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The photochemical activation of methane over a substrate containing Rh'(C0)z species has been studied using transmission infrared spectroscopy. At 233 K, methane activation is achieved by the oxidative addition of the C-H bond to a postulated 16-electron surface species, Rh'(CO), which is produced by UV (325 nm) photodecomposition of the Rh1(CO)2 on the surface. The oxidative addition product, Rh(CO)(H)(CH3), further undergoes a migratory-insertion reaction in the presence of CO to form a proposed Rh(CO)(H)(COCH3) surface species. Isotopic experiments using CI8O have been performed to confirm the product assignment.An IR spectroscopic study of acetaldehyde and acetone adsorption following the photoreaction suggests that other CH3CO-containing species may also be formed on the surface as a result of C-H bond activation followed by CH3 insertion into the Rh-CO bond region.