Degradation of polyaniline films electrodeposited on optically transparent gold electrodes has been followed by thin-layer bidimensional spectroelectrochemistry. The influence of the anodic potential reached during multiple potential scans has been assessed. Correlation of changes in the spectral signals in normal and parallel arrangement has enabled identifying species of different nature, both soluble and insoluble, electroactive and inert, during the degradation of the polymer film. The three bidimensional spectroelectrochemistry signals have demonstrated the occurrence of different types of degradation processes depending on the applied potential, ranging from the simple release of oligomers and hydrolysis products retained in the film during electropolymerization to more dramatic modifications of the film.