Electrochemical copolymerization of diphenylamine (DPA) with o-chloroaniline (OCA) was performed in aqueous 4M sulfuric acid using the pulse potentiostatic method (PPSM). By employing the tunable parameters in PPSM, polymeric films were deposited under different conditions. Cyclic voltammetry was used for evaluating the characteristics of the deposited polymeric films. A suitable growth equation for the deposition of polymer, relating the charge associated for the film deposition and the pulse parameters in PPSM, was deduced. Various surface parameters are evaluated. The formation of copolymer during PPSM deposition was revealed through critical analysis of the results. The characteristic differences between the individual homopolymers, poly(diphenylamine) and poly(o-chloroaniline) and the copolymer, poly(diphenylamine-co-o-chloroaniline), were brought out. The copolymer was also synthesized through a chemical method and characterized through infrared and ultraviolet-visible spectroscopic analysis. (C) 2003 Wiley Periodicals, Inc.