Device and method for analyzing impurities in hydrogen isotope gas

A hydrogen isotope and impurity analysis technology, applied in the field of gas chromatography analysis, can solve the problems of high analysis results and difficult effective separation

Active Publication Date: 2022-05-27
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Oxygen and argon are often difficult to separate effectively in a 5A capillary column with hydrogen as the carrier gas at room temperature, which leads to high analysis results of oxygen impurity content in the presence of argon impurities
[0005] Therefore, using a conventional chromatograph to analyze impurities in hydrogen isotope gas, how to change the current situation of poor analysis accuracy and easy mixing with other gases to affect the analysis results has become an urgent problem to be solved by those skilled in the art

Method used

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  • Device and method for analyzing impurities in hydrogen isotope gas
  • Device and method for analyzing impurities in hydrogen isotope gas
  • Device and method for analyzing impurities in hydrogen isotope gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] for calibrating instruments 4 He sensitivity

[0075](1), set the temperature of the chromatographic column box 18 and the temperature of the thermal conductivity detector 14 to 200°C, close the second six-way valve 13 (at this time, the first chromatographic column 16 is communicated with the thermal conductivity detector 14), use a high Purging the hydrogen purifier 15 and the chromatographic column with pure argon, the purging time is not less than 4 hours;

[0076] (2), cooling the chromatographic column and the hydrogen purifier 15 to 30°C, and the temperature of the thermal conductivity detector 14 to 70°C;

[0077] (3), will 4 The standard gas source 2 (the main component is argon) with a He content of 0.1% is as follows figure 2 The position shown is connected to the vacuum sampling system;

[0078] (4) Evacuate the chromatograph pipeline and perform vacuum leak detection to ensure air tightness;

[0079] (5), observe the baseline, open the first six-way v...

Embodiment 2

[0088] for calibrating instruments 3 He sensitivity.

[0089] (1), set the temperature of the chromatographic column box 18 and the temperature of the thermal conductivity detector 14 to 200°C, close the second six-way valve 13 (at this time, the first chromatographic column 16 is communicated with the thermal conductivity detector 14), use a high Purging the hydrogen purifier 15 and the chromatographic column with pure argon, the purging time is not less than 4 hours;

[0090] (2), cooling the chromatographic column and the hydrogen purifier 15 to 30°C, and the temperature of the thermal conductivity detector 14 to 70°C;

[0091] (3), will be pure 3 He gas is used as the standard gas source 2, according to the appendix figure 2 The position shown is connected to the vacuum sampling system;

[0092] (4) Evacuate the chromatograph pipeline and perform vacuum leak detection to ensure air tightness;

[0093] (5), observe the baseline, open the first six-way valve 12 after t...

Embodiment 3

[0103] O to calibrate the instrument 2 , N 2 , CH 4 , CO sensitivity

[0104] (1) The temperature of the chromatographic column box 18 and the temperature of the thermal conductivity detector 14 are both set to 200°C to 250°C, and the second six-way valve 13 is opened (at this time, the second chromatographic column 17 is communicated with the thermal conductivity detector 14), The second chromatographic column 17 is purged with high-purity argon, and the purge time is not less than 4 hours;

[0105] (2), cooling the chromatographic column and the hydrogen purifier 15 to 30°C, and the temperature of the thermal conductivity detector 14 to 70°C;

[0106] (3), the main component is hydrogen, O 2 , N 2 , CH 4 , standard gas with CO content of 1.00%, 1.00%, 1.00% and 1.00% respectively, according to the attached figure 2 The position shown is connected to the vacuum sampling system;

[0107] (4) Evacuate the chromatograph pipeline and perform vacuum leak detection to ensu...

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Abstract

The invention discloses a device for analyzing impurities in hydrogen isotope gas, which comprises a carrier gas source, a standard gas source, a sample container, a chromatographic column box, a hydrogen purifier and a thermal conductivity detector, the chromatographic column box comprises a first chromatographic column and a second chromatographic column, and the hydrogen purifier can adsorb the hydrogen isotope gas. According to the invention, the hydrogen purifier is connected in series in front of the first chromatographic column, and the hydrogen purifier can adsorb hydrogen isotope gas below the detection limit of the thermal conductivity detector so as to eliminate the overlap between deuterium and tritium peaks and helium peaks, so that the analysis precision of helium impurities in the hydrogen isotope gas is improved; the invention further provides a method for analyzing the impurities in the hydrogen isotope gas, argon is used as carrier gas, analysis is carried out through the second chromatographic column, and therefore interference of argon impurities in a hydrogen isotope sample on analysis of oxygen impurities is avoided. According to the invention, high-precision analysis of impurities such as nitrogen, methane and carbon monoxide is realized while high-precision analysis of impurities such as helium and oxygen in the hydrogen isotope gas is realized.

Description

technical field [0001] The invention relates to the technical field of gas chromatography analysis, in particular to a device and method for analyzing impurities in hydrogen isotope gas. Background technique [0002] The International Thermonuclear Experimental Reactor (ITER) and the China Fusion Engineering Test Reactor (CFETR) are major projects to promote fusion power generation, among which the tritium fuel cycle and tritium balance are related to Technology requires rapid, precise analysis and control of impurity levels in hydrogen isotope gases. [0003] Because hydrogen isotope mixed gas often contains deuterium and tritium isotopes, the chromatographic analysis of impurities in hydrogen isotope mixed gas is different from the analysis of ordinary hydrogen. The chromatographic analysis of impurities in ordinary hydrogen often uses high-purity hydrogen as the carrier gas. Since there is no deuterium and tritium in the sample gas, helium ( 3 He or 4 The chromatograph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14G01N30/46G01N30/66
CPCG01N30/02G01N30/14G01N30/468G01N30/66G01N2030/025G01N2030/143Y02E30/10
Inventor 雷强华武志刚寇化秦张光辉熊义富蒋富冬
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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