Human urine is responsible for almost 75% of the nitrogen found in wastewater. Various effective methods for urea splitting are nowadays developed (Urbańczyk et al, 2016), and urea electro-oxidation (UEO) is one promising option (Boggs et al, 2009), easy to implement and operating at room temperature. Nickel and its alloys have proven to be effective and low-cost electrocatalysts for UEO, making large-scale pollution control feasible (Zhu et al, 2020). In addition, the cathodic hydrogen production during the electrochemical process offers an indirect energy source, allowing the nitrogen pollution valorization. The present work aims to get a better understanding of the UEO processes occurring at the electrodeelectrolyte interface that consist in an indirect oxidation in alkaline medium by the Ni(III)/Ni(II) electromediation.