In this work, the electrochemical quartz crystal microbalance has been employed to monitor directly the in situ growth of the zinc hexacyanoferrate film during the electrodeposition. Mass changes of the platinum|crystal working electrode were correlated with cyclic voltammetry data. Effects of the sorption of counter-cations (K(+), Na(+), and ) during redox reactions were studied. The electrocatalytic oxidation properties of procaine by the zinc hexacyanoferrate films were performed.Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)