5种多溴联苯纯度定值的核磁法研究及不确定度评定  

Study on purity determination of five polybrominated biphenyls using quantitative NMR with uncertainty assessment

作　　者：李娅 邵明武[2] 黄挺[2] 朱翔 任昀 LI Ya;SHAO Ming-wu;Huang Ting;ZHU Xiang;REN Yun(The Hunan Institute of Metrology and Testing,Changsha 410014;Division of Metrology in Chemistry,National Institute of Metrology,Beijing 100029)

机构地区：[1]湖南省计量检测研究院,长沙140014 [2]中国计量科学研究院,北京100029

出　　处：《分析试验室》2018年第12期1393-1397,共5页Chinese Journal of Analysis Laboratory

基　　金：国家重点基础专项(2016YFF0201102)资助

摘　　要：建立了5种多溴联苯(PBB-15,PBB-26,PBB-30,PBB-31,PBB-49)纯度的核磁定值方法。采用安赛蜜为内标,以氘代丙酮和氘代二甲亚砜混合溶液(1:3,V/V)作为溶剂,采取不积卫星峰方式对样品进行1H NMR谱图进行分析,并对仪器参数进行优化,测得5种多溴联苯纯度分别为:99.14%,99.13%,99.23%,99.11%,98.17%,且RSD均小于0.15%,与质量平衡法定值结果一致。对5种纯品定量核磁法引入的不确定度进行系统评定,其合成相对标准不确定度均不超过0.35%。A quantitative nuclear magnetic resonance( qNMR) method was established for purity determination of five types of polybrominated biphenyls( PBB-15,PBB-26,PBB-30,PBB-31 and PBB-49). The selection of internal standard, solvents and quantitative peak were investigated.Without integral of satellite peak,the qNMR detection was analyzed using acesulfame as internal standard substance and the mixture of deuterated acetone and deuterated dimethylsulfoxide( Vd-Acetone/Vd-DMSO= 1: 3) as solvent. The detection conditions of q NMR for five polybrominated biphenyls were optimized and the purity results were 99. 14%, 99. 13%, 99. 23%, 99. 11% and 98. 17%,respectively. The results were in accordance with the result of mass balance method with the RSD value less than 0. 15%. Meanwhile,the results of systematic uncertainty assessment for quantitative NMR was 0. 35% at most.

关 键 词：多溴联苯 溴化阻燃剂 标准物质 定量核磁 质量平衡法 

分 类 号：O657.2[理学—分析化学]