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中国无机分析化学:2020,10(1):70-75
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熔融制样-X射线荧光测定钨钼锡矿中的主次成分
刘恒杰1, 贾海峰2, 谭清月3
(1.湖北冶金地质研究所(中南冶金地质研究所);2.湖北冶金地质研究所(中南冶金地质研究所);3.中南冶金地质研究所,湖北 宜昌 443003)
Determination of Primary and Secondary Components in Tunggium-molybdenum Tin Mine by Melt Sampler-X-ray Fluorescence
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投稿时间:2019-05-31    修订日期:2019-06-07
中文摘要: 本文采用熔融制样-X射线荧光光谱法测定矿物中的Cu、Pb、Zn、Mo、W、Al、Fe、Si、K、Na、Ti、Ca、Sn等13个主次量元素,采用混合均匀的三混熔剂,以硝酸锂为氧化剂,溴化锂为脱膜剂。进行实验条件优化选择,在650℃下对样品进行预氧化,在1100℃下高温熔融,熔融时间为300s,最后制成均匀透明,表面光滑无气孔的熔片,以部分国家一级标准物质和自制的钨钼锡标准样品,熔融制片进行测定,线性拟合建立标准曲线,并通过测量谱线选择、基体校正,使钨钼锡的测定范围扩宽,从微量到主量均能够进行测定,并且适用于多种不同矿石的分析。样品的组成和含量变化会对分析线强度造成吸收、增强以及谱线重叠的影响,采用理论α系数和经验系数相结合的方法来校正其产生的基体效应。相同条件下熔融10个标样进行测定,其RSD均小于5%,表明方法的准确度、精密度均满足国家相关质量标准的要求。选用一些含量不同的标样进行测定,本法的最终测定结果与标准值相符,表明本法可用于钨钼锡矿的测定。
Abstract:In this paper, the melting sample preparation - X ray fluorescence spectrometry determination of Cu, Pb, Zn, Mo, W, Al, Fe, Si, K, Na, Ti, Ca, Sn 13 primary and secondary elements, such as by mixing 3 mixed solvent, with lithium nitric acid as oxidizing agent, lithium bromide as remover. Optimal selection experiment condition, the samples under 650 ℃ to oxidation, and then under the 1100 ℃ high temperature melting, melting time of 300 s, the last made uniform transparent, smooth surface, no stomata fuse link, as part of a national level standard substance and homemade molybdenum tungsten tin standard sample, melting production were determined, linear fitting to establish standard curve, and by measuring the spectral line selection, the matrix correction, expanding the area of the determination of molybdenum tungsten tin, from the trace to the quantity can be measured, and suitable for a variety of different analysis of the ore. Changes on the analysis of the composition and content of the sample line intensity due to absorption, enhance, and the influence of the spectral overlap, by adopting the combination of theory of alpha coefficient and experience coefficient method to correcting the matrix effect. The same conditions the molten 10 sample determination, the RSD are less than 5%, shows that accuracy and precision of the method are meet the requirements of relevant national quality standards. Choose some content determination of different sample, the final determination results of this method are consistent with the standard values, indicating that this method can be used for the determination of tungstenandMolybdenum tin ore.
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刘恒杰,贾海峰,谭清月.熔融制样-X射线荧光测定钨钼锡矿中的主次成分[J].中国无机分析化学,2020,10(1):70-75.
LIU Heng Jie,Jia Haifeng,TAN Qingyue.Determination of Primary and Secondary Components in Tunggium-molybdenum Tin Mine by Melt Sampler-X-ray Fluorescence[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(1):70-75.

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