实验室土壤质控样品重金属测试结果允许相对误差判据研究
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摘要
实验室内部质控体系对于维护检测实验室正常运转具有重要意义。定期核查质控样品分析结果并进行准确度评估,是质控体系正常运行的基本要求。合理选择评估判据是质控规范的重要内容。论文以土壤、沉积物系列标准样品中土壤详查目标重金属元素(As、Be、Cd、Co、Cr、Cu、Hg、Mo、Mn、Ni、Pb、Sb、Tl、V、Zn等)含量认定值及扩展不确定度数据为基础,利用非线性拟合工具,建立了目标元素允许相对误差经验模型,探讨并提出了实验室内部质控样品重金属元素分析结果合格性新判据,并与目前正在执行的地质部门质控规范和生态环境部相关质控技术规定进行了比较。提出的技术途径对于正在修订的地质部门实验室质控规范具有参考价值。
The internal quality control system of laboratory is of great significance to maintain the normal operation of testing laboratory.The periodic verification of analysis results of quality control samples as well as accuracy evaluation is the basic requirement for the normal operation of quality control system.The reasonable selection of evaluation criterion is an important content in quality control specifications.Based on the certified values and expanded uncertainty data for the contents of target heavy metals(As,Be,Cd,Co,Cr,Cu,Hg,Mo,Mn,Ni,Pb,Sb,Tl,V and Zn,etc)in series standard samples of soil and sediment,the empirical model of allowable relative error for target elements was established using the nonlinear fitting tool.New criterion for the analysis results of heavy metal elements in internal quality control samples of laboratory was discussed and proposed.It was compared with the related quality control specifications which were being executed by the departments of geology and ecological environment.The proposed technological approach had reference value for the quality control specifications in laboratory which were being revised by department of geology.
The internal quality control system of laboratory is of great significance to maintain the normal operation of testing laboratory.The periodic verification of analysis results of quality control samples as well as accuracy evaluation is the basic requirement for the normal operation of quality control system.The reasonable selection of evaluation criterion is an important content in quality control specifications.Based on the certified values and expanded uncertainty data for the contents of target heavy metals(As,Be,Cd,Co,Cr,Cu,Hg,Mo,Mn,Ni,Pb,Sb,Tl,V and Zn,etc)in series standard samples of soil and sediment,the empirical model of allowable relative error for target elements was established using the nonlinear fitting tool.New criterion for the analysis results of heavy metal elements in internal quality control samples of laboratory was discussed and proposed.It was compared with the related quality control specifications which were being executed by the departments of geology and ecological environment.The proposed technological approach had reference value for the quality control specifications in laboratory which were being revised by department of geology.
引文
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[12]殷惠民,杜祯宇,李玉武,等.能量色散X射线荧光光谱仪和简化的基体效应校正模型测定土壤、沉积物中重金属元素[J].冶金分析,2018,38(4):1-10.YIN Hui-min,DU Zhen-yu,LI Yu-wu,et al.Determination of heavy metal elements in soil and sediment by energy dispersive X-ray fluorescence spectrometer and simplified matrix effect correction model[J].Metallurgical Analysis,2018,38(4):1-10.
[13]Thomas Linsinger.Application Note 1:Comparison of a measurement result with the certified value[EB/OL].(2005-01)[2018-9-24].https://www.researchgate.net/publication/284405063_Comparison_of_a_measurement_result_with_the_certified_value.
[14]李玉武,狄一安,孙海容,等.用经验模型评估环境样品测量不确定度[J].中国无机分析化学,2012,2(1):1-8.LI Yu-wu,DI Yi-an,SUN Hai-rong,et al.Evaluation of measurement uncertainty for environmental sample by empirical model[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(1):1-8.
[15]Horwitz W.Evaluation of analytical methods used for regulation of foods and drugs[J].Anal.Chem.,1982,54:67A-76A.
[16]DesiréL Massart,Johanna Smeyers-Verbeke,Yvan Vander Heyden.Benchmarking for analytical methods:The Horwitz curve[J].LCGC EUROPE,2005,18(10):528-531.
[17]Boyer K W,Horwitz W,Albert R.Interlaboratory variability in trace element analysis[J].Anal.Chem.,1985,57:454-459.
[18]Horwitz W,Kamps L R,Boyer I W,et al.Quality assurance in the analysis of foods for trace constituents[J].J.Assoc.Off.Anal.Chem.,1980,63:1344-1354.
[19]Margosis M,Horwitz W,Albert R.Performance characteristics of methods of analysis used for regulatory purposes.I.Drug dosage forms.F.Gravimetric and titrimetric methods[J].J.Assoc.Off.Anal.Chem.,1988,71:619-635.
[20]Horwitz W,Britton P,Chitrel S J.A simple method for evaluating data from an interlaboratory study[J].J.Assoc.Off.Anal.Chem.,1998,81:1257-1265.
[2]生态环境部.农用地土壤污染状况详查质量保证与质量控制技术规定[EB/OL].(2017)[2018-09-15].http://www.docin.com/p-2059522788.html.
[3]生态环境部.重点行业企业用地调查质量保证与质量控制技术规定[EB/OL].(2017)[2018-09-15].http://www.docin.com/p-2069182395.html.
[4]环境保护部科技标准司.HJ/T 166-2004土壤环境监测技术规范[S].北京:中国环境科学出版社,2004.
[5]环境保护部科技标准司.HJ 780-2015土壤和沉积物无机元素的测定波长色散X射线荧光光谱法[S].北京:中国环境科学出版社,2015.
[6]土壤和沉积物22种无机元素的测定酸溶/电感耦合等离子发射光谱法(征求意见稿)[EB/OL].(2018-06-06)[2018-09-15].http://www.mee.gov.cn/gkml/sthjbgw/stbgth/201806/W020180620510928672563.pdf.
[7]土壤和沉积物铜、锌、铅、镍、铬的测定火焰原子吸收分光光度法(征求意见稿)[EB/OL].(2018-08-24)[2018-09-15].http://www.mee.gov.cn/gkml/sthjbgw/stbgth/201808/W020180831567410880879.pdf.
[8]杨冬雪.土壤监测几种质量控制指标及评价方法探讨[J].中国环境监测,2010,26(4):78-82.YANG Dong-xue.Research on quality control index system and evaluation method of soil monitoring[J].Environmental Monitoring in China,2010,26(4):78-82.
[9]环境保护部办公厅,国土资源部办公厅,农业部办公厅.关于印发全国土壤污染状况详查样品分析测试方法系列技术规定的通知附件.全国土壤污染状况详查土壤样品分析测试方法技术规定[EB/OL].(2017-10-23)[2018-9-24].http://www.zhb.gov.cn/gkml/hbb/bgth/201711/t20171106_425226.htm.
[10]中国地质科学院地球物理地球化学勘察研究所.国家一级地球化学标准物质证书集(1982-2012)[EB/OL].(2017-09-15)[2018-01-05].https://wenku.baidu.com/view/a0613b370a4e767f5acfa1c7aa00b52acfc79c1c.html.
[11]殷惠民,杜祯宇,任立军,等.波长色散X射线荧光光谱谱线重叠和基体效应校正系数有效性判断及在土壤、沉积物重金属测定中的应用[J].冶金分析,2018,38(7):1-11.YIN Hui-min,DU Zhen-yu,REN Li-jun,et al.Coefficient effectiveness judgment of overlapping line and matrix effect correction in wavelength dispersive X-ray fluorescence spectrometry and its application in determination of heavy elements in soil and sediment samples[J].Metallurgical Analysis,2018,38(7):1-11.
[12]殷惠民,杜祯宇,李玉武,等.能量色散X射线荧光光谱仪和简化的基体效应校正模型测定土壤、沉积物中重金属元素[J].冶金分析,2018,38(4):1-10.YIN Hui-min,DU Zhen-yu,LI Yu-wu,et al.Determination of heavy metal elements in soil and sediment by energy dispersive X-ray fluorescence spectrometer and simplified matrix effect correction model[J].Metallurgical Analysis,2018,38(4):1-10.
[13]Thomas Linsinger.Application Note 1:Comparison of a measurement result with the certified value[EB/OL].(2005-01)[2018-9-24].https://www.researchgate.net/publication/284405063_Comparison_of_a_measurement_result_with_the_certified_value.
[14]李玉武,狄一安,孙海容,等.用经验模型评估环境样品测量不确定度[J].中国无机分析化学,2012,2(1):1-8.LI Yu-wu,DI Yi-an,SUN Hai-rong,et al.Evaluation of measurement uncertainty for environmental sample by empirical model[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(1):1-8.
[15]Horwitz W.Evaluation of analytical methods used for regulation of foods and drugs[J].Anal.Chem.,1982,54:67A-76A.
[16]DesiréL Massart,Johanna Smeyers-Verbeke,Yvan Vander Heyden.Benchmarking for analytical methods:The Horwitz curve[J].LCGC EUROPE,2005,18(10):528-531.
[17]Boyer K W,Horwitz W,Albert R.Interlaboratory variability in trace element analysis[J].Anal.Chem.,1985,57:454-459.
[18]Horwitz W,Kamps L R,Boyer I W,et al.Quality assurance in the analysis of foods for trace constituents[J].J.Assoc.Off.Anal.Chem.,1980,63:1344-1354.
[19]Margosis M,Horwitz W,Albert R.Performance characteristics of methods of analysis used for regulatory purposes.I.Drug dosage forms.F.Gravimetric and titrimetric methods[J].J.Assoc.Off.Anal.Chem.,1988,71:619-635.
[20]Horwitz W,Britton P,Chitrel S J.A simple method for evaluating data from an interlaboratory study[J].J.Assoc.Off.Anal.Chem.,1998,81:1257-1265.
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