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Core–shell Fe2O3@C nanoparticles are very studied due to its biocompatibility with plant and animals cells and due its special properties of chemical adsorption. Thus, the definition of an easy synthesis method of these nanoparticles is very important to the scientific studies and to future applications of these materials. For example, the properties of these nanoparticles depend of the combination between some processing parameters, as the temperature, time, chemical composition, atmosphere and others. The mass yield of the synthesis processes depend of these parameters and are important information. In this work the effect of temperature and of the concentration of the iron precursor were evaluated on the characteristics of the proposed nanoparticles. The nanostructures of Fe2O3 coated with carbon (Fe2O3@C) were synthetized by adapted co-precipitation hydrothermal rote. In 40.0 ml of distilled water was added 1.800 g of glucose, 6.006 g of urea, 0.500 g of polyethylene Glycol (PEG 1500) and different concentrations of iron nitrate Fe (NO2)3.9H2O and different temperature values were applied. The Fe2O3@C core-shell were characterized by scanning electron microscopy (SEM/FEG), Energy Dispersive Scanning (EDS) and X-ray Diffractions (XRD). Results showed that nanoparticles form clusters with different sizes that are dependent on the temperature values and Fe (NO3)3.9H2O concentration. The core-shell mass has a linear relation with the iron precursor mass and the reaction temperatures influences the microstructure of the core-shell nanoparticles.