Nanocrystalline MgAl2O4 spinel powder was synthesized by pyrolysis of complex compounds of aluminum and magnesium with triethanolamine (TEA). The soluble metal ion-TEA complexes formed the precursor material on complete dehydration of the complexes of aluminum-TEA and magnesium-TEA. Single-phase MgAl2O4 spinel powder resulted after heat treatment of the precursor material at 675 degrees C. The precursor and the heat-treated powders mere characterized by X-ray diffractometry (XRD), differential thermal and thermogravimetric analysis, and transmission electron microscopy (TEM). The average crystallite size as measured from the X-ray line broadening was around 14 nm and the average particle size from TEM studies was around 20 nm.