电感耦合等离子体发射光谱法测定多金属矿石中的钼

摘要

样品经盐酸-硝酸-氢氟酸-高氯酸-硫酸(五酸)加热分解完全,利用浓硫酸的氧化性,可将钼转化为钼酸盐进入溶液中,盐酸溶解盐类至溶液清亮,用电感耦合等离子体发射光谱法在波长202.0 nm处测定多金属矿石中的钼,克服了盐酸-硝酸-氢氟酸-高氯酸(四酸)分解样品测定结果偏低的问题,同时解决了国标方法分析流程长、成本高、使用试剂较多且不易操作的难题.方法检出限为2.8μg/g,经国家一级标准物质分析验证,测定值与标准值相符.对自制监控样品测定6次,方法精密度(RSD)为2.16％.通过不同溶矿方法、不同检测方法及不同实验室进行验证,证明该方法线性范围宽(0 ～ 50 mg/mL),操作简单,适用于批量多金属矿石样品中0.001％～2.00％钼的测定.%Metallic ore samples were digested completely with HC1-HNO3-HF-HC1O4-H2SO4. The Mo was oxidized to molybdate by concentrated H2SO4. The HC1 was used to dissolve salt to clear solution, in preparation for measurement by inductively coupled plasma emission spectrometry at 202 nm. This method avoids the errors of the HC1-HNO3-HF-HC104 method and has the benefits of improved accuracy, decreased time, lower cost and less materials. Results are in agreement with the certified values of national standard reference materials. The secondary grade standard reference materials were tested 6 times giving RSD of less than 2. 16%. The detection limit of the method is 2. 8 (xg/g and the linear range is from 0 to 50 mg/mL. Tested by different dissolution methods and detection methods at different labs, this method is suitable for the detection of 0.001% to 2.00% Mo in metallic ores with satisfactory results.