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MgAl2O4 spinel was synthesized by a novel route method of sol-gel technique. Spinel powders were sintered at various temperatures to investigate the phase contents and crystallinity. The characterization of the samples was carried out by using various techniques. The formation of the spinel phase was inferred by differential thermal analyzer, while crystalline and structural properties were studied by X-ray diffraction, Fourier transform infrared spectroscopy and magic angle spinning nuclear magnetic resonance (MAS-NMR). These studies infer the formation of spinel phase at much lower temperature (around 375 °C) and order-disorder transition in the spinel around 700 °C. The studies also indicate the formation of the spinel with better crystallinity. The inversion parameter was also calculated using MAS-NMR and its value is found to be approximately 0.30 for a sample sintered around 1000 °C. [ABSTRACT FROM AUTHOR]