A novel experimental/numerical method is set up in order to decouple water and oxygen diffusion phenomena and to prove the occurrence of thermo-oxidation during hygrothermal aging of thermosetting resins for RTM composite applications. The method consists of creating artificial environmental conditions under pure water, pure oxygen and a water/oxygen mixture and in following the mass uptake of polymer samples during aging. Global and local (ultra-microindentation) mechanical properties of samples are then measured during and after aging, for each environmental conditioning. By analyzing the gravimetric curves with the aid of diffusion-reaction models and the results of mechanical tests, it is shown that water and oxygen diffusion phenomena are coupled in a complex way and that diffusion/reaction phenomena between water and oxygen take place during hygrothermal aging.