Polyaniline(PAN)/polysulfone (PSF) composite film electrodes were successfully prepared by electropolymerization using cyclic votammetry technique. The composite film electrodes show a great enhancement in electron transfer kinetics, and the separation between oxidation and reduction peaks (Delta E(p)) decreases from 200 to 35 mV for hydroquinone (H(2)Q) and from 275 to 42 mV for catechol (CC) at bare Pt and composite film electrodes respectively. In their mixed systems, the redox peak of H(2)Q and two pairs of redox peaks of CC on this composite film electrode could be obviously distinguished which indicates the composite film electrodes have excellent electrocatalytic activity and reversibility towards the oxidation of two diphenols (hydroquinone and catechol). The linear relationships between the peak current and concentration are observed for single solute and mixed systems within the certain concentration range, implying that the composite film electrodes have potential application in the qualitative or quantitative analysis of diphenol. (C) 2011 Elsevier B.V. All rights reserved.