Nanostructured materials are very promising for technological applications such as sensors, magnetic recording technology and magnetic liquids for drug delivery, hence driving systematic studies to tailor their structural and morphological properties for specific (bio)physical and/or (bio)chemical properties. In this way, chemical methods based on adding chelating agents are widely used to control their structural and morphological properties. We have recently showed that samples grown adding sucrose and glycerol result on particles with different morphologies and sizes, that in turn drastically influence their magnetic behavior changed, i.e. for the obtained nanoparticles we observed an increase of the Morin transition with the diminution of particle size. Neutron Powder Diffraction is thus fundamental for elucidating the influence of the structural changes in the magnetic behavior of these nanostructured Hematite samples.