Polyaniline (PANI)-molybdenum trisulfide (MoS3) electrode, prepared by a multi-step procedure, and polyaniline electrode were characterized in non-aqueous electrolyte (0.5 M LiClO4/acetonitrile) by cyclic voltammetry, electrochemical impedance spectroscopy and the electrochemical quartz crystal microbalance (EQCM). The voltammetric charge decreased slightly (20%) upon incorporation of MoS3 in the PANI film electrode. The normalized low frequency capacitance defined as the low frequency capacitance/voltammetric charge ratio is identical for both PANI and PANI-MoS3 electrodes suggesting that MoS3 does not contribute to the capacitance measured. The EQCM data is consistent with mixed transport of anions and cations. Upon oxidation in 0.5 M LiClO4/acetonitrile, a mass change of 43 g/mol is observed for PANI-MoS3 and this suggests that solvent is also involved in addition to ClO4- ingress and Li+ expulsion.