气相色谱-质谱联用法和气相色谱法对多功能控暴剂中臭味气体的定性、定量分析
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摘要
采用气相色谱-质谱联用法对含叔丁基硫醇、二乙基硫醚、邻氯苯亚甲基丙二腈等多种组分的多功能控暴剂进行了定性分析,实现了各物质的完全分离和各色谱峰的归属确认。使用注射器配气法实现了标准气的配制,并采用气相色谱法对多功能控暴剂中叔丁基硫醇进行定量分析。叔丁基硫醇气体样品的质量浓度在5~1 000μg·L~(-1)内与其对应的峰高呈线性关系,进样量为1mL时,检出限(3S/N)为5μg·L~(-1)。加标回收率在97.2%~105%之间,对同一样品连续进样测定,测定值的相对标准偏差(n=6)为3.2%。
The multifunctional riot control agent composed of 2-methyl-2-propanethiol,diethyl sulfide and 2-chlorobenzylidene malononitrile were analysed qualitatively by gas chromatography in hyphenation with mass spectrometry.Complete separation of the analytes was achieved and assoting of the chromatographic peaks was affirmed.2-Methyl-2-propanethiol in multifunctional riot control agent was determined by gas chromatography using syringe dispensing method in preparation of gas standards.Linear relationship between values of peak height and mass concentration of 2-methyl-2-propanethiol was kept in the range of 5-1 000μg·L~(-1).Detection limit(3 S/N)of 5μg·L~(-1) was found when 1 mL of the sample was introduced.Values of recovery obtained by standard addition method were in the range of 97.2%-105%.By replicate introduction of a same sample,RSD(n=6)was 3.2%.
The multifunctional riot control agent composed of 2-methyl-2-propanethiol,diethyl sulfide and 2-chlorobenzylidene malononitrile were analysed qualitatively by gas chromatography in hyphenation with mass spectrometry.Complete separation of the analytes was achieved and assoting of the chromatographic peaks was affirmed.2-Methyl-2-propanethiol in multifunctional riot control agent was determined by gas chromatography using syringe dispensing method in preparation of gas standards.Linear relationship between values of peak height and mass concentration of 2-methyl-2-propanethiol was kept in the range of 5-1 000μg·L~(-1).Detection limit(3 S/N)of 5μg·L~(-1) was found when 1 mL of the sample was introduced.Values of recovery obtained by standard addition method were in the range of 97.2%-105%.By replicate introduction of a same sample,RSD(n=6)was 3.2%.
引文
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[2]周振中.防暴刺激剂公共安全性能评述[J].武警工程大学学报,2008(2):34-38.
[3]马宝龙.美国非致命武器的研究:镇静剂和臭味剂[J].国外防化科技动态,2002(2):2-7.
[4]王红英,牟瑛琳,郝焕明,等.新型控暴剂辣椒素研究进展[J].警察技术,2011(2):71-73.
[5] WITTEN B,WAGMAN W,SHAFFER R,et al.Malodorous substances as riot control and troop training agents[R].[S.l.]:[s.n.],1970.
[6] PINNEY V R.Malodorant compositions,related nonlethal weapon systems,and methods of their use:US6352032[P].2002-03-05.
[7]闫瑾,鲍峰伟,牛丽娜,等.气相色谱-质谱法确定主流烟气中的植物碱[J].理化检验-化学分册,2015,51(9):932-935.
[8]王红英,郝焕明,牟瑛琳,等.气相色谱法测定催泪喷射器中的刺激剂中刺激组分[J].分析仪器,2012(4):30-32.
[9]魏学锋,费旭东,吴颖,等.气相色谱-硫化学发光检测器测定车用汽油中8种硫醇[J].分析试验室,2015,34(10):1178-1182.
[10]吕建霞,梁立娜.吹扫捕集-气相色谱/质谱联用法测定水中臭味物质[J].环境化学,2013,32(11):2223-2224.
[11]冯桂学,王明泉,刘莉,等.顶空固相微萃取-气相色谱-质谱联用技术测定水中8种致臭味物质方法优化[J].给水排水,2014,40(12):17-20.
[12]薛田,崔庆忠,吕宁,等.邻氯苯亚甲基丙二腈的热分解性能研究[J].质谱学报,2016,37(1):23-30.
[13]周黎明,顾惠芬.GC-MS检定刺激剂CN,CS和CR[J].防化学报,1995(4):37-39.
[14]闫凤美,黄绍重.喷射催泪器中有效成分的GC/MS分析[J].中外医疗,2006(12):49-50.
[15]梁政勇,章亚东,张剑,等.三相相转移催化剂制备叔丁基硫醇新工艺研究[J].高校化学工程学报,2011,25(4):627-631.
[16]赵冲林,许大年,陈志升.毒剂及相关化合物气体发生与采集分析[J].分析测试学报,2008,27(3):304-306.
[17]孔令昌.野外气体取样器和取样方法的研究[J].地震地质,1992(3):96-98.
[18]李永福,付新民,张冬梅.一种简易气体取样器[J].仪器仪表与分析监测,2001(4):38-39.
[19]魏刚,王淑英.侧柏叶挥发油化学成分气质联用分析[J].时珍国医国药,2001,12(1):18-19.
[20]张岚,蒋兰,鄂学礼,等.饮用水中痕量挥发性有机物吹扫捕集-气质联用测定法[J].环境与健康杂志,2008,25(5):431-432.
[21]刘永波,刘海山,王红芳.固相萃取-气相色谱-质谱联用法测定蔬菜、水果中吡虫啉残留量[J].理化检验-化学分册,2007,43(1):23-25.
[22]程万影,郝雪颖,马士洲,等.新型控暴器材爆炸分散研究[J].火工品,2012(6):1-4.