电感耦合等离子体原子发射光谱法测定钼矿石中的钨钼

运用过氧化钠碱熔法处理钼矿样, 直接以盐酸-柠檬酸-过氧化氢混合酸提取熔融物来避免硅胶的产生和钨酸、钼酸沉淀的生成。以W 207.912 nm和Mo 202.031 nm谱线作为钨、钼的分析线, Co 240.725 nm为内标线, 消除了基体干扰效应和仪器信号漂移的影响, 建立了电感耦合等离子体原子发射光谱法测定试液中钨和钼的方法。钨的检出限为0.010 μg/mL, 测定范围为0.013%～12.50%, 回收率为98%～102%;钼的检出限为0.005 μg/mL, 测定范围为0.006%～12.50%, 回收率为99%～102%。对钼标准矿样测试, 所测得钼、钨结果与认定值相符, 相对标准偏差(RSD, n=8)为1.2%~3.6%。

Determination of tungsten and molybdenum in molybdenum ore by inductively coupled plasma atomic emission spectrometry

With ore samples decomposed by sodium peroxide alkali fusion, the fusion samples were directly extracted with mixed acid of hydrochloric acid-citric acid-hydrogen peroxide in order to effectively avoid the production of silicone and the generation of tungstic acid and molybdenic acid precipitates. With spectral lines of W 207.912 nm and Mo 202.031 nm as the analytical line of tungsten and molybdenum and spectral line of Co 240.725 nm as internal standard, the effects of matrix interference and instrument drift were eliminated and a method for the determination of tungsten and molybdenum in the test solution was established by inductively coupled plasma atomic emission spectrometry. The detection limit of tungsten was 0.010 μg/mL, the detection range was 0.013%-12.50% and recoveries were 98%-102%. The detection limit of molybdenum was 0.005 μg/mL, the detection range was 0.006%-12.50%, and recoveries were 99%-102%. The method was applied to determination of tungsten and molybdenum in molybdenum ore certified reference materials. The results were consistent with the certified values and the relative standard deviations (RSD, n=6) were 1.2%-3.6%.