3-Aminophenylcalixpyrrole (3APCP) was grafted to a glassy carbon (GC) surface during the electrochemical oxidation process in 0.1 M tetrabutylammoniumtetra-fluoroborate (TBATFB) containing acetonitrile solution. The presence of a surface film was confirmed electrochemically by comparing voltammograms of dopamine and ferricyanide redox probes at the bare and modified electrodes. Reflection-absorption infrared spectroscopy (RAIRS), XPS, atomic force microscopy (AFM), ellipsometry and the contact angle measurements were also employed to characterize 3APCP film on GC electrode. RAIRS analysis revealed that calixpyrrole was bonded to the glassy carbon surface via the etheric linkage. The stability of the modified GC electrode was also studied. Copyright (C) 2011 John Wiley & Sons, Ltd.