Mn0.25Fe2.75O4-PEG nanoparticles based on local iron sand were synthesized using the coprecipitation method. The characterization of sample was conducted using the X-ray Diffraction (XRD) instrument, Fourier Transform Infrared (FTIR), Small Angle X-Ray Scattering (SAXS), and Magneto-thermal each has a purpose to find out the formed phase structure, the adsorption pattern of sample functional group, nanoparticle distribution, and thermal effect of the sample. The results of characterization using XRD showing that the formed sample phase was in the form of the magnetite spinel structure. Through Rietica analysis and calculation using Debye-Scherrer, the sizes of nanoparticle samples were 7.9, 6.4, and 5.3 nm respectively with the addition of PEG concentration of 1000, 2000, and 4000. The adsorption of nanoparticle functional group was confirmed well with the appearance of Fe-O and Mn-O bound adsorption, at the wavenumbers of 430 cm-1 and 482 cm-1 respectively which were the representations of Mn0.25Fe2.75O4 material. Furthermore, the SAXS data analysis using the two lognormal method showed that the primary size of the particle sample was around 3 nm. Meanwhile, the secondary sizes of the sample were 8.5, 7.1, and 5.9 nm with the addition of PEG concentration of 1000, 2000, and 4000. Interestingly, Mn0.25Fe2.75O4-PEG nanoparticles of 1000, 2000, and 4000 characterized using the Magneto thermal instrument have the value of 1.079, 1.082, and 1.105 W/g respectively and was able to improve the temperature of 37 °C up to 38°C. These characteristics showed that the Mn0.25Fe2.75O4-PEG nanoparticles have potentials to become a unique material which can function as the material for hyperthermia therapy.