ICP-MS和ICP-AES测定地球化学勘查样品及稀土矿石中铌钽方法体系的建立

高会艳

高会艳.ICP-MS和ICP-AES测定地球化学勘查样品及稀土矿石中铌钽方法体系的建立[J].岩矿测试,2014,33(3):312-320

View Full Text 查看/发表评论 EndNote BibTeX 下载PDF阅读器

Determination Systems of Nb and Ta in Geochemical Samples and Rare Earth ores by ICP-MS and ICP-AES

投稿时间：2013-07-29

DOI：

Key words: geochemical exploration samples rare earth ores Nb Ta constant temperature-electric heating plate digestion Na₂O₂ fusion Inductively Coupled Plasma-Mass Spectrometry Inductively Coupled Plasma-Atomic Emission Spectrometry

作者	单位
高会艳	中铁资源集团中心实验室, 河北廊坊 065000

摘要点击次数: 7157

全文下载次数: 2399

Abstract:

A method to deal with the conditions of incomplete digestion of geological samples, and the complexity of the analysis for present technologies, along with the routine methods of wet digestion on constant temperature electric heating plate with mixed acids and Na₂O₂ fusion pre-treatment method and to ease the hydrolysis of Nb and Ta are describe in this paper. Both Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) were applied to establish two sets of analysis methods which can be used to detect the contents of Nb and Ta in geochemical exploration samples and rare earth ores. Wet digestion on constant temperature electric heating plate is suitable for low content and easy decomposition of samples with nitric acid-hydrofluoric acid-sulfuric acid by ICP-MS. Na₂O₂ fusion pre-treatment method is suitable for high content and insoluble samples by using ICP-AES. Through the analysis of a series of national certified reference samples of soil, stream sediments, rocks and rare earth ores, the results show that mixed acid pre-treatment coupled with ICP-MS had a linear range of 0-200 ng/mL and detection limits of Nb and Ta were 0.01 μg/g and 0.05 μg/g, respectively. The relative error was less than 10%, and the relative standard deviation (RSD) was less than 6%. The Na₂O₂ fusion pre-treatment coupled with ICP-AES had a linear range of 0-30 μg/mL, detection limits of Nb and Ta were 0.2 μg/g and 2.5 μg/g, respectively. The relative error was less than 10%, and the precision (RSD) was less than 7%. The two sets of analysis method satisfy the demand of analysis of Nb and Ta in samples with a complex matrix, a large range of content and large quantities of samples.