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    熔融制样-X射线荧光光谱法测定钨矿石中10种主次量成分

    Determination of 10 Major and Minor Components in Tungsten Ore by X-Ray Fluorescence Spectrometry with Fusion Sample Preparation

    • 摘要: 钨矿石是重要的战略物资,开发简单、快速、准确的钨矿石中10种成分含量的测定方法对选矿具有重要作用,因此进行了题示研究。取8.000 0 g质量比3∶7的四硼酸钠-四硼酸锂混合熔剂、0.100 0 g五氧化二钽(三氧化钨的内标)、0.400 0 g预先烘干的样品置于铂-金坩埚中,搅拌均匀后于650 ℃预氧化30 min,滴加12滴300 g·L−1碘化锂溶液,于1 050 ℃熔融19 min,制得的样片中主次量成分采用X射线荧光光谱法测定,其中硅、铝、钙、镁、铁、钛、磷、锰、钾的测定数据采用基于基本参数法的校正公式校正,三氧化钨校准曲线线性欠佳以及测定准确度较低的问题采用钽内标法消除。结果显示:10种成分的质量分数均在一定范围内和对应的荧光强度与钽荧光强度的比值(三氧化钨)或荧光强度(其他9种成分)呈线性关系,检出限(3s)分别为10.00~48.00 mg·kg−1(锰、钛和磷)和0.010%~0.12%(其余7种成分)。方法用于钨矿石标准物质GBW07241、多金属矿标准物质GBW07369及两个实际样品中10种成分的12次重复测定,测定值与认定值基本一致,相对标准偏差均小于7.0%;实际样品中10种成分测定结果与传统化学方法所得数据吻合良好。

       

      Abstract: Tungsten ore is an important strategic material, and establishing a simple, rapid, and accurate method for determining the content of 10 components in tungsten ore plays a crucial role in ore beneficiation. Therefore, the research mentioned by the title was conducted. The 8.000 0 g of mixture flux of sodium tetraborate and lithium tetraborate at mass ratio of 3∶7, and 0.100 0 g of tantalum pentoxide (the internal standard for tungsten trioxide), and 0.400 0 g of pre-dried sample were placed in a platinum-gold crucible. The mixture was stirred evenly, and pre-oxidized at 650 ℃ for 30 min. Then, 12 drops of the 300 g · L-1 lithium iodide solution were added, and the mixture was melted at 1 050 ℃ for 19 min. The major and minor components in prepared sample pellets were analyzed using X-ray fluorescence spectrometry. Determination data of silicon, aluminum, calcium, magnesium, iron, titanium, phosphorus, manganese, and potassium were corrected using correction formulas based on the fundamental parameter method. The issues of poor linearity of the tungsten trioxide calibration curve and low determination accuracy were eliminated using the tantalum internal standard method. It was shown that linear relationships between the mass fractions of 10 components and the fluorescence intensity ratio of tungsten to tantalum (tungsten trioxide) or fluorescence intensities (the other 9 components) were kept in definite ranges, with detection limits (3s) in the ranges of 10.00-48.00 mg·kg-1 for manganese, titanium, and phosphorus, and 0.010%-0.12% for the remaining 7 components. This method was applied to the 12 times repeated determination of 10 components in tungsten ore reference material GBW07241, polymetallic ore reference material GBW07369, and 2 actual samples. The determined values were basically consistent with the certified values, and RSDs were all less than 7.0%. The determination results of 10 components in the actual samples were in good agreement with the data obtained by traditional chemical methods.

       

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