ポーラログラフ法によるバナジウムとモリブデンの定量
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概要
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A method for the simultaneous polarographic determination of vanadium and molybdenum in 0.1 <I>M</I> EDTA-0.1 <I>M</I> sodium acetate supporting electrolyte has been studied. In the presence of quinquevalent vanadium the relation between the limiting current and the concentration of molybdenum is not linear, and therefore, a calibration procedure is required for overcoming this interference. Since the limiting current of molybdenum varies linearly with vanadium concentration, the corrected value, <I>h</I><SUB>2</SUB>, against the measured step height of molybdenum, <I>h</I><SUB>1</SUB>, is then given by <I>h</I><SUB>2</SUB>= <I>h</I><SUB>1</SUB><I>k</I>(<I>c</I><SUB>1</SUB>-<I>c</I><SUB>2</SUB>), in which <I>c</I><SUB>1</SUB>, <I>c</I><SUB>2</SUB> and <I>k</I> are, respectively, the standard concentration of vanadium used in preparing a calibration curve, the concentration of vanadium coexisting in the sample solution and the slope of the curve relating <I>h</I><SUB>1</SUB> to <I>c</I><SUB>2</SUB>, and the value of <I>k</I> is got by adding a difinite quantity of vanadium to the same sample solution and measuring the increased step height of molybdenum. The concentration <I>c</I><SUB>1</SUB> should be an approximate average of vanadium concentration expected to increase analytical accuracy. It seems that the cathodic reduction wave of sexvalent molybdenum in this supporting electrolyte is produced by its reduction to tervalent molybdenum, and it is chemically oxidized in the vicinity of the electrode by the coexisting quinque- and quardrivalent vanadium by which sexvalent molybdenum is regenerated.
- 社団法人 日本分析化学会の論文
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