甲醇等5种强极性有机物污染事故中的监测分析方法
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摘要
建立了在突发性水污染事故中定量分析水样中甲醇、丙酮、乙腈、N,N-二甲基甲酰胺和N,N-二甲基乙酰胺等5种极性有机物的实验室和现场应急监测分析方法。采用顶空-车载气相色谱质谱法用于现场快速定性定量分析;顶空-气相色谱法用于实验室准确定量分析。通过优化顶空及气相参数,在最佳实验条件下测得顶空-气相色谱质谱法中甲醇、丙酮、乙腈、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺等5种化合物的检出限分别为1.0、0.06、0.5、10.0、15.0 mg/L,平行测定7次结果的相对标准偏差分别为2.1%~3.8%,加标回收率为69.4%~104%;顶空-气相色谱法灵敏度高于气相色谱质谱法,检出限分别为0.08、0.01、0.03、1.7、1.7 mg/L,平行测定7次结果的相对标准偏差分别为2.5%~4.1%,加标回收率为78.1%~116%。
A simple method was developed to rapidly quantitative and qualitative analyse methonal,acetone,acetonitrile,N,Ndimethyl formamide and N,N-dimethyl-Acetamide in sudden water pollution accidents. A headspace-vehicular GC-MS method was adopted to rapidly detect five strong polar volatile organic compounds at water pollution accidents site; a headspace-GC-ECD method was used in laboratory analysis. Under optimum conditions,the detect limitation of GC-MSD method of methonal,acetone,acetonitrile,N,N-dimethyl formamide and N,N-dimethyl-Acetamide were 1. 0,0. 06,0. 5,10. 0 and 15. 0 mg/L respectively,and the relative standard deviation were between 2. 1%-3. 8%( n = 7) reapectively; the spiked recovery of these five compounds were between 69. 4%-104%; the detect limitation of GC-ECD method of methonal,aceton,acetonitrile,N,Ndimethyl formamide and N,N-dimethyl-Acetamide were 0. 08,0. 01,0. 03,1. 7 and 1. 7 mg/L respectively,and the relative standard deviation were between 2. 5%-4. 1%( n = 7) reapectively; the spiked recovery of these five compounds were between78. 1%-116%.
A simple method was developed to rapidly quantitative and qualitative analyse methonal,acetone,acetonitrile,N,Ndimethyl formamide and N,N-dimethyl-Acetamide in sudden water pollution accidents. A headspace-vehicular GC-MS method was adopted to rapidly detect five strong polar volatile organic compounds at water pollution accidents site; a headspace-GC-ECD method was used in laboratory analysis. Under optimum conditions,the detect limitation of GC-MSD method of methonal,acetone,acetonitrile,N,N-dimethyl formamide and N,N-dimethyl-Acetamide were 1. 0,0. 06,0. 5,10. 0 and 15. 0 mg/L respectively,and the relative standard deviation were between 2. 1%-3. 8%( n = 7) reapectively; the spiked recovery of these five compounds were between 69. 4%-104%; the detect limitation of GC-ECD method of methonal,aceton,acetonitrile,N,Ndimethyl formamide and N,N-dimethyl-Acetamide were 0. 08,0. 01,0. 03,1. 7 and 1. 7 mg/L respectively,and the relative standard deviation were between 2. 5%-4. 1%( n = 7) reapectively; the spiked recovery of these five compounds were between78. 1%-116%.
引文
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[2]李海燕.顶空-毛细管气相色谱法同步测定水中丙酮吡啶乙腈[J].中国环境监测,2011,27(2):56-58.LI Haiyan.Headspace Capillary Gas Chromatography Determination of Pyridine,Acetone,Acetonitrile Synchronization[J].Environmental Monitoring in China,2011,27(2):56-58.
[3]李韵谱,董小艳,吴亚西.气相色谱-质谱法分析环境空气中的甲醇和丙酮[J].环境卫生医学杂志,2013,3(5):445-448.LI Yunpu,DONG Xiaoyan,WU Yaxi.Determination of Methanol and Acetone in Ambient Air by Gas Chromatography-Mass Spectrometry[J].Journal of Environmental Hygiene,2013,3(5):445-448.
[4]环境保护部.突发环境事件应急监测规范:HJ589-2010[S].北京:中国环境科学出版社,2010.
[5]唐访良,朱文.气相色谱法测定废水中的N,N-二甲基甲酰胺和N,N-二甲基乙酰胺[J].理化检验-化学分册,2006,42(11):941-942.TANG Fangliang,ZHU Wen.Determination of N,N-Dimethyl Formamide and N,N-Dimethyl-Acetamide in Waste Water by Gas Chromatography[J].Physical Testing and Chemical Analysis-Chemical Analysis,2006,42(11):941-942.
[6]朱辉,耿艳.毛细管柱气相色谱法测定废气和废水中的N,N-二甲基甲酰胺[J].环境监测管理与技术,2013,25(1):43-45.ZHU Hui,GENG Yan.Determination of N,N-Dimethyl Formamide in Industrial Waste Gas and Waster Water by Capillary Gas Chromatographic Method[J].The Administration and Technique of Environmental Monitoring,2013,25(1):43-45.
[7]江建彪,朱高文.顶空毛细管气相色谱法同时测定水中丙酮甲醇乙腈[J].环境监测管理与技术,2012,24(6):64-66.JIANG Jianbiao ZHU Gaowen,Headspace Capillary Gas Chromatography Method for the Simultaneous Determination of Acetone,Methanol and Acetonitrile in Water[J].The Administration and Technique of Environmental Monitoring,2012,24(6):64-66.