作者：李志昂1, 阮俊2, 王潇1, 王凯1, 刘仁红1, 周鑫1
作者单位：1. 中国测试技术研究院，四川 成都 610021;
2. 云南省计量测试技术研究院，云南 昆明 650228
关键词：磷化氢;气体标准物质;火焰光度气相色谱法;傅里叶变换红外光谱法;F-检验;t-检验
摘要：
针对微量磷化氢气体标准物质难以制备且定值不准确的难题，采用称量法制备10–6级氮中磷化氢气体标准物质，并建立测定微量磷化氢气体的火焰光度气相色谱法和傅里叶变换红外光谱法。分别对两种分析方法的测量重复性（相对标准偏差）、线性及测定下限进行比对研究，采用统计学原理F-检验法和t-检验法检验两种方法表明不存在显著性差异（系统误差）。选择性能较优的火焰光度气相色谱法考察磷化氢气体标准物质制备过程的一致性等实验，结果显示研制的磷化氢气体标准物质量值准确、一致性良好。
Study on preparation and analysis method of trace phosphine gas reference material in nitrogen
LI Zhiang1, RUAN Jun2, WANG Xiao1, WANG Kai1, LIU Renhong1, ZHOU Xin1
1. National Institute of Measurement and Testing Technology, Chengdu 610021, China;
2. Yunnan Institute of Metrology and Testing Technology, Kunming 650228, China
Abstract: In view of the difficulty of preparing trace phosphine gas reference material and the inaccurate value, the phosphine gas reference material in nitrogen in grade 10–6 was prepared by gravimetric method, along with the flame photometric gas chromatography and Fourier transform infrared spectrometry were established for the determination of trace phosphine gas. In the experiment, the repeatability (relative standard deviation, RSD), linearity and lower limit of measurement of the two methods were compared. The F-test method and t-test method of statistical principle were used to judge that there was no significant difference between the two methods. Through the established flame photometric gas chromatography, the consistency of the preparation process and other evaluations were investigated, the results showed that the quality value of the prepared phosphine gas reference material was accurate and the consistency was good.
Keywords: phosphine;gas reference material;flame photometric gas chromatography;Fourier transform infrared spectrometry;F-test;t-test
2022, 48(4):61-67 收稿日期: 2021-09-27;收到修改稿日期: 2021-10-30
基金项目: 云南省质量技术监督局科技计划项目（2017ynzjkj02）
作者简介: 李志昂（1989-），男，山东嘉祥县人，助理研究员，硕士，主要从事气体分析标准化研究及气体标准物质研发
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