A surfactant assisted co-precipitation method was employed for the low temperature synthesis of magnesium aluminate spinel with nanocrystalline size and high specific surface area. Pluronic P123 triblock copolymer and ammonia solution were used as surfactant and precipitation agent, respectively. The prepared samples were characterized by thermal gravimetric and differential thermal gravimetric analyses (TG/DTG), X-ray diffraction (XRD), N-2 adsorption (BET) and transmission electron microscopy (TEM) techniques. The effects of several process parameters such as refluxing temperature, refluxing time, pH, P123 to metals mole ratio (P123/metals) and calcination temperature on the structural properties of the samples were investigated. The obtained results showed that, among the process parameters pH and refluxing temperature have a significant effect on the structural properties of samples. The results revealed that increase in pH from 9.5 to 11 and refluxing temperature from 40 degrees C to 80 degrees C increased the specific surface area of prepared samples in the range of 157-188 m(2) g(-1) and 162-184 m(2) g(-1), respectively. The XRD analysis showed the single-phase MgAl2O4 was formed at 700 degrees C. (C) 2012 Elsevier Ltd. All rights reserved.