分析测试学报2017，Vol.36Issue(3)：414-417,4.DOI:10.3969/j.issn.1004-4957.2017.03.021
定量核磁法测定CL-20标准物质中有机杂质的含量
Determination of Organic Impurity in Reference Materials CL-20 by Quantitative Nuclear Magnetic Resonance(qNMR)
摘要
Abstract
A quantitative nuclear magnetic resonance(qNMR) method was established for the determination of the organic impurities contents in the reference material hexanitrohexaazaisowurtzitane(CL -20).The main impurities in the reference material were confirmed to be ethyl acetate and monoacetylpentanitrohexaazais-owurtzitane (MPIW) by analyzing the NMR spectrum.Hexamethyldisiloxane in CC14 solution with its NMR peak of δ 0.06 was selected as the internal standard which was added into the CL-20 in acetone-d6 solution without tetramethylsilane (TMS).After investigating the effect of delay time (D1) and number of sampling(NS) on quantitative NMR experiments,the experimental parameters were chosen with D1 of 20 s and NS of 32.Using the optimized experiment parameters,it was found that the contents of ethyl acetate and MPIW were 0.035 16％ and 0.156 2％,with RSDs of 0.91％ and 0.86％,respectively.关键词
定量核磁共振/核磁共振氢谱/六硝基六氮杂异伍兹烷(CL-20)/有机杂质Key words
quantitative nuclear magnetic resonance(qNMR)/1 H NMR/CL-20/organic impurity分类
数理科学引用本文复制引用
刘可,王民昌,徐敏,张丽涵,张皋,陈智群..定量核磁法测定CL-20标准物质中有机杂质的含量[J].分析测试学报,2017,36(3):414-417,4.基金项目
国家自然科学基金国际(地区)合作与交流项目(5151130036) （地区）
