1,3⁃二氯⁃2,4,6⁃三硝基苯纯度的高效液相色谱分析方法  

Purity Analysis of 1,3⁃Dichloro⁃2,4,6⁃Trinitrobenzene by High Performance Liquid Chromatography

作　　者：刘云章 何佳远 肖芸 陈丽珍 王建龙 LIU Yun-zhang;HE Jia-yuan;XIAO Yun;CHEN Li-zhen;WANG Jian-long(School of Chemical Engineering and Technology,North University of China,Taiyuan 030051,China;Norinco Group Hubei DongFang Chemical Industry Co.Ltd,Xiangyang 441404,China)

机构地区：[1]中北大学化学工程与技术学院,山西太原030051 [2]湖北东方化工有限公司,湖北襄阳441404

出　　处：《含能材料》2022年第6期564-570,共7页Chinese Journal of Energetic Materials

摘　　要：为准确测定1,3⁃二氯⁃2,4,6⁃三硝基苯(DCTNB)产品的纯度,建立了DCTNB及其合成过程中产生的杂质(1,5⁃二氯⁃2,4⁃二硝基苯(DCDNB)、2,3,4⁃三氯⁃1,5⁃二硝基苯(TCDNB))的高效液相色谱分析方法,研究了流动相体系及比例、流速及进样量等色谱条件对DCTNB高效液相色谱分离效果的影响,定量分析采用外标法进行。结果表明,最优的色谱条件为:Hypersil ODS2色谱柱(250 mm×4.6 mm,5μm),紫外检测波长240 nm,流动相为V_(ACN)/V_(Water)=55/45,流速1.2 mL·min^(-1),柱温25℃,进样量10μL。在上述色谱条件下,DCDNB,DCTNB和TCDNB的保留时间分别为9.20,10.50,14.17 min,各紫外吸收峰的分离度均大于3.70,分离效果良好。DCDNB,DCTNB和TCDNB分别在5~250,5~500,5~250 mg·L^(-1)浓度范围内线性关系良好,线性相关系数R^(2)>0.999,检出限分别为0.47,0.68,0.85 mg·L^(-1),定量限分别为1.58,2.28,2.82 mg·L^(-1),相对标准偏差为1.01%~1.27%,加标回收率为98.82%~102.13%。To determine the purity of 1,3⁃dichloro⁃2,4,6⁃trinitrobenzene(DCTNB)product accurately,a high⁃performance liq⁃uid chromatography(HPLC)real⁃time(or in⁃situ)method for the determination of DCTNB and its impurities,1,5⁃dichloro⁃2,4⁃dinitrobenzene(DCDNB)and 2,3,4⁃trichloro⁃1,5⁃dinitrobenzene(TCDNB)was established..The effect of different mobile phase system,mobile phase ratio,flow rate and injection volume etc.conditions on the separation of high performance liquid chromatography for DCTNB was discussed.The quantitative analysis method was carried out by an external standard method.Re⁃sults show that The optimal chromatographic conditions obtained are as follows:hypersil ODS2 chromatographic column(250 mm×4.6 mm,5μm),UV detection wavelength 240 nm,acetonitrile/water with a volume ratio of 55∶45 as mobile phase,flow rate 1.2 mL·min^(-1),column temperature 25℃,injection volume 10μL.Under the above chromatographic condi⁃tions,the retention times of DCDNB,DCTNB and TCDNB are 9.20,10.50,and 14.17 min in sequence with good resolution of all peaks(greater than 3.70).DCDNB,DCTNB and TCDNB show a good linear relationships in the concentration ranges of 5-250,5-500 and 5-250 mg·L^(⁃1),respectively,and the linear correlation coefficient R^(2) is greater than 0.999.The detection lim⁃its of DCDNB,DCTNB and TCDNB are 0.47,0.68,0.85 mg·L^(-1),the quantification limits are 1.58,2.28,2.82 mg·L^(-1),respec⁃tively,the relative standard deviation of 1.01%-1.27%,and the standard recovery rates are 98.82%-102.13%.

关 键 词：1 3⁃二氯⁃2 4 6⁃三硝基苯(DCTNB) 1 5⁃二氯⁃2 4⁃二硝基苯(DCDNB) 2 3 4⁃三氯⁃1 5⁃二硝基苯(TCDNB) 高效液相色谱法(HPLC) 纯度分析方法 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O65[理学—分析化学]