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MgFe₂O₄ nanoparticles have been synthesized by coprecipitation method. Magnetic measurements in combination with neutron diffraction have determined the existence of a superparamagnetic state in this metal oxide system. The superparamagnetic relaxation of magnetization in these nanoparticles has been studied by using Mössbauer spectroscopy. The relaxation time has been correlated with the particle size and temperature and is consistent with Néel theory.