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The dip in the current-potential plateau in the first reduction step of hexaammine cobalt(III) ion (I) and the resulting minimum of the current near -0.8 volt (vs. S.C.E.) have been investigated. A normal polarogram is obtained at relatively high concentrations of sodium perchlorate, nitrate or chloride, the exact concentration required for elimination of the dip increasing with increasing concentration of I. The concentration of barium salt to eliminate the dip is more than five times smaller than that of sodium salt. The cationic surfactants dedecylammonium and tetrabutylammonium perchlorate in a concentration of less than 10M eliminate the dip. At higher concentrations than 10-5 M they cause the first reduction wave of I to become extremely irreversible. The appearance of the dip is correlated with the structure of the double layer on the negative side of the isoelectric point and the adsorption of the positively charged particles formed by interaction of the reduction product Co(NH3)62+ of I with water. No dip occurs when the diffuse double layer is compressed or when its charge is the same as that of the precipitate formed at the surface of the electrode.

Effect on Polarograms of the Product Formed in the One-Electron Reduction of Hexaammine Cobalt (III) Ion (I).