Synchrotron radiation at the European Synchrotron Radiation Facility has been used to characterize oxide thin films and multilayers grown by metal organic chemical vapor deposition (MOCVD). Reflectometry measurements were performed in the low angle region to get information on the quality of film/substrate and film/film interfaces of the heterostructures. The experimental data were compared to simulated spectra. High angle diffraction experiments were performed on superlattices of (BaTiO3/SrTiO3)15 and (La2/3Sr1/3Mn03/SrTiO3)15. The multilayers are oriented with the [001] direction perpendicular to the substrate plane. The 001 diffraction peaks were recorded up to the 008 one. The satellite peaks observed for both types of multilayers indicate the good coherence over the whole stacking. For the (BaTiO3/SrTiO3)15 systems, the diffraction peaks were particularly well resolved even for the highest order (008 peak), showing excellent epitaxial quality with abrupt interfaces for periods up to 16 nm.