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The effects of reaction parameters on Hurn:xwiley:23670932:media:cptc202000216:cptc202000216-math-0001 production from ethanol photocatalysis in the gas phase have been investigated. The photocatalytic activity evolves from an early mass‐transfer limited regime to an independent one at later irradiation times, which is interpreted in terms of a photocatalytic site activity distribution. Ethanol molar fraction exhibits two different domains, with Hurn:xwiley:23670932:media:cptc202000216:cptc202000216-math-0002 production increasing up to a molar fraction of 0.12, beyond which it plateaus. Hurn:xwiley:23670932:media:cptc202000216:cptc202000216-math-0003 :AcH ratios are very sensitive to reaction conditions, reaching 1.8 at low reactant flows. UV light is converted to Hurn:x-wiley:23670932:media:cptc202000216:cptc202000216-math-0004 with an efficiency of nearly 3 %.