Determination of 7 Metal Elements in Agricultural Soil by Automatic Graphite Digestion-Inductively Coupled Plasma Mass Spectrometry
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建立全自动石墨消解-电感耦合等离子体质谱(ICP-MS)法测定土壤中Cd、As、Pb、Cr、Cu、Ni、Zn 7种元素.采用 8 mL HNO3+5 mL HCl+5 mL HF+1 mL HClO4 酸体系消解 3 h,设定 160℃赶酸温度,以Rh-Re为内标定量,电感耦合等离子体质谱仪选取碰撞模式测定土壤样品.结果显示:7种不同元素在一定线性范围内相关性良好,相关系数均大于 0.999,检出限为 0.02～0.5 mg/kg,定量限为 0.08～2.0 mg/kg.土壤有证标准物质测定结果的相对标准偏差为 0.9%～6.1%,相对误差为-8.9%～7.6%.水稻田、果园、人工草地 3种典型农用地土壤样品中 7种元素加标回收率分别为 85.4%～109.0%、86.4%～102.0%、85.8%～99.0%.方法的检出限低、精密度和正确度高,满足农用地土壤污染状况详查质量保证与质量控制的技术规定.
An automatic graphite digestion-inductively coupled plasma mass spectrometry(ICP-MS)has been established for the determination of 7 elements,Cd,As,Pb,Cr,Cu,Ni and Zn in soil.The soil samples were digested with 8 mL HNO3+5 mL HCl+5 mL HF+1 mL HClO4 system for 3 h,with a acid driving temperature of 160℃.After digestion,the soil samples were quantified by Rh-Re as the internal standard and determined using the collision mode of inductively coupled plasma mass spectrometer.The results showed that the 7 elements had good correlation within a certain linear range,with correlation coefficients all greater than 0.999.The limits of detection were 0.02～0.5 mg/kg,and the limits of quantitation were 0.08～2.0 mg/kg.The relative standard deviation of the determination results of certified reference materials in soil was 0.9%～6.1%,and the relative error was-8.9%～7.6%.The spiked recoveries of the 7 elements in three typical agricultural soils,namely paddy fields,orchards,and artificial grasslands,were 85.4%～109.0%,86.4%～102.0%,and 85.8%～99.0%,respectively.The method has a low detection limit,high precision and accuracy,and can meet the technical requirements for quality assurance and quality control of detailed investigation of pollution in agricultural soil.
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