二酸化鉛懸濁液とシュウ酸ナトリウムの酸化還元反応の検討 : 終点検出法及び反応生成物の定量

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タイトル別名
  • 二酸化鉛懸濁液としゅう酸ナトリウムの酸化還元反応の検討　　終点検出法及び反応生成物の定量
  • Investigation of the redox reaction of lead dioxide suspension with sodium oxalate
  • 2サンカ ナマリ ケンダクエキ ト シュウサン ナトリウム ノ サンカ カンゲ
  • 終点検出法及び反応生成物の定量

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説明

The methods for detecting end point in the heterogeneous redox reaction system in which a suspension of lead dioxide was titrated with a standard solution of sodium oxalate, were investigated. The derivative polarographic titration method (the conventional potentiometric titration method at a constant current, so called DPT method) using a pair of platinum electrodes, and the visual titration method in which the suspension changes to become the clear solution just at the end point, were investigated. The reaction products, CO2 and Pb(II), were also determined. The value of optimum current density for the DPT method was estimated from the current-potential curves obtained by the DPT method, on the basis of the polarograms using a rotating platinum electrode. It was found that the shape of the titration curve at the end point in the DPT method depends on the behavior of the anodic wave of oxalate ion, added in slight excess of the equivalent amount. From the results of this titration method, the error for the calculated value on the assumption that the equivalence point is located at the point in 1 : 1 molar ratio, was within about ± 1 %, and the relative standard deviation was ± 0.7%. Effect of the titration condition, i.e., current density, concentration of HNO3, concentration of Pb(IV) and temperature of the solution, was investigated.

収録刊行物

  • 分析化学

    分析化学 26 (10), 687-691, 1977

    公益社団法人 日本分析化学会

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