利用电感耦合等离子体质谱法测定肥料重金属砷、镉、铅、铬含量  

The determination of arsenic,cadmium,lead and chromium in fertilizer by inductively coupled plasma mass spectrometer method

作　　者：李亚丽 刘蜜 郭伟[1,2,3] 王孝钢 汪洪 LI Ya-li;LIU Mi;GUO Wei;WANG Xiao-gang;WANG Hong(State Key Laboratory of Efficient Utilization of Arid and Semi-arid Arable Land in Northern China/Institute of Agricultural Resources and Regional Planning,Chinese Academy of Agricultural Sciences,Beijing 100081;China National Center for Quality Supervision and Test of Chemical Fertilizers(Beijing),Beijing 10081;Laboratory of Quality and Safety Risk Assessment for Agricultural Products from Fertilizer Sources(Beijing),Ministry of Agriculture and Rural Affairs,Beijing 100081;Qingdao Academy of Agricultural Sciences,Qingdao Shandong 266109)

机构地区：[1]北方干旱半干旱耕地高效利用全国重点实验室/中国农业科学院农业资源与农业区划研究所,北京100081 [2]国家化肥质量检验检测中心(北京),北京100081 [3]农业农村部农产品质量安全肥料源性因子风险评估实验室(北京),北京100081 [4]青岛市农业科学研究院,山东青岛266109

出　　处：《中国土壤与肥料》2024年第2期235-243,共9页Soil and Fertilizer Sciences in China

基　　金：国家重点研发计划项目(2022YFD1700603);国家农产品质量安全风险评估项目(GJFP2019035,GJFP2019037);中央级公益性科研院所基本科研业务费专项(Y2019PT20-04,1610132019018)。

摘　　要：选取7个不同的肥料样品,采用硝酸-盐酸(王水)消解,消解液中砷(As)、镉(Cd)、铅(Pb)、铬(Cr)重金属元素含量采用电感耦合等离子体质谱(ICP-MS)法氦碰撞模式测定。结果显示,根据固体称重量为0.2 g,定容体积50 mL,Cr、As、Cd、Pb方法检出限分别为0.018、0.008、0.005、0.021 mg/kg,定量限分别为0.061、0.025、0.016、0.069 mg/kg,根据液体称重量1.0 g,定容体积50 mL,Cr、As、Cd、Pb方法检出限分别为0.004、0.002、0.001、0.004 mg/kg,定量限分别为0.012、0.005、0.003、0.014 mg/kg,待测样品分别进行6组重复测定,结果显示Cr相对标准偏差(RSD)在3.8%~16.8%之间,As的RSD为3.9%~56.5%,Cd的RSD为0.0%~25.7%,Pb的RSD为4.2%~24.5%,样品加标回收率为67.4%~122.0%。4家实验室对不同肥料种类抽取样品进行实验室比对测定,分析显示所有参与实验室测试值之间存在一致性,经柯克伦检验剔除离群值,保留歧离值后,将格拉布斯检验应用于通过柯克伦检验后的单元平均值,各元素均未发现有单个或成对歧离值或离群值存在。方法精密度和准确度满足要求,结论认为ICP-MS可用于肥料中As、Cd、Pb、Gr含量的测定分析。Seven different fertilizer samples were selected for digestion by nitric acid-hydrochloric acid(aqua regia).The contents of heavy metals such as arsenic(As),cadmium(Cd),lead(Pb)and chromium(Cr)in the digestion solution were determined by helium collision mode using an inductively coupled plasma mass spectrometer(ICP-MS)method.The results showed that:based on the solid weight of 0.2 g and the constant volume of 50 mL,the detection limits of Cr,As,Cd and Pb were 0.018,0.008,0.005 and 0.021 mg/kg,respectively,and the limits of quantification were 0.061,0.025,0.016 and 0.069 mg/kg,respectively.According to the liquid weight of 1.0 g and the constant volume of 50 mL,the detection limits of Cr,As,Cd and Pb were 0.004,0.002,0.001 and 0.004 mg/kg,respectively,and the limits of quantification were 0.012,0.005,0.003 and 0.014 mg/kg,respectively.The relative standard deviation of Cr,As,Cd and Pb(n=6)were 3.8%-16.8%,3.9%-56.5%,0-25.7%and 4.2%-24.5%,respectively.The recoveries were 67.4%-122.0%.Samples of different fertilizer types were extracted from four laboratories for laboratory comparison,and the analysis showed that there was consistency between the test values of all the participating laboratories.After the outliers were removed by the Cochran test and the outliers were retained,the Grubbs test was applied to the unit average after passing the Cochran test,and no single or pairs of outliers or outliers were found for each element.The precision and accuracy of the method meet the requirements.Conclusion suggested that ICP-MS could be used for the determination of As,Cd,Pb and Cr in fertilizer.

关 键 词：重金属 电感耦合等离子体质谱 实验室比对 

分 类 号：TQ440.72[化学工程—化学肥料工业] O657.63[理学—分析化学]