激光剥蚀电感耦合等离子体质谱法测定氧化镧中14种稀土杂质  

Determination of 14 Rare Earth Impurities in Lanthanum Oxide by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

作　　者：田佳[1] 刘鹏宇[1] 冯流星[2] 张殿凯[1] 鲍叶琳 

机构地区：[1]北京有色金属研究总院国标(北京)检验认证有限公司,北京100088 [2]中国计量科学研究院,北京100013

出　　处：《稀有金属》2018年第1期106-112,共7页Chinese Journal of Rare Metals

基　　金：国家科技部创新方法工作专项项目(2012IM030500)资助

摘　　要：将氧化镧粉末与微晶纤维素（MCC）粘结剂研磨均匀后压片，采用激光剥蚀电感耦合等离子体质谱法（LA-ICP-MS）定量分析了氧化镧中稀土杂质的含量，并对压片条件和激光剥蚀参数进行了探索和优化。实验确定了氧化镧与微晶纤维素的最佳质量比为92：8，混合粉末的研磨时间至少为15min；在线扫描的剥蚀方式下，选择激光能量为750V，剥蚀孔径为150μm，扫描速率为60μm·s-1，能获得灵敏度高、稳定性好的信号。在最佳实验条件下，用GSB04-2602—2604-2010系列氧化镧标样建立工作曲线，并以La为内标进行校正，得到各稀土杂质的线性相关系数为0．9966—0．9999。对空白样片进行了11次平行测定，统计各元素的检出限为0．01～0．15μg·g-1。对3种不同含量的氧化镧样品中14种稀土杂质进行了测定，测定结果与ICP—MS法的结果基本吻合，相对标准偏差RSD在3．4％～11．2％之间。该方法准确度和精密度良好，能够实现2—4N氧化镧中稀土杂质的定量分析要求。Lanthanum oxide powder was mixed evenly with microcrystalline cellulose （ MCC, used as the binder）, and tableted. The contents of rare earth impurities in lanthanum oxide were quantitative analyzed by laser ablation inductively coupled plasma mass spec- trometry （LA-ICP-MS）. Tableting conditions and laser ablation parameters were explored and optimized. Experiments showed that the optimum mass ratio of lanthanum oxide and MCC was 92 to 8 and the grinding time need to be at least 15 min. Stable signal intensity and high sensitivity could be obtained when laser energy was 750 V, spot size was 150 Ixm and scan rate was 60 Ixm＇s-I by using sin- gle line scan mode. Under the best experimental conditions, GSB04-2602 - 2604-2010 lanthanum oxide standard samples were used to establish working curves, the linear correlation coefficients of rare earth impurities were between 0. 9966 and 0. 9999 after calibrated by laSLa internal standard. The detection limits of each element were from 0.01 to 0.15 μg-g-1 after 11 times＇ blank sample determina- tion. Fourteen kinds of rare earth impurities in three lanthanum oxide samples with different contents were determined by LA-ICP-MS, the results were consistent with ICP-MS, and the relative standard deviations were from 3.4% to 11.2%. The accuracy and precision were favorable, which showed that LA-ICP-MS could satisfy the quantitative analysis requirement for rare earth impurities in lanthanum oxide.

关 键 词：激光剥蚀电感耦合等离子体质谱法(LA-ICP-MS) 氧化镧 稀土杂质 压片 激光剥蚀参数 

分 类 号：O657.63[理学—分析化学]