Magnesium aluminate (MgAl2O4) spinel nanoparticles were synthesized by reverse microemulsion process in cyclohexane by using two kinds of surfactants, n-amyl alcohol as cosurfactant and mixture of aluminic/magnesic salt aqueous solution as basic reagents. The effects of surfactant types and titration methods on the morphologies and sizes of the MgAl2O4 nanoparticles were characterized by TEM, TGA-DTA, XRD, HR-TEM and FT-IR. TEM images show that the particles prepared by forward-titration method with SPAN-80/Triton X-100 compound emulsifier have uniform spherical shape and good monodispersity with an average size of 9.5 nm. However, the average size of the particles prepared by reverse-titration method was about 10 nm and some particles have irregular platelike appearance. The products prepared with NP-40 surfactant and forward-titration method were agglomerated with an average size of 13 nm. TGA and XRD results show that the reverse microemulsion method has dramatically lowered the calcination temperature of MgAl2O4 with a degree of 700 °C, and the precursor can transform to single spinel phase at 900 °C.