以柠檬酸和过氧化氢为络合剂电感耦合等离子体原子发射光谱法测定选矿样品中钨和钼

以盐酸、硝酸、氢氟酸、硫酸、柠檬酸和过氧化氢溶解样品，选择W239.709 nm和Mo 284.823 nm的谱线分别作为钨和钼的分析线，用ICP-AES光谱法测定了样品中钨和钼含量。利用柠檬酸和过氧化氢与钨酸、钼酸络合作用，抑制钨酸和钼酸的析出，促使样品的快速溶解，确保了钨、钼测定结果的准确性。钨和钼的检出限分别为0.015 μg/mL 和0.003 μg/mL，测定下限分别为0.075 μg/mL和 0.015 μg/mL。当钨、钼含量分别在0.1~100 μg/mL范围内，其校准曲线均呈线性关系，且线性相关系数都在0.999 5以上。采用本方法测定钼矿石标准样品和选矿流程样品中钨、钼时，测定值与认定值或硫氰酸盐光度法或重量法的测定值相符。用钨矿石标准样品和选矿流程样品进行加标回收试验，测得钨的加标回收率在96%～105%之间，钼的加标回收率在94%～102%之间。

Inductively coupled plasma atomic emission spectrometric determination of tungsten and molybdenum in mineral processing samples with hydrogen peroxide and citric acid as complexing agent

The sample was dissolved in hydrochloric acid,nitric acid,hydrofluoric acid,sulfuric acid,citric acid and hydrogen peroxide.W239.709 nm and Mo 284.823 nm were used as the analytical lines for tungsten and molybdenum,respectively.The contents of tungsten and molybdenum in sample were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The precipitation of tungsten acid and molybdenum acid was inhibited by the complexing action of citric acid and hydrogen peroxide to accelerate the dissolution of sample and guarantee the determination accuracy of tungsten and molybdenum.The detection limit was 0.015 μg/mL and 0.003 μg/mL,and the limit of quantitation was 0.075 μg/mL and 0.015 μg/mL for tungsten and molybdenum,respectively.When the content of tungsten and molybdenum was in range of 0.1-100 μg/mL,the calibration curve was linear,with correlation coefficient more than 0.9995.The determination results of tungsten and molybdenum in molybdenum ore standard sample and mineral processing samples by this method were consistent with the certified values or those obtained by thiocyanate spectrophotometry or gravimetric method.The recovery tests of tungsten ore standard sample and mineral processing samples were conducted.The found recoveries of tungsten and molybdenum were 96%-105% and 94%-102%,respectively.