建立了电感耦合等离子体质谱法( ICP-MS)测定高纯二氧化锡电极材料中Cu, Cr, Mn, Co, Ni, Cd, Fe和Pb等关键性杂质离子的新方法。以2 mL浓HCl为介质,基于高温高压密闭溶样技术,在230℃时保持3 h可将0.1 g样品完全分解。进一步结合氮气吹扫氯化物基体分离技术,实现了150℃挥发温度时和1.5 h时间内单次>99.9％的基体去除效率,有效消除了后续ICP-MS测定的基体效应以及潜在的质谱干扰。全分析流程加标回收率在100％±5％以内,6次样品平行测定值的相对标准偏差( RSD)在0.09％~3.68％之间,方法检出限(3σ)在0.002~0.034 mg/kg之间,表明本方法不仅具有较好的精确度,而且具有较高的灵敏度,可适用于纯度高达6N的二氧化锡电极材料中杂质离子的检测。应用此法成功测定了3个标称为4N纯度的二氧化锡电极材料实际样品。%A new method for determination of trace Cu, Cr, Mn, Co, Ni, Cd, Fe and Pb impurities in high pure tin oxide material was proposed. 0. 1 g of sample was successfully digested at 230℃ in 3 h when autoclaves with high pressure and high temperature were used. After that, over 99. 9% of the matrix Sn was removed by chloride volatilization at 150℃ for 1. 5 h, which eliminated the matrix effect and spectra interference in the following ICP-MS detection. The recoveries for all the analytes of the spiked test were 100%±5%, the RSDs for 6 runs of sample analysis were from 0. 09% to 3. 68%, and the limits of detection (LOD, 3σ) were from 0. 002 mg/kg to 0. 034 mg/kg, which indicated that the established method were of both accuracy and high sensitivity, and could be applied for the analysis of samples with purity up to 6N. Finally, three samples specified with 4N purity were analyzed by this method.
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