Monodisperse NiFe nanoparticles with different compositions have been successfully synthesized by surfactant free simple modified polyol method. In the process, polyethylene glycol was used as a solvent media and it has been found to play a key role to act as a reducing agent as well as a stabilizer simultaneously. XRD, TEM, and EDS analysis techniques were used to characterize the synthesized nanoparticles. TEM images displayed formation of a thin oxide layer around the nanoparticles, and confirmed by detection of some oxygen element using EDS measurement. The magnetic properties of the synthesized NiFe NPs samples were measured by vibrating sample magnetometer (VSM) at room temperature, and the saturation magnetization value was found to be iron content dependent. (C) 2013 Elsevier B. V. All rights reserved.