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作 者:秦婷[1] 张旭龙[1] 热孜婉[1] 全小盾[1]
出 处:《理化检验(化学分册)》2013年第7期827-830,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:提出了应用X射线荧光光谱法测定钼精矿样品中钼、铁、铅、铜、硅和钙等6种元素。样品以四硼酸锂与硝酸锂为熔剂于1100℃熔融,15min后倒入铂-金模具中成型,脱摸所得熔块用于X射线荧光光谱分析。以高纯三氧化钼、三氧化二铁、二氧化硅、碳酸钙、铜标准溶液和铅标准溶液等物质为基础,配制10个校准样品用于制作工作曲线。优化了各元素的基体校正数学模型。方法的检出限在0.003%~0.015%之间;对同一钼精矿试样重复测定¨次,测得其相对标准偏差(n=11)在0.066%~2.5%之间。方法用于2个钼精矿样品分析,所得结果与化学法测定结果相符合。XRFS was proposed for determination of 6 elements (i. e. , Mo, Fe, Pb, Cu, Si and Ca) in sample of molybdenum concentrates. The sample was fused at 1 100℃ using Li2B4O7 and LiNO3 as flux for 15 min, and the sample in molten state was poured into a Pt-Au mould to have it shaped upon cooling, and the melt demoulded was used for XRFS analysis. Working curve was prepared with a set of 10 calibration samples, which were prepared with higln purity oxides (i. e. , MOO3, Fe203, SiO2) and CaCO3 as well as standard solutions (Cu and Pb). The mathematical models of matrix correction of the 6 elements were optimized. Values of detection limit of the method found were in the range of 0. 003%-0. 015%. Values of RSD's (n= 11) were found to be in the range of 0. 066%--2. 5% in the analysis of a sample of molybdenum concentrates. The proposed method was used in analyzing 2 samples of molybdenum concentrate, giving results in consistency with those obtained by chemical methods.
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