CoFe2O4 nanoparticles were synthesized by co-precipitating Co(II) and Fe(III) ions in alkaline medium following temperature annealing, aiming to study the influence of the sintering temperature on the structure of the nanosized cubic ferrite. A group of powder samples were submitted to thermal treatment at 373, 623, 1023, 1273, and 1473 K during 30 minutes in atmospheric air. For the purpose of our investigation cobalt ferrite nanoparticles were evaluated by atomic absorption spectrophotometry, X-ray diffraction (XRD), Raman, and Mössbauer spectroscopy. The chemical composition of cobalt ferrite samples, expressed as the [Fe]/[Co] ratio, was found as 2.1. Our results reveal that the increase of the sintering temperature modifies the cation distribution profile, resulting in an improvement of the nanomaterial’s properties.