X-ray and Mössbauer studies have been made on Co 0.5−x Mn x Zn 0.5 Fe 2 O 4 prepared by the co-precipitation method from stoichiometric aqueous solutions. In these compositions x varies from 0.0to 0.5in steps of 0.1. The as-synthesized powders were characterized by the X-ray diffraction analysis (XRD), transmission electron microscopy, Fourier transform infrared spectroscopy (FTIR), vibrating sample magnetometer (VSM) and Mössbauer spectroscopy at room temperature. The XRD results revealed the production of a broad single cubic phase with the average crystallite size of about 5–8nm. The FTIR measurements between 400 and 4000cm −1 confirmed the intrinsic cation vibrations of the spinel structure. The Mössbauer spectral studies showed that the substitution of magnetic Mn 2+ is responsible for the increase in the intensity of the central paramagnetic doublet. The VSM results showed that as the Mn content increases up to 0.4the Curie point, the coercivity and saturation magnetization decrease.