Vinasse, a dark-colored aqueous byproduct of bioethanol production, contains a variety of organic compounds and inorganic salt ions. In this study, vinasse was utilized as a sacrificial agent in the water splitting reaction using Pt/TiO₂ as a photocatalyst under UV irradiation. The gaseous products generated were analyzed, revealing the formation of hydrogen (H₂) along with other gases, including CO₂, CH₄, CO, C₂H₆, C₂H₄, C₃H₈, and C₄H₁₀. When using filtered vinasse as the sacrificial agent, H₂ and other gaseous products were produced solely through photolysis, even in the presence of the Pt/TiO₂ photocatalyst. Notably, H₂ production from the water splitting reaction was enhanced when inorganic salt ions were removed from the vinasse, and a lower concentration of vinasse was employed in the reaction medium.