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萃取色谱分离 - 电感耦合等离子体质谱法测定高纯氧化铽中痕量稀土杂质的研究

Determination of Rare Earth Impurities in High Purity Tb4O7 by ICPMS with P507 Extraction Chromatography

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【作者】 曹心德尹明李冰张岩

【Author】 Cao Xinde ( Department of Chemistry, University of Science and Technology of China, Hefei, 230026 ) Yin Ming, Li Bing, Zhang Yan ( Institute of Rock and Mineral Analysis, Ministry of Geology and Mineral Resources, Beijing, 100037 )

【机构】 地矿部岩矿测试技术研究所

【摘要】 考察了源于基体Tb的多原子离子质谱干扰及基体Tb对稀土杂质测定信号的影响,研究了P507HCl萃取色谱体系分离高纯Tb4O7基体与痕量稀土杂质的条件,采用Re内标补偿直接测定与分离基体后测定相结合的方式,建立了分析高纯Tb4O7中痕量稀土杂质的电感耦合等离子体质谱(ICPMS)法,检出限为5~21ng/L,加标回收率为90%~109%,3次测量的相对标准偏差为1.3%~6.5%,分离周期近9h。方法可用于纯度(质量分数,w)为99.99%~99.9999%的Tb4O7中痕量稀土杂质的分析。

【Abstract】 The matrix effect of Tb4O7 on signals of rare earth impurities and the mass spectra interferences originated from polyatomic ions of Tb4O7 were studied. The optimum conditions for separation of Tb4O7 and rare earth impurities by 2-ethylhexyl hydrogen2-ethylhexylphosphonate (P507) extraction chromatography were investigated. A method was developed for the determination of rare earth impurities in high purity Tb4O7 by ICPMS, based on the combination of direct determination and determination after separation . The detection limits for REEs were 5~21 ng/L. The recoveries of REEs for spiked samples were 90%~109% with the precision of 1.3%~6.5% RSD( n =3). The method can be applied to the analysis of 99.99%~99.9999% high purity Tb4O7.

  • 【文献出处】 岩矿测试 ,ROCK AND MINERAL ANALYSIS , 编辑部邮箱 ,1998年02期
  • 【分类号】P624.4
  • 【被引频次】8
  • 【下载频次】89
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