含磷毒剂及其降解产物的气相色谱－质谱测定方法研究  

Analysis of Organophosphorus Warfare Agents and Their Degradation Products by Gas Chromatography-Mass Spectrometry

作　　者：顾惠芬[1] 周黎明[1] 蔡冠梁[1] 钟玉征[1] 

机构地区：[1]防化指挥工程学院分析测试中心

出　　处：《色谱》1996年第1期41-44,共4页Chinese Journal of Chromatography

摘　　要：研究了用台式气相色谱－质谱仪分析测定含磷毒剂及其降解产物，并对降解产物的衍生化方法及它们的色谱行为进行了研究，总结分析了它们的质谱裂解特点及规律，测定了水样中的含磷毒剂及降解产物。Organophosphorus chemical warfare agents sarin, soman,tabun, VX and their degradation products were determined in environmental samples with full scanning electron impact gas chromatography-mass spectrometry (EI-GC-MS).The gas chromatograph was fit with a 25m×0.2mm i.d. HP-5 capillary column, with film thickness of 0.33 μm.Helium at 90 kPa was used as carrier gas, at the flow rate of 0.5mL/min.The oven was held at 40℃ for 2 min, then programmed from 40 to 280℃ at 10℃/min and held at 280℃ for 10 min.Split/splitless injection was used at injection temperature 250℃.The interface was held at 280℃.Water samples were extracted with dichloromethane under neutral,acidic and alkaline conditions. The polar degradation products,organophosphonic acids,were methylated with diazomethane at room temperature for 15 min or silylated with BSTFA at 60-70℃ for 30 min to form volatile compounds which could be analyzed by gas chromatography-mass spectrometry. The remaining aqueous soltuion was evaporated to dryness and dissolved with acidic MeOH and derivatized with dizomethane and analyzed.Names,formula and mass spectral fragments of organophosphorus chemical warfare agents and derivatives of organophosphorus acids are presented in tables.Total ion current chromatograms of these compounds are shown in three figures.The mass spectral fragments are interpreted and discussed.Tabun, ethyl phosphonate and methylphosphonic acid in the water were quantitatively determined. The recoveries range from 23% to 28% in 10× 10-6 level.

关 键 词：气相色谱 质谱 水样 含磷毒剂 降解产物 

分 类 号：E929.1[军事—军事装备学] O657.71[兵器科学与技术—武器系统与运用工程]