一缩二乙二醇二硝酸酯中有机杂质的定性和定量分析  

Qualitative and Quantitative Analysis of Organic Impurities in Diethylene Glycol Dinitrate

作　　者：陈爽[1] 康莹[2] 胡银[2] 索志荣[1] 孟俞富 宁艳利[2] CHEN Shuang;KANG Ying;HU Yin;SUO Zhi-rong;MENG Yu-fu;NING Yan-li(School of Materials Science and Engineering,Southwest University of Science and Technology,Mianyang Sichuan 621010,China;Xi′an Modern Chemistry Research Institute,Xi′an 710065,China)

机构地区：[1]西南科技大学材料科学与工程学院,四川绵阳621010 [2]西安近代化学研究所,陕西西安710065

出　　处：《火炸药学报》2019年第5期516-520,I0006,共6页Chinese Journal of Explosives & Propellants

基　　金：国防科工局技术基础科研项目(No.JSJL2014208A006)

摘　　要：为了对含能增塑剂一缩二乙二醇二硝酸酯(DEGDN)中的有机杂质进行定性和定量分析,采用气相色谱-质谱联用法,利用NIST标准质谱库检索、对照品比对以及杂质形成机理分析,对DEGDN中的有机杂质进行定性,然后采用外标法对杂质进行定量。结果表明,在DEGDN中检测到4种有机杂质,杂质1、3、4分别为2-(羟甲基)-1,3-二氧戊环、正癸烷和乙二醇二硝酸酯,杂质2可能为2-羟基-1,4-二氧六环;外标法中各物质线性关系良好,线性相关系数为0.999 5~0.999 9,平均加标回收率为96.72%~103.33%,RSD为0.31%~1.25%,表明该方法精密度和准确度高,可用于DEGDN中有机杂质的检测分析。In order to qualitatively and quantitatively determine the organic impurities in diethylene glycol dinitrate(DEGDN),the gas chromatography-tandem mass spectrometric method was established and organic impurities in DEGDN were qualitatively determined by retrieving the NIST library,comparing with the authentic samples and analyzing formation mechanism of impurities.An external standard method was used to determine the contents of the identified organic impurities.The results show that four organic impurities are detected in DEGDN,impurity 1 is identified as 2-(hydroxymethyl)-1,3-dioxolane,impurity 3 is identified as decane,impurity 4 is identified as ethylene glycol dinitrate(EGDN),and impurity 2 may be 2-hydroxy-1,4-dioxane.In the external standard method,the linear relationship between the materials is good,the correlation coefficients are in the range of 0.999 5—0.999 9,the average recoveries are in the range of 96.72%—103.33%and the relative standard deviations(RSD)are in the range of 0.31%—1.25%,showing that the proposed method has high precision and accuracy and can be used for the determination of the organic impurities in the DEGDN.

关 键 词：分析化学 含能增塑剂 一缩二乙二醇二硝酸酯(DEGDN) 气相色谱-质谱联用法 有机杂质 外标法 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O657[理学—分析化学]