四酢酸鉛標準溶液中の鉛(II)のポーラログラフ法による定量;鉛(IV)水酸化物の沈殿分離法の適用

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Lead(II) contained as an impurity in standard solution of lead tetraacetate was determined by the use of the polarographic method, after the separation of lead(IV) hydroxide. In order to prevent the co-precipitation of lead(II), the hydrolysis of lead(IV) was carried out in an acid solution in the presence of a large amount of aluminum(III). Relations between the concentration of lead(II) in the supernatant solution and the concentration of aluminum(III) added, pH and temperature of the solution, and the agitating time were inveotigated. The proposed procedure is as follows: In the solution (197cm^3) containing 0.5M Al(NO_3)_3, 0.1M HNO_3, and 0.1M KNO_3, and maintained in a thermostat at (25±0.2)℃, 3.00ml of 0.05M lead tetraacetate standard solution is added dropwise and hydrolyzed. After the mixture is stirred for 2 hours, lead(IV) hydroxide is centrifuged from the solution. The resu1ting supernatant solution is taken into a polarographic cell and the polarogram is recorded after removal of oxygen. The concentration of lead(II) in the solution is calculated directly from the calibration curve. By using this method, it was found that lead(II) of 1 to 2% in mole fraction was contained as an impurity in a freshly prepared standard solution of lead tetraactate. These results agreed with the amount of lead(II) estimated in the previous paper.
社団法人日本分析化学会の論文
1975-03-10