Alumina gels were prepared by the sol-gel method using alumatrane or tris(alumatranyloxy-i-propyl)amine as precursor synthesised directly from the reaction of inexpensive and readily available compounds, aluminium hydroxide and triisopropanolamine (TIS), via the one step process. Sol-gel process parameters, such as gel time, were correlated to variables of the initial stage of the process, such as pH, temperature of hydrolysis and hydrolysis ratio. The sol-gel transition of alcoholic alumatrane solutions was monitored by multiple waveform rheological measurements. The gel time could be determined from the evolution of the storage (G ) and loss (G ) moduli versus time at different frequencies using the Winter Chambon criterion (convergence of the loss tangents at the gel point). Increasing pH values, hydrolysis ratio and/or temperature accelerated the kinetics of hydrolysis-condensation reactions and thus reduced the gel time. The apparent activation energy of the cross-linking leading to the gelation calculated from the gel times at various temperatures was found to be approximately 139 kJ mol −1 and independent of hydrolysis ratio. Alumina materials prepared from the heat treatment of obtained gel at 500 • C were analysed using X-ray diffraction and the BET method.