Liquid-solid separation of cobalt(Ⅱ)with phenanthroline- potassium thiocyanate-water system
ZUO Guoqiang1,WANG Yongkui2, LIU Gaiyun1, GU Zengxin1, QIN Bohan1
1. Department of Metallurgy and Chemical Engineering, Jiyuan Vocational and Technical College,Jiyuan 459000, China; 2. School of Municipal and Environmental Engineering,Henan University of Urban Construction, Pingdingshan 467036, China
摘要 当分析元素含量极低时,往往要求在测定之前辅以化学分离预富集手段以纯化富集待测物和除去干扰基体。实验利用邻菲罗啉和硫氰酸钾作为微痕量Co2+的络合剂,建立了一种液固体系分离富集微痕量Co2+的新方法。分别考察了邻菲罗啉溶液用量、硫氰酸钾溶液用量、酸度对分离效率的影响。结果表明,当体系中Co2+含量为100 μg时,控制体系pH=2~6,加入1.00 mL 1.5 g/L邻菲罗啉溶液、1.00 mL 0.1 mol/L硫氰酸钾溶液、1.00 mL 10 g/L EDTA溶液、1.00 mL 40 g/L硫脲溶液,震荡静置后,Co2+与邻菲罗啉、硫氰酸钾反应生成的离子缔合物定量沉淀到溶液底部,而Cd2+、Fe3+、Zn2+、Ni2+、Cu2+、Pb2+、Al3+、Ag+等离子仍留在水相中,从而实现了Co2+与这些离子的定量分离。方法成功用于合成水样中微痕量Co2+的定量分离,富集率在97.2%～98.6%之间。
Abstract：When the content of test element was very low, the chemical separation and enrichment method are usually required before determination for the pyrification enrichment of analytes and the removal of interference matrix. A new method for the separation and enrichment of micro or trace Co2+ in liquid-solid separation system was proposed with phenanthroline and potassium thiocyanate as the complexing agent. The effect of phenanthroline solution dosage, potassium thiocyanate solution dosage and solution acidity on the separation yields were investigated, respectively. The results showed that in the presence of 1.00 mL of 1.5 g/L phenanthroline solution, 1.00 mL of 0.1 mol/L potassium thiocyanate solution, 1.00 mL of 10 g/L EDTA solution, and 1.00 mL of 40 g/L thiourea solution, 100 μg of Co2+ could react with phenanthroline and potassium thiocyanate to form ion association complex at pH 2-6 after oscillation and stillness, which could be quantitatively precipitated to the bottom of the solution.Whereas Cd2+,Fe3+,Zn2+,Ni2+,Cu2+,Pb2+,Al3+,Ag+ remained in the water phase, thus realizing the quantitative separation of Co2+ from these ions. The proposed method was successfully applied to the quantitative separation of micro or trace Co2+ in synthetic water samples. The enrichment yields were between 97.2% and 98.6%.
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