某些火炸药色谱分析中的样品前处理技术  

Sample Pretreatment Techniques for the Chromatographic Analysis of Energetic Materials

作　　者：贾林[1] 张皋[1] 张林军[1] 张冬梅[1] 杜姣姣[1] 王琼[1] 杨彩宁[1] 任春燕[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《含能材料》2015年第3期279-284,共6页Chinese Journal of Energetic Materials

基　　金：国家国防科技工业局"十一五"科研计划项目(Z092009T001)

摘　　要：用色谱法分析火炸药样品时,首先要将待测物从固体基质中萃取到溶剂中。传统的火炸药样品前处理方法,如:索式提取(SE)法、溶剂溶解水沉淀(SDWP)法,所需时间太长,不能满足现代快速检测的需求。本研究考察了超声辅助萃取(UAE)、开放式聚焦微波辅助萃取(MAE)、加压加热萃取(PLE)对某些火炸药的萃取效果。结果表明,MAE、PLE需选择不溶解硝化棉(NC)仅溶解待测物的萃取溶剂。UAE、MAE、PLE比SE、SDWP萃取时间短。UAE适用于以非NC聚合物作粘合剂的疏松质地的火炸药样品的萃取。MAE由于硝化甘油(NG)在常压下加热后挥发明显,限制了较高萃取温度的使用,即限制了微波的作用,萃取效率相对于昂贵仪器的性价比不高。PLE可抑制NG的挥发和分解,对包括黑索今(RDX)在内的待测物有很强的溶解能力,有萃取效率高、适用面广的优点,缺点是运行成本较高。When the explosive and propellant samples are analyzed by chromatography,firstly,the tested substances need to be extracted into solvent from solid matrices.The time required for traditional pretreatment methods of explosive and propellant samples such as Soxhlet′s extraction（SE）method and solvent-dissolve-water-precipitation extraction（SDWP）method is too long,which can not meet the needs of modern rapid detection.The extraction effect of some explosive and propellant samples by the ultrasound-assisted extraction（UAE）,microwave-assisted extraction（MAE）and pressurized-liquid extraction（PLE）were examied.Results show that MAE and PLE have to choose the extraction solvent,which can not dissolve nitrocellulose（NC）,only dissolve the tested substances.The extraction time of UAE,MAE and PLE is shorter than that of SE and SDWP.UAE is used to extract the explosive and propellant samples with loose texture and without NC polymer as binder.The use of higher MAE temperature is limited due to volatile obviously after nitroglycerin（NG）heating under normal pressure,i.e.the effect of microwave is restricted,the price ratio of extraction efficiency relative to expensive instrument is not high.PLE can restrain the volatilization and decomposition of NG,having the very strong dissolution ability for the tested substances,including cyclotrimethylene trinitramine（RDX）,and the advantages of high extraction efficiency and wide application.Its shortcoming is that running cost is higher.

关 键 词：萃取 色谱法 硝化甘油 硝化棉 黑索今(RDX) 

分 类 号：TQ560.72[化学工程—炸药化工] O657.7[理学—分析化学]