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偏振能量色散X射线荧光光谱法测定硫化物矿石中的铜铅锌
引用本文:蒯丽君,詹秀春,樊兴涛,温宏利,袁继海.偏振能量色散X射线荧光光谱法测定硫化物矿石中的铜铅锌[J].岩矿测试,2013,32(6):903-908.
作者姓名:蒯丽君  詹秀春  樊兴涛  温宏利  袁继海
作者单位:国家地质实验测试中心, 北京 100037;国家地质实验测试中心, 北京 100037;国家地质实验测试中心, 北京 100037;国家地质实验测试中心, 北京 100037;国家地质实验测试中心, 北京 100037
基金项目:国家自然科学基金资助项目(41203022);中国地质大调查项目(1212011120276)
摘    要:X射线荧光光谱法用于分析矿石主成分的常规制样方法有粉末压片法与玻璃熔融法,但分析硫含量高的地质样品时,前者存在矿物效应和粒度效应问题、后者可能腐蚀贵金属坩埚。为满足矿产勘查的需要,急需一种适应于硫化物矿石主成分分析的制样方法。本文建立了一种硝酸+氢氟酸封闭消解试样,标准溶液校准,偏振能量色散X射线荧光光谱(PE-EDXRF)同时测定硫化物样品中铜、铅、锌三种元素的分析方法。用GBW 07162~GBW 07168等7种矿石国家一级标准物质进行精密度和准确度实验。结果表明,当样品中铜、铅、锌元素含量大于1%时,几乎所有样品中的铜、铅、锌元素的精密度(RSD,n=6)优于5%,检测结果与标准值一致性良好。本方法通过样品消解、直接液体进样等技术的应用,消除了粒度效应和矿物效应等基体效应对分析结果的影响,解决了因缺乏基体匹配的标准物质而造成的含量校准的问题,使PE-EDXRF技术可以在硫化物矿石分析中得到比较方便的应用。这种分析方法为实验室矿石分析提供了新手段,也为野外现场PE-EDXRF分析高矿化度样品提供了新途径。

关 键 词:硫化物矿石        偏振能量色散X射线荧光光谱法  溶液法  酸消解
收稿时间:2013/4/11 0:00:00
修稿时间:2013/5/14 0:00:00

Determination of Cu, Pb and Zn in Sulfide Ores by Polarized Energy Dispersive X-ray Fluorescence Spectrometry
KUAI Li-jun,ZHAN Xiu-chun,FAN Xing-tao,WEN Hong-li and YUAN Ji-hai.Determination of Cu, Pb and Zn in Sulfide Ores by Polarized Energy Dispersive X-ray Fluorescence Spectrometry[J].Rock and Mineral Analysis,2013,32(6):903-908.
Authors:KUAI Li-jun  ZHAN Xiu-chun  FAN Xing-tao  WEN Hong-li and YUAN Ji-hai
Institution:National Research Center for Geoanalysis, Beijing 100037, China;National Research Center for Geoanalysis, Beijing 100037, China;National Research Center for Geoanalysis, Beijing 100037, China;National Research Center for Geoanalysis, Beijing 100037, China;National Research Center for Geoanalysis, Beijing 100037, China
Abstract:The traditional sample preparation methods are pressed powder pellets and glass melting to determine major components for sulfide ores by X-ray Fluorescence Spectrometry. However, for high sulfur geological samples, the preparation method of pressed powder pellet has mineralogical effects and particle size effects, and the glass melting method has the disadvantage of being corrosive to precious metal crucibles. Development of a simple sample preparation method for principal components analysis is essential to meet the requirements for exploration of mineral deposits. In this paper a method is presented to determine Cu, Pb, Zn contained in sulfide ores. This method utilizes Polarized Energy Dispersive X-ray Fluorescence Spectrometry (PE-EDXRF) along with nitric acid and fluoric acid digestion, and is calibrated by standard solution. The accuracy and precision of the method were examined by analyzing reference materials GBW 07162 to GBW 07168. The test results indicate that the relative standard deviations (RSD, n=6) of the most elemental components are less than 5%, when the concentrations of copper, zinc and lead are more than 1%. The results are in good agreement with certified values of reference materials. The impact of matrix effects such as particle size effect and mineral effect on analytical elements has been eliminated by digestion sample and direct solution inlet. The problem of calibrating concentrations that were short of standard materials has been solved with the matrix matching. The technology of PE-EDXRF provides a new means of ore analysis in the laboratory and a new technical support for PE-EDXRF field analysis for high sulfide samples.
Keywords:sulfide ores  copper  lead  zinc  Polarized Energy Dispersive X-ray Fluorescence Spectrometry  solution method  acid digestion
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