摘要
对不同底气中微量CO,CO2和CH4进行定量分析。考察了在HayeSep D,Porapak Q和5A分子筛色谱柱上,不同底气中2μmol/mol的CO,CO2和CH4在气相色谱氢火焰离子化检测器(FID)上的响应值,并且对这3种气体在不同色谱柱上的出峰情况进行了讨论。选择氮气为底气的混合气作为标准,分别对氢气,氩气和氦气为底气的混合气进行校准,比较不同底气相同浓度的3种气体在FID上校准值和重量值的相对偏差。在5A分子筛柱上,以氢气为底气的混合气中一氧化碳和甲烷的校准偏差分别为-19%和-20%;在Porapak Q柱上,以氢气为底气的混合气中二氧化碳和甲烷的校准偏差小于1.0%。当采用以氮气为底气的混合气校准氦气、氩气、氢气为底气的混合气时,在5A分子筛柱上,以氢气为底气的一氧化碳和甲烷校准偏差最大。该方法具有良好的重复性和准确度,适用于高纯气体中常见杂质的测定。
Trace CO,CO2 and CH4 in different matrix gases was quantitative analysis.The response values of carbon monoxide,carbon dioxide and methane mixtures of 2μmol/mol in different matrix gases on HayeSep D,Porapak Q and 5A molecular sieve column on gas chromatography with hydrogen flame ionization detector(FID)were investigated.Also,situation of the peaks on different chromatographic columns were discussed.Using the mixture gas in nitrogen as standard,hydrogen,argon and helium as the matrix gases was calibrated respectively.The relative standard deviation of calibration values and gravimetric values of the three gases with the same concentration of different matrix gases on FID were compared.The experimental results show that on 5A molecular sieve column,the calibration deviations of carbon monoxide and methane in the mixture with hydrogen as the matrix gas were-19%and-20%,respectively.On the Porapak Q column,the calibration deviation of carbon dioxide and methane in the mixture with hydrogen as the matrix gas was less than 1.0%.The experimental results show that when the mixture of helium,argon and hydrogen was used to calibrate the mixture of helium,argon and hydrogen,the deviation of carbon monoxide and methane on 5A molecular sieve column was the largest.The method has good repeatability and accuracy and is suitable for the determination of common impurities in high purity gases.
作者
刘雨佳
李增和
胡树国
Liu Yujia;Li Zenghe;Hu Shuguo(Beijing University of Chemical Technology,Beijing 100013,China;National Institute of Metrology,Beijing 100029,China)
出处
《化学分析计量》
CAS
2019年第6期16-19,共4页
Chemical Analysis And Meterage
基金
国家重点研发计划课题“氢燃料电池用高纯氢标准物质的研制及检测技术研究”(2018YFF0212904)
关键词
氢火焰离子化检测器
一氧化碳
二氧化碳
甲烷
底气
hydrogen flame ionization detector
carbon monoxide
carbon dioxide
methane
matrix gases.
