A series of alumina samples were prepared with aluminium secondary butoxide (ASB) as precursor. The effect of variations in preparation parameters like nature of hydrolysing solvents and pH during hydrolysis were investigated. The total surface area (SA), pore size distribution, pore volume (PV), alumina phase and morphology were determined for various samples. It was observed that alumina prepared in this method has a high surface ml/g. A major part of the surface area is present in mesoporous region with radii around the dominant pore radius of 105 Angstrom. Changes in the pore-structure and pore size distribution could be observed by : (i) varying the medium of hydrolysis from water to a mixture of water and isopropyl alcohol and(ii) carrying out hydrolysis at base/alkoxide mole ratios 0.3 to 1.1. For a given ratio of water/ASB, PV and SA increased with base/alkoxide ratio.