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建立了氢化物发生-原子荧光光谱法快速测定钨矿石中砷的分析方法。对盐酸硝酸溶样方法及共存元素的干扰进行了研究,并优化了仪器条件。结果发现,用盐酸硝酸溶解样品完全,通过加入酒石酸和硫脲-抗坏血酸抑制基体钨等其他金属离子的干扰。方法的定量限为0.20mg/kg,回收率为87.5%—105.6%。在0.0005—0.2400水平范围(质量分数,单位%)内,实验室间的重复性限r和重现性限R分别为lgSr=0.976lgm-1.53,lgSR=0.9932lgm-1.52。方法具有操作简便、快速,灵敏度高等优点,可用于钨矿石中痕量砷的测定。
A method for the rapid determination of arsenic in tungsten ores by hydride generation-atomic fluorescence spectrometry was established. The method of dissolving hydrochloric acid in nitric acid and the interference of coexisting elements were studied, and the instrument conditions were optimized. As a result, it was found that the sample was completely dissolved with hydrochloric acid and nitric acid to restrain the interference of other metal ions such as matrix tungsten by adding tartaric acid and thiourea-ascorbic acid. The limit of quantification of the method was 0.20 mg / kg and the recovery was 87.5% -105.6%. In the range of 0.0005-0.2400 (mass fraction, unit%), the repeatability limit r and repeatability limit R between laboratories are respectively lgSr = 0.976lgm-1.53 and lgSR = 0.9932lgm-1.52. The method has the advantages of simple operation, rapidity and high sensitivity, and can be used for the determination of trace amounts of arsenic in tungsten ores.