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采用盐硝混酸+氢氟酸溶解样品,氢溴酸挥发除锑的方法,避免高含量锑在溶液中不稳定及对铊测定的干扰,采用电感耦合等离子体质谱法测定了铅锑精矿中铊的含量。铅锑精矿经过前处理后,样品溶液中锑的残留量均小于10μg/m L。选择铱作内标,将方法应用于实际样品中铊的测定,相对标准偏差小于5%,回收率为97.2%~107%,选择6家试验室协同验证,经统计检验测试结果间无明显差异。方法适用于铅锑精矿中铊的测定。
The method of dissolving samples with salt and nitric acid mixed acid and hydrofluoric acid and removing volatile antimony by hydrobromic acid is adopted to avoid the instability of the high content of antimony in the solution and the interference to the determination of thallium. The content of antimony in the lead antimony concentrate by ICP- Thallium content. Lead antimony concentrate after pre-treatment, the sample solution of antimony residues were less than 10μg / m L. The method was applied to the determination of thallium in real samples with the relative standard deviation of less than 5% and the recovery of 97.2% -107%. Six laboratories were selected to verify the results. There was no significant difference between the test results . The method is suitable for the determination of thallium in lead-antimony concentrate.