In this study nanocrystalline MgAl2O4 spinel powders were synthesized with a new synthesis method using ethylene diamine as precipitation agent. The prepared samples were characterized by X-ray diffraction (XRD), N2 adsorption (BET), thermal gravimetric and differential thermal analysis (TGA/DTA), Fourier-transform infrared spectroscopy (FT-IR), and transmission electron microscope (TEM). The obtained results showed a nanocrystalline structure with relatively high surface area and mesoporous structure. Increase in calcination temperature slightly decreased the specific surface area and increased the crystallite size.