电感耦合等离子体质谱（ICP-MS）法测定垃圾焚烧飞灰中的重金属

Determination of Heavy Metals in Fly Ash of Waste Incineration by Inductively Coupled Plasma Mass Spectrometry

基于全自动消解仪优化程序,以HNO3-HF-HClO4消解体系消解飞灰样品,通过选择合适的待测同位素以及干扰元素校正方程校正质谱干扰,建立了全自动消解-电感耦合等离子质谱(ICP-MS)法测定飞灰样品中铍、钒、铬、锰、镍、铜、锌、镉、铅等9种元素的新方法。采用嵌片技术和碰撞模式消除基体干扰,采用单一内标103Rh进行信号漂移校正,9种元素校准曲线的线性相关系数均大于0.999,方法检出限在0.01~0.3μg/g。用飞灰标准物质SRM1633C进行验证,平均相对标准偏差RSD在0.54%~2.4%,加标回收率为85%~120%,各元素的测定值与标准值吻合。方法具有较好的准确度和精密度,适合垃圾焚烧产生飞灰样品中全量金属的测定。

To understand the contents of metal elements in fly ash,the new method which comprised the automatic digestion system optimization program,and the efficient mixed acid digestion system(HNO 3+HF+HClO 4) was established to measure the 9 elements in fly ash samples.Through selecting suitable isotopes and calibrating equation of interference elements to correct the mass spectrometry interference,the chip technology and collision mode were used to eliminate matrix interference,and the single internal standard 103 Rh was used to correct signal drift.ICP-MS arose highly representation on beryllium,vanadium,chromium,manganese,nickel,copper,zinc,cadmium and lead elements analysis.The calibration curve r >0.999,the detection limit of the method between 0.01-0.30 μg/g.The method was validated by SRM1633C,average RSD was between 0.54%-2.4%,and the recovery rate was 85%-120%,the measured values of each element were in agreement with the standard values.The method is suitable for the determination of total metals in fly ash samples from waste incineration with its good accuracy and precision.