Résumé : A novel way has been proposed to follow the formation of nanocrystalline magnetite. Iron oxide nanoparticles were synthesized by the thermal decomposition of Fe(acac)(3) in the presence of oleic acid and oleylamine surfactants at high temperature. The species produced during the synthetic process are characterized through their effects on the proton nuclear magnetic relaxation of the reaction medium and their sizes. As shown by transmission electron microscopy, photon correlation spectroscopy and x-ray diffraction, the diameter of nano-objects increases when the time synthesis is longer. Magnetic properties evaluated by nuclear magnetic resonance (NMRD profiles, T(1) and T(2) measurements) were correlated with the size parameters.