The synthesis and characterization of seven nanostructured NiFe2O4 ferrite samples with spinel type structure were studied. The samples were synthesized by the sal-gel autocombustion method, using cellulose, a cellulose-citric add mixture, hexamethylenetetramine, citric acid, tartaric acid, glycine and urea as chelating/fuel agents. For the first time in the nickel ferrite synthesis developed by this method, hexamethylenetetramine and tartaric add were used as chelating/fuel agents. The as-obtained samples were characterized by IR spectroscopy, XRD SEM and BET techniques. The catalytic properties of nanostructured NiFe2O4 samples were tested for hydrogen peroxide decomposition. The influence of chelating/fuel agents was highlighted in terms of combustion process development with consequences on particle size, interionic distance values, surface area, microstructure and catalytic activity. The best catalytic properties were recorded for NiFe2O4 obtained with urea as a chelating/fuel agent. (C) 2013 Elsevier B.V. All rights reserved.