My research focuses on the study of chemical and structural changes of model and applied electrodes surfaces at the interface with liquid electrolytes during Oxygen Evolution Reaction (OER), relevant for corrosion and electrocatalysis. The aim is to gain a fundamental atomic scale understanding of the surface dynamics under electrochemical (EC) polarization, shining light on the mechanism that leads to electrode instability and degradation at high EC potentials. In this context, a combination of operando/in situ surface sensitive techniques is required, but the experimental challenges are considerable. In some conditions, synchrotron based intense x-ray techniques provide a sufficient high signal to noise ratio, despite electrolyte attenuation, to detect nanoscale features at the sample surface revealed during the electrochemical reaction. Particularly relevant for these purposes is Total Reflection X-ray Absorption Spectroscopy, a not so common technique which although can provide unique structural and chemical information in operando conditions from the electrode surface.