We propose quantitative analysis of chemical and phase composition of Zn−Ni alloy depending on the film thickness, using potentiodynamic stripping in an alkaline ammonia‐glycinate electrolyte. The mechanism of dissolution of zinc‐enriched Zn−Ni alloy films in this electrolyte comprises sequential stages of dissolution of zinc‐phase and zinc from a γ‐phase of various structures, followed by dissolution of the nickel‐enriched residue, formed by dezincification, and matrix nickel.