CN101126750B - Xenon impurity chromatogram analysis method - Google Patents
Xenon impurity chromatogram analysis method Download PDFInfo
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- CN101126750B CN101126750B CN2007100533326A CN200710053332A CN101126750B CN 101126750 B CN101126750 B CN 101126750B CN 2007100533326 A CN2007100533326 A CN 2007100533326A CN 200710053332 A CN200710053332 A CN 200710053332A CN 101126750 B CN101126750 B CN 101126750B
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Abstract
The utility model discloses a chromatographic study method of all impurities in the xenon, aiming at solving the problems of enabling to analyze all impurities in the xenon in particular to the fluoride, reducing the analysis time, and other problems. The utility model adopts the technical proposal that the analysis steps comprises: firstly, analyzing H2, O2, N2, Kr, CO, CO2, CH4 and N2O impurityin xenon, which comprises: selecting the helium as standard gas and selecting the chromatographic instrument PDD, setting the chromatographic condition of PDD and carrying on the analysis; secondly, analyzing the impurity SF6 in xenon, which comprises: setting the chromatogram condition, leading the xenon into the molecular sieve chromatographic column after the gas chromatography working 8 to 10minutes, then cutting down the xenon getting into the molecular sieve chromatographic column after the gas chromatography working 10 to 12 minutes, and analyzing the impurity SF6; thirdly, analyzing the impurity C2F6 in the xenon, which comprises: setting the chromatogram condition, carrying on analysis after the working condition is stable, analyzing the impurities CH4, C2H4, C2H6 and C3H8 with chromatographic instrument FID, which comprises: choosing the standard gas, setting the working conditions of chromatographic instrument FID and analyzing the content of the impurity CH4, C2H4, C2H6 and C3H8.
Description
Technical field
The present invention relates to chromatogram analysis method, specifically be more suitable for the chromatogram analysis method of all impurity in the xenon.
Background technology
Everybody knows, in the xenon except H
2, O
2, N
2, K
r, CO
2, CO, CH
4, N
2Outside several conventional impurity of O, also there is SF
6, C
2F
6, C
2H
4, C
2H
6In hydrocarbon, this is because in recent years along with industry especially developing rapidly of fluorine chemistry industry, and the fluorine chemical product is also increasing, and as the C of waste gas
2F
6, SF
6Discharging also grow with each passing day and enter due to the atmosphere.The C that also has trace in addition in the air
2H
4, C
2H
6In hydrocarbon.And producing of krypton xenon is to be raw material with the air, and C
2F
6, SF
6, C
2H
4, C
2H
6Boiling point be respectively-78.95 ℃ ,-63.25 ℃ ,-103.75 ℃ ,-88.65 ℃, all be higher than the boiling point-108.05 ℃ of Xe, all might be concentrated in the product xenon with the above impurity of the rectifying of knockout tower.
At present, in the analytical approach of xenon, there is following problem: 1, can not multianalysis go out the impurity in the xenon, can only analyze the H in the xenon
2, O
2, N
2, K
r, CO
2, CO, CH
4, N
2Several conventional impurity of O; 2, analysis time long, need one and a half hours the interval time that per two bottles of gas are analyzed under the normal condition; 3, the instrument of analysis needs is more, and per minute is analysed one bottle of xenon, needs to use three instruments just can finish, and causes energy resource consumption excessive.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of can multianalysis go out impurity, analysis time in the xenon shortly promptly only need half an hour, to analyze the instrument that needs less and analyze the chromatogram analysis method of impurity in the xenon accurately.
Realize the technical measures of above-mentioned purpose:
The chromatogram analysis method of impurity in the xenon, its step comprises:
1), at first analyzes H in the xenon
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2O impurity step:
A) selecting the helium spirit for use is standard gas and PDD chromatograph;
B) start the PDD chromatograph;
C) set the PDD chromatographic condition:
Furnace temperature: 60～90 ℃, working time: 20～15 minutes, detector temperature: 130～200 ℃, 75～90 ℃ of clack box temperature, enter the nebulizer gas pressure of molecular sieve chromatography post: 0.23～0.29MPa, enter the nebulizer gas pressure of polymer microsphere chromatographic column: 0.3～0.38MPa;
D) the PDD condition of work is analyzed after stablizing;
2) analyse SF in the xenon
6Impurity, its step:
A) set chromatographic condition:
Furnace temperature: 70 ℃, working time: 17 minutes, detector temperature: 130～160 ℃, 75～90 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.3～0.38MPa;
B) run to 8～10 minutes at gas chromatographicanalyzer, xenon is imported the molecular sieve chromatography post, running to 10～12 minutes, cut off the xenon that enters the molecular sieve chromatography post, analysing impurity SF
6
3) analyse C in the xenon
2F
6Impurity, its step:
A) set chromatographic condition:
Furnace temperature: 30～50 ℃, working time: 25～17 minutes, detector temperature: 130～200 ℃, 75～90 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.3～0.38MPa;
B) treat to analyze after condition of work is stablized;
4) adopt FID chromatograph analysing impurity: CH
4, C
2H
4, C
2H
6, C
3H
8Step:
A), selection standard gas
B), set FID chromatograph condition of work:
Furnace temperature: 90～120 ℃, working time: 8～4 minutes, detecting device base temperature: 190～210 ℃, Al
2O
3The nebulizer gas pressure of chromatographic column: 0.16～0.2MPa; Air mass flow: hydrogen: carrier gas=1～10: 1: 1;
C) analysing impurity CH
4, C
2H
4, C
2H
6, C
3H
8Content.
It is: analyze the C in the xenon
2F
6The chromatographic condition of impurity: 35～43 ℃ of furnace temperature, 22～18 minutes working times.
It was: cut off the xenon that enters molecular sieve at 11～12 minutes.
The present invention compares with the existing impurity of analyzing in the xenon, have that the impurity of analyzing in the xenon is comprehensive, short promptly be reduced to two by shortening to the instrument that only needs half an hour just can finish, analyze to need in original 1 and a half hours by original three analysis time, analyzes advantages such as accurate, that work efficiency is improved, cuts down the consumption of energy.
Embodiment
Following embodiment all is the same equally gas that adopts, the analysis of carrying out under different chromatographic conditions.
Embodiment 1
1), at first analyzes H in the xenon
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2O impurity step:
A), selecting the helium spirit for use is standard gas and PDD chromatograph;
B), start the PDD chromatograph;
C), set the PDD chromatographic condition:
Furnace temperature: 65 ℃, working time: 19 minutes, detector temperature: 150 ℃, 80 ℃ of clack box temperature, enter the nebulizer gas pressure of molecular sieve chromatography post: 0.27MPa enters the nebulizer gas pressure of polymer microsphere chromatographic column: 0.37MPa;
D), the PDD condition of work analyzes after stable, by analysis, H
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2The content of O is respectively:
2), the SF in the analysis xenon
6Impurity, its step:
Selection standard gas is German import (CF4:9.2 * 10
-6SF
6: 9.72 * 10
-6).
A) set chromatographic condition:
Furnace temperature: 70 ℃, working time: 14 minutes, detector temperature: 150 ℃, 75 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.38MPa;
B), run to 8 minutes, xenon is imported the molecular sieve chromatography post, running to 10 minutes and 5 seconds, cut off the xenon that enters the molecular sieve chromatography post, analysing impurity SF at gas chromatographicanalyzer
6, calculate SF by analysis
6Content is:
3) C in the analysis xenon
2F
6Impurity, its step:
Selection standard gas is German import (CF4:9.37 * 10
-6C2F6:11.5 * 10
-6).
A) set chromatographic condition:
Furnace temperature: 30 ℃, working time: 25 minutes, detector temperature: 130 ℃, 75 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.38MPa;
B) treat to analyze after condition of work is stablized, calculate C by analysis
2F
6Content is:
4), adopt FID chromatograph analysing impurity: CH
4, C
2H
4, C
2H
6, C
3H
8Step:
A), select German import standard gas (CH for use
4: 2.04 * 10
-6C
2H
4: 1.79 * 10
-6C
2H
6: 1.81 * 10
-6C
3H
8: 1.78 * 10
-6);
B), set FID chromatogram condition of work:
Furnace temperature: 95 ℃, working time: 7 minutes, detecting device base temperature: 200 ℃, Al
2O
3The nebulizer gas pressure of chromatographic column: 0.16MPa; Air mass flow: hydrogen: carrier gas=1: 0.1: 0.086, promptly air mass flow is 350ml/min, and hydrogen flowing quantity is 35ml/min, and carrier gas flux is 30ml/min;
C), analysing impurity CH
4, C
2H
4, C
2H
6, C
3H
8Content.Calculate CH by analysis
4, C
2H
4, C
2H
6, C
3H
8Content is:
Embodiment 2
1), at first analyzes H in the xenon
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2O impurity step:
A), selecting the helium spirit for use is standard gas and PDD chromatograph;
B), start the PDD chromatograph;
C), set the PDD chromatographic condition:
Furnace temperature: 70 ℃, working time: 17 minutes, detector temperature: 160 ℃, 75 ℃ of clack box temperature, enter the nebulizer gas pressure of molecular sieve chromatography post: 0.25MPa enters the nebulizer gas pressure of polymer microsphere chromatographic column: 0.35MPa;
D), the PDD condition of work analyzes after stable, by analysis, H
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2The content of O is respectively:
2) SF in the analysis xenon
6Impurity, its step:
Selection standard gas is German import (CF4:9.2 * 10
-6SF
6: 9.72 * 10
-6).
A) set chromatographic condition:
Furnace temperature: 70 ℃, working time: 14 minutes, detector temperature: 150 ℃, 83 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.35MPa;
B), run to 9 minutes and 16 seconds, xenon is imported the molecular sieve chromatography post, running to 11 minutes and 00 second, cut off the xenon that enters the molecular sieve chromatography post, analysing impurity SF at gas chromatographicanalyzer
6Calculate SF by analysis
6Content is:
3) the C2F6 impurity in the analysis xenon, its step:
Selection standard gas is German import (CF4:9.37 * 10
-6C2F6:11.5 * 10
-6).
A) set chromatographic condition:
Furnace temperature: 39 ℃, working time: 21 minutes, detector temperature: 150 ℃, 83 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.35MPa;
B) treat to analyze after condition of work is stablized.Calculate C by analysis
2F
6Content is:
4), adopt FID chromatograph analysing impurity: CH
4, C
2H
4, C
2H
6, C
3H
8Step:
A), select German import standard gas (CH for use
4: 2.04 * 10
-6C
2H
4: 1.79 * 10
-6C
2H
6: 1.81 * 10
-6C
3H
8: 1.78 * 10
-6);
B), set FID chromatogram condition of work:
Furnace temperature: 110 ℃, working time: 7 minutes, detecting device base temperature: 200 ℃, Al
2O
3The nebulizer gas pressure of chromatographic column: 0.18MPa; Air mass flow: hydrogen: carrier gas=10: 1: 0.95, promptly air mass flow is 354ml/min, and hydrogen flowing quantity is 35ml/min, and carrier gas flux is 33.25ml/min;
D) analyse impurity CH
4, C
2H
4, C
2H
6, C
3H
8Content.Calculate CH by analysis
4, C
2H
4, C
2H
6, C
3H
8Content is:
Embodiment 3
1), at first analyzes H in the xenon
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2O impurity step:
A), selecting the helium spirit for use is standard gas and PDD chromatograph;
B), start the PDD chromatograph;
C), set the PDD chromatographic condition:
Furnace temperature: 85 ℃, working time: 16 minutes, detector temperature: 190 ℃, 85 ℃ of clack box temperature, enter the nebulizer gas pressure of molecular sieve chromatography post: 0.29MPa enters the nebulizer gas pressure of polymer microsphere chromatographic column: 0.38MPa;
D), the PDD condition of work analyzes after stable, by analysis, H
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2The content of O is respectively:
2) SF in the analysis xenon
6Impurity, its step:
Selection standard gas is German import (CF4:9.2 * 10
-6SF
6: 9.72 * 10
-6).
A) set chromatographic condition:
Furnace temperature: 70 ℃, working time: 14 minutes, detector temperature: 150 ℃, 80 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.30MPa;
B), run to 9 minutes and 56 seconds, xenon is imported the molecular sieve chromatography post, running to 11 minutes and 50 seconds, cut off the xenon that enters the molecular sieve chromatography post, analysing impurity SF at gas chromatographicanalyzer
6, calculate SF by analysis
6Content is:
3) the C2F6 impurity in the analysis xenon, its step:
Selection standard gas is German import (CF4:9.37 * 10
-6C2F6:11.5 * 10
-6).
A) set chromatographic condition:
Furnace temperature: 49 ℃, working time: 18 minutes, detector temperature: 140 ℃, 90 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.30MPa;
B) treat to analyze after condition of work is stablized, calculate C by analysis
2F
6Content is:
4), adopt FID chromatograph analysing impurity: CH
4, C
2H
4, C
2H
6, C
3H
8Step:
A), select German import standard gas (CH for use
4: 2.04 * 10
-6C
2H
4: 1.79 * 10
-6C
2H
6: 1.81 * 10
-6C
3H
8: 1.78 * 10
-6);
B), set FID chromatogram condition of work:
Furnace temperature: 105 ℃, working time: 7 minutes, detecting device base temperature: 200 ℃, Al
2O
3The nebulizer gas pressure of chromatographic column: 0.18MPa; Air mass flow: hydrogen: carrier gas=10: 1: 0.95, promptly air mass flow is 354ml/min, and hydrogen flowing quantity is 35ml/min, and carrier gas flux is 33.25ml/min;
5) analysing impurity CH
4, C
2H
4, C
2H
6, C
3H
8Content.Calculate CH by analysis
4, C
2H
4, C
2H
6, C
3H
8Content is:
Claims (3)
1. the chromatogram analysis method of impurity in the xenon, its step comprises:
1) at first analyzes H in the xenon
2, O
2, N
2, Kr, CO, CO
2, CH
4, N
2O impurity step:
A) selecting the helium spirit for use is standard gas and PDD chromatograph;
B) start the PDD chromatograph;
C) set the PDD chromatographic condition:
Furnace temperature: 60～90 ℃, working time: 20～15 minutes, detector temperature: 130～200 ℃, 75～90 ℃ of clack box temperature, enter the nebulizer gas pressure of molecular sieve chromatography post: 0.23～0.29MPa, enter the nebulizer gas pressure of polymer microsphere chromatographic column: 0.3～0.38MPa;
D) the PDD condition of work is analyzed after stablizing;
2) SF in the analysis xenon
6Impurity, its step:
A) set chromatographic condition:
Furnace temperature: 70 ℃, working time: 17 minutes, detector temperature: 130～160 ℃, 75～90 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.3～0.38MPa;
B) run to 8～10 minutes at gas chromatographicanalyzer, xenon is imported the molecular sieve chromatography post, running to 10～12 minutes, cut off the xenon that enters the molecular sieve chromatography post, analysing impurity SF
6
3) C in the analysis xenon
2F
6Impurity, its step:
A) set chromatographic condition:
Furnace temperature: 30～50 ℃, working time: 25～17 minutes, detector temperature: 130～200 ℃, 75～90 ℃ of clack box temperature entered the nebulizer gas pressure of polymer microsphere chromatographic column: 0.3～0.38MPa;
B) treat to analyze after condition of work is stablized;
4) adopt FID chromatograph analysing impurity: CH
4, C
2H
4, C
2H
6, C
3H
8, its step:
A) selection standard gas
B) set FID chromatograph condition of work:
Furnace temperature: 90～120 ℃, working time: 8～4 minutes, detecting device base temperature: 190～210 ℃, Al
2O
3The nebulizer gas pressure of chromatographic column: 0.16～0.2MPa; Air mass flow: hydrogen: carrier gas=1～10: 1: 1;
C) analysing impurity CH
4, C
2H
4, C
2H
6, C
3H
8Content.
2. the chromatogram analysis method of impurity in the xenon as claimed in claim 1 is characterized in that: analyze the C in the xenon
2F
6The chromatographic condition of impurity: 35～43 ℃ of furnace temperature, 22～18 minutes working times.
3. the chromatogram analysis method of impurity in the xenon as claimed in claim 1 is characterized in that: cut off the xenon that enters molecular sieve at 11～12 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100533326A CN101126750B (en) | 2007-09-21 | 2007-09-21 | Xenon impurity chromatogram analysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100533326A CN101126750B (en) | 2007-09-21 | 2007-09-21 | Xenon impurity chromatogram analysis method |
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|---|---|
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| CN101126750B true CN101126750B (en) | 2010-07-28 |
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|---|---|---|---|
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487543B (en) * | 2013-09-17 | 2015-08-05 | 武汉钢铁(集团)公司 | The analytical approach of Krypton and xenon content in krypton xenon unstripped gas |
| CN104678034B (en) * | 2013-11-27 | 2017-12-15 | 上海宝钢工业技术服务有限公司 | Determine the analysis system and assay method of impurity component in high-purity gas |
| CN104316617A (en) * | 2014-11-06 | 2015-01-28 | 上海华爱色谱分析技术有限公司 | Gas chromatograph for analysis on trace light dydrocarbon impurity in electronic-grade propylene |
| CN105259291A (en) * | 2015-11-11 | 2016-01-20 | 中国核动力研究设计院 | Analysis method of fission gas |
| CN107014940A (en) * | 2017-05-09 | 2017-08-04 | 上海大学 | Rapid analysis method when carbon monoxide, carbon dioxide and nitrous oxide coexist |
| CN108931585A (en) * | 2017-05-25 | 2018-12-04 | 中国石油化工股份有限公司 | Carbon impurity on-line monitoring method in a kind of liquefaction hydrocarbon raw material |
| CN111830149B (en) * | 2020-06-23 | 2022-05-20 | 中国辐射防护研究院 | TCD gas chromatography multi-stage circulating Kr separation system and method |
| CN112858514B (en) * | 2021-01-18 | 2022-12-13 | 中昊光明化工研究设计院有限公司 | Method for measuring krypton, xenon and methane in air separation oxygen and device for measuring krypton, xenon and methane in air separation oxygen |
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| EP0677852B1 (en) * | 1994-04-15 | 1997-10-01 | General Electric Company | Apparatus and process for krypton-xenon concentration, separation and measurement |
| CN2285900Y (en) * | 1996-04-10 | 1998-07-08 | 中国科学院大连化学物理研究所 | High purity argon analyzer |
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| EP0677852B1 (en) * | 1994-04-15 | 1997-10-01 | General Electric Company | Apparatus and process for krypton-xenon concentration, separation and measurement |
| CN2285900Y (en) * | 1996-04-10 | 1998-07-08 | 中国科学院大连化学物理研究所 | High purity argon analyzer |
| CN2687669Y (en) * | 2004-02-16 | 2005-03-23 | 臧牧 | Fully-automatic high-sensitivity helium mass spectra leak detecting in strument |
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