Octahedral molecular sieves (OMS) are used as novel heterogeneous catalysts in the selective oxidation of benzyl alcohol to benzaldehyde [1]. Only the chemisorbed oxygen on the surface (O-) and the lattice oxygen in the layers close to the surface are involved in the oxygen transfer during selective oxidation of alcohols [1]. Manganese oxides with tunnel structures (OMS-2) were protonated (HKOMS-2) through an exchange process using concentrated nitric acid, leading to weaker Mn-O bonds. Temperature programmed desorption (TPD) results [1] showed the lattice oxygen in the layers close to the surface to be greatly selective to the reaction. This directly correlates to the increased activity in alcohol oxidation. Potentiometric titrations determined an increase in the average oxidation state of manganese with oxidation of the alcohol. Soft X-ray photoelectron spectroscopy (sXPS) and O K-edge NEXAFS techniques performed at beamline U12A (NSLS BNL) were employed to study pre- and post reaction surface changes in the catalyst material.