As shown in another communication to Symposium V, nano-sized aluminasenriched in pentacoordinated aluminum (Alv) are obtained throughthe limited hydrolysis of aluminum alkoxides. Here the surface properties ofthese aluminas are investigated from the catalytic point of view. The goalis to obtain geometrical information on the Lewis acid sites. 1H→27A1 (cross-polarization) high resolution MASNMR, using chemisorbed NH3 which acts as a XH spinreservoir, allows the direct observation of surface Al involved in thecatalytic site. The polarization transfer from these protons to surface Alis remarkably efficient because of the relatively short A1:N-H distance. Itis observed that the main Lewis acid sites are located on distortedtetrahedral aluminum and pentacoordinated Al. These results are compared tolow temperature infrared data of adsorbed CO.