回転白金電極を用いるシアン化物,塩化物およびシアン酸塩混合物の逐次電流滴定

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Successive amperometric titration of cyanide, chloride and cynate with silver nitrate solution at rotating platinum electrode (1000 rpm) has been investigated at zero applied potential with a saturated calomel electrode. Suspended silver cyanide does not cathodically depolarize the rotating platinum electrode. Silver chloride and silver cyanate readily undergo electroreduction at the rotating platinum electrode in the absence of an inhibitor such as gelatin. Therefore, cyanide in 0.1F potassium nitrate can be titrated in the presence of chloride and cyanate if no gelatin is added to prevent the electroreduction of silver chloride and silver cyanate. Since silver chloride is not electroactive in the presence of 0.02% gelatin, the current remains essentially at zero during the precipitation of chloride, after which continued titration give rises to the cathodic current due to excess of silver ion. Finally cyanate can be titrated at 5°C by adding 25 vol.% methanol to decrease the solubility of silver cyanate as previously reported {this journal, 13, 433 (1965)}. Carbonate ion must be removed by adding barium nitrate prior to the titration. The possible concentration range was as follows; 110×10-3F for cyanide, 210×10F-3 for chloride, 520×10-3F for cyanate. The errors were about 2% for equimolar mixtures of 0.01F solution of cyanide, chloride, and cyanate, respectively. The duration consumed was about 90 minutes.
社団法人日本分析化学会の論文

回転白金電極を用いるシアン化物,塩化物およびシアン酸塩混合物の逐次電流滴定

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