Anodic polymerization of the azo dye methoxy red (4-methoxybenzene azo-1,3-diaminobenzene) on platinum electrodes in 1 M HCl in 50% v/v ethanol/water was found to yield thin and stable polymeric films. The films were electroactive in acidic solutions and the activity diminished as the acidity decreased. The pair of symmetrical redox peaks at a formal redox potential, (E degrees)(pH=0) = 0.61 V vs SCE, with a Nernstian slope dE/dpH = 0.06 V, is attributed to a 1:1 proton + electron elimination (on oxidation)/addition (on reduction) at the amino/imino linkages which connect the aromatic nuclei. Chronocoulometric plots indicated that the transport of the solvated protons, and probably Cl- ions, through the film is the rate-determining step of the above redox processes. The rate of electron transfer reactions of the redox couple [Fe(CN)(6)](3-/4-) on poly-methoxy red-covered platinum electrodes decreased by a factor of more than two orders of magnitude, compared to the bare electrodes.