锗(Ⅳ)-没食子酸示波极谱电流增敏机理研究Ⅰ.高温合金中锗的测定及有关研究  

Study on the Enhancement Mechanism of the Oscillopolarographic Current of Germanium(Ⅳ)—Gallic Acid System Ⅰ.Determination of Germanium in Superalloys and Investigation

作　　者：张月霞[1] 吴永明[2] 

机构地区：[1]冶金部钢铁研究总院,北京100081 [2]北京科技大学

出　　处：《冶金分析》1997年第3期8-11,14,共5页Metallurgical Analysis

基　　金：国家自然科学基金会及中科院长春应用化学研究所电分析化学开放研究实验室资助课题

摘　　要：研究表明,锗(Ⅳ)-没食子酸在稀硫酸介质中的络合吸附电流,由于钒(Ⅳ)及 EDTA 的加入生产高灵敏络合吸附平行催化电流,共增敏1200余倍。计算得化学反应速率常数 k_1=14.4×10~6L/mol·s^(-1)。锗(Ⅳ)浓度0.04～20ng/ml 与其电流峰高呈线性关系。线性回归方程式:(μA·s^(-2)=0.78+85(μg/25ml),相关系数r=0.9996。检出限为5×10^(-11)mol/LGe(Ⅳ).为迄今同类测定锗的最灵敏方法之一,用于高温合金中痕量锗的测定,结果准确,与光度法及 ICP-MS 测得结果一致。The experimental results demonstrated that the complex adsorptive current of germanium(Ⅳ)-gallic acid in the medium of dilute sulfuric acid could produce a sensitive complex adsorptive parallel catalytic current after adding vanadium(Ⅳ) and EDTA.The peak height was about 1200 times higher than that of the original current.The rate constant(k_1)of chemical reaction was calculated to be 14.4×10~6L/mol·s^(-1).Under the optimum conditions the linear range and the detection limit were 0.04-20ng/ml and 5×10^(-11)mol/L for Ge(Ⅳ),respectively.The linear regression equation was Y(μA·s^(-2))=0.78+85X(μg/25ml) and the correlation coefficient(r)was 0.9996.The method is one of the most sensitive methods among that of the same kinds and has been applied to determine the micro amounts of germanium in superalloys with satisfactory results which were in good agreement with that of spectrophotometry and ICP-MS.

关 键 词：锗分析 没食子酸 示波极谱法 高温合金 

分 类 号：TG132.32[一般工业技术—材料科学与工程] TG115.334[金属学及工艺—合金]