Preliminary exploration on statistical distribution analysis of dysprosium rod by laser ablation-inductively coupled plasma mass spectrometry
YANG Li-xia1,LI Dong-ling1,ZHANG Xiao-wei2,MIAO Rui-ying2,LI Xiao-jia*1
1.Beijing Key Laboratory of Metal Material Characterization,Central Iron and Steel Research Institute,Beijing 100081,China; 2.National Engineering Research Center for Rare Earth Materials,General Research Institute for Nonferrous Metals,Beijing 100088,China
Abstract：The development of high-efficiency and high-sensitivity in situ microanalysis technology for rare earth purification process, such as solid state electromigration, is of great significance. The dysprosium rods after purification by solid state electrotransport were investigated. The laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for the micro-area distribution analysis of high-purity rare-earth metals. The effect of laser ablation rate on sample surface coverage and analysis time was studied. The optimized ablation rate was 50 μm/s. Moreover, the influence of ablation cell and ICP-MS carrier gas flow on the elemental signal intensity, oxide yield and elemental fractionation effect was also investigated. The optimized carrier gas flow was 0.60 L/min (He) and 1.0 L/min (Ar). By using 158Dy as the internal standard, the two-dimensional relative intensity distribution of various impurity elements in different electromigration areas was obtained in line scanning mode. The migration patterns of impurity elements were preliminarily explored. The results showed that Al, Si, Ti, Fe, Mo and W migrated from cathode to anode in electromigration process, while Ni and Cu migrated from the mid-region towards two poles, which was consistent with results obtained by glow discharge mass spectrometry (GD-MS). In addition, more abundant micro-area statistical distribution information could be obtained by LA-ICP-MS. The maximum segregation degree, relative standard deviation (RSD) and maximum segregation position of impurity elements in different electromigration regions revealed that the migration status of elements was possibly related to the process of solid state electromigration. Therefore, LA-ICP-MS perhaps provided a new and effective tool for the process analysis and optimization of purification of rare-earth metals.
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