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将氧化镧粉末与微晶纤维素(MCC,作为粘合剂)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138La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。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2N~4N氧化镧中稀土杂质的定量分析要求。
Lanthanum oxide powder and microcrystalline cellulose (MCC, as a binder) after grinding uniform tablet using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) quantitative analysis of lanthanum oxide rare earth impurities, The conditions and laser ablation parameters were explored and optimized. The optimum mass ratio of lanthanum oxide to microcrystalline cellulose was 92: 8. The grinding time of the mixed powder was at least 15 min. Under the condition of online scanning, the laser energy was 750V, the pore size was 150μm and the scanning rate was 60μm · s-1, to obtain high sensitivity and good stability of the signal. Under the optimal experimental conditions, the working curve was established with the standard samples of GSB04-2602 ~ 2604-2010 lanthanum oxide, and the calibration curve was 138La. The linear correlation coefficients of all rare earth impurities were 0.9966 ~ 0.9999. The blank samples were 11 times parallel determination, the detection limit of each element of 0.01 ~ 0.15μg / g. The determination of 14 kinds of rare earth impurities in three kinds of lanthanum oxide samples with different contents basically coincided with the results of ICP-MS, and the relative standard deviations RSD ranged from 3.4% to 11.2%. The method has good accuracy and precision, and can meet the quantitative analysis requirements of rare earth impurities in 2N ~ 4N lanthanum oxide.