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Membrane–electrode assemblies (MEAs) designed for a polymer electrolyte membrane (PEM) water electrolyser based on a short-side chain (SSC) perfluorosulfonic acid (PFSA) membrane, Aquivion®, and an advanced Ir-Ru oxide anode electro-catalyst, with various cathode and anode noble metal loadings, were investigated. Electrochemical impedance spectroscopy (EIS), in combination with performance and durability tests, provided useful information to identify rate-determining steps and to quantify the impact of the different phenomena on the electrolysis efficiency and stability characteristics as a function of the MEA properties. This technique appears to be a useful diagnostic tool to individuate different phenomena and to quantify their effect on the performance and degradation of PEM electrolysis cells.