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In situ diffuse reflectance infrared Fourier transform spectrometry (DRIFTS) and density functional theory (DFT) calculations reveal the reaction mechanism of HCHO. This strategy provides crucial enlightenment for designing novel Mn-based catalysts for application in the HCHO oxidation field.While photoredox catalysis continues to transform modern synthetic chemistry, detailed mechanistic studies involving direct observation of reaction intermediates and rate constants are rare. By use of a combination of steady state photochemical measur