作者：黄林艳, 赵彦辉, 赵亚娴, 鲁炳闻, 杨刚, 刘海萍, 房丽萍
作者单位：国家环境保护污染物计量和标准样品研究重点实验室 环境保护部标准样品研究所, 北京 100029
关键词：标准样品;多氯联苯;纯度;不确定度;气相色谱法
摘要：
为保证环境监测过程中使用的标准样品量值准确，需要对其原料纯度进行测定。分别使用GC-MS、GC-FID和GC-ECD3 种具有不同检测器的气相色谱法，对7种指示性多氯联苯（PCBs）纯品纯度进行测定，采用峰面积归一化法计算纯度，并对纯度不确定度进行评定。结果显示，PCBs纯品中的主要杂质均为具有不同氯取代数或取代位的PCBs同类物。GC-MS法测得的PCBs纯度值与标称值最接近，不同方法测得的纯品纯度值大小关系基本为：GC-MS GC-FID GC-ECD。纯度不确定度采用不同测定方法不确定度的合成，合成标准不确定度为0.40%~4.42%。
Purity comparison of indicative PCBs determined by gas chromatographic methods
HUANG Linyan, ZHAO Yanhui, ZHAO Yaxian, LU Bingwen, YANG Gang, LIU Haiping, FANG Liping
Institute for Environmental Reference Materials of Ministry of Environmental Protection, State Environmental Protection Key Laboratory of Environmental Pollutant Metrology and Reference Materials Study, Beijing 100029, China
Abstract: In order to ensure the accurate value of the environmental reference material (RM) used in environmental monitoring, it is necessary to determine the purity of the RM raw material. The purities of 7 indicative polychlorinated biphenyls (PCBs) pure materials were determined by GC-MS, GC-FID and GC-μECD, respectively, and were calculated based on area normalization method. Furthermore, the purity uncertainties were evaluated. The results showed that the main impurities of the 7 indicative PCBs were PCBs or structural analogues with the same or similar number of chlorine substitutions and different substitution positions. The purity values of PCBs measured by GC-MS were the closest to the labelled values, and the relation of purity values measured by different methods was basically as follows: GC-MS > GC-FID > GC-μECD. The uncertainties of 7 indicative PCBs purity were synthesized by the uncertainties of different methods, which were between 0.40% and 4.42%.
Keywords: reference materials;polychlorinated biphenyls;purity;uncertainty;gas chromatography
2018, 44(11): 127-134 收稿日期: 2018-08-03;收到修改稿日期: 2018-09-05
基金项目: 国家环境保护标准制修订项目（2017-31）；环境保护部环境发展中心重点实验室开放课题项目（ZDSY-2018-02）
作者简介: 黄林艳(1987-),女,江西抚州市人,工程师,博士,主要从事环境分析与标准样品相关研究
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