School of Chemical Engineering and the Environment, Beijing Institute of Technology, Beijing 10081, China.
Xi'an Modern Chemistry Research Institute, Xi'an, Shaanxi 710065, China.
Anal Methods. 2022 Aug 25;14(33):3203-3208. doi: 10.1039/d2ay00770c.
A novel qNMR method was developed for the simultaneous determination of the component ratio and moisture content in triethyleneglycol dinitrate (TEGDN) and nitroglycerin (NG) composites. Using the ERETIC module technique of NMR spectrometry, moisture in the solvent and internal standard were eliminated by the integral value subtraction method, and the component ratio and moisture content in TEGDN/NG composites could be accurately calculated. Method validation was carried out in terms of the precision, stability, linearity, recovery, robustness, limit of quantification (LOQ) and limit of detection (LOD). The results of the qNMR method show good accuracy compared with the HPLC and Karl Fischer methods. Statistical Student's -test and -test at the 95% confidence level proved that there was no significant difference between the qNMR method and the other two methods. For TEGDN/NG composites of high-energy and high-sensitivity explosives, the low dose and high efficiency of the qNMR method could effectively avoid the danger of explosion and burning.
一种新的 qNMR 方法被开发用于同时测定三乙二醇二硝酸酯(TEGDN)和硝化甘油(NG)复合材料的组成比和水分含量。利用 NMR 光谱的 ERETIC 模块技术,通过积分值减法方法消除溶剂和内标中的水分,可准确计算 TEGDN/NG 复合材料的组成比和水分含量。该方法通过精密度、稳定性、线性、回收率、稳健性、定量限(LOQ)和检测限(LOD)进行了验证。qNMR 方法的结果与 HPLC 和卡尔费休法相比具有良好的准确性。在 95%置信水平下的统计学生 t 检验和 t 检验证明,qNMR 方法与其他两种方法之间没有显著差异。对于高能和高灵敏度炸药的 TEGDN/NG 复合材料,qNMR 方法的低剂量和高效率可以有效地避免爆炸和燃烧的危险。