Abstract

A procedure is developed for the separate determination of the Sn(II) and Sn(IV) in the range of 0.05–0.25 M in acidic aqueous and ethylene glycol solutions in the presence of Ni(II), Cu(II), F^–, a surfactant (OS-20), and citric or oxalic acids. The direct iodatometric titration of Sn(II) is used before and after the reduction of Sn(IV) with aluminum. The procedure is applicable to the analysis of electrolytes for the deposition of tin and Ni–Sn and Cu–Sn alloys and can be used to monitor changes in the concentrations of Sn(II and IV) as a result of redox processes in electrolytes and the hydrolysis of tin compounds. The interfering effect of copper consists in the interaction of Cu(II) with Sn(II) and Al with the formation of Cu(I) ions, reacting with iodate ions, and is eliminated by the introduction of oxalic acid. The relative error in determining the concentration of tin in the absence of copper(II) ions and in the presence of other components does not exceed 2.2%, and in the presence of Cu(II) the error is 4.3%.

中文翻译：

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滴定法测定电镀中用于沉积 Sn、Cu-Sn 和 Ni-Sn 涂层的电解质中的锡 (II, IV)

摘要

开发了一种程序，用于在 Ni(II)、Cu(II)、F 的存在下，在酸性水溶液和乙二醇溶液中分别测定 0.05–0.25 M 范围内的 Sn(II) 和 Sn(IV) ^–、表面活性剂 (OS-20) 和柠檬酸或草酸。在用铝还原 Sn(IV) 之前和之后使用 Sn(II) 的直接碘量滴定。该程序适用于分析用于沉积锡、Ni-Sn 和 Cu-Sn 合金的电解液，并可用于监测电解液中氧化还原过程引起的 Sn（II 和 IV）浓度变化以及锡化合物的水解。铜的干扰作用在于 Cu(II) 与 Sn(II) 和 Al 的相互作用，形成 Cu(I) 离子，与碘酸盐离子反应，并通过引入草酸消除。在不存在铜（II）离子和存在其他成分的情况下，确定锡浓度的相对误差不超过 2.2%，存在铜（II）时的误差为 4.3%。