The role of different basic media for the preparation of Zn-Al based hydroxy compounds, leading to the formation of ZnAl2O4 spinel at low temperature was investigated. Nitrate salts of respective cations with molar ratio for ZnO:Al2O3 as 1:1 were used for coprecipitation. DTA, TGA, XRD, IR spectroscopy and SEM technique were utilised for characterization of the precursor hydroxy compounds as well as the final products obtained by heat treatment of the hydroxy compounds at different temperatures. It had been found that spinel formation was very much influenced by the nature of mixed hydroxide precursors obtained by using different basic media. The thermal treatment of the coprecipitated gel powders led to the formation of ZnAl2O4 at relatively low temperature (500°). Mixed hydroxide gel powder obtained by using NH4OH- hexamethylene tetramine (HMT) as basic medium was observed to exhibit best results so far as spinel formation at low temperature was concerned.