Inert gas condensation was employed to prepare nanoparticles of Mg and MgH2 which morphology, clustering degree and structural stability have been investigated by X-ray diffraction and electron microscopy. Thermodynamic functional properties of the Mg and Mgr2 nanostructured samples were investigated by high pressure differential scanning calorimetry. Some specific features of the morphology of the samples prepared by inert gas condensation are compared with powders obtained by ball milling through desorption kinetics behavior. © 2008 Materials Research Society.