三酸消解-电感耦合等离子体质谱法测定土壤中钆、镝、铒、镱

Determination of Gd,Dy,Er,Yb in soil by triacid digestioninductively coupled plasma mass spectrometry

基于硝酸、氢氟酸、高氯酸三酸消解体系,采用全自动消解仪对土壤进行消解,建立三酸消解-电感耦合等离子质谱法测定土壤样品中钆、镝、铒、镱4种重稀土元素的新方法。采用物理技术-嵌片模式减缓土壤高盐基体对测试的影响,选择合适的待测同位素以及编辑干扰元素校正方程去除质谱干扰,采用碰撞模式去除基体干扰,实现用单一内标185Re进行土壤测试信号漂移校正,4种元素标准工作曲线的线性相关系数均大于0.999,方法检出限为0.009~0.05μg/g。基于10 ng/mL的185Re内标溶液校正基体效应,校正后的加标回收率可达到93%~107%。对空白样品进行加标回收试验,测定结果的平均相对标准偏差为2.4%~7.9%(n=6),加标回收率为94.1%~110%。该分析方法适宜土壤中钆、镝、铒、镱4种重稀土元素的测试。

A new method for the determination of four heavy rare earth elements,gadolinium,dysprosium,erbium and ytterbium,in soil samples by inductively coupled plasma mass spectrometry(ICP-MS)was established using a fully automatic digestion instrument based on nitric acid,hydrofluoric acid,and perchloric acid digestion systems.This method used physical technology embedded mode to mitigate the impact of high salinity soil matrix on testing.By selecting appropriate isotopes to be tested and editing the interference element correction equation to remove mass spectrometry interference,collision mode was used to remove matrix interference,and a single internal standard 185Re was used for soil testing signal drift correction.The linear correlation coefficients of the calibration curves for all four elements were more than 0.999,and the detection limits of the method were between 0.009-0.05μg/g.Based on 10 ng/mL 185Re internal standard solution to correct the matrix effect,the corrected spiked recovery rate could reach 93%-107%.A spiked recovery test was conducted on blank samples,with the average relative standard deviation of 2.4%-7.9%(n=6)and a spiked recovery rate of 94.1%to 110%.The measured values of each element match the standard values.This analysis method is suitable for testing and promoting the four heavy rare earth elements of gadolinium dysprosium erbium ytterbium in soil.