A combustion route of synthesizing highly crystalline single phase nickel ferrite (NiFe 2 O 4 ) spinel nanoparticles using various amounts of dl-alanine as fuel has been reported in this paper. The role of the amount of fuel is found to be significant in the size control and phase purity of nano crystalline samples. The structural, thermal, morphological and magnetic studies have been carried out. XRD patterns reveal the formation of highly crystalline nano NiFe 2 O 4 with high degree of phase purity when fuel concentration is maintained at 1M and 2M. FTIR spectra also prove the formation of pure nano NiFe 2 O 4 . The temperature and fuel effects are found to have strong influence on size, structural, and magnetic properties of materials. The magnetic measurements show that the nano NiFe 2 O 4 samples exhibit soft ferromagnetism with the highest saturation magnetization Ms at room temperature as 42.53emu/g.