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This study introduces an electro-dehydrogenation method for converting amines into nitriles in aqueous environments, simultaneously releasing two moles of H2 using nickel electrodes. This eco-friendly process is selective and operates at room temperature, in contrast to traditional thermal methods that require high temperatures and where condensation products are usually observed. Detailed impedance spectroscopy analysis reveals that the dehydrogenation of amines in aqueous media is facilitated by efficient charge transfer, with the diffusion of amines to the electrode surface identified as the kinetically slowest step. Our study underscores the potential of electrochemistry to enhance the reversible dehydrogenation and hydrogenation of the amine/nitrile pair. By demonstrating the practicality and efficiency of this approach, we highlight the amine/nitrile pair as a promising candidate for liquid organic hydrogen carriers. This has significant implications for the future of hydrogen storage and transport technologies, paving the way for more sustainable and efficient energy solutions. [ABSTRACT FROM AUTHOR]