A new methodology is presented to offer the possibility of simultaneously obtaining two different spectroscopic signals in a single spectroelectrochemical experiment. Taking the plane of the electrode surface as a spatial reference, normal-beam and parallel-beam UV−vis absorbance signals are jointly analyzed, revealing important experimental differences between the two kinds of signals. Two different chemical systems are selected to show the possibilities of the bidimensional spectroelectrochemistry: a simple diffusive process and an adsorptive electrode reaction. Comparative results show clearly that the two kinds of spectroscopic signals, both normal and parallel to the electrode surface, have to be used together in the study of any electrode reaction scheme.
