MS Analysis of Purity Standard Reference Material of Hexanitrostilbene and Determination of Its Organic Impurities
摘 要
采用气相色谱-质谱法对六硝基芪纯度标准物质(简写作HNS)中易气化、热稳定性好的有机杂质(包括3,5-二溴吡啶、2,4,6-三硝基苯、2,4,6-三硝基甲苯及4,6-二硝基苯异唑等)进行结构鉴定。利用液相色谱-大气压化学电离源-质谱法对HNS中难气化,热稳定性差的杂质(主要是非极性较强的中间体二苦基乙烷,简写作DPE)作结构鉴定,并检测到HNS和DPE的特征加合离子。以上两方面的工作有效地测定了HNS中的有机杂质,为这些杂质的去除提供了依据,对制备HNS纯度标准物质具有重要意义。
Abstract
GC-MS was applied to the identification of chemical structure of easily gasifiable and thermo-stable organic impurities (i.e., 3.5-dibromopyridine, 2,4,6-trinitrobenzene, 2,4,6-trinitrotoluene and 4,6-dinitrobenzoisoxazole) in the purity SRM of hexanitrostilbene (abbr. as HNS); and LC-MS with APCI was applied to the structural identification of hardly gasifiable and poorly thermo-stable impurities, especially the non-polar intermediate of 1,2-bis(2,4,6-trinitrophenyl) ethane, (abbr. as DPE). Characteristic adduct ions of HNS and DPE were also detected by LC-MS with APCI. Organic impurities in HNS were successfully determined by the above mentioned methods which gave a sound base to eliminate the impurities from HNS and was beneficial for preparation of the purity SRM.
中图分类号 O657.63
所属栏目 工作简报
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收稿日期 2013/2/11
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备注李文杰(1980-),男,山东烟台人,工程师,硕士,主要从事有机质谱研究工作。
引用该论文: LI Wen-jie,NING Yan-li,HU Yin,SU Peng-fei,ZHANG Lin-jun,CHEN Zhi-qun,ZHANG Gao. MS Analysis of Purity Standard Reference Material of Hexanitrostilbene and Determination of Its Organic Impurities[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(4): 462~466
李文杰,宁艳利,胡银,苏鹏飞,张林军,陈智群,张皋. 六硝基芪纯度标准物质的质谱分析及其有机杂质的测定[J]. 理化检验-化学分册, 2014, 50(4): 462~466
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参考文献
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【2】雷波,史春红.六硝基芪纯化工艺研究[J].火工品, 2007(4):13-16.
【3】李佩芳,夏红,念东,等.混合炸药中TNT与HNS的分离与测定[J].华东工学院学报, 1992,61(1):54-59.
【4】张敏.RDX和HMX的大气压电喷雾电离质谱分析[J].火炸药学报, 2006(2):77-80.
【5】张敏,孙莉霞,陈智群.BTTN与NG混合物的大气压电喷雾质谱研究[J].含能材料, 2004,12(3):165-167.
【6】GILBERT E E. The preparation of hexanitrostilbene from hexanitrobibenzyl[J]. Propellants and Explosives, 1980,5:168-172.
【7】KAYSER E G. An investigation of the Shipp hexanitrostilbene (HNS) process[J]. Journal of Energetic Materials, 1983,1:325-348.
【8】BELLAMY A J. Identification of α-chloro-2,2′,4,4′,6,6′-hexanitrobibenzyl as an impurity in hexanitrostilbene[J]. Journal of Energetic Materials, 2010,28(1):1-1.
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