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Cyclic voltametric studies were carried out on mixtures of nickel sulphate, ferrous ammonium sulphate containing ethylene diamine tetra acetic acid, triammonium citrate, boric acid, Sodium chloride in the pH range of 8.5‐10.5 on platinum. The deposition of iron was found to involve the formation of FeOH+ and the second electron transfer is slow. The formation of iron nickel alloy film is anomalous. The charge transfer rates of FeOH+ and NiOH+ determine the deposition. Stripping voltametric curves revealed the dissolution of iron from an intermediate phase rich of iron in the iron‐nickel films.

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