微波消解/ICP-MS测定水系沉积物中的9种重金属元素

优化了微波消解进行沉积物样品前处理的方法,选择了HNO3-H2O2-HF体系。以Ge,In,Bi为内标元素,建立了电感耦合等离子体质谱(ICP-MS)同时测定Cr,Mn,Ni,Co,Cu,Zn,Cd,Sb,Pb九种重金属元素含量的方法。该方法的相关系数都在3个9以上,测定了国家标准物质ESS-1GSBZ50011-88土壤中的元素,测定值与标准值或参考值一致,相对标准偏差0.48%～5.73%,加标回收率98.0%～100.7%,检出限在0.011～0.328μg.L-1。利用建立的方法测定了白洋淀11个代表性点位的水系沉积物中的九种重金属元素含量,为环境中土壤及水系沉积物中重金属元素含量的测定提供了可靠的分析方法。

Determination of 9 heavy metal elements in sediment by ICP-MS using microwave digestion for sample preparation

A method for determining 9 heavy metal elements in soil and sediment was developed by using microwave digestion-ICP-MS. The mixture of HNO3-H2O2-HF was found to give the best digestion results for soil and sediment of samples. Under the optimized conditions, the samples were analyzed by ICP-MS with the triple internal standard elements Ge, In and Bi. The results showed that all their correlation coefficients were over 0.999. The national standard soil referenee material (ESS-1 GSBZ50011-88) was analyzed by the described method and the results were accorded with the reference values. The measurement precision range was from 0.48% to 5.73% in terms of relative standard deviation. The recoveries and the limits of detection were in the ranges of 98.0% to 100.7% and 0.011 to 0.328 microg x L(-1) respectively, and 11 sediment samples were determined by the proposed method. It was indicated that the method was reliable for determining heavy metal elements in soil and sediment samples.