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作 者:王铭 WANG Ming(Kunming Metallurgical Research Institute,Kunming,Yunnan 650031,China)
出 处:《云南冶金》2018年第4期79-82,共4页Yunnan Metallurgy
摘 要:在酸性底液中,Pb^(2+)极谱峰电位为-0.47 V,Sn^(2+)、Sn^(4+)都为-0.5 V(vs.SCE),峰电流重叠严重。实验选择适当的硫酸酸度,加入一定量的EDTA、氯化钡、硫酸钾,既保证Pb完全沉淀,又防止Sn沉淀。针对样品溶解后既有Sn^(2+)也有Sn^(4+),而且两个价态的锡占比没有规律,无法测定,选择三氯化铁把锡完全氧化为稳定的Sn^(4+),测定时加入抗坏血酸除去多余的Fe3+,防止在电极反应过程中产生的Sn^(2+)再被氧化为Sn^(4+)。实验也证明:电极反应是分步进行的推论。锡的浓度在0.02~200 mg/L线性良好。In the acid base solution, Pb^2+ polarographic peak electric potential is -0.47V, Sn^2+ , Sn^4+ , which voltage is - 0.5V ( vs. SCE) , the peak current overlapped seriously. The proper acidity of sulfuric acid shall be selected in the lab, and a certain EDTA, barium chloride, potassium sulphate shall be added, which can guarantee the complete precipitation of Pb, and can prevent precipitation of Sn. Once the sample dissolves, both Sn^2+ and Sn^4+ are contained, two valence stated tin ratio has no regulation, it cannot be measured, so ferric trichloride is selected to stabilizes Sn^4+ by complete oxidation of tin, and the ascorbic acid is added to remove the redundant Fe^3+ during determination, which can prevent Sn^2+ oxidated to Sn^4+ again in the electrode reaction process. The experiment also proved: the electrode reaction shall be carried out step by step. The linear is good when tin concentration is 0.02 - 200mg/L.
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