Precipitation of magnesium aluminate hydrate with faster addition of ammonia at desired pH causes agglomeration. Agglomerated powder, without any further treatment, on calcination forms intermediate compounds at low temperatures (≤ 900°C). The intermediate compounds on further heat treatment (≥ 1000°C) decompose into MgO, MgAl 2 O 4 and α-Al 2 O 3 . Effect of agglomeration and absorption of foreign ions such as Cl -, SO 2 4-, and NH + 4 in complex compounds probably cause loss of Al 3+ and Mg 2+ ions during heat treatment, and stoichiometry changes. Powders prepared by continuous method with better control of process parameters than batch process yields better spinellization.