三重四极杆电感耦合等离子体质谱(ICP-MS)法测定氧化铕中13种稀土杂质元素  

Determination of 13 Rare Earth Impurities in Europium Oxide by Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry

作　　者：李维涵 李鹰 李剑 杨萌 LI Weihan;LI Ying;LI Jian;YANG Meng(Hangzhou Puyu Technology Co.,Ltd.,Hangzhou,Zhejiang 311300,China)

机构地区：[1]杭州谱育科技发展有限公司,杭州311300

出　　处：《中国无机分析化学》2024年第3期343-349,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2021YFF0700804)。

摘　　要：稀土杂质元素直接影响高纯单金属稀土材料的整体性能,是高科技领域许多材料的重要组成部分。通过考察消解酸量、温度、时间,氧气反应气流量,稀释气流量,建立了基于三重四极杆电感耦合等离子体质谱(ICP-MS/MS)法直接测定氧化铕中13种稀土杂质元素的分析方法。采用0.1%基体直接进样,可以很大程度提高前处理分析效率。利用碰撞模式测定氧化铕稀土中的Y、La、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Yb、Lu元素,氧气质量转移模式测定氧化铕中的Tm,两种模式结合可以有效去除多原子干扰,实现氧化铕的稳定测试。通过对氧化铕标准物质(GBW02902)直接测定,结果表明,在碰撞和氧气质量转移模式下,各元素线性相关系数(r)均大于0.9999,方法检出限为0.001~0.023 mg/kg,测试精密度优于2.0%,13种元素的测定值都在认定值的不确定度范围之内。方法操作简单、测定稳定、效率高,为实验室进行氧化铕材料中REE杂质的准确测定提供思路和借鉴。Rare earth impurity elements directly affect the overall performance of high-purity monometallic rare earth materials,which are an important part of many materials in high-tech fields.By investigating the optimal digestion acid amount,temperature,time,oxygen reaction gas flow and dilution gas flow,an analysis method for the direct determination of 13 rare earth impurity elements in europium oxide based on triple quadrupole inductively coupled plasma mass spectrometer(ICP-MS/MS)was established.This method used 0.1%matrix for direct injection,which greatly improved the efficiency of pretreatment analysis.Y,La,Pr,Nd,Sm,Gd,Tb,Dy,Ho,Er,Yb and Lu elements in europium oxide rare earth were determined by collision mode.Furthermore,Tm in europium oxide was determined by oxygen mass transfer mode.The combination of the two modes effectively removed the multi-atomic interference,realized the stability test and analysis of europium oxide.Through direct determination and analysis of europium oxide reference material(GBW02902),the results showed that under the mode of collision and oxygen mass transfer,the linear correlation coefficient(r)of each element was greater than 0.9999,the detection limit of the method was 0.001-0.023 mg/kg,the test precision was better than 2.0%,and the test values of 13 elements were within the uncertainty range of the certified value.The analytical method is simple in operation,stable in test and high in efficiency,which can provide ideas and references for the accurate test and analysis of REE impurities in europium oxide materials in the laboratory.

关 键 词：ICP-MS/MS 氧化铕稀土 碰撞模式 氧气质量转移模式 REE杂质元素 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]