电感耦合等离子体质谱同时测定沉积物中12种重金属元素

SIMULTANEOUS DETERMINATION OF TWELVE HEAVY METALS IN SEDIMENT BY ICP-MS

比较了王水回流、密闭容器消解及微波消解3种不同方法对海洋沉积物的消解效果,结果表明微波消解效果较好;优化了消解体系和程序,HNO3-HF-H2O2消解体系对重金属的溶出效果较好;并建立了电感耦合等离子体质谱测定沉积物中Cr、Co、Ni、Cu、Zn、Mo、Cd、Sn、Hg、Tl、Pb、U等12种重金属元素的分析方法,各元素的线性关系良好(r=0.9998-1.0000),检出限为2.2—66.0 ng.g-1,Rh和Re元素的加标回收率均在91.2%—106.9%之间,利用该方法分析了标准物质MESS-3,测定值与参考值吻合较好,相对标准偏差(RSD)为1.2%—5.7%,该方法的精密度和准确性良好.

Three digestion methods were investigated to compare their effects on the determination of twelve heavy metal elements（Cr,Co,Ni,Cu,Zn,Mo,Cd,Sn,Hg,Tl,Pb,U） in certified reference materials.The results showed that the efficiency of microwave digestion was better than the other two digestion methods.A mixed digestion system of HNO3-HF-H2O2 was used with a better digestion effect.A method based on inductively coupled plasma-mass spectrometric（ICP-MS） analysis was established for the determination of the twelve heavy metals in sediments.Good linearity of the calibration curves was obtained for these elements（r=0.9998—1.0000）.Detection limits for these twelve elements were in the range of 2.2 ng · g-1 to 66.0 ng · g-1,and the recoveries of Rh and Re elements were in the range of 91.2% to 106.9%.The MESS-3 standard reference material was determined with this method,and the results of twelve elements were in good agreement with the reference values.The RSD varied from 1.2% to 5.7%,which showed that the method had high precision.