环境监测用氮气中多组分VOCs标准物质的研制
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摘要
介绍了采用称量法制备瓶装1μmol/mol氮气中42个组分挥发性有机物(VOCs)标准物质的研制方法。建立了选择离子模式,气相色谱-质谱联用的分析方法,对目标组分在气瓶中的长期稳定性进行了考察。所选择的42种目标组分完全满足中国环境保护标准《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)和美国环保署《使用特殊处理的采样罐/气相色谱仪检测环境大气中的挥发性有机物》(EPA TO—14A)这2个方法标准中所规定的环境空气中挥发性有机有害成分的监测要求。将研制的气体标准物质与中国计量科学研究院(NIM)和英国国家物理实验室(NPL)分别进行了比对测试,取得了良好的比对结果与国际等效度。结果表明,1μmol/mol氮气中42种组分VOCs标准物质的有效期为一年,相对扩展不确定度为5.0%(包含因子k=2),并取得国家标准物质证书GBW(E)062231。
The development of multi-component VOCs reference material in nitrogen gas at 1 μmol/mol level by gravimetric preparation method was described in this paper. The stability of target analytes in cylinder was checked using GC coupled with a quadruple mass selective detector. All the selected 42 target analytes could meet the requirements on monitoring VOCs in ambient air, according to the China environmental protection method HJ 644-2013 and the U.S. Environmental Protection Agency method TO-14 A. The validation result between NIM and NIMTT showed a reliable consistency, and an international equivalence degree was also obtained from the comparison result between NPL and NIMTT. All the research results indicated that an estimated relative expanded uncertainty of 5.0%(k=2) and one year shelf life has been achieved. This gas reference material has acquired the certificate of national secondary gas reference material GBW(E)062231.
The development of multi-component VOCs reference material in nitrogen gas at 1 μmol/mol level by gravimetric preparation method was described in this paper. The stability of target analytes in cylinder was checked using GC coupled with a quadruple mass selective detector. All the selected 42 target analytes could meet the requirements on monitoring VOCs in ambient air, according to the China environmental protection method HJ 644-2013 and the U.S. Environmental Protection Agency method TO-14 A. The validation result between NIM and NIMTT showed a reliable consistency, and an international equivalence degree was also obtained from the comparison result between NPL and NIMTT. All the research results indicated that an estimated relative expanded uncertainty of 5.0%(k=2) and one year shelf life has been achieved. This gas reference material has acquired the certificate of national secondary gas reference material GBW(E)062231.
引文
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[17] 郑力文,董了瑜,李志昂,等.氮气中多组分挥发性有机物(VOCs)气体标准物质的气相色谱-质谱分析方法研究[J].化工技术与开发,2017,46(1):25-28.ZHENG Liwen,DONG Liaoyu,LI Zhiang,et al.Study on 42 Components Volatile Organic Compounds Gas Standard Materials in Nitrogen Measured by GC-MS[J].Technology & Development of Chemical Industry,2017,46(1):25-28.
[18] 全国标准物质计量技术委员会.气体标准物质研制(生产)通用技术要求: JF 1344—2012[S].北京:中国标准出版社,2012.
[2] YANG K L,LO J G.Evaluation of Capillary Gas Chromatography for the Measurement of Hydrocarbons by Participating in an Intercomparison Experiment[J].Chromatographia,1997,44(7):405-417.
[3] 赵利容,王新明,何秋生.广州市城市街道中四氯化碳、三氯乙烯和四氯乙烯的暴露特征[J].中国环境监测,2005,21(4):72-74.ZHAO Lirong,WANG Xinming,HE Qiusheng,et al.Characteristics of Halocarbons in Urban Guangzhou Streets[J].Environmental Monitoring of China,2005,21(4):72-74.
[4] 李宁,范洁,王倩,等.环境监测用5种氯代烯烃混合气体标准样品制备[J].中国环境监测,2014,30(5):101-104.LI Ning,FAN Jie,WANG Qian,et al.Development of a Standard Reference Material Containing 5 Chlorinated Hydrocarbons for Environmental Monitoring[J].Environmental Monitoring of China,2014,30(5):101-104.
[5] 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.
[6] SCHMIDT W P,ROOK H L.Preparation of Gas Cylinder Standards for the Measurement of Trace Levels of Benzene and Tetrachloroethylene[J].Anal Chem,1983,55(2):290-294.
[7] RHODERICK G C.Development of a Gas Standard Reference Material Containing Eighteen Volatile Organic Compunds[J].Fresenius Journal of Analytical Chemistry,1991,341(9):524-531.
[8] RHODERICK G C.Development of a Fifteen Component Hydrocarbon Gas Standard Reference Material at 5 nmol/mol in Nitrogen[J].Fresenius Journal of Analytical Chemistry,1997,359(6):477-483.
[9] 吴忠祥,彭洪俊,田文,等.氮气中苯系物(高压) 标准气体的研制[J].低温与特气,2001,19(4):29-34.WU Zhongxiang,PENG Hongjun,TIAN Wen,et al.Development of Standard Gas BTEX(High Pressure) in Nitrogen[J].Low Temperature and Specialty Gas,2001,19(4):29-34.
[10] 李宁,王倩,郭健,等.氮气中六种氯代烷烃混合标准气体的研制[J].色谱,2010,28(5):521-524.LI Ning,WANG Qian,GUO Jian,et al.Development of Standard Gas Mixture of Six Chlorinated Hydrocarbons in Nitrogen[J].Chinese Journal of Chromatography,2010,28(5):521-524.
[11] 周泽义,王德发,胡树国.挥发性有机物气体标准物质的研制[J].计量学报,2008,29(4):215-221.ZHOU Zeyi,WANG Defa,HU Shuguo.Preparation of Volatile Organic Compounds Certified Reference Materials[J].Acta Metrologica Sinica,2008,29(4):215-221.
[12] International Organization for Standardization.Gas Analysis-Preparation of Calibration Gas Mixtures-Gravimetric Method:ISO 6142:2001 [S/OL].[2001-04].https://www.iso.org/standard/24663.html.
[13] 吴忠祥,彭鸿俊,田文,等.甲烷气体标准样品的研制[J].中国环境监测,1999,15(6):30-35.WU Zhongxiang,PENG Hongjun,TIAN Wen,et al.Development on Standard Gas of Methane in Nitrogen[J].Environmental Monitoring of China,1999,15(6):30-35.
[14] 周鑫,李志昂,董了瑜,等.注射称量法配气中的称量线性研究及不确定度评定[J].化学试剂,2017,39(5):505-508.ZHOU Xin,LI Zhiang,DONG Liaoyu,et al.Weighing Linearity and Uncertainty Evaluation for Gravimetric Preparation of Reference Gas Mixture Using Injection Method[J].Chemical Reagents,2017,39(5),505-508.
[15] 方正,周鑫,霍玉朋,等.电子质量比较器在重量法配气中的称量不确定度评定[J].中国测试,2016,42(12):38-41.FANG Zheng,ZHOU Xin,HUO Yupeng,et al.Weighing Uncertainty Evaluation on Electronic Mass Comparator for Gravimetric Preparation of Reference Gas Mixture[J].China Measurement & Test,2016,42(12):38-41.
[16] 李宁,范洁,王倩,等.环境监测用5种氯代烯烃混合气体标准样品研制[J].中国环境监测,2014,30(5):101-104.LI Ning,FAN Jie,WANG Qian,et al.Development of a Standard Reference Material Containing 5 Chlorinated Hydrocarbons for Environmental Monitoring[J].Environmental Monitoring of China,2014,30(5):101-104.
[17] 郑力文,董了瑜,李志昂,等.氮气中多组分挥发性有机物(VOCs)气体标准物质的气相色谱-质谱分析方法研究[J].化工技术与开发,2017,46(1):25-28.ZHENG Liwen,DONG Liaoyu,LI Zhiang,et al.Study on 42 Components Volatile Organic Compounds Gas Standard Materials in Nitrogen Measured by GC-MS[J].Technology & Development of Chemical Industry,2017,46(1):25-28.
[18] 全国标准物质计量技术委员会.气体标准物质研制(生产)通用技术要求: JF 1344—2012[S].北京:中国标准出版社,2012.