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文章摘要
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
GAO Hui-yan.Determination Systems of Nb and Ta in Geochemical Samples and Rare Earth ores by ICP-MS and ICP-AES[J].Rock and Mineral Analysis,2014,33(3):312-320.DOI:
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
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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:
中文关键词: 地球化学勘查样品  稀土矿      恒温电热板消解  碱熔  电感耦合等离子体质谱法  电感耦合等离子体发射光谱法
英文关键词: 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
基金项目:国家自然科学基金资助项目(41103013)
作者单位
高会艳 中铁资源集团中心实验室, 河北 廊坊 065000 
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中文摘要:
      针对目前铌钽分析中出现的样品溶解不完全、元素易水解及现有分析技术流程复杂的情况,本文对常用的混合酸恒温电热板溶解和过氧化钠碱熔两种样品前处理方式进行优化,运用电感耦合等离子体质谱法(ICP-MS)、电感耦合等离子体发射光谱法(ICP-AES)两种技术手段,建立了测定地球化学勘查样品及稀土矿石中不同含量水平的铌、钽两套分析方法。对于铌、钽含量较低且易于分解的样品,采用硝酸-氢氟酸-硫酸混合酸恒温电热板消解ICP-MS方法测定;对于铌、钽含量高且难溶的样品,采用过氧化钠高温熔融ICP-AES方法测定。ICP-MS用于分析低含量样品更具优势,而高含量样品更适合运用ICP-AES。通过分析土壤、水系沉积物、岩石、稀有稀土矿石系列国家标准物质,结果表明混合酸处理ICP-MS分析方法的线性范围为0~200 ng/mL;检出限为铌0.01 μg/g,钽0.05 μg/g;相对误差小于10%,精密度(RSD)小于6%;碱熔处理ICP-AES分析方法的线性范围为0~30 μg/mL,检出限为铌0.2 μg/g,钽2.5 μg/g,相对误差小于10%,精密度(RSD)小于7%。这两套分析方法可以满足基体复杂、铌钽含量变化范围大、试样批量大的检测要求。
英文摘要:
      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.
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