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、GCFID和GC-μECD3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-μECD。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%。
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%.
作者
黄林艳
赵彦辉
赵亚娴
鲁炳闻
杨刚
刘海萍
房丽萍
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)
出处
《中国测试》
CAS
北大核心
2018年第11期127-134,共8页
China Measurement & Test
基金
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)。
关键词
标准样品
多氯联苯
纯度
不确定度
气相色谱法
reference materials
polychlorinated biphenyls
purity
uncertainty
gas chromatography
