The present investigation is a follow-up of studies on glycine-nitrate autoignition technique for production of magnesium aluminate nano-particles. The technical characteristics of powders were studied in relation to a wide range of pH, 2.5-10.5. The effect of pH on particle formation was particularly emphasized to achieve a powder in nano-scale. In preparation of precursors the Mg/Al mole ratio was considered to be 0.50 and the level of fuel/NO3 was adjusted at 0.75. The thermal behavior of precursors was evaluated by DTA-TG technique. Also, the obtained powders were calcined at 600, 800, 1000 and 1200 degrees C and characterized by XRD, BET, TEM and elemental analysis methods. The results indicated that the physico-chemical characteristics of products are strongly influenced by the pH of synthesis environment. The precursor prepared in pH of 2.5 exhibits flaming type ignition, while the precursors synthesized at neutral and alkali environments show underwent smoldering type combustion. In conclusion, the optimum characteristics were achieved when precursor is manufactured at neutral condition. (C) 2015 Elsevier B.V. All rights reserved.