CN107014940A - Rapid analysis method when carbon monoxide, carbon dioxide and nitrous oxide coexist - Google Patents

Rapid analysis method when carbon monoxide, carbon dioxide and nitrous oxide coexist Download PDF

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Publication number
CN107014940A
CN107014940A CN201710320390.4A CN201710320390A CN107014940A CN 107014940 A CN107014940 A CN 107014940A CN 201710320390 A CN201710320390 A CN 201710320390A CN 107014940 A CN107014940 A CN 107014940A
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gas
temperature
mixture body
normal mixture
detector
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王锦花
付文芳
王平
吴明红
欧阳应根
肖松涛
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/64—Electrical detectors
    • G01N30/66—Thermal conductivity detectors

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

Rapid analysis method when being coexisted the invention provides a kind of carbonoxide, carbon dioxide and nitrous oxide, i.e., with gas chromatography associated with shincarbon T packed columns and thermal conductivity detector (TCD), while Analysis for CO, CO2And N2O.Carrier gas is hydrogen, and flow is 30 ml/min.The room temperature that gasifies is 100 DEG C, and detector temperature is 100 DEG C, column temperature：Temperature programming, initial temperature：100 DEG C, retention time：7min；Heating rate：35 DEG C/min, final temperature：220℃；Retention time：1min.CO and CO2Lowest detection volume fraction be 1.00 × 10‑3, N2O lowest detection volume fraction is 3 × 10‑3。CO、CO2And N2The standard relative deviation of O analysis is respectively 2.0,3.1 and 2.6%.It is short and simple to operate the time required to this method.

Description

Rapid analysis method when carbon monoxide, carbon dioxide and nitrous oxide coexist
Technical field
The present invention relates to CO, CO2And N2Rapid analysis method when O coexists.
Background technology
With the fast development of China's Nuclear Electricity, the spentnuclear fuel that nuclear power station is produced will be more and more, spentnuclear fuel post processing Can China's Nuclear Electricity is related to sustainable development.Hydroxy amino urea（HSC）Be it is a kind of be expected to be used for spentnuclear fuel post processing it is new The salt-free reducing agent of type.In spentnuclear fuel post processing flow, reducing agent coexists with nitric acid.HSC is the reducing agent of moderate strength, Nitric acid has certain oxidisability, and there may be CO, CO with nitric acid reaction by HSC2And N2O, these materials may influence spentnuclear fuel The normal operation of flow is post-processed, therefore, it is necessary to these gaseous products of qualitative and quantitative analysis, this relates to CO, CO2And N2O coexists When analysis method.Once there is document*Reported with gas chromatography while Analysis for CO, CO2And N2O (including O2、NO、NO2With C3H6), this method uses Ni catalytic converters by CO, CO2Methane is converted into, is then analyzed again.This method need to reequip gas phase Chromatograph, then, using 5A molecular sieves, 10%OV-101/Chromosorb W, GDX-502 and four kinds of packed columns of silicagel column, is adopted Analyzed with two kinds of detectors of hydrogen flame ionization detector and electron capture detector, system is extremely complex.The present invention is used Gas chromatography associated with shincarbon T packed columns and thermal conductivity detector (TCD) is while Analysis for CO, CO2And N2O, system is simple, behaviour Facilitate.
The content of the invention
The present invention provides a kind of while quick Analysis for CO, CO2And N2O new method, i.e., with shincarbon T packed columns and Gas chromatography associated with thermal conductivity detector (TCD) is while quick Analysis for CO, CO2And N2O.CO and CO2Lowest detection volume fraction be 1.00×10-3, N2O lowest detection volume fraction is 3 × 10-3。 CO、CO2And N2The standard relative deviation difference of O analysis For 2.0,3.1 and 2.6%.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of CO, CO2And N2Analysis method when O coexists, it is characterised in that this method has following process and step：
A. by CO, CO2And argon gas is with 5:5:90 volume ratios are mixed as normal mixture body 1, by N2O and nitrogen are with 3：97 volumes Than mixing as normal mixture body 2；
B. using gas chromatography associated with shincarbon T packed columns and thermal conductivity detector (TCD)；By shincarbon T packed columns Correctly it is fitted into gas chromatograph, and is passed through hydrogen, adjusts its flow for 30 ml/min, after 20min, set column temperature as 100 DEG C, temperature of vaporization chamber is set as 100 DEG C, and detector temperature is 100 DEG C；
C. column temperature is worked as, vaporizer when detector all reaches 100 DEG C, sets bridge stream as 120mA, column temperature is temperature programming, initial temperature： 100 DEG C, retention time：7min；Heating rate：35 DEG C/min, final temperature：220℃；Retention time：1min；
D. Data Processing in Chromatography Workstation power supply is opened, computer is opened, into the station that works online, thermal conductivity detector (TCD) passage, input is selected Appropriate word and parameter；Select " data acquisition ", return to zero, walk baseline；
E. when baseline is steady, draw standard mixed gas 1 and normal mixture body 2 respectively, and it is rapidly injected gas chromatograph, The RPB and " startup " button of respective channel are pressed simultaneously；
F. after sampling analysis terminates, stopping sampling button is pressed；The peak area of certain gas is obtained from chromatogram, you can draw out The peak area of three kinds of gas-normal mixture body volume relationship figure, i.e., the standard working curve of three kinds gas；
G. under the same conditions, under test gas sample is injected, the peak area of certain gas is found out from chromatogram, then, from it Standard working curve checks in corresponding volume, the volume of this kind of gas in sample size and normal mixture body further according to sample Fraction, so that it may calculate the volume fraction of certain gas contained by sample.
The method have the advantages that：In 20 minutes, while Analysis for CO, CO2And N2O, the degree of accuracy is high, and simple to operate.
Brief description of the drawings
Fig. 1 is normal mixture body 1（Containing CO, CO2Deng）Gas chromatogram.In figure, abscissa is the time（Point）, indulge and sit It is designated as response（mV）.CO retention time is 4.35 min, CO2Retention time be 11.64 min.
Fig. 2 is with normal mixture body 2（Containing N2O etc.）Gas chromatogram.In figure, abscissa is the time（Point）, indulge and sit It is designated as response（mV）.N2O retention time is 14.63 min.
Fig. 3 is the Typical gas chromatograph figure for the gaseous sample that HSC-6M salpeter solutions place certain time generation.It is horizontal in figure Coordinate is the time（Point）, ordinate is response（mV）.The chromatogram of this figure and normal mixture body is compared and understood：Gas sample There is CO in product2And N2O, but without CO.
Fig. 4 be different temperatures under, 0.2M HSC-6M salpeter solutions produce CO2Volume fraction and the graph of a relation of time, Abscissa is the time, and unit is " hour ", and ordinate is the CO produced2Volume fraction, unit be " 10-2”.It is different bent in figure Line represented under different temperatures, the CO that 0.2M HSC-6M salpeter solutions are produced2Volume fraction and the relation of time.
Fig. 5 be different temperatures under, 0.2M HSC-6M salpeter solutions produce N2O volume fraction and the graph of a relation of time, Abscissa is the time, and unit is " hour "；Ordinate is the N produced2O volume fraction, unit is " 10-2”.It is different bent in figure Line represented under different temperatures, the N that 0.2M HSC-6M salpeter solutions are produced2O volume fraction and the relation of time.
Embodiment
After now the specific embodiment of the present invention is described in.
Embodiment 1：Referring to Fig. 1-Fig. 5, the present embodiment is comprised the following steps that：
（1）Calibrating gas is got out first, containing CO and CO2Deng for normal mixture body 1, containing N2O etc. for normal mixture Body 2；
（2）Shincarbon T packed columns are correctly fitted into gas chromatograph, hydrogen is passed through, its flow are adjusted for 30 ml/ After min, 20min, column temperature is set as 100 DEG C, temperature of vaporization chamber is 100 DEG C, detector temperature is 100 DEG C；
（3）Work as column temperature, vaporizer, when detector all reaches 100 DEG C of design temperature, set bridge stream as 120mA, program liter is set Temperature, initial temperature：100 DEG C, retention time：7min；Heating rate：35 DEG C/min, final temperature：220℃；Retention time：1min；
（4）Data Processing in Chromatography Workstation power supply is opened, computer is opened, into the station that works online, thermal conductivity detector (TCD) passage, input is selected Appropriate word and parameter；Select " data acquisition ", return to zero, walk baseline；
（5）When baseline is steady, draw standard mixed gas 1 and normal mixture body 2 are distinguished with gastight syringe, and quickly note Enter gas chromatograph, while pressing the RPB and " startup " button of respective channel；
（6）After sampling analysis terminates, i.e., after appearance terminates, press stopping sampling button；Subsequently into qualitative analysis and quantitative analysis Stage；Qualitative analysis uses retention time counter point；Quantitative analysis uses appearance method, i.e. quantitative sample injection-working curve method；Institute Quantitative sample injection-the working curve method stated is exactly：Under certain operating conditions, the normal mixture body of certain volume, root are injected According to the peak area of certain component in obtained sample chromatogram figure, peak area-normal mixture body sample introduction spirogram is drawn out, is The standard working curve of certain component；
（7）Under the same conditions, gaseous sample is injected, the peak area of wherein certain component peaks is obtained, then from the standard work of the component The sample size of calibrating gas corresponding thereto is checked in as curve, then by the sampling volume of sample and the component in normal mixture Content in body, you can calculate the volume fraction of certain component contained by sample.

Claims (1)

  1. Rapid analysis method when 1. a kind of carbonoxide, carbon dioxide and nitrous oxide coexist, it is characterised in that this method has There is following process and step：
    A. by CO, CO2And argon gas is with 5:5:90 volume ratios are mixed as normal mixture body 1, by N2O and nitrogen are with 3：97 volumes Than mixing as normal mixture body 2；
    B. using gas chromatography associated with shincarbon T packed columns and thermal conductivity detector (TCD)；By shincarbon T packed columns Correctly it is fitted into gas chromatograph, and is passed through hydrogen, adjusts its flow for 30 ml/min, after 20min, set column temperature as 100 DEG C, temperature of vaporization chamber is set as 100 DEG C, and detector temperature is 100 DEG C；
    C. column temperature is worked as, vaporizer when detector all reaches 100 DEG C, sets bridge stream as 120mA, column temperature is temperature programming, initial temperature： 100 DEG C, retention time：7min；Heating rate：35 DEG C/min, final temperature：220℃；Retention time：1min；
    D. Data Processing in Chromatography Workstation power supply is opened, computer is opened, into the station that works online, thermal conductivity detector (TCD) passage, input is selected Appropriate word and parameter；Select " data acquisition ", return to zero, walk baseline；
    E. when baseline is steady, draw standard mixed gas 1 and normal mixture body 2 respectively, and it is rapidly injected gas chromatograph, The RPB and " startup " button of respective channel are pressed simultaneously；
    After sampling analysis terminates, stopping sampling button is pressed；The peak area of certain gas is obtained from chromatogram, you can draw out three The peak area of kind gas-normal mixture body volume relationship figure, i.e., the standard working curve of three kinds gas；
    Under the same conditions, under test gas sample is injected, the peak area of certain gas is found out from chromatogram, then, from its mark Quasi- working curve checks in corresponding volume, the volume integral of this kind of gas in sample size and normal mixture body further according to sample Number, so that it may calculate the volume fraction of certain gas contained by sample.
CN201710320390.4A 2017-05-09 2017-05-09 Rapid analysis method when carbon monoxide, carbon dioxide and nitrous oxide coexist Pending CN107014940A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110988106A (en) * 2020-03-04 2020-04-10 中国农业科学院农业环境与可持续发展研究所 Nitrous oxide isotope delta15N correction method
CN111239281A (en) * 2020-02-12 2020-06-05 西南石油大学 Improved gas chromatography carrier gas system

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2854595Y (en) * 2005-09-12 2007-01-03 上海华爱色谱分析技术有限公司 Gas chromatograph for analysing tail gas of vehicle
CN101126750A (en) * 2007-09-21 2008-02-20 武汉钢铁(集团)公司 Xenon impurity chromatogram analysis method
CN102495158A (en) * 2011-11-22 2012-06-13 中国科学院地质与地球物理研究所兰州油气资源研究中心 Method for analyzing N2O, CO, CH4 and CO2 in atmosphere with one injection by gas chromatography
WO2014034524A1 (en) * 2012-08-27 2014-03-06 三井金属鉱業株式会社 Exhaust gas purifying catalyst

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2854595Y (en) * 2005-09-12 2007-01-03 上海华爱色谱分析技术有限公司 Gas chromatograph for analysing tail gas of vehicle
CN101126750A (en) * 2007-09-21 2008-02-20 武汉钢铁(集团)公司 Xenon impurity chromatogram analysis method
CN102495158A (en) * 2011-11-22 2012-06-13 中国科学院地质与地球物理研究所兰州油气资源研究中心 Method for analyzing N2O, CO, CH4 and CO2 in atmosphere with one injection by gas chromatography
WO2014034524A1 (en) * 2012-08-27 2014-03-06 三井金属鉱業株式会社 Exhaust gas purifying catalyst

Non-Patent Citations (4)

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RUSSELL N.DIETZ等: "Gas chromatographic determination of nitric oxide on treated molecular sieve", 《ANALYTICAL CHEMISTRY》 *
卢冠等: "O2、CO、CO2、N2O、NO、NO2和C3H6混合气的同时色谱检测", 《华东化工学院学报》 *
曹美秋等: "气相色谱同时测定NO、CO、N2O、CO2", 《环境化学》 *
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111239281A (en) * 2020-02-12 2020-06-05 西南石油大学 Improved gas chromatography carrier gas system
CN110988106A (en) * 2020-03-04 2020-04-10 中国农业科学院农业环境与可持续发展研究所 Nitrous oxide isotope delta15N correction method
CN110988106B (en) * 2020-03-04 2020-06-12 中国农业科学院农业环境与可持续发展研究所 Nitrous oxide isotope delta15N correction method

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Application publication date: 20170804