Electropolymerization of Azure A on indium-tin oxide (ITO) and gold electrodes have been carried out from KNO3 aqueous solution. After repetitive voltammetry cycles (electrochemical ageing process), surface morphology of the resulting film is altered involving a deactivation of its pristine electroactivity. Aged and pristine PAA films have been characterized by hyphenated techniques based on spectroelectrochemistry and electrogravimetry (cyclic voltammetry, electrochemical quartz crystal microbalance, and Vis-NIR spectroscopy). Correlation of these techniques allows to obtain the very subtle qualitative and quantitative difference between both films. Accumulation of hydrogen gas inside films is postulated to be the cause of the electrochemical deactivation. In addition, the electroactivity renovation by a soft thermal treatment in oven at 60 degrees C during 24 h is evaluated. (C) 2017 The Electrochemical Society. All rights reserved.