Magnesium ferrite (MgFe 2 O[Formula: see text] being a soft magnetic material with fast frequency response, high a.c. heat power generation and high biocompatibility, is widely used in biomedical fields such as targeted drug delivery, magnetic hyperthermia, etc. This paper reports the synthesis of magnetic MgFe 2 O 4 nanoparticles by hydrothermal method using chloride salts of metal ions. The effect of calcination on the structural and magnetic properties is studied by XRD, FTIR, VSM and Mossbauer spectrum analysis. Fine particles in the size range 3–24[Formula: see text]nm are obtained. On calcination, crystallite size increases and lattice parameter decreases. From the magnetic characterization, it is seen that the magnetic properties mainly depend on crystallite size and cation distribution. The mixed spinel states of the prepared materials are confirmed from the FTIR and Mossbauer spectrum analysis. The doublet spectrum obtained in the Mossbauer studies indicates the superparamagnetic relaxation at room temperature.