In order to reduce the cost of producing hydrogen through water electrolysis, novel technologies must be improved. Recently, the merging of conventional alkaline electrolysis (AEL) and proton exchange membrane electrolysis (PEM) has led to the development of anion exchange membrane electrolysis (AEMWE), which offers several advantages over AEL and PEM. In a nutshell, this technique employs cheap, abundant, and easily available (non-geostrategic) transition metals with anionic exchange membranes, overcoming the drawbacks of AEL and PEM.[1] To reach the readiness level of this technology, new and scalable synthetic routes for catalysts that lower the overpotential of the sluggish oxygen evolution reaction (OER) are required. Amongst all the OER catalysts reported in the literature, Layered Double Hydroxides (LDHs) have gained increasing attention due to their low overpotentials and stabilities.[2] Besides, electrochemical protocols to determine the activity and stability of these catalysts in different electrochemical cells must be established to understand their properties. Thus, this work focuses on the advantages and limitations of different electrochemical techniques, such as rotating disk electrode (RDE), three-electrode cells, and single-cell tests, to determine the activity and stability of two different LDHs. Unlike laboratory scale LDHs ‒prepared by hydrothermal treatment (HT-LDH)‒ room temperature synthesized LDHs (RT-LDH) can be prepared in kilogram quantities and present chemical structure and morphology differences. In this work, the LDHs have been characterized with spectroscopic techniques to correlate the chemical structure and morphology of the materials to their electrochemical response by RDE, three-electrode cells, and single-cell measurements. All in all, the scalable RT-LDH presents higher activity compared to HT-LDH in all three techniques. On the one hand, small current densities can only be reached by RDE, and the short-term stability of the materials is affected by the catalyst layer interface. On the other side, single-cell test measurements require long operational times, and the contribution of the membrane degradation to the overall cell voltage is still unclear. Thus, three-electrode cell measurements offer the possibility of characterizing LDHs at relevant current densities in a fast and straightforward manner, without membrane contributions, and are further employed in this work to study the stability of these systems. References: [1] N. Du, C. Roy, R. Peach, M. Turnbull, S. Thiele and C. Bock, Chemical Reviews, 122, 11830 (2022). [2] R. Sanchis-Gual, A. Seijas-Da Silva, M. Coronado-Puchau, T. F. Otero, G. Abellán, E. Coronado, Electrochimica Acta, 338, 138613 (2021).