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)

作　　者：刘可[1,2] 王民昌[1,2] 徐敏[1,2] 张丽涵[1,2] 张皋[1,2] 陈智群[1,2] LIU Ke WANG Min-chang XU Min ZHANG Li-han ZHANG Gao CHEN Zhi-qun(Xi＇an Modern Chemistry Researeh Institure, Xi＇an 710065, China State Key Laboratory of Fluorine ＆ Nitrogen Chemicals, Xi＇an 710065, China)

机构地区：[1]西安近代化学研究所,陕西西安710065 [2]氟氮化工资源高效开发与利用国家重点实验室,陕西西安710065

出　　处：《分析测试学报》2017年第3期414-417,共4页Journal of Instrumental Analysis

基　　金：国家自然科学基金国际(地区)合作与交流项目(5151130036)

摘　　要：采用定量核磁共振波谱法(qNMR)测定六硝基六氮杂异伍兹烷(CL-20)标准物质中有机杂质的含量。核磁谱图解析证明,主要有机杂质成分为残余溶剂乙酸乙酯和中间体五硝基-乙酰基六氮杂异伍兹烷(MPIW),以不含四甲基硅烷(TMS)的氘代丙酮为溶剂,将六甲基二硅醚的四氯化碳标准溶液加入待测液中作为内标,以其谱峰(δ=0.06)作为内标峰对两种有机杂质进行定量分析。考察了延迟时间和采样次数对准确定量的影响,结果显示为确保定量结果的准确性,延迟时间D_1应不小于20 s,采样次数为32次。采用优化后的实验参数进行纯度分析,测得CL-20标准物质中有机杂质乙酸乙酯和MPIW的质量分数分别为0.03516%和0.156 2%,相对标准偏差(RSD)分别为0.91%和0.86%。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 CCl4 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 

分 类 号：O482.532[理学—固体物理] TQ564.42[理学—物理]