【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0.03516%和0.156 2%,相对标准偏差（RSD）分别为0.91%和0.86%。更多还原

【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 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.更多还原