In this study, films of poly[1-(4-methoxyphenyl)-1H-pyrrole] [poly(MPPy)] were electrochemically grown on carbon fiber microelectrodes (CFMEs) in 0.05 M of tetraethyl ammonium perchlorate-dichloromethane. The effect of different monomer concentrations (range = 1-10 mM) on electrochemical properties of resulting polymers was characterized by cyclic voltammetry, Fourier transform infrared reflectance-attenuated total reflection spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), and electrochemical impedance spectroscopy. All modified CFMEs were found to have capacitance on the basis of Nyquist, Bode-magnitude, Bode-phase, and Admittance plots. An equivalent circuit model of (R(C(R(QR)))(CR)) gave the best fit for all monomer concentrations used. Furthermore, SEM and AFM results showed that poly(MPPy) was formed as a continuous and well-adhered film onto CFME. (C) 2009 Wiley Periodicals, Inc. Adv Polym Techn 28: 120-130, 2009; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.20152