CN105866228A - Method for quantitative determination of hydrogen gas and deuterium gas in mixed gas - Google Patents
Method for quantitative determination of hydrogen gas and deuterium gas in mixed gas Download PDFInfo
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- CN105866228A CN105866228A CN201610020752.3A CN201610020752A CN105866228A CN 105866228 A CN105866228 A CN 105866228A CN 201610020752 A CN201610020752 A CN 201610020752A CN 105866228 A CN105866228 A CN 105866228A
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Abstract
The invention relates to a method for quantitative determination of hydrogen gas and deuterium gas in mixed gas; the mixed gas of the hydrogen gas and the deuterium gas is injected into a quantitative gas analyzer, the hydrogen gas and the deuterium gas are separated, and response curves of the hydrogen gas and the deuterium gas are subjected to area integral by using Masssoft 7.0; a to-be-tested sample is injected to the quantitative gas analyzer, response curves of the hydrogen gas and the deuterium gas are collected by using the Masssoft 7.0 sortware, the response curves of the hydrogen gas and the deuterium gas after each-time sample injection are subjected to area integral by Origin 8.0, the area integral of the hydrogen gas and the deuterium gas are respectively led to hydrogen gas and deuterium gas linear regression equations, and the volume of the hydrogen gas and the volume of the deuterium gas are calculated. By making the standard curves of hydrogen gas, deuterium gas and hydrogen deuteride in the mixed gas, the hydrogen gas and the deuterium gas in the mixed gas composed of unknown gases are determined; and the method used for quantitative determination of the hydrogen gas and the deuterium gas in the mixed gas and having low cost and easy operation is provided.
Description
Technical field
The present invention relates to the technical field of stable state isotopic separation and mensuration, more specifically to one and utilize quantitative gas
Hydrogen and the method for deuterium content in analysis-e/or determining mixed gas.
Background technology
Deuterium (deuterium) is a kind of isotope of hydrogen, containing a proton and a neutron, relative atom in its atomic nucleus
Amount is 2 times of hydrogen atom.Deuterium is usually used in thermonuclear reaction, is referred to as " following natural fuel ", its grinding at chemistry and biology
Study carefully and work is used as isotopic tracer.
The method being presently used for measuring hydrogen isotope has neutron heat energy spectrometry, nuclear magnetic resonance method, gas chromatography, gas phase color
Spectrum-MS and mass spectrography.These methods implement condition determination the harshest (as gas chromatography need liquid nitrogen environment and
Special gas chromatogram and chromatographic column), or must (need to use nuclear magnetic resonance analyser, gas phase color by the expensive precision instrument of Price-dependent
Spectrum-GC-MS etc.).Such as, in using mass spectrometric determination mixed gas during hydrogen isotope content, the method for report at present
Rely primarily on stable isotope mass spectrograph MAT253.The price of this instrument is up to millions of unit, and general unit is difficult to bear.
Summary of the invention
It is an object of the invention to solve hydrogen and deuterium content difficulty in existing mensuration mixed gas, with high costs lacks
Falling into and provide under a kind of normal condition, cost of determination is low, operate hydrogen and deuterium method for quantitatively determining in easy gaseous mixture.
To achieve these goals, the present invention is by the following technical solutions:
Hydrogen and the method for quantitatively determining of deuterium in a kind of gaseous mixture, described assay method comprises the following steps:
(1) mixed gas of hydrogen and deuterium is injected quantitative gas analyser, hydrogen and deuterium are separated, and uses Masssoft
The response curve of 7.0 pairs of hydrogen and deuterium carries out area integral；
(2) testing sample is injected quantitative gas analyser, uses Masssoft 7.0 software collection hydrogen and the response curve of deuterium,
Origin8.0 is used the response curve of hydrogen and deuterium after each sample introduction to be carried out area integral, by hydrogen and the area integral of deuterium
Bring hydrogen described in (1) and deuterium equation of linear regression respectively into, calculate hydrogen and the volume of deuterium.
As preferably, hydrogen equation of linear regression is YH2=124.36 × XH2-0.0033(R2=0.9997).
As preferably, deuterium equation of linear regression is YD2=436.28 × XD2-0.0033(R2=0.9998).
As preferably, described in concretely comprise the following steps:
1) graticule makes:
Gas production bag is evacuated, injects 0,0.5,1,2,4,6,8, the hydrogen of 10mL and deuterium calibrating gas the most wherein,
And add nitrogen to gas production bag, in making gas production bag, volume of gas is fixed as 10mL, and gas production bag is accessed gasometric analysis mass spectrum
Instrument, uses MASsoft7.0 monitoring to analyze hydrogen and the response curve of deuterium, derives data, use Origin8.0 to entering every time
The data obtained after sample carry out area integral, using area integral as the volume of variable, hydrogen and deuterium as dependent variable, do hydrogen
Gas and the regression curve of deuterium；
2) sample analysis:
Use body transfer utensil to draw mixed gas to be measured, be injected in gas production bag, and add nitrogen to gas production bag, in record gas production bag
Volume of gas, injects gasometric analysis instrument by mixed gas in gas production bag, uses hydrogen in MASsoft7.0 monitoring gaseous mixture
With the response curve of deuterium, use Origin8.0 that the data obtained after each sample introduction are carried out area integral, use hydrogen and deuterium
Regression curve calculate each gas component content.
As preferably, quantitative mass spectral instrument model is QGA.
Beneficial effects of the present invention: the present invention uses price at the quantitative gas analyser of about 200,000 yuan, mixes by making
In conjunction gas, the standard curve of hydrogen, deuterium and hydrogen deuteride measures hydrogen and deuterium in the gaseous mixture that unknown gas forms, it is provided that one
Planting under normal condition, cost of determination is low, operate hydrogen and deuterium method for quantitatively determining in easy gaseous mixture.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following example.Described side
Method is conventional method if no special instructions.Described raw material the most all can be either commercially available from open.
Below the present invention is described in further detail, it should be pointed out that embodiment described below is intended to be easy to the present invention
Understanding, and it is not played any restriction effect.
Mass spectrograph model used by the present invention is QGA, purchased from Hiden, England.
Embodiment
Hydrogen regression curve equation makes: taking the gas production bag that 8 dischargeable capacitys are more than 10ml, numbering 1-8, successively to numbered 1-8
Gas production bag in add 0,0.5,1,2,4,6,8,10ml hydrogen calibrating gas (purity be more than 99.99%), depend on the most again
Secondary in the gas production bag of numbered 1-8, add 10,9.5,9,8,6,4,2,0ml nitrogen calibrating gas (purity be more than 99.99%).
Then hydrogen and nitrogen mixed gas are implanted sequentially quantitative gas analyser (Quantitative Gas Analyser, QGA,
Hidden, England), use the response curve of Masssoft 7.0 (Hidden, England) software collection hydrogen.Use
Origin8.0 carries out area integral to the data obtained after each sample introduction.Area integral (X with hydrogen response curveH2) it is horizontal seat
Mark, the actual volume (Y of hydrogenH2, ml) and it is that vertical coordinate makes regression curve.Obtain YH2And XH2Equation of linear regression.
YH2=124.36 × XH2-0.0033(R2=0.9997).
Deuterium regression curve equation makes: taking the gas production bag that 8 dischargeable capacitys are more than 10ml, numbering 1-8, successively to volume
Number be the gas production bag of 1-8 adds 0,0.5,1,2,4,6,8,10ml deuterium calibrating gas (purity is more than 99.99%),
The most successively in the gas production bag of numbered 1-8 add 10,9.5,9,8,6,4,2,0ml nitrogen calibrating gas (purity
More than 99.99%).Then deuterium and nitrogen mixed gas are implanted sequentially quantitative gas analyser (Quantitative Gas
Analyser, QGA, Hidden, England), use the sound of Masssoft 7.0 (Hidden, England) software collection deuterium
Answer curve.Use Origin8.0 that the data obtained after each sample introduction are carried out area integral.Area integral with deuterium response curve
(XD2) it is abscissa, the actual volume (Y of deuteriumD2, ml) and it is that vertical coordinate makes regression curve.Obtain YD2And XD2's
Equation of linear regression: YD2=436.28 × XD2-0.0033(R2=0.9998).
Sample determination: take 4 parts of cumulative volumes and be 10ml, but nitrogen, hydrogen and deuterium gaseous mixture that each component ratio is different,
Every part of sample is divided into two equal portions, the first equal portions 4 sample numbering 1-4 respectively, another equal portions numbering 5-8, is noted by 1-4 sample
Enter quantitative gas analyser, use Masssoft 7.0 (Hidden, England) software collection hydrogen and the response curve of deuterium,
Origin8.0 is used the response curve of hydrogen and deuterium after each sample introduction to be carried out area integral, by hydrogen and the area integral of deuterium
Bring hydrogen and deuterium equation of linear regression respectively into:
(1)YH2=124.36 × XH2-0.0033(R2=0.9997)
(2)YD2=436.28 × XD2-0.0033(R2=0.9998).
Calculating hydrogen and the actual volume (ml) of deuterium and degree in 1-4 sample, result of calculation is as shown in table 1.
The table 1 gasometric analysis instrument analysis result to test sample
5-8 sample is delivered to Shanghai Chemical Research Inst, this chief minister carries out quantitative analysis with MAT253 stable isotope mass spectrograph,
Analysis result is as shown in table 2.
Table 1 MAT253 analysis result to test sample
| Sample number into spectrum | H2Content (%) | D2Content (%) |
| 5 | 0.27 | 0.23 |
| 6 | 0.27 | 0.90 |
| 7 | 0.35 | 1.9 |
| 8 | 0.47 | 17.8 |
By comparing Tables 1 and 2 it can be seen that gasometric analysis instrument to the analysis result of 1-4 sample with MAT253 to 5-8
The test result of number sample is completely the same.Therefore, the present invention is in analytic routines gaseous sample when hydrogen and deuterium content, completely
The use mass spectrometric method of stable isotope can be substituted, be that one is with low cost, operate hydrogen and deuterium in easy gaseous mixture
Method for quantitatively determining.
Embodiment described above is the one preferably scheme of the present invention, and the present invention not makees any pro forma limit
System, also has other variant and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (5)
1. hydrogen and the method for quantitatively determining of deuterium in a gaseous mixture, it is characterised in that described assay method comprises the following steps:
(1) mixed gas of hydrogen and deuterium is injected quantitative gas analyser, hydrogen and deuterium are separated, and uses Masssoft 7.0 that the response curve of hydrogen and deuterium is carried out area integral；
(2) testing sample is injected quantitative gas analyser, use Masssoft 7.0 software collection hydrogen and the response curve of deuterium, use Origin8.0 that the response curve of hydrogen and deuterium after each sample introduction is carried out area integral, the area integral of hydrogen and deuterium is brought into respectively hydrogen described in (1) and deuterium equation of linear regression, calculates hydrogen and the volume of deuterium.
Hydrogen and the method for quantitatively determining of deuterium in a kind of gaseous mixture the most according to claim 1, it is characterised in that hydrogen equation of linear regression is Y H2=124.36×XH2-0.0033(R2=0.9997)。
Hydrogen and the method for quantitatively determining of deuterium in a kind of gaseous mixture the most according to claim 1, it is characterised in that deuterium equation of linear regression is Y D2=436.28×XD2-0.0033(R2=0.9998)。
Hydrogen and the method for quantitatively determining of deuterium in a kind of gaseous mixture the most according to claim 1, it is characterised in that described in concretely comprise the following steps:
1) graticule makes:
Gas production bag is evacuated, inject 0,0.5,1,2,4,6,8, the hydrogen of 10mL and deuterium calibrating gas the most wherein, and add nitrogen to gas production bag, in making gas production bag, volume of gas is fixed as 10mL, gas production bag is accessed gasometric analysis mass spectrograph, MASsoft7.0 monitoring is used to analyze hydrogen and the response curve of deuterium, derive data, use Origin8.0 that the data obtained after each sample introduction are carried out area integral, using area integral as variable, the volume of hydrogen and deuterium, as dependent variable, does the regression curve of hydrogen and deuterium；
2) sample analysis:
Body transfer utensil is used to draw mixed gas to be measured, it is injected in gas production bag, and add nitrogen to gas production bag, volume of gas in record gas production bag, mixed gas in gas production bag is injected gasometric analysis instrument, use hydrogen and the response curve of deuterium in MASsoft7.0 monitoring gaseous mixture, use Origin8.0 that the data obtained after each sample introduction are carried out area integral, use the regression curve of hydrogen and deuterium to calculate the content of each gas component.
Hydrogen and the method for quantitatively determining of deuterium in a kind of gaseous mixture the most according to claim 1, it is characterised in that quantitative mass spectral instrument model is QGA.
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| CN201610020752.3A CN105866228A (en) | 2016-01-13 | 2016-01-13 | Method for quantitative determination of hydrogen gas and deuterium gas in mixed gas |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988104A (en) * | 2019-12-26 | 2020-04-10 | 中国工程物理研究院材料研究所 | Hydrogen isotope gas quadrupole mass spectrometry based on double correction |
| CN111307921A (en) * | 2019-11-26 | 2020-06-19 | 中国工程物理研究院材料研究所 | Absolute measurement quadrupole mass spectrum hydrogen isotope gas abundance analysis method and device |
| CN112924522A (en) * | 2021-01-27 | 2021-06-08 | 中国科学院合肥物质科学研究院 | Method for accurately measuring partial pressure of hydrogen, deuterium and helium by using conventional four-stage mass spectrometer |
Citations (4)
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| US4066404A (en) * | 1976-08-02 | 1978-01-03 | Phillips Petroleum Company | Determination of deuterium concentration in water |
| JPS59180458A (en) * | 1983-03-31 | 1984-10-13 | Rikagaku Kenkyusho | Quantitative analysis of deuterium in water |
| CN1580779A (en) * | 2003-08-13 | 2005-02-16 | 浙江普康生物技术股份有限公司 | Biological sample structure hydrogen-deuterium substitution verification and deuterium percentage content determining method |
| CN101349679A (en) * | 2007-07-19 | 2009-01-21 | 柯香文 | Method for quantitatively measuring hydrogen, deuteration hydrogen and deuterium hydrogen isotope element |
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2016
- 2016-01-13 CN CN201610020752.3A patent/CN105866228A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4066404A (en) * | 1976-08-02 | 1978-01-03 | Phillips Petroleum Company | Determination of deuterium concentration in water |
| JPS59180458A (en) * | 1983-03-31 | 1984-10-13 | Rikagaku Kenkyusho | Quantitative analysis of deuterium in water |
| CN1580779A (en) * | 2003-08-13 | 2005-02-16 | 浙江普康生物技术股份有限公司 | Biological sample structure hydrogen-deuterium substitution verification and deuterium percentage content determining method |
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Non-Patent Citations (1)
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| 蒋昌勇 等: "氕氘比CH/CD的四极质谱计测量", 《原子能科学技术》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111307921A (en) * | 2019-11-26 | 2020-06-19 | 中国工程物理研究院材料研究所 | Absolute measurement quadrupole mass spectrum hydrogen isotope gas abundance analysis method and device |
| CN111307921B (en) * | 2019-11-26 | 2022-11-25 | 中国工程物理研究院材料研究所 | Absolute measurement quadrupole mass spectrum hydrogen isotope gas abundance analysis method and device |
| CN110988104A (en) * | 2019-12-26 | 2020-04-10 | 中国工程物理研究院材料研究所 | Hydrogen isotope gas quadrupole mass spectrometry based on double correction |
| CN110988104B (en) * | 2019-12-26 | 2022-06-24 | 中国工程物理研究院材料研究所 | Hydrogen isotope gas quadrupole mass spectrometry based on double correction |
| CN112924522A (en) * | 2021-01-27 | 2021-06-08 | 中国科学院合肥物质科学研究院 | Method for accurately measuring partial pressure of hydrogen, deuterium and helium by using conventional four-stage mass spectrometer |
| CN112924522B (en) * | 2021-01-27 | 2023-05-30 | 中国科学院合肥物质科学研究院 | Method for accurately measuring partial pressure of hydrogen, deuterium and helium by using conventional four-stage mass spectrometer |
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Application publication date: 20160817 |