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    熔融制样-X射线荧光光谱法测定锡矿和钨钼矿中16种组分

    XRFS Determination of 16 Components in Tin Ore and Tungsten Molybdenum Ore with Fused Sample Preparation

    • 摘要: 锡矿或钨钼矿样品以四硼酸锂为熔剂,以硝酸铵为氧化剂,预氧化后,以溴化锂为脱模剂,在1 100℃下熔融10 min,冷却后制成熔融片,采用X射线荧光光谱法测定熔融片中锡、钨、钼、砷、铅、锌、锑、铜和三氧化二铝、二氧化硅、三氧化二铁、一氧化锰、二氧化钛、氧化钙、五氧化二磷、三氧化硫等16种组分的含量。以五氧化二钽为内标,采用理论系数法校正基体效应,16种组分的检出限为50~155 μg·g-1。方法应用于锡矿样品的分析,测定值与已知值相符,测定值的相对标准偏差(n=10)为0.15%~1.2%。

       

      Abstract: After preoxidation, the sample of tin ore or tungsten molybdenum ore was fused at 1 100 ℃ for 10 min using Li2B4O7, NH4NO3 and LiBr as flux, oxidant and release agent respectively. The melt sheet was prepared after cooling. XRFS was applied to the determination of 16 components, i.e. Sn, W, Mo, As, Pb, Zn, Sb, Cu, Al2O3, SiO2, Fe2O3, MnO, TiO2, CaO, P2O5, SO3 in the melt sheet. Ta2O5 was used as internal standard. Theoretical coefficient method was used to correct matrix effect. Detection limits of the 16 components ranged from 50 to 155 μg·g-1. The proposed method was applied to the analysis of tin ore sample, giving results in consistency with the known values and values of RSDs (n=10) of determined values were in the range of 0.15%-1.2%.

       

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