农药乳油中有害溶剂混合二级标准物质的研制
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摘要
对研制的农药乳油中有害溶剂(甲醇、苯、甲苯、二甲苯、N,N-二甲基甲酰胺)混合元素二级标准物质进行了均匀性、稳定性的评估和检测。确立了气相色谱检测方法,采用氢火焰离子化检测器(FID),DB-1301毛细管色谱柱,以正癸烷为内标,并用8家实验室联合定值的方法对标准物质进行了定值及不确定度评定。所研制的混合元素二级标准物质均匀性良好,保质期至少可达7个月。定值方法正确、可靠,量值准确,符合二级标准物质的规范要求。
The evaluation and detection of the uniformity and stability of secondary standard material for harmful solvents(methanol;benzene;methylbenzene;dimethylbenzene;N,N-dimethylformamide)in emulsifiable concentrate pesticide were carried out.The detection was performed with an Agilent 7890 gas chromatography equipped with a flame ionization detector(FID)and a DB-1301 capillary packed column.nDecane was selected as internal standard and we cooperated with other seven laboratories to get the fixed value of the standard material for making the uncertainty evaluation.The secondary standard material has good uniformity and remains stable for at least 7 months.The evaluation method is correct,reliable,and accurate and it complies with the standard requirements of the two level standards.
The evaluation and detection of the uniformity and stability of secondary standard material for harmful solvents(methanol;benzene;methylbenzene;dimethylbenzene;N,N-dimethylformamide)in emulsifiable concentrate pesticide were carried out.The detection was performed with an Agilent 7890 gas chromatography equipped with a flame ionization detector(FID)and a DB-1301 capillary packed column.nDecane was selected as internal standard and we cooperated with other seven laboratories to get the fixed value of the standard material for making the uncertainty evaluation.The secondary standard material has good uniformity and remains stable for at least 7 months.The evaluation method is correct,reliable,and accurate and it complies with the standard requirements of the two level standards.
引文
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[3]QUAN H,HAN Y Z.Standard Material and its Application Technique(2nd Edition)[M].Beijing:Standards Press of China,2003(in Chinese).(全浩、韩永志.标准物质及其应用技术(第二版)[M].北京:中国标准出版社,2003.)
[4]HUA N Z Crisis and Development Trend of Emulsifiable Concentrate[J].Pestic Mark News,2012,(10):4-6(in Chinese).(华乃震,乳油的危机与今后发展趋势[J].农药市场信息,2012(10):4-6.)
[5]China Pesticide Industry Association.Limit of harmful solvent of emulsifiable concentrate pesticide:HG/T 4576-2013[S].Beijing:Chemical Industry Press,2014(in Chinese).(中国农药工业协会.农药乳油中有害溶剂限量:HG/T 4576-2013[S].北京:化学工业出版社,2014.)
[6]National Research Center for Certified Reference Materials.Technical Specification for Grade A Certified Reference Materials:JJG 1006-1994[S].Beijing:China Metrology Publishing House,1994(in Chinese).(国家标准物质研究中心.一级标准物质计量技术规范:JJG 1006-1994[S].北京:中国计量出版社,1994.)
[7]National Chemical Standard Materials Committee.Analytical Test and Quality Assurance[M].Liaoniang:Liaoning University Press,2004(in Chinese).(全国化工标准物质委员会.分析测试质量保证[M].辽宁:辽宁大学出版社,2004.)
[8]JIANG Z G,GU X M.Mathematical Statistics and Quality Assurance in Analysis and Testing[M].Shanghai:East China Institute of Chemical Technology Press,1991(in Chinese).(蒋子刚,顾雪梅.分析测试中的数理统计与质量保证[M].上海:华东化工学院出版社,1991.)
[9]Secretariat of National Standard Sample Technical Committee.Directives for the Work of Reference Materials(3)-Reference Materials-General and Statistical Principles for Certification GB/T 15000.3-2008[S].Beijing:Standards Press of China,2008(in Chinese).(全国标准样品技术委员会秘书处.标准样品工作导则(3)标准样品定值的一般原则和统计方法GB/T15000.3-2008[S].北京:中国标准出版社,2008.)
[10]The Management Committee of the National Standards.Development,Management and Application of Reference Materials[M].Beijing:China Metrology Publishing House,2010(in Chinese).(全国标准物质管理委员会.标准物质的研制、管理与应用[M].北京:中国计量出版社,2010.)
[11]Jiangsu Academy of Metrology.Evaluation and Expression of Uncertainty in Measurement JJF 1059.1-2012[S].Beijing:China Zhijian Publishing House,Standards Press of China,2013(in Chinese).(江苏省计量科学研究院.测量不确定度评定与表示JJF 1059.1-2012[S].北京:中国质检出版社,中国标准出版社,2013.)