• Yamada Masuyoshi
• Nishimura Kazushige
• Morokuma Hidetoshi

Classifications

• H01J49/0431 Primary

  for liquid samples (interfaces to liquid chromatographs G01N30/7233) · CPC title

• H01J49/168

  field ionisation, e.g. corona discharge (atmospheric pressure corona discharge per se H01T19/00) · CPC title