CN111007031A - Method for measuring trace hydrogen or trace oxygen - Google Patents

Method for measuring trace hydrogen or trace oxygen Download PDF

Info

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
Authority
CN
China
Prior art keywords
hydrogen
oxygen
trace
water vapor
content
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201911365247.2A
Other languages
Chinese (zh)
Inventor
汪献忠
***
李新田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henan Relations Co Ltd
Original Assignee
Henan Relations Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henan Relations Co Ltd filed Critical Henan Relations Co Ltd
Priority to CN201911365247.2A priority Critical patent/CN111007031A/en
Publication of CN111007031A publication Critical patent/CN111007031A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/39Investigating 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

Method for measuring trace hydrogen or trace oxygen
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.
CN201911365247.2A 2019-12-26 2019-12-26 Method for measuring trace hydrogen or trace oxygen Pending CN111007031A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911365247.2A CN111007031A (en) 2019-12-26 2019-12-26 Method for measuring trace hydrogen or trace oxygen

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911365247.2A CN111007031A (en) 2019-12-26 2019-12-26 Method for measuring trace hydrogen or trace oxygen

Publications (1)

Publication Number Publication Date
CN111007031A true CN111007031A (en) 2020-04-14

Family

ID=70118937

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911365247.2A Pending CN111007031A (en) 2019-12-26 2019-12-26 Method for measuring trace hydrogen or trace oxygen

Country Status (1)

Country Link
CN (1) CN111007031A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
Title
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 *
汪涛 等: "《纳米与化学》", 30 April 2018, 苏州大学出版 *
钟秦 等: "《化工原理 第4版》", 30 September 2019, 国防工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
Kamieniak et al. The latest developments in the analytical sensing of methane
CN108717106A (en) The device and its detection method of total sulfur content in a kind of detection natural gas
Langenberg et al. Determination of binary gas-phase diffusion coefficients of unstable and adsorbing atmospheric trace gases at low temperature–arrested flow and twin tube method
US20040180448A1 (en) Analytical sensitivity enhancement by catalytic transformation
JP2004511797A (en) Improved detection method of carbon monoxide by infrared absorption spectroscopy
Kaiser et al. Intercomparison of Hantzsch and fiber-laser-induced-fluorescence formaldehyde measurements
CN111007031A (en) Method for measuring trace hydrogen or trace oxygen
Chen et al. Solvent effects on chemical composition and optical properties of extracted secondary brown carbon constituents
Geiger et al. Trace analysis of specialty and electronic gases
CN112415059A (en) Sensing device, detection device and detection method for hydrogen concentration in mixed gas
Wang et al. Cavity-Enhanced Raman Spectroscopy for Detection of Trace Gaseous Impurities in Hydrogen for Fuel Cells
Løkken Water vapour measurements in natural gas in the presence of ethylene glycol
Persijn Purity analysis of gases used in the preparation of reference gas standards using a versatile OPO-based CRDS spectrometer
Hjorth et al. Reaction between nitrate radical and formaldehyde in air: a determination of the rate constant at 295.+-. 2 K
CN208255220U (en) The device of total sulfur content in a kind of detection natural gas
CN216117321U (en) Full-range methane detection device for leakage quantification
CN106841530A (en) Solid engines state monitoring apparatus based on chemical atmosphere sensor
CN112824875A (en) Method for detecting ultraviolet differential nitrogen dioxide gas
CN114441505B (en) Water vapor in-situ calibration device for Raman probe, calibration method and application
CN114166920B (en) Method and system for measuring concentration of gaseous nitrous acid in ambient atmosphere
Yun et al. Infrared absorption properties analysis of dissolved gases in transformer oil
Guo et al. Effects of nitrogen dioxide and carbon monoxide on the determination of sulfur dioxide by flue gas analyzer
Alage et al. A Nitrate Ion Chemical Ionization Atmospheric Pressure interface Time-of-Flight Mass Spectrometer (NO 3− ToFCIMS): calibration and sensitivity study
CN117288827A (en) N is measured based on chemical ionization mass spectrometer 2 O 5 Calibration device system and calibration method thereof
Craig et al. Tunable diode laser absorption spectrometer for detection of hydrogen fluoride gas at ambient pressure

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20200414

RJ01 Rejection of invention patent application after publication