Element analysis device and element analysis method

Patent metadata

Field	Value
Publication number	US-10978285-B2
Application number	US-201716333879-A
Country	US
Kind code	B2
Filing date	Sep 22, 2017
Priority date	Sep 23, 2016
Publication date	Apr 13, 2021
Grant date	Apr 13, 2021

Abstract

An objective of this invention is to conduct an accurate quantitative analysis on the Ar element contained in a sample gas by an element analysis device comprising a heating furnace and a mass spectrometer for conducting a quantitative analysis on an element in a vacuum atmosphere. The element analysis device comprises: a heating furnace that heats a graphite crucible containing a sample while introducing a carrier gas into the heating furnace, thereby vaporizing the sample to generate a sample gas; a quadrupole mass spectrometer that conducts the quantitative analysis on the Ar element contained in the sample gas in a mixed gas comprising the carrier gas and the sample gas discharged from the heating furnace, a first pressure regulator that controls the pressure of the carrier gas to be introduced into the heating furnace, and a second pressure regulator that controls the pressure of the mixed gas discharged from the heating furnace.

First claim

The invention claimed is:

1. An element analysis device comprising
a heating furnace that produces a sample gas by heating a crucible that contains a sample while introducing a carrier gas so as to evaporate at least a part of the sample,
a mass spectrometer that extracts an element contained in the sample gas in a mixed gas comprising the carrier gas and the sample gas discharged from the heating furnace in a vacuum atmosphere and that conducts a quantitative analysis on the element,
a first pressure regulator that controls pressure of the carrier gas to be introduced into the heating furnace, and
a second pressure regulator that controls pressure of the mixed gas to be introduced into the mass spectrometer.

2. The element analysis device according to claim 1 , further comprising
a vacuum chamber to which the mass spectrometer is connected, wherein
total amount of the mixed gas discharged from the second pressure regulator is introduced into the vacuum chamber.

3. The element analysis device according to claim 1 , further comprising
a suction pump that is arranged on a branch line that branches and extends from a position between the second pressure regulator and the mass spectrometer and that sucks the mixed gas whose pressure is controlled by the second pressure regulator.

4. The element analysis device according to claim 1 , wherein
the pressure of the carrier gas to be introduced into the heating furnace is controlled by the first pressure regulator within a range more than or equal to 20 kPa and less than or equal to 80 kPa.

5. The element analysis device according to claim 1 , wherein
the sample is an Ar containing sample.

6. The element analysis device according to claim 1 , wherein
the mass spectrometer is a quadrupole mass spectrometer, and comprising
an information processing unit that conducts a quantitative analysis on the element contained in the sample gas based on
a reference analysis data that indicates a chronological change of current intensity obtained (i) by heating the crucible into which a bath agent containing a main component of the sample is put while introducing the carrier gas into the heating furnace, (ii) by heating the crucible without putting the sample into the crucible while introducing the carrier gas into the heating furnace and (iii) by introducing the carrier gas discharged from the heating furnace into the quadrupole mass spectrometer, and
a measurement analysis data that indicates the chronological change of the current intensity obtained (i) by putting the sample into the crucible and heating the crucible while introducing the carrier gas into the heating furnace, and (ii) by introducing the mixed gas comprising the carrier gas and the sample gas discharged from the heating furnace into the quadrupole mass spectrometer.

7. The element analysis device according to claim 1 , wherein the second pressure regulator is provided on a discharging line which guides the mixed gas discharged from the heating furnace to the mass spectrometer.

8. The element analysis device according to claim 1 , further comprising a flow rate adjuster that limits a flow rate of the mixed gas, the flow rate adjuster being arranged in series with the second pressure regulator.

9. An element analysis method for conducting a quantitative analysis on an element contained in a sample gas produced by evaporating a sample, comprising
heating a crucible in a heating furnace into which a bath agent containing a main component of the sample is put while introducing a carrier gas whose pressure is within a range more than or equal to 20 kPa and less than or equal to 80 kPa into the heating furnace,
producing the sample gas by heating the crucible into which an Ar containing sample is put while introducing the carrier gas into the heating furnace,
reducing pressure of a mixed gas comprising the carrier gas and the sample gas discharged from the heating furnace to less than or equal to 1.5 Pa and introducing the decompressed mixed gas into a mass spectrometer, and
extracting the element contained in the sample gas and conducting the quantitative analysis on the element.

10. The element analysis method according to claim 9 , comprising
heating the crucible in the heating furnace into which the bath agent containing the main component of the sample is put while introducing the carrier gas whose pressure is within the range more than or equal to 20 kPa and less than or equal to 80 kPa into the heating furnace,
obtaining a reference analysis data that indicates a chronological change of current intensity by heating the crucible in the heating furnace into which no sample is put while introducing the carrier gas into the heating furnace, by reducing the pressure of the carrier gas discharged from the heating furnace to less than or equal to 1.5 Pa and by introducing the decompressed carrier gas into the mass spectrometer, and
obtaining a measurement analysis data that indicates the chronological change of the current intensity by producing the sample gas by heating the crucible in the heating furnace into which the Ar containing sample is put while introducing the carrier gas into the heating furnace, by reducing the pressure of the mixed gas comprising the carrier gas and the sample gas discharged from the heating furnace to less than or equal to 1.5 Pa and by introducing the decompressed mixed gas into the mass spectrometer, and
conducting the quantitative analysis on the element contained in the sample gas based on the reference analysis data and the measurement analysis data.

11. The element analysis method according to claim 9 , wherein the mass spectrometer into which the decompressed mixed gas is introduced is a quadrupole mass spectrometer.

Assignees

• Horiba Ltd
• Horiba Stec Co Ltd

Inventors

• Inoue Takahito
• Uchihara Hiroshi
• Sasai Kohei
• Ikeyama Toshihiro

Classifications

• G01N31/12 Primary

  using combustion (G01N25/20 takes precedence) · CPC title

• G01N33/0016

  by regulating a physical variable, e.g. pressure or temperature · CPC title

• G01N33/0026

  using an alternating circulation of another gas · CPC title

• H01J49/24

  Vacuum systems, e.g. maintaining desired pressures · CPC title

• G01N30/32

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