The nanocrystalline NiFe 2 O 4 particles prepared by solution combustion synthesis technique using different fuels such as ethylene-diamine-tetra-acetic acid (NA sample) and urea (NB sample) were studied using magnetic measurement and 57 Fe Mössbauer spectroscopy with a high velocity resolution. The temperature dependence of magnetization is different for the two samples. Mössbauer spectra demonstrate the necessity to use more than two magnetic sextets, usually used to fit the NiFe 2 O 4 nanoparticles spectra. Evaluation of the different local microenvironments for Fe in both tetrahedral (A) and octahedral (B) sites, caused by different Ni 2+ occupation of octahedral sites, demonstrates at least five different local microenvironments for both A and B sites. Therefore, the Mössbauer spectra were fitted by using ten magnetic sextets which are related to the spread 57 Fe location in octahedral and tetrahedral sites.