The influence of the cationic composition on the electrochemical deposition of zinc on plane cathodes was investigated. Electrochemical deposition of zinc from aqueous feed needs high purity of the feed electrolyte owing to sensitivity of the hydrogen over-voltage. In contrast to sulfate-based electrolytes, the hydrogen overvoltage in acetic acid can be kept high in electrodeposition of zinc and several heavy metals such as nickel. As a consequence, electrochemical deposition of zinc is possible even at nickel concentrations of 50 mg/l and above. Depending on the electrolyte composition in acetate-based systems the deposition of granular zinc of different particle size, from the micron to the submicron range, is possible on plane electrodes. The chemical composition of granular deposits from several acetate-based electrolytes was analysed by inductively coupled plasma (ICP) analysis and their structure and morphology were detected by scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometry (EDXS).