负压进样-气相色谱法测定氢气体系中痕量气体组分  

Determination of Trace Gas Components in Hydrogen System by Gas Chromatography with Sub-Atmospheric Sampling

作　　者：祝刘正 吴展华[1] 杨小军 陈帅 王淑敏 占鑫星 任英[1] 韩国强 ZHU Liuzheng;WU Zhanhua;YANG Xiaojun;CHEN Shuai;WANG Shumin;ZHAN Xinxing;REN Ying;HAN Guoqiang(China Institute of Atomic Energy,Beijing 102413,China)

机构地区：[1]中国原子能科学研究院,北京102413

出　　处：《理化检验（化学分册）》2022年第3期275-278,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：以氢气体系样品为研究对象,采用负压进样方式,分析样品前,对整个进样管道进行吹扫清洗3次,再抽真空。以阀进样方式调节样品的进样压力,采用附氦离子化检测器气相色谱法测定其中氧气、氮气、一氧化碳、甲烷的含量。结果表明,进样压力在10 100~101 225 Pa内与各气体组分对应的峰面积呈线性关系,4种气体组分的检出限(3S/N)依次为4.0,3.8,5.2,3.6 nmol·mol^(-1)。对一组混合标准气体平行测定6次,其峰面积的相对标准偏差为0.011%~0.72%。对另一组混合标准气体进行测定,测定值与已知值相符。此外,负压进样方式的样品用量仅为常(正)压进样的1/4 200,测定过程总耗时仅为常(正)压进样方式的1/3。The sample of hydrogen system was taken as the investigation object, and sub-atmospheric sampling was used. Before analyzing the sample, the whole injection pipeline was purged and cleaned 3 times, and then kept in vacuum. The injection pressure of the sample was adjusted by valve injection, and oxygen, nitrogen, carbon monoxide, methane were determined by gas chromatography with helium ionization detector. As shown by the results, linear relationships between injection pressure of the sample and values of peak area of 4 components were kept in the range of 10 100-101 225 Pa, with detection limits(3 S/N) of 4.0, 3.8, 5.2, 3.6 nmol·mol^(-1), respectively. A set of mixed standard gas were analyzed 6 times in parallel by the proposed method, with RSDs of values of peak area in the range of 0.011%-0.72%. Another set of mixed standard gas were analyzed by the proposed method, and the determined values were in accordance with the known values. In addition, the sample amount of sub-atmospheric sampling was only 1/4 200 of that of normal(positive)-atmospheric sampling, and the total time consuming of determination process was only 1/3 of that of normal(positive)-atmospheric sampling.

关 键 词：气相色谱法 负压进样 氦离子化检测器 气体组分 

分 类 号：O657.7[理学—分析化学]