四溴双酚A中有机杂质测量及不确定度评估  

Measurement of Organic Impurities in Tetrabromobisphenol A and Evaluation of Measurement Uncertainty

作　　者：刘思[1,2] 彭子娟 万康妮 李彭辉 宋善军[2] LIU Si;PENG Zijuan;WAN Kangni;LI Penghui;SONG Shanjun(Tianjin University of Technology,Tianjin 300384,China;National Institute of Metrology,Beijing 100029,China;Beijing University of Chemical Technology,Beijing 100029,China)

机构地区：[1]天津理工大学,天津300384 [2]中国计量科学研究院,北京100029 [3]北京化工大学,北京100029

出　　处：《计量科学与技术》2023年第6期54-62,共9页Metrology Science and Technology

基　　金：国家自然科学基金项目(21806158);中国计量科学研究院基本科研业务费项目(AKY1720)。

摘　　要：为更好的满足有机纯度标准物质中有机杂质的准确测量需求,以常见溴代阻燃剂——四溴双酚A为例,通过面积归一法及标准曲线法,测量了其主要有机杂质——三溴双酚A的含量并进行了不确定度评估。此外,进一步采用定量核磁技术对该杂质的含量进行了测量,通过数据比较可知,面积归一法测得的杂质含量为0.70%,引入的不确定度为0.04%;标准曲线法测得的杂质含量为1.16%,引入的不确定度为0.09%。二者合成后的纯度为0.93%,不确定度为0.24%,该结果可覆盖定量核磁法测量结果(0.76%,不确定度0.03%)。综上,在实际定值工作中,当面积归一法和标准曲线法产生较大差异时(>0.1%),可采用二者合成的结果作为杂质含量测量值,以保证测量结果的准确性。To ensure accurate determination of organic impurities in certified reference materials for organic purity,we studied the brominated flame retardant tetrabrombisphenol A(TBBPA).Using the area normalization and standard curve methods,we quantified its primary organic impurity,tribromobisphenol A,and evaluated the associated uncertainties.Additionally,the impurity's content was measured using quantitative nuclear magnetic resonance(qNMR).The impurity levels derived from the area normalization and standard curve methods were 0.70%±0.04%and 1.16%±0.09%,respectively.A combined purity estimate yielded 0.93%±0.24%,encompassing the qNMR result of 0.76%±0.03%.When significant discrepancies(>0.1%)arise between the area normalization and standard curve methods,their combined result can be adopted to guarantee the accuracy of the measurement.

关 键 词：计量学 四溴双酚A 有机杂质测量 不确定度评估 面积归一法 标准曲线法 定量核磁法 

分 类 号：TB99[一般工业技术—计量学]