H-1 and H-2 MAS NMR spectroscopy were utilized for investigating the interaction of surface complexes upon adsorption of cyclohexanone and cyclododecanone oxime on MFI-type zeolites and [Al]SBA-15. Signals of hydrogen-bonded and protonated complexes were identified and evidenced the diffusion of cyclohexanone oxime into the micropores of silicalite-1 and ZSM-5 and limited accessibility of acid sites in [Al]SBA-15 for cyclododecanone oxime.