1. 西安近代化学研究所
2. 氟氮化工资源高效开发与利用国家重点实验室
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刘可, 王民昌, 徐敏, 等. 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.
Determination of Organic Impurity in Reference Materials CL-20 by Quantitative Nuclear Magnetic Resonance(qNMR)[J]. 2017,36(3):414-417.
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D1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0.035 16%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.
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
quantitative nuclear magnetic resonance(qNMR)1H NMRCL-20organic impurity
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