In this work, we use xylan as a model compound for hemicellulose, dissolved in an aqueous 1 M NaOH solution as the reaction medium. The experimental setup consists of a RuO₂ anode, a platinized titanium cathode, and an Ag/AgCl reference electrode. The reactions are conducted under ambient conditions (room temperature and atmospheric pressure) with constant stirring to ensure uniform mixing. Electrochemical techniques including cyclic voltammetry (CV), linear sweep voltammetry (LSV), and constant current experiments (chronopotentiometry, CP) are employed, with the reactions proceeding until a total charge of 25 kilocoulombs (kC) has passed. To evaluate the degradation of xylan and understand the reaction’s products, analytical techniques such as Liquid Chromatography (LC), Total Organic Carbon (TOC), and Chemical Oxygen Demand (COD) are employed. These methods help track the composition of the solution before and after the reaction. Following the successful oxidation of xylan, the study offers innovative solutions for the valorization of waste biogenic polymers into valuable chemicals and fuels.