A novel nitrate-citrate gel combustion route was used to prepare fine particle of a series Mg1-xNixFeCrO4 (0.0 <= x <= 1.0) and its structural properties were investigated. The in situ oxidizing environment provided by the nitrate ions in the gel increases the rate of oxidation and lowers the decomposition temperature of component. All the samples after sintering were characterized at room temperature by X-ray diffraction (XRD) method and Mossbauer spectroscopy techniques. The X-ray and Mossbauer studies confirmed the single phase cubic spinel structure with all Fe ions in 3+ charge state. XRD and Mossbauer studies revealed that the samples of x = 0.0, and 0.2 are random spinet and show rather broad lines, while x = 0.4-1.0 are inverse spinel. (C) 2013 Elsevier Ltd. All rights reserved.