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机构地区:[1]信阳师范学院化学化工学院,河南信阳464000 [2]郑州铁路职业技术学院,河南郑州450052
出 处:《冶金分析》2013年第6期76-79,共4页Metallurgical Analysis
基 金:河南省教育厅自然科学研究计划项目(2006150023)
摘 要:研究了氯化钠-正丙醇-硫氰酸铵-水体系析相萃取分离和富集Sn(Ⅳ)的行为及与一些金属离子分离的条件。结果表明,氯化钠能使正丙醇的水溶液分成两相,在分相过程中,Sn(Ⅳ)和硫氰酸铵生成的[Sn(SCN)5~6][(5~6)-4]-与质子化正丙醇C3H7OH2+形成的缔合物[Sn(SCN)5~6][C3H7OH2]1-2能被正丙醇相完全萃取。固定溶液酸度为pH 2,当正丙醇、硫氰酸铵和氯化钠的浓度分别为30%(V/V)、0.09mol/L和0.17g/mL时,Sn(Ⅳ)的萃取率在98.3%以上,Fe(Ⅳ)、Ni(Ⅳ)、Pb(Ⅳ)、Al(Ⅲ)、Mg(Ⅳ)、Mn(Ⅳ)、Ce(Ⅲ)、Cr(Ⅲ)、Zn(Ⅳ)、Ag(Ⅰ)、Cd(Ⅳ)和V(Ⅴ)不被萃取,实现了Sn(Ⅳ)与上述金属离子的分离。方法用于Pb-Ca-Sn-Al合金中Sn的分离和测定,平均回收率为97.4%,相对标准偏差(n=7)为2.1%。The behavior and conditions for extraction separation and enrichment of stannum (Ⅳ) from other metal ions in sodium chloride-1-propanol-ammonium thiocyanate-water system were investigated.The results showed that 1-propanol aqueous solution could be well divided into two phases in presence of sodium chloride.During the phase separation process,[Sn(SCN)5~6]^[(5~6)-4]-formed from stannum (Ⅳ) and ammonium thiocyanate could reacted with protonized 1-propanol of C3H7OH2+ to form associated complex of[Sn(SCN)5~6][C3H7OH2]1-2,which could be fully extracted by 1-propanol phase.When acidity of the solution was fixed at pH 2.0,and the concentration of 1-propanol,ammonium thiocyanate and sodium chloride was 30%(V/V),0.09mol/L and 0.17g/mL,respectively,the extraction yield of stannum? was more than 98.3%.Simultaneously,Fe(Ⅳ)、Ni(Ⅳ)、Pb(Ⅳ)、Al(Ⅲ)、Mg(Ⅳ)、Mn(Ⅳ)、Ce(Ⅲ)、Cr(Ⅲ)、Zn(Ⅳ)、Ag(Ⅰ)、Cd(Ⅳ) and V(Ⅴ) could not be extracted,realizing the separation of stannum (Ⅳ) from these metal ions.The method has been applied to the separation and determination of stannum (Ⅳ) in Pb-Ca-Sn-Al alloy sample with recovery of 97.4%and relative standard deviation(n=7)of 2.1%.
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