X射线荧光光谱(XRF)法测定土壤污染样品中9种重金属元素
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摘要
采用粉末压片法制样,利用理学ZSX PrimusⅡX射线荧光光谱仪,用国家标准物质土壤(GSS系列)、沉积物(GSD系列)、环境保护部标准样品研究所研制的土壤标准样品GSB Z 50011-88(黑钙土)、GSB Z 50012-88(棕壤)、GSB Z 50013-88(红壤)、GSB Z 50014-88(褐土)、湖南污染土壤标准(GBW0732729)作标准样品,建立了X射线荧光光谱(XRF)法测定农业地质土壤污染物样品中的Cu、Pb、Cr、Ni、Zn、Co、As、Mn、V等9种重金属元素的方法,采用经验系数法校正谱线重叠干扰和基体校正。用3个土壤考核样品和环境保护部标准样品研究所研制的GSB07-3272-2015作为样品评估方法的准确度和精密度,结果符合《全国土壤污染状况详查土壤样品分析测试方法技术规定》中规定的Cu、Pb、Cr、Ni、Zn、Co、As、Mn、V元素检测方法质量要求。
Soil standard samples GSB Z 50011-88(black calcareous soil),GSB Z 50012-88(brown soil),GSB Z 50013-88(red soil),GSB Z 50014-88(cinnamon soil)developed by National Standard Soil(GSS series),Sediment(GSD series)and Institute of Standard Samples of Ministry of Environmental Protection(Institute of Standard Samples)were prepared by powder pressing method and ZSX Primus II X-ray fluorescence spectrometer.The dyed soil standard(GBW0732729)was used as the standard sample to establish an XRF method for the determination of nine heavy metal elements,namely,Cu,Pb,Cr,Ni,Zn,Co,As,Mn and V,in agricultural geological soil pollutant samples.Empirical coefficient method was used to correct overlapping interference of spectral lines and matrix correction.GSB07-3272-2015,developed by the Institute of Standard Samples of the Ministry of Environmental Protection,was used as a sample to evaluate the accuracy and precision of the method.The results met the quality requirements of the above-mentioned elements in the Technical Regulations for the Analysis and Testing of Soil Samples for the National Detailed Investigation of Soil Pollution.
Soil standard samples GSB Z 50011-88(black calcareous soil),GSB Z 50012-88(brown soil),GSB Z 50013-88(red soil),GSB Z 50014-88(cinnamon soil)developed by National Standard Soil(GSS series),Sediment(GSD series)and Institute of Standard Samples of Ministry of Environmental Protection(Institute of Standard Samples)were prepared by powder pressing method and ZSX Primus II X-ray fluorescence spectrometer.The dyed soil standard(GBW0732729)was used as the standard sample to establish an XRF method for the determination of nine heavy metal elements,namely,Cu,Pb,Cr,Ni,Zn,Co,As,Mn and V,in agricultural geological soil pollutant samples.Empirical coefficient method was used to correct overlapping interference of spectral lines and matrix correction.GSB07-3272-2015,developed by the Institute of Standard Samples of the Ministry of Environmental Protection,was used as a sample to evaluate the accuracy and precision of the method.The results met the quality requirements of the above-mentioned elements in the Technical Regulations for the Analysis and Testing of Soil Samples for the National Detailed Investigation of Soil Pollution.
引文
[1]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)[2017-11-07]http://www.zhb.gov.cn/g km l/hbb/bgth/201711/t20171106_425226.htm.
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[3]李可及,赵改红,赵朝辉,等.变稀释比熔融制样-X射线荧光光谱分析钼矿石[J].分析仪器(Analysis instrument),2018(2):188-192.
[4]马景治.X射线荧光光谱法快速测定灰岩样品中主、次量组分[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(6):42-45.
[5]常利民,刘峰,王晓霞,等.基于熔融制样测量钛铁中5种成份的研究[J].中国测试(China Test),2017(增刊1):68-71.
[6]邓述培,苏卫汉.波长色散XRF法测定湘西李家桥测区2.3万个化探样品中6种微量元素[J].湖南有色金属(Hunan Nonferrous Metals),2012(3):72-74.
[7]邓述培,徐红柳,肖立青,等.理学ZSX PrimusⅡX射线荧光光谱仪日常维护及常见故障维修[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(5):67-70.
[8]邓述培,范鹏飞,孙云超,等.理学ZSX PrimusⅡX射线荧光光谱仪E-Z扫描在盲矿石样中的应用[J].世界有色金属(World Nonferrous Metals),2018(14):190-192.
[9]张勤,樊守忠,潘宴山,等.X射线荧光光谱法测定多目标地球化学调查样品中主次痕量组分[J].岩矿测试(Rock and Mineral Testing),2004,23(1):19-24.
[10]全国国土资源标准化技术委员会.区域地球化学样品分析方法第1部分:三氧化二铝等24个成分测定粉末压片-X射线荧光光谱法:DZ/T 0279.1-2016[S].北京:中国地质出版社,2016.
[11]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会土壤质量总汞、总砷、总铅的测定原子荧光法第2部分:土壤中总砷的测定:GBT 22105.2—2008[S].北京:中国标准出版社,2008.