罐采样/气相色谱-质谱法分析环境空气中57种臭氧前体物
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摘要
针对中国当前臭氧污染问题,建立了苏玛罐采样-低温浓缩/气相色谱-质谱法分析环境空气中57种臭氧前体物的方法。样品经三级冷阱预浓缩仪富集、除干扰组分并进行冷聚焦后利用冷柱温分离,气相色谱-质谱法分析。笔者优化了阱的关键温度和时间参数,在最佳实验条件下进行方法性能实验,结果表明,57种目标化合物的方法检出限为0.03×10~(-6)～0.39×10~(-6),高、中、低3组浓度水平的相对标准偏差(RSD)为0.5%～11%(n=6),空白加标回收率为80.1%～112%。方法成功应用于山东省17个采样城市环境空气样品的分析。
In order to analyze the cause of severe O_3 pollution in China, this study proposed a method to determine 57 ozone precursors compounds in ambient air based on canister sampling-cryogenic traping/GC-MS. Samples were cryogenically preconcentrated and focused after interfering substances removed, then determined by GC-MS. In this paper, key temperature and time parameters of cold traps were optimised, experiment performances of the method were conducted under optimum conditions. The results showed that under the optimized conditions, the method detection limits of 57 compounds were between 0.03×10~(-6)-0.39×10~(-6). The method showed high accuracy and validity, three levels of the relative standard(RSD) were in the range of 0.5%-11%(n=6), spiked sample recoveries were in the range of 80.1%-112%. This method was successfully used for the determination of ambient air samples in 17 citis of Shangdong province.
In order to analyze the cause of severe O_3 pollution in China, this study proposed a method to determine 57 ozone precursors compounds in ambient air based on canister sampling-cryogenic traping/GC-MS. Samples were cryogenically preconcentrated and focused after interfering substances removed, then determined by GC-MS. In this paper, key temperature and time parameters of cold traps were optimised, experiment performances of the method were conducted under optimum conditions. The results showed that under the optimized conditions, the method detection limits of 57 compounds were between 0.03×10~(-6)-0.39×10~(-6). The method showed high accuracy and validity, three levels of the relative standard(RSD) were in the range of 0.5%-11%(n=6), spiked sample recoveries were in the range of 80.1%-112%. This method was successfully used for the determination of ambient air samples in 17 citis of Shangdong province.
引文
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[10] WEI W,CHENG S Y.Characteristics of Volatile Organic Compounds (VOCs) Emitted from Petroleum Refinery in Beijing,China[J].Atmospheric Environment,2014,89(1):358-366.
[11] 环境保护部.环境空气挥发性有机物的测定罐采样/气相色谱-质谱法:HJ 759—2015[S].北京:中国环境科学出版社,2015.
[12] 环境保护部.环境空气挥发性有机物的测定吸附管采样-热脱附/气相色谱-质谱法:HJ 644—2013[S].北京:中国环境科学出版社,2013.
[13] United States Environmental Protection Agency.Technical Assistance Document for Sampling and Analysis of Ozone Precursors:EPA/600-R-98/161 [S].Washington DC:United States Environment Protection Agency,1998.
[14] WANG W K D,AUSTIN C C.Determination of Complex Mixtures of Volatile Organic Compounds in Ambient Air:Canister Methodology[J].Anal Bioanal Chem,2006,368(4):1 099-1 120.
[15] BARLETTA B,MEINARDI S,ROWLAND F S,et al.Volatile Organic Compounds in 43 Chinese Cities[J].Atmospheric Environment,2005,39(32):5 979-5 990.
[16] 徐慧,邓君俊,邢振雨,等.厦门不同功能区VOCs的污染特征及健康风险评价[J].环境科学学报,2015,35(9):2 701-2 709.XU Hui,DENG Junjun,XING Zhenyu,et al.Pollution Characteristics and Health Risk Assessment of VOCs in Different Functional Zones of Xiamen[J].Acta Scientiae Circumstanyiae,2015,35(9):2 701-2 709.
[17] SHINJI S.Characteristics of Ambient C2-C12 Non-methane Hydrocarbons in Metropolitan Nagoya,Japan[J].Atmospheric Environment,2009,43(29):4 384-4 395.
[2] 段菁春,彭艳春,谭吉华,等.北京市冬季灰霾期NMHCs空间分布特征研究[J].环境科学,2013,34(12):4 533-4 557.DUAN Jingchun,PENG Yanchun,TAN Jihua,et al.Spatial Distribution Characteristics of NMHCs During Winter Haze in Beijing[J].Environmental Science,2013,34(12):4 533-4 557.
[3] 林旭,朱彬,安俊琳,等.南京北郊VOCs对臭氧和二次有机气溶胶潜在贡献的研究[J].中国环境科学,2015,35(4):976-986.LIN Xu,ZHU Bin,AN Junlin,et al.Potential Contribution of Secondary Organic Aerosols and Ozone of VOCs in Northern Suburb of Nanjing[J].China Environmental Science,2015,35(4):976-986.
[4] 徐慧,张晗,邢振雨,等.厦门冬春季大气VOCs的污染特征及臭氧生成潜势[J].环境科学,2015,36(1):11-17.XU Hui,ZHANG Han,XING Zhenyu,et al.Pollution Characteristics and Ozone Formation Potential of Ambient VOCs in Winter and Spring in Xiamen[J].Environmental Science,2015,36(1):11-17.
[5] SOU N M.Evaluation of Non-methane Hydrocarbon (NMHC) Emissions Based on an Ambient Air Measurement in Tokyo Area,Japan[J].Atmospheric Environment,2010,44(38):4 982-4 993.
[6] 刘丹,解强,张鑫,等.北京冬季灰霾频发期VOCs源解析及健康风险评价[J].环境科学,2016,37(10):3 693-3 701.LIU Dan,XIE Qiang,ZHANG Xin,et al.Source Apportionment and Health Risk Assessment of VOCs During the Haze Period in the Winter in Beijing[J].Environmental Science,2016,37(10):3 693-3 701.
[7] USEPA.Technical Assistance Document for Sampling and Analysis of Ozone Precursors:EPA/600-R-98/161[S].Washington DC:United States Environment Protection Agency,1998.
[8] 孔琴心,刘广仁.近地面臭氧浓度变化及其对人体健康的可能影响[J].气候与环境研究,1999,4(1):61-66.KONG Qinxin,LIU Guangren.Surface Ozone Concentration Variation and Possible Influence on Human[J].Climatic and Environmental Research,1999,4(1):61-66.
[9] 刘峰,朱永官,王效科.我国地面臭氧污染及其生态环境效应[J].生态环境,2008,17(4):1 674-1 679.LIU Feng,ZHU Yongguan,WANG Xiaoke.Surface Ozone Pollution and Its Eco-environmental Impactsin China[J].Ecology and Environment,2008,17(4):1 674-1 679.
[10] WEI W,CHENG S Y.Characteristics of Volatile Organic Compounds (VOCs) Emitted from Petroleum Refinery in Beijing,China[J].Atmospheric Environment,2014,89(1):358-366.
[11] 环境保护部.环境空气挥发性有机物的测定罐采样/气相色谱-质谱法:HJ 759—2015[S].北京:中国环境科学出版社,2015.
[12] 环境保护部.环境空气挥发性有机物的测定吸附管采样-热脱附/气相色谱-质谱法:HJ 644—2013[S].北京:中国环境科学出版社,2013.
[13] United States Environmental Protection Agency.Technical Assistance Document for Sampling and Analysis of Ozone Precursors:EPA/600-R-98/161 [S].Washington DC:United States Environment Protection Agency,1998.
[14] WANG W K D,AUSTIN C C.Determination of Complex Mixtures of Volatile Organic Compounds in Ambient Air:Canister Methodology[J].Anal Bioanal Chem,2006,368(4):1 099-1 120.
[15] BARLETTA B,MEINARDI S,ROWLAND F S,et al.Volatile Organic Compounds in 43 Chinese Cities[J].Atmospheric Environment,2005,39(32):5 979-5 990.
[16] 徐慧,邓君俊,邢振雨,等.厦门不同功能区VOCs的污染特征及健康风险评价[J].环境科学学报,2015,35(9):2 701-2 709.XU Hui,DENG Junjun,XING Zhenyu,et al.Pollution Characteristics and Health Risk Assessment of VOCs in Different Functional Zones of Xiamen[J].Acta Scientiae Circumstanyiae,2015,35(9):2 701-2 709.
[17] SHINJI S.Characteristics of Ambient C2-C12 Non-methane Hydrocarbons in Metropolitan Nagoya,Japan[J].Atmospheric Environment,2009,43(29):4 384-4 395.
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