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徐爽, 徐聪聪, 郭腾达, 林培军, 李凤春, 王继林, 顾清宇, 栾日坚, 张玉强, 李增胜, 杨慧, 魏玮. 电子探针技术测定稀有多金属矿中微量元素硅钽钨的实验条件设定[J]. 岩矿测试, 2022, 41(2): 251-259. DOI: 10.15898/j.cnki.11-2131/td.202109080120
引用本文: 徐爽, 徐聪聪, 郭腾达, 林培军, 李凤春, 王继林, 顾清宇, 栾日坚, 张玉强, 李增胜, 杨慧, 魏玮. 电子探针技术测定稀有多金属矿中微量元素硅钽钨的实验条件设定[J]. 岩矿测试, 2022, 41(2): 251-259. DOI: 10.15898/j.cnki.11-2131/td.202109080120
XU Shuang, XU Congcong, GUO Tengda, LIN Peijun, LI Fengchun, WANG Jilin, GU Qingyu, LUAN Rijian, ZHANG Yuqiang, LI Zengsheng, YANG Hui, WEI Wei. The Experimental Conditions for Quantitative Determination of Trace Elements Si, Ta and W in Rare Polymetallic Ore by Electron Probe Microanalyzer[J]. Rock and Mineral Analysis, 2022, 41(2): 251-259. DOI: 10.15898/j.cnki.11-2131/td.202109080120
Citation: XU Shuang, XU Congcong, GUO Tengda, LIN Peijun, LI Fengchun, WANG Jilin, GU Qingyu, LUAN Rijian, ZHANG Yuqiang, LI Zengsheng, YANG Hui, WEI Wei. The Experimental Conditions for Quantitative Determination of Trace Elements Si, Ta and W in Rare Polymetallic Ore by Electron Probe Microanalyzer[J]. Rock and Mineral Analysis, 2022, 41(2): 251-259. DOI: 10.15898/j.cnki.11-2131/td.202109080120

电子探针技术测定稀有多金属矿中微量元素硅钽钨的实验条件设定

The Experimental Conditions for Quantitative Determination of Trace Elements Si, Ta and W in Rare Polymetallic Ore by Electron Probe Microanalyzer

  • 摘要: 近年来对稀有多金属矿的研究越来越趋向于微区化、微量化,作为其重要研究手段之一,电子探针定量分析在微量元素测试方面取得很大的进展。在微量测试过程中,除了增大测试束流,提高测试时间来降低检出限以外,更要注意去除来自其他元素,特别是主量元素的干扰。在日常测试稀有多金属样品的过程中,Si、Ta、W三个元素存在相互干扰,这种干扰对影响微量元素的测试结果,且因含量低不易被察觉,从而影响最终结论的准确性。本文以SPI标样公司的SiO2、金属Ta和W为研究对象,查明Si、Ta、W三者之间在不同测试条件下的干扰关系并给出建议:硅酸盐测试中,Si建议使用TAP-Kα,Ta和W建议使用LIF-Lα;铌钽矿测试中,Si、Ta、W建议分别使用PET-Kα、PET-Mα和TAP-Mβ,并配合Ta对Si的干扰校正测试结果更为准确。

     

    Abstract:
    BACKGROUNDIn recent years, the study of rare polymetallic ore tends to be increasingly detailed. As one of the important research methods, electron probe quantitative analysis has made great progress in trace element measurement. During analysis, in addition to increasing the beam size and time to reduce the detection limit, more attention should be paid to removing the interference from other elements, especially the main elements. During the routine testing of rare polymetallic samples, Si, Ta, W interfere with each other. Such interference affects the analytical results of trace elements, and is not easily detected due to its low content, thus affecting the accuracy of the final conclusion.
    OBJECTIVESTo determine the interference relationship among Si, Ta and W under different analytical conditions.
    METHODSTaking SiO2, metal Ta and W of SPI as the research object, each element was analyzed under different conditions by electron probe microanalyzer.
    RESULTSIn the analysis of silicate, TAP-Kα is used for Si, and LIF-Lα is recommended for Ta and W. In the analysis of niobium tantalum ore, it is suggested to use PET-Kα, PET-Mα and TAP-Mβ for Si, Ta and W, respectively; since 100% Ta will produce about 0.1% Si, therefore, the results are more accurate with the interference correction of Ta on Si.
    CONCLUSIONSIt is important to understand the spectral peak stripping method and the principle of element interference and spectral peak overlap, adjusting the parameters according to the actual situation to ensure the accuracy of data.

     

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