气相色谱-脉冲火焰光度法测定环境气体中沙林  

Determination of sarin in environmental gas by gas chromatography-pulse flame photometric detector

作　　者：王红英 郝焕明 王金生 陈言坤 陈鹏[1] WANG Hongying;HAO Huanming;WANG Jinsheng;CHEN Yankun;CHEN Peng(Research Institute of Chemical Defense,Academy of Mlitary Sciences,Beijing 102205)

机构地区：[1]军事科学院防化研究院,北京102205

出　　处：《分析试验室》2020年第10期1218-1220,共3页Chinese Journal of Analysis Laboratory

摘　　要：建立了气相色谱-脉冲火焰光度法(GC-PFPD)测定气体沙林的方法。对环境气体中沙林的采集方式、环境湿度对采集回收率的影响、色谱柱类型、色谱条件、检测器条件进行了研究。确立了沙林气体样品经乙腈吸收采集、毛细管色谱柱分离、脉冲火焰光度检测器检测的技术途径。采用5%聚苯基甲基硅氧烷(30 m×0.32 mm×0.25"m)石英毛细管柱,回收率为90.4%~100.0%,相对标准偏差为5.0%,对气态沙林的最低检出浓度为0.3 ng/L,在39.4~630.6 ng/m L范围内有良好的线形关系(r^2=0.9999),方法可以用于定量分析环境气体中沙林。A novel method of determination of sarin in environmental gas by gas chromatography-pulse flame photometric detector(GC-PFPD)was described.The collection method of environmental sarin gas,influence of environmental humidity on sarin collection recovery,the chromatographic column type,chromatographic conditions and detector parameters were studied.Sarin in the gas was absorbed by acetonitrile,separated by capillary column and detected by pulse flame photometric detector.Samples of sarin were separated on the capillary column HP-5(5%Polyphenylmethylsiloxane,30 m×0.32 mm×0.25μm)with N2 as carrier gas at a flow rate of 1.3 m L/min.Inlet and detector temperature were 250℃and 300℃,Temperature program was from60℃(held for 0.5 min)to 250℃(held for 5.0 min)at a rate of 20℃.The detector selected phosphorus mode with the flow rate of hydrogen and air at 9.0 m L/min and 10.0 m L/min,respectively.The recoveries of standard additions were in the range of 90.4%-100.0%and the relative standard deviation(RSD)was 5%.The detection limit of sarin in gas was 0.3 ng/L(signal-to-noise ratio of 3)and the linear relationship was good in the range of 39.4-630.6 ng/m L.The method could be applied to quantitative determination of sarin gas sample.

关 键 词：气相色谱-脉冲火焰光度法(GC-PFPD) 沙林 气体监测 

分 类 号：X132[环境科学与工程—环境科学] O657.7[理学—分析化学]