Thermal analysis of alumina precursors prepared by two different PFHS (precipitation from homogeneous solution) methods and a conventional method is described. All three precursors exhibit distinct thermal behaviour patterns, marked by multiple phase transformations, to yieldγ-Al2O3 ultimately. Thermal analysis studies, coupled with XRD, IR and elemental analysis data, indicate that the precursors obtained by the PFHS methods are monophasic in nature, and hence yield relatively small, uniform microspheroidal alumina in comparison with the alumina obtained by the conventional method.