Nickel zinc ferrite (Ni 0.5 Zn 0.5 Fe 2 O 4 ) nanoparticles were synthesized via solution auto ignition combustion method. The ferrite samples were synthesized with different pH values 3, 5, 7 and 8. The as synthesized samples were calcined at 800 o C for 4 hours. These synthesized nanopowder have been characterized by XRD, SEM and VSM and effect of pH value on the properties of the ferrite samples were studied. XRD pattern confirmed that samples were crystalline in nature. Crystallite size of ferrite powder increased with increase in basic nature of ferrite nanopaticles. Crystallite size of sample was found 24.86nm, 28.10nm, 33.51nm and 39.61nm at pH values 3, 5, 7 and 8 respectively. The magnetization of samples prepared at different pH values 3, 5, 7 and 8 were found 55.490e.m.u./g, 61.420e.m.u./g, 65.541e.m.u./g and 66.512e.m.u./g respectively.