Two-Dimensional GC Determination of 6 Components in Air After TNT Explosion
摘 要
采用二维气相色谱法(2DGC)测定三硝基甲苯爆炸后空气中6种组分的含量。试验选用5A色谱柱(3 m×2 mm,0.18~0.25 mm,用于测定一氧化碳、甲烷、氢气、氮气、氧气)和Porapark Q色谱柱(3 m×2 mm,0.18~0.25 mm,用于测定二氧化碳)。为克服基线波动的影响,在检测器前端增加气阻,在进样口出口端增加气容。选用10号气阻,使基线波动幅度减小至100 μV,平稳时间为10 s。气容和气阻的组合有效改善了阀切换操作引起的基线波动及流量归零引起的基线波动。按所选定的2DGC的分析流程和色谱条件,可完成上述6种组分的测定,各组分无损失,分析时间为1 h。一氧化碳、二氧化碳、甲烷、氢气的检出限(3S/N)依次为0.001 5%,0.001 0%,0.001 5%,0.15%。上述4种气体组分测定值的相对标准偏差(n=10)依次为0.50%,0.20%,0.20%,0.40%。经显著性检验,2DGC的分析结果与质谱和一氧化碳检测仪的分析结果之间不存在显著性差异。方法应用于实际样品的分析,结果表明三硝基甲苯爆炸后空气中一氧化碳、二氧化碳、甲烷、氢气、氮气和氧气为常量成分。
Abstract
Two-dimensional GC (2DGC) was applied to the determination of 6 components in air after TNT explosion. Chromatographic columns of 5A and Porapark Q (3 m×2 mm, 0.18-0.25 mm for both columns) were chosen for determination of CO, CH4, H2, N2 and O2 with the former column and for determination of CO2 with the latter one. To overcome the interference of baseline fluctuation, a gas resistance was set in front of the detector, and a gas capacitance was placed at the outlet of sample introducer. By using the gas resistance No.10, the amplitude of baseline fluctuation was lowered to 100 μV with stablizing time of 10 s, and by the combined effect of gas resistance and gas capacitance, baseline fluctuations due to valve switching and flow rate zeroizing were significantly decreased. By the optimized analytical procedure and chromatographic conditions of 2DGC, determination of the 6 components was completed within 1 h without lossing of any of the components. Detection limits (3S/N) found for CO, CO2, CH4 and H2 were 0.001 5%, 0.001 0%, 0.001 5% and 0.15% respectively. Values of RSDs (n=10) found for the above 4 gas components were 0.50%, 0.20%, 0.20% and 0.40% respectively. As shown by the results of test for significance, no significant differences were found among the analytical results found by 2DGC, by the MS and by CO detector. The proposed method had been applied to the analysis of actural samples, and as shown by the results of determination, CO, CO2, CH4, H2, N2 and O2 were the main components in air after TNT explosion.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201902007
所属栏目 工作简报
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收稿日期 2018/4/16
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备注王伟超,助理工程师,硕士,研究方向为气相色谱,wangweichao1205@163.com
引用该论文: WANG Weichao,DU Jixing,GAN Zongyu,XIE Haifeng. Two-Dimensional GC Determination of 6 Components in Air After TNT Explosion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(2): 156~161
王伟超,杜继星,甘宗煜,谢海峰. 二维气相色谱法测定三硝基甲苯爆炸后空气中6种组分[J]. 理化检验-化学分册, 2019, 55(2): 156~161
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参考文献
【1】王新建.炸药氧平衡理论在铵油炸药管理中的应用研究[J].中国人民公安大学学报(自然科学版), 2014(3):76-79.
【2】STOLTZ C, PEIRIS S. T-jump/FTIR studies of poly-glycidyl nitrate (PGN) pyrolysis[J]. AIP Conference Proceedings, 2007,955(1):1263-1266.
【3】丁卉.阀切换离子色谱的构建和应用[D].上海:华东理工大学, 2012.
【4】徐小民.串联毛细管气相色谱柱分离原理及应用[D].杭州:浙江大学, 2016.
【5】肖细炼,李季,张彩明,等.三检测通道-气相色谱法快速分析天然气的组成[J].理化检验-化学分册, 2012,48(6):678-681.
【6】张齐,徐立英,乐毅.多维气相色谱技术在炼厂气分析中的应用[J].精细石油化工, 2013,30(5):83-86.
【7】许国旺.现代实用气相色谱法[M].北京:化学工业出版社, 2004.
【2】STOLTZ C, PEIRIS S. T-jump/FTIR studies of poly-glycidyl nitrate (PGN) pyrolysis[J]. AIP Conference Proceedings, 2007,955(1):1263-1266.
【3】丁卉.阀切换离子色谱的构建和应用[D].上海:华东理工大学, 2012.
【4】徐小民.串联毛细管气相色谱柱分离原理及应用[D].杭州:浙江大学, 2016.
【5】肖细炼,李季,张彩明,等.三检测通道-气相色谱法快速分析天然气的组成[J].理化检验-化学分册, 2012,48(6):678-681.
【6】张齐,徐立英,乐毅.多维气相色谱技术在炼厂气分析中的应用[J].精细石油化工, 2013,30(5):83-86.
【7】许国旺.现代实用气相色谱法[M].北京:化学工业出版社, 2004.
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