邻菲罗啉-硫氰酸钾-水体系液固分离钴(Ⅱ)  

Liquid-solid separation of cobalt(Ⅱ)with phenanthroline-potassium thiocyanate-water system

作　　者：左国强[1] 王永奎 刘改云[1] 顾增鑫 秦博涵 ZUO Guoqiang;WANG Yongkui;LIU Gaiyun;GU Zengxin;QIN Bohan(Department of Metallurgy and Chemical Engineering,Jiyuan Vocational and Technical College,Jiyuan 459000,China;School of Municipal and Environmental Engineering,Henan University of Urban Construction,Pingdingshan 467036,China)

机构地区：[1]济源职业技术学院冶金化工系,河南济源459000 [2]河南城建学院市政与环境工程学院,河南平顶山467036

出　　处：《冶金分析》2022年第12期95-101,共7页Metallurgical Analysis

基　　金：河南省2020年科技发展计划(No.202102210259);济源市2020年度科技发展计划(No.20022008);济源职业技术学院青年骨干教师资助项目。

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Co^(2+)的络合剂,建立了一种液固体系分离富集微痕量Co^(2+)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Co^(2+)含量为100μg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,Co^(2+)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Cd^(2+)、Fe^(3+)、Zn^(2+)、Ni^(2+)、Cu^(2+)、Pb^(2+)、Al^(3+)、Ag+等离子仍留在水相中,从而实现了Co^(2+)与这些离子的定量分离。方法成功用于合成水样中微痕量Co^(2+)的定量分离,富集率在97.2%~98.6%之间。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 Co^(2+)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,100μg of Co^(2+)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 Cd^(2+),Fe^(3+),Zn^(2+),Ni^(2+),Cu^(2+),Pb^(2+),Al^(3+),Ag+remained in the water phase,thus realizing the quantitative separation of Co^(2+)from these ions.The proposed method was successfully applied to the quantitative separation of micro or trace Co^(2+)in synthetic water samples.The enrichment yields were between 97.2%and 98.6%.

关 键 词：钴 分离富集 邻菲罗啉 硫氰酸钾 

分 类 号：O657[理学—分析化学] X832[理学—化学]