针对环境评价性土壤,采用HNO3-HClO4-HF消解样品、HNO3提取技术,以52 Cr、65 Cu、114 Cd、208 Pb作为测定同位素,采用间接经验公式校正质谱干扰,最终实现了电感耦合等离子体质谱法(ICP-MS)同时对Cr、Cu、Cd、Pb等4种重金属的测定.详细对比分析了HCl-HNO3-HClO4-HF、HCl-HNO3-H2 SO4-HF、HNO3-HClO4-HF消解法等3种试样处理方法对土壤成分分析标准物质的分析数据,结果表明:HNO3-HClO4-HF消解法测定值与认定值相符.Cr、Cu、Cd、Pb的校准曲线相关系数均达0.9999以上,方法测定限(μg·L-1)分别为:Cr 1.54,Cu 0.83,Cd 0.024,Pb 0.29.将方法应用于土壤4种重金属元素的测定,结果与认定值基本一致,相对标准偏差(RSD,n=12)均小于8％,加标回收率在96.7％ ～102.3％.方法应用于实际环境评价性土壤样品分析,结果与X射线荧光光谱法(XRF)相吻合.%The environmental evaluation soils were decomposed by mixed acid of HNO3-HF-HClO4 and extracted by HNO3. 52Cr,65 Cu,114 Cd and 208 Pb were chosen as determining isotopes and the mass spectral interference were calibrated by the indirect experi-ence formula. Four trace elements of Cr,Cu,Cd and Pb were successfully determined by inductively coupled plasma-mass spectrom-etry(ICP-MS). The experimental data were contrasted in details with the other three digestion methods such as HCl-HNO3-HClO4-HF,HCl-HNO3-H2 SO4-HF and HNO3-HClO4-HF. The results show that the correlation coefficients of calibration curves were both up to 0. 9999. The detection limits(10SD,μg·L-1 )are1. 54 for Cr,0. 83 for Cu,0. 024 for Cd and 0. 29 for Pb. The measured val-ues with the proposed method were in consistent with the certified values,the relative standard deviations(RSD,n=12)were less than 8％,and the recoveries were between 96. 7％ ～102. 3％. In the analysis of the actual environmental evaluation soil samples, the results were consistent with those obtained by XRF.
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