A compact photomicroreactor assembly consisting of a capillary microreactor and small-scale LEDs was developed for the study of reaction kinetics in the gas-liquid photocatalytic oxidation of thiophenol to phenyl disulfide within Taylor flow. The importance of photons was convincingly shown by a suction phenomenon due to the fast consumption of oxygen. Mass transfer limitations were evaluated and an operational zone without mass transfer effects was chosen to study reaction kinetics. Effects of photocatalyst loading and light sources on the reaction performance were investigated. Reaction kinetic analysis was performed to obtain reaction orders with respect to both thiophenol and oxygen based on heterogeneous and homogeneous experimental re...