BackgroundIn the face of escalating water pollution challenges, the study explores the efficacy of Electro-Fenton (EF) treatment using NiTiO3 perovskite-modified cathodes for methylene blue (MB) removal from wastewater. MethodsEmploying a Central Composite Design (CCD) methodology, significant factors influencing the EF process, including initial MB concentration, pH, applied current, and reaction time, were optimized. The NiTiO3 catalyst was meticulously characterized, revealing its rhombohedral crystal structure, uniform particle distribution, and efficient charge transfer properties. FindingsElectrochemical analyses demonstrated the superior performance of the NiTiO3/Graphite electrode, emphasizing its increased electroactive sites, enhanced oxygen reduction capability, and reduced charge transfer resistance compared to the bare Graphite electrode. The EF process was finely tuned, demonstrating a 95.38 % removal efficiency of MB at optimal conditions (initial concentration: 25 mg L−1, pH: 4.5, current: 40 mA, time: 110 min). This study underscores the promising potential of NiTiO3-modified cathodes in advanced water treatment applications, highlighting their robust efficiency and environmental significance in combating persistent organic pollutants.