Exposure to radiation can lead to the breakdown of water into reactive oxygen species (ROS), such as hydroxyl radicals (OH·), through a process called radiolysis. The presence of hydroxyl radicals (OH·) and other ROS can cause mutations to DNA in the human body. While hydrogen peroxide (H₂O₂), a product of radiolysis, may not be a strong ROS on its own, it can react with certain metal ions such as iron(II) to produce hydroxyl radicals in a process called the Fenton reaction. This study investigates the optimal conditions for the Fenton reaction using a cost-effective spectroscopic analysis of ferric thiocyanate and degradation of methyl orange to detect the presence of Fe3+ and OH·. Understanding conditions and methods of detection for the Fenton reaction is relevant due to the carcinogenic nature of the hydroxyl radicals produced (Kumar et al., 2021). The results of the spectroscopic analysis suggest that the Fenton reaction occurs ideally in acidic environments (p = 0.00354) with low temperature dependence. Additionally, both spectroscopic methods are effective for detecting the efficiency of Fenton processes. This study provides valuable insights for future research on the Fenton reaction and its potential applications.