Most recently, magnetic ceramic nanoparticles have attracted considerable scientific interest from the basic research point of view and for their prospective use in chemical sensing, catalysis and electrochemical applications. In this paper we report the successful synthesis of xSnO2-(1-x)α-Fe2O3 system by hydrothermal synthesis and that of xZrO2-(1-x)α-Fe2O3 system by mechanochemical activation. The two nanoparticle systems were analyzed side-by-side using X-ray diffraction (XRD) and Mössbauer spectroscopy. The latter technique was used in its complexity, including the determination of the recoilless fraction using our dual absorber method. This was correlated with the onset of new phases in the systems of interest.