The textural and structural properties of a skeletal Ni catalyst prepared by alkali leaching of aluminum from the rapidly quenched Ni50Al50 alloy have been investigated by elemental analysis (ICP-AES), nitrogen physisorption, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and H-2 thermal desorption techniques. As compared to Raney Ni, such a skeletal catalyst has a residual Ni2Al3 phase, lower surface area, higher average pore diameter and porosity, larger mean crystallite size, and unit-cell parameter. These differences are attributable to the metastable character of the pristine rapidly quenched alloy and their relationship with the catalytic behavior is discussed and correlated. (C) 2003 Published by Elsevier Inc.