| ^1HNMR双内标法测定2,4-DNT标准物质中的有机杂质 |
| |
| 引用本文： | 王民昌,张皋,徐敏,栾洁玉,陈智群,李遵来,齐珠钗. ^1HNMR双内标法测定2,4-DNT标准物质中的有机杂质[J]. 化学分析计量, 2012, 21(3): 52-55 |
| |
| 作者姓名： | 王民昌 张皋 徐敏 栾洁玉 陈智群 李遵来 齐珠钗 |
| |
| 作者单位： | 西安近代化学研究所,西安,710065 |
| |
| 摘 要： | 利用^1HNMR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O．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。
|
| 关 键 词： | ^1HNMR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 |
Quantification of the Organic Impurities in Reference Material 2,4-DNT by Double Internal Standards of 1H NMR |
| |
| Wang Minchang , Zhang Gao , Xu Min , Luan Jieyu , Chen Zhiqun , Li Zunlai , Qi Zhuchai. Quantification of the Organic Impurities in Reference Material 2,4-DNT by Double Internal Standards of 1H NMR[J]. Chemical Analysis And Meterage, 2012, 21(3): 52-55 |
| |
| Authors: | Wang Minchang Zhang Gao Xu Min Luan Jieyu Chen Zhiqun Li Zunlai Qi Zhuchai |
| |
| Affiliation: | (Xi’an Modern Chemistry Research Institute,Xi’an 710065,China) |
| |
| Abstract: | 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 CCl4 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. |
| |
| Keywords: | quantification of 1H NMR reference material of 2,4-DNT double internal standards 1,1,2,2-tetrachloroethane hexamethyldisiloxane |
| 本文献已被 CNKI 维普 万方数据 等数据库收录！ |
|
