岩矿测试2013，Vol.32Issue(2)：334-339,6.
质量平衡法分析1,2,3,4-四氯苯的纯度分析与不确定度评定
Analysis of Purity and Uncertainty for 1, 2, 3, 4-Tetrachlorobenzene with the Mass Balance Method
摘要
Abstract
A traceable method is presented, to study the purities of certified reference material of 1,2,3,4-tetrachlorobenzene with the assessment of uncertainties. The purities of 1, 2, 3, 4-tetrachlorobenzene were determined by the mass balance method. The qualitative analysis of main non-volatile impurities was identified as 1,2,3 ,5-tetrachlorobenzene with Gas Chromatography-Mass Spectrometry (GC-MS) and standard addition. The quantitative analysis for the impurities was measured by Gas Chromatography-Flame Ionization Detector (GC-FID). The content of water and ash in 1 ,2,3,4-tetrachlorobenzene were respectively measured by Karl-Fischer titrator and ignited at 900 °C in a muffler roaster. The residuals of solvent were confirmed as ethyl ether by Headspace Gas Chromatography-Mass Spectrometry. The certified result with the mass balance method was 98. 79% and the expanded uncertainty was 0. 20% (k =2). The good homogeneity result in the 95% confidence interval was validated by F-test and t-test statistical methods with samples from 500 different bottles. The stability inspection was carried out on short-term ( one month) and long-term ( 12 months) tests, and the results indicate that the stability period for 1 ,2,3,4-tetrachlorobenzene of storage is no less than 12 months at 20℃.关键词
质量平衡法/1,2,3,4-四氯苯/标准物质/纯度分析/不确定度评定Key words
mass balance method/ 1,2,3,4-tetrachlorobenzene/ certified reference materials/ purity analysis/ uncertainty evalution分类
化学化工引用本文复制引用
马康,杨冉,王海峰,何雅娟,刘菲..质量平衡法分析1,2,3,4-四氯苯的纯度分析与不确定度评定[J].岩矿测试,2013,32(2):334-339,6.基金项目
科技基础性工作专项计划项目(2008FY130200) （2008FY130200）
水体污染控制治理科技重大专项(2009ZX07420-008-02) （2009ZX07420-008-02）
