CN111007031A - Method for measuring trace hydrogen or trace oxygen - Google Patents
Method for measuring trace hydrogen or trace oxygen Download PDFInfo
- Publication number
- CN111007031A CN111007031A CN201911365247.2A CN201911365247A CN111007031A CN 111007031 A CN111007031 A CN 111007031A CN 201911365247 A CN201911365247 A CN 201911365247A CN 111007031 A CN111007031 A CN 111007031A
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- Prior art keywords
- hydrogen
- oxygen
- trace
- water vapor
- content
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000001301 oxygen Substances 0.000 title claims abstract description 59
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 59
- 239000001257 hydrogen Substances 0.000 title claims abstract description 55
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 55
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000007789 gas Substances 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000005259 measurement Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001745 non-dispersive infrared spectroscopy Methods 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 230000001737 promoting effect Effects 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 2
- 238000000041 tunable diode laser absorption spectroscopy Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 238000000691 measurement method Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000001285 laser absorption spectroscopy Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
Abstract
A method for spectroscopic measurement of trace hydrogen or trace oxygen, comprising the steps of: drying the mixed gas containing trace oxygen or trace hydrogen; measuring the content of water vapor in the dried mixed gas to obtain an initial water vapor content A; carrying out chemical reaction on oxygen and hydrogen in the mixed gas to generate water vapor; measuring the content of water vapor in the reacted gas to obtain the content B of the reacted water vapor; according to the chemical reaction formula: 2H2+O2=2H2O, knowing that the difference between B and a and the concentration of the trace hydrogen participating in the reaction are equal to 1: 1, the difference to the concentration of the trace oxygen participating in the reaction is equal to 2: 1, so that the content of trace hydrogen or trace oxygen contained in the initial mixed gas can be estimated. The measuring method of the invention has simple operation, convenience and rapidness, and the measuring result is more accurate。
Description
Technical Field
The invention belongs to the field of gas content detection, and particularly relates to a spectral measurement method of trace hydrogen or trace oxygen.
Background art o
Oxygen is an important gas and is used in many situations. Oxygen is a strong oxidant, and the requirement on the oxygen content is high in some occasions, so that substance damage can be caused once the oxygen content exceeds the standard. Oxygen has an absorption peak near 0.76um, and the oxygen content can be measured by using an infrared spectroscopy method, but the infrared absorption capacity of the oxygen is weak. The direct infrared absorption spectrum measurement of oxygen is difficult to realize higher precision, even use laser, adopt TDLAS to measure, also is difficult to realize higher detection precision.
Hydrogen is also an important gas and is used in many applications. Hydrogen energy and hydrogen-cooled generators are required to be utilized in large quantities, hydrogen is flammable and explosive gas, and once the content exceeds the standard, explosion is possibly caused. Hydrogen is a molecule with a symmetrical diatomic structure, and because the molecular structure is symmetrical, the infrared absorption spectrum is extremely weak, and infrared spectrum measurement is difficult to realize.
The oxygen and the hydrogen are subjected to combustion reaction or catalytic reaction to generate water, and the infrared absorption capacity of the gaseous water is very strong, so that the detection accuracy of less than 0.1ppm can be realized. Therefore, the trace oxygen or the trace hydrogen is respectively reacted with the hydrogen or the oxygen to generate water, and then the high-precision detection of the water can be realized through the characteristic that the gaseous water has very strong infrared absorption energy, so that the high-precision detection of the trace oxygen or the trace hydrogen can be indirectly realized.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the spectral measurement method of trace hydrogen or trace oxygen, which is convenient to operate and accurate in measurement result.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for measuring the spectrum of trace hydrogen or trace oxygen includes such steps as measuring the trace hydrogen or oxygen,
(1) introducing a mixed gas containing a trace of oxygen or hydrogen to be detected;
(2) drying the mixed gas to reduce the content of water vapor in the mixed gas so as to improve the monitoring sensitivity;
(3) introducing the dried mixed gas into a first water vapor measurement gas chamber, and measuring the content of water vapor in the mixed gas to obtain an initial water vapor content A;
(4) introducing the mixed gas into a catalytic reaction gas chamber to enable oxygen and hydrogen to generate chemical reaction to generate water vapor;
(5) introducing the gas after the catalytic reaction into a second water vapor measurement air chamber, and measuring the content of water vapor to obtain the content B of the water vapor after the reaction;
(6) calculating the difference value between the water vapor content B after the reaction and the initial water vapor content A;
(7) according to the chemical reaction formula: 2H2+O2=2H2O, the difference is known to be equal to the concentration of the trace hydrogen participating in the reaction, equal to 1: 1, the difference to the concentration of the trace oxygen participating in the reaction is equal to 2: 1, so that the content of a trace amount of hydrogen or oxygen contained in the initial mixed gas in the step (1) can be estimated.
In the step (1), if only hydrogen and no oxygen exist in the gas to be detected, high-concentration oxygen or air needs to be mixed; if only oxygen exists in the gas to be detected and no hydrogen exists, high-concentration hydrogen needs to be mixed; thereby forming a mixed gas of oxygen and hydrogen.
And (3) performing adsorption treatment on the water vapor by adopting a molecular sieve or other adsorbents in a drying mode in the step (2).
The method for measuring the water vapor content in step (3) and step (5) includes, but is not limited to, TDLAS (Tunable Laser Absorption Spectroscopy) or NDIR (Non-Dispersive InfraRed Spectroscopy).
The catalyst used in the catalytic reaction chamber in step (4) includes, but is not limited to, palladium catalyst or platinum catalyst capable of promoting the reaction between oxygen and hydrogen.
By adopting the technical scheme, the mixed gas containing trace hydrogen or trace oxygen is subjected to catalytic reaction to generate water vapor, the water vapor is subjected to spectral measurement, and the content of trace hydrogen or trace oxygen in the original mixed gas is calculated according to the molecular proportion of hydrogen and oxygen to water in the chemical reaction.
Detailed Description
The invention relates to a spectral measurement method of trace hydrogen or trace oxygen, which comprises the following steps:
(1) introducing a mixed gas containing a trace amount of hydrogen or oxygen to be detected;
(2) drying the mixed gas to reduce the content of water vapor in the mixed gas so as to improve the monitoring sensitivity;
(3) introducing the dried mixed gas into a first water vapor measurement gas chamber, and measuring the content of water vapor in the mixed gas to obtain an initial water vapor content A;
(4) introducing the mixed gas into a catalytic reaction gas chamber to enable oxygen and hydrogen to generate chemical reaction to generate water vapor;
(5) introducing the gas after the catalytic reaction into a second water vapor measurement air chamber, and measuring the content of water vapor to obtain the content B of the water vapor after the reaction;
(6) calculating the difference value between the water vapor content B after the reaction and the initial water vapor content A;
(7) according to the chemical reaction formula: 2H2+O2=2H2O, the difference is known to be equal to the concentration of the trace hydrogen participating in the reaction, equal to 1: 1, the difference to the concentration of the trace oxygen participating in the reaction is equal to 2: 1, so that the content of a trace amount of hydrogen or oxygen contained in the initial mixed gas in the step (1) can be estimated.
In the step (1), if only hydrogen and no oxygen exist in the gas to be detected, high-concentration oxygen or air needs to be mixed; if only oxygen exists in the gas to be detected and no hydrogen exists, high-concentration hydrogen needs to be mixed; thereby forming a mixed gas of oxygen and hydrogen.
And (3) performing adsorption treatment on the water vapor by adopting a molecular sieve or other adsorbents in a drying mode in the step (2).
The method for measuring the water vapor content in step (3) and step (5) includes, but is not limited to, TDLAS (Tunable Laser Absorption Spectroscopy) or NDIR (Non-Dispersive InfraRed Spectroscopy).
The catalyst used in the catalytic reaction chamber in step (4) includes, but is not limited to, palladium catalyst or platinum catalyst capable of promoting the reaction between oxygen and hydrogen.
The present embodiment is not intended to limit the shape, material, structure, etc. of the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (5)
1. A method for measuring a trace amount of hydrogen or a trace amount of oxygen by a spectrum, characterized in that: comprises the following steps of (a) carrying out,
(1) introducing a mixed gas containing a trace amount of hydrogen or oxygen to be detected;
(2) drying the mixed gas to reduce the content of water vapor in the mixed gas so as to improve the monitoring sensitivity;
(3) introducing the dried mixed gas into a first water vapor measurement gas chamber, and measuring the content of water vapor in the mixed gas to obtain an initial water vapor content A;
(4) introducing the mixed gas into a catalytic reaction gas chamber to enable oxygen and hydrogen to generate chemical reaction to generate water vapor;
(5) introducing the gas after the catalytic reaction into a second water vapor measurement air chamber, and measuring the content of water vapor to obtain the content B of the water vapor after the reaction;
(6) calculating the difference value between the water vapor content B after the reaction and the initial water vapor content A;
(7) according to the chemical reaction formula: 2H2+O2=2H2O, the difference is known to be equal to the concentration of the trace hydrogen participating in the reaction, equal to 1: 1, the difference to the concentration of the trace oxygen participating in the reaction is equal to 2: 1, so that the content of a trace amount of hydrogen or oxygen contained in the initial mixed gas in the step (1) can be estimated.
2. The method for spectroscopic measurement of trace hydrogen or trace oxygen as set forth in claim 1, wherein: in the step (1), if only hydrogen and no oxygen exist in the gas to be detected, high-concentration oxygen or air needs to be mixed; if only oxygen exists in the gas to be detected and no hydrogen exists, high-concentration hydrogen needs to be mixed; thereby forming a mixed gas of oxygen and hydrogen.
3. The method for spectroscopic measurement of trace hydrogen or trace oxygen as set forth in claim 1, wherein: and (3) performing adsorption treatment on the water vapor by adopting a molecular sieve or other adsorbents in a drying mode in the step (2).
4. The method for spectroscopic measurement of trace hydrogen or trace oxygen as set forth in claim 1, wherein: the measuring method of the water vapor content in the step (3) and the step (5) includes, but is not limited to, a TDLAS technique or an NDIR technique.
5. The method for spectroscopic measurement of trace hydrogen or trace oxygen as set forth in claim 1, wherein: the catalyst used in the catalytic reaction chamber in step (4) includes, but is not limited to, palladium catalyst or platinum catalyst capable of promoting the reaction between oxygen and hydrogen.
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CN201911365247.2A CN111007031A (en) | 2019-12-26 | 2019-12-26 | Method for measuring trace hydrogen or trace oxygen |
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CN201911365247.2A CN111007031A (en) | 2019-12-26 | 2019-12-26 | Method for measuring trace hydrogen or trace oxygen |
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CN201911365247.2A Pending CN111007031A (en) | 2019-12-26 | 2019-12-26 | Method for measuring trace hydrogen or trace oxygen |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111739673A (en) * | 2020-05-12 | 2020-10-02 | 中国原子能科学研究院 | Oxidation adsorption experiment system and method for trace hydrogen in oxygen atmosphere |
Citations (6)
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EP0310053A2 (en) * | 1987-09-30 | 1989-04-05 | Messer Griesheim Gmbh | Method for determining hydrogen concentrations |
JPH02245658A (en) * | 1989-03-18 | 1990-10-01 | Nisshin Steel Co Ltd | Method and apparatus for measuring concentration of oxygen in gas |
CN1080397A (en) * | 1992-06-18 | 1994-01-05 | 刘永军 | The aquation mensuration of micro amount of oxygen |
CN104569282A (en) * | 2015-01-08 | 2015-04-29 | 中昊光明化工研究设计院有限公司 | Method for determining content of hydrogen and oxygen in hydrogen-containing gas and integrally determining content of water and oxygen |
CN104697951A (en) * | 2006-04-19 | 2015-06-10 | 光学传感公司 | Measuring water vapor in hydrocarbons |
CN105806806A (en) * | 2016-05-12 | 2016-07-27 | 河南省日立信股份有限公司 | TDLAS based escaped ammonia concentration detection device and method |
-
2019
- 2019-12-26 CN CN201911365247.2A patent/CN111007031A/en active Pending
Patent Citations (6)
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EP0310053A2 (en) * | 1987-09-30 | 1989-04-05 | Messer Griesheim Gmbh | Method for determining hydrogen concentrations |
JPH02245658A (en) * | 1989-03-18 | 1990-10-01 | Nisshin Steel Co Ltd | Method and apparatus for measuring concentration of oxygen in gas |
CN1080397A (en) * | 1992-06-18 | 1994-01-05 | 刘永军 | The aquation mensuration of micro amount of oxygen |
CN104697951A (en) * | 2006-04-19 | 2015-06-10 | 光学传感公司 | Measuring water vapor in hydrocarbons |
CN104569282A (en) * | 2015-01-08 | 2015-04-29 | 中昊光明化工研究设计院有限公司 | Method for determining content of hydrogen and oxygen in hydrogen-containing gas and integrally determining content of water and oxygen |
CN105806806A (en) * | 2016-05-12 | 2016-07-27 | 河南省日立信股份有限公司 | TDLAS based escaped ammonia concentration detection device and method |
Non-Patent Citations (3)
Title |
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李国刚: "《环境监测科技进展报告:第九次全国环境监测学术论文集 上》", 31 August 2009, 中国环境科学出版社 * |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111739673A (en) * | 2020-05-12 | 2020-10-02 | 中国原子能科学研究院 | Oxidation adsorption experiment system and method for trace hydrogen in oxygen atmosphere |
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