^1HNMR双内标法测定2,4-DNT标准物质中的有机杂质  

Quantification of the Organic Impurities in Reference Material 2,4-DNT by Double Internal Standards of ^1HNMR

作　　者：王民昌[1] 张皋[1] 徐敏[1] 栾洁玉[1] 陈智群[1] 李遵来[1] 齐珠钗[1] 

机构地区：[1]西安近代化学研究所,西安710065

出　　处：《化学分析计量》2012年第3期52-55,共4页Chemical Analysis And Meterage

摘　　要：利用1H NMR确定了2,4-DNT标准物质中的有机杂质为乙醇,根据化合物的核载量定义,采用不含四甲基硅烷(TMS)的氘代丙酮为溶剂,将1,1,2,2-四氯乙烷与六甲基二硅醚的四氯化碳标准溶液加入待测液中作为双内标,用乙醇的甲基质子峰为定量峰对其含量进行了测定。双内标法测定结果分别为0.075%,0.074%,标准偏差分别为0.005,0.006,t检验证实该结果与色谱法定值结果一致。该方法专属、准确、简便、快速,适用于标准物质中有机杂质的测定。One kind of organic impurities in reference material 2,4-DNT was identified as ethanol by ^1H NMR. 1,1,2,2-tetrachloroethane and hexamethyldisiloxane of CC14 solution were added to 2,4-DNT of acetone-d6 solution without tetramethylsilane（TMS） as double internal standards. The quantitative analysis of the impurity ethanol was achieved by measuring the selected methyl proton peak intensity, according to the nucleus-carrying mass（NCM） of every component. It was found that the content of ethanol were 0.075%,0.074%, and RSD were 0.005,0.006 respectively, which were accordant with that of the gas chromatography by t test. The method is specificity, accurate, simple, rapid and suitable for the quantitative determination of the organic impurities in reference material content.

关 键 词：1H NMR定量 2 4-DNT标准物质 双内标 1 1 2 2-四氯乙烷 六甲基二硅醚 

分 类 号：O657.1[理学—分析化学]