高温高压微波消解-电感耦合等离子体质谱法测定煤及粉煤灰中稀土元素  

Determination of Rare Earth Elements in Coal and Fly Ash by Inductively Coupled Plasma Mass Spectrometry with High-temperature and High-pressure Microwave Digestion

作　　者：孙凯茜 李晓敬 于聪灵 宋娟娟 刘璐 王泽宇 冉卓 刘玥 SUN Kaixi;LI Xiaojing;YU Congling;SONG Juanjuan;LIU Lu;WANG Zeyu;RAN Zhuo;LIU Yue(Hebei Research Center for Geoanalysis,Baoding 071051,China;Key laboratory of Mineral Resources and Ecological Environment Monitoring of Hebei Province,Baoding 071051,China)

机构地区：[1]河北省地质实验测试中心,河北保定071051 [2]河北省矿产资源与生态环境监测重点实验室,河北保定071051

出　　处：《湿法冶金》2025年第2期271-279,共9页Hydrometallurgy of China

基　　金：保定市科技计划项目(2341ZF165)。

摘　　要：针对现有煤系样品中稀土元素的测定存在前处理效率低、质谱干扰较大等问题,建立了一种在HNO_(3)-HF-HClO_(4)-H_(2)SO_(4)混酸体系中采用高温高压微波消解-电感耦合等离子体质谱法测定煤及粉煤灰样品中稀土元素的方法,并考察了前处理方式、称样量、消解体系、质谱干扰等对测定结果的影响。结果表明:方法校准曲线线性相关系数均大于0.9996,检出限为0.0037~0.042μg/g,各元素测定值的相对标准偏差(RSD,n=11)均在5.85%以内,加标回收率为95.0%~107.2%,相对误差均小于6.95%。该方法准确性高,稳定性好,可极大提高工作效率。Aiming at the problems of low pre-treatment efficiency and significant mass spectrometry interference in the determination of rare earth elements in coal-related samples,a method for the determination of rare earth elements in coal and fly ash samples by high-temperature and high-pressure microwave digestion-ICP-MS in a mixed acid system of HNO_(3)-HF-HClO_(4)-H_(2)SO_(4) was established.The effects of pre-treatment methods,sample weight,digestion system and mass spectrometry interference on the determination results were investigated.The results show that the linear correlation coefficients of the calibration curves are all greater than 0.9996,the detection limits are 0.0037~0.042μg/g,the relative standard deviations(RSD,n=11)of the determination results of each element are all within 5.85%,the recoveries of standard addition are 95.0%~107.2%,and the relative errors are all less than 6.95%.The method has high accuracy and good stability,which greatly improves the determination efficiency.

关 键 词：高温高压微波消解 电感耦合等离子体质谱法 煤 粉煤灰 稀土元素 测定 

分 类 号：O657.63[理学—分析化学]