气相质谱仪校准用氮气中4组分混合气体标准物质的研制
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摘要
介绍0.1μmol/mol气相质谱仪校准用氮气中4组分混合气体标准物质的研制方法。标准气体的组分为溴氯甲烷、1,4-二氟苯、氯苯-D5和4-溴氟苯,所采用的制备及分析方法分别为注射称量法和GC-MS法。通过瓶内压力及各组分浓度随时间的变化考察其浓度的均匀性和稳定性。对标准气体的制备过程及均匀性和稳定性引入的不确定度进行评定。实验结果表明,4组分混合气体标准物质在0.5～10 MPa范围内具有较好的压力均匀性和稳定性,其相对扩展不确定度为5.0%(k=2),使用有效期为1年。
The development method of gas chromatography-mass spectrometry calibration of 4 components that containing bromochloromethane, 1,4-difluorobenzene, chlorobenzene-D5 and 4-bromofluorobenzene at0.1 μmol/mol in nitrogen gas reference material is described The gas standard is prepared by gravimetric preparation method and is intercompared to the existing gas cylinder standard using gas chromatography with a mass spectrometry detector. Relationships between time or pressure and homogeneity or stability were also investigated. The paper also evaluated the uncertainties from preparation using gravimetric method, uniformity and stability. All the research results indicated that have been better homogeneity and stability between0.5 MPa and 10 MPa and an estimated relative expanded uncertainty of 5%(k=2) with one year shelf life have been achieved.
The development method of gas chromatography-mass spectrometry calibration of 4 components that containing bromochloromethane, 1,4-difluorobenzene, chlorobenzene-D5 and 4-bromofluorobenzene at0.1 μmol/mol in nitrogen gas reference material is described The gas standard is prepared by gravimetric preparation method and is intercompared to the existing gas cylinder standard using gas chromatography with a mass spectrometry detector. Relationships between time or pressure and homogeneity or stability were also investigated. The paper also evaluated the uncertainties from preparation using gravimetric method, uniformity and stability. All the research results indicated that have been better homogeneity and stability between0.5 MPa and 10 MPa and an estimated relative expanded uncertainty of 5%(k=2) with one year shelf life have been achieved.
引文
[1]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.
[2] YANG K L. Evaluation of capillary gas chromatography for the measurement of hydrocarbons by participating in an intercomparison experiment[J]. chromatographia, 1997,44(7/8):11-15.
[3] SCHM D T.William P, et al Preparation of gas cylinder standards for the measurement of trace levels of benzene and tetrachloroethylene[J]. Anal Chem, 1983(55):290-294.
[4] RHODERICK G C. Development of a fifteen component hydrocarbon gas standard reference material at 5nmol/mol in nitrogen[J]. Fresenius J Anal Chem, 1997(359):477-483.
[5]环境空气挥发性有机物的测定罐采样/气相色谱-质谱法:HJ759-2015[S].北京:中国环境科学出版社,2015.
[6]董了瑜,舒琳雅,李志昂,等.瓶装氮气中22组分挥发性卤代烃混合气体标准物质的研制[J].中国测试,2017, 43(10):32-36.
[7] MILTON M J T,VARGHA G M,BROWN A S. Gravimetric methods for the preparation of standard gas mixtures[J].Metrologia,2011,48(5):1-9.
[8] Gas analysis-Preparation of calibration gas mixtures Gravimetricmethod:ISO 6142-2001[S]. Geneva:International Organization for Standardization, 2001.
[9]中国国家标准管理化委员会.中华人民共和国国家标准:GB/T 5274-2008气体分析校准用混合气体的制备称量法[S].北京:中国标准出版社,2008:6
[10]气体标准物质研制(生产)通用技术要求:JJF 1344-2012[S].北京:中国质检出版社,2012.
[11]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(5):101-104.
[12]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.
[13]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.
[14] ALINK A, VAN D V. Uncertainty calculations for the preparationof primary gas mixtures[J]. Metrologia,2000,37(6):641-650.
[15]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.
[16]方正,周鑫,潘义.氮气中1μmol·mol~(-1)硫化氢气体标准物质的研制[J].化学研究与应用,2014, 26(11):1809-1812.
[2] YANG K L. Evaluation of capillary gas chromatography for the measurement of hydrocarbons by participating in an intercomparison experiment[J]. chromatographia, 1997,44(7/8):11-15.
[3] SCHM D T.William P, et al Preparation of gas cylinder standards for the measurement of trace levels of benzene and tetrachloroethylene[J]. Anal Chem, 1983(55):290-294.
[4] RHODERICK G C. Development of a fifteen component hydrocarbon gas standard reference material at 5nmol/mol in nitrogen[J]. Fresenius J Anal Chem, 1997(359):477-483.
[5]环境空气挥发性有机物的测定罐采样/气相色谱-质谱法:HJ759-2015[S].北京:中国环境科学出版社,2015.
[6]董了瑜,舒琳雅,李志昂,等.瓶装氮气中22组分挥发性卤代烃混合气体标准物质的研制[J].中国测试,2017, 43(10):32-36.
[7] MILTON M J T,VARGHA G M,BROWN A S. Gravimetric methods for the preparation of standard gas mixtures[J].Metrologia,2011,48(5):1-9.
[8] Gas analysis-Preparation of calibration gas mixtures Gravimetricmethod:ISO 6142-2001[S]. Geneva:International Organization for Standardization, 2001.
[9]中国国家标准管理化委员会.中华人民共和国国家标准:GB/T 5274-2008气体分析校准用混合气体的制备称量法[S].北京:中国标准出版社,2008:6
[10]气体标准物质研制(生产)通用技术要求:JJF 1344-2012[S].北京:中国质检出版社,2012.
[11]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(5):101-104.
[12]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.
[13]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.
[14] ALINK A, VAN D V. Uncertainty calculations for the preparationof primary gas mixtures[J]. Metrologia,2000,37(6):641-650.
[15]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.
[16]方正,周鑫,潘义.氮气中1μmol·mol~(-1)硫化氢气体标准物质的研制[J].化学研究与应用,2014, 26(11):1809-1812.