To develop a method for the preparation of MgO nanoparticles, precatalyst synthesis from magnesium nitrate with ammonia and calcination was performed in presence of PEG in air. Without PEG, the catalysts are inactive. The conversion to hydroxide was performed using a PEG/MgO mo-lar ratio of 1, but, before the calcination, excess of PEG was either saved (PEG1) or increased to 2, 3, or 4 (PEG 2-4). Catalysts were calcined at 400–660 °C and characterized using XRD, N2 adsorption-desorption, TGA, FTIR, and SEM. The FAME yield in the reactions with methanol depend on the PEG ratio used and the calcination temperature. The optimal calcination temperature and highest FAME yield in the 6 h reactions for catalysts PEG1, PEG2, PEG3 and PEG4 were 400 °C, 74%; 500 °C, 80%; 500 °C, 51% and 550 °C, 31%, respectively. The yield dependence on calcination temperature for catalysts with a constant PEG ratio is similar to that of a bell curve, which becomes wider and flatters with an increase in PEG ratio. For most catalysts, the FAME yield increases as the size of the crystallites decreases. The dependence of FAME and the intermediate yield on oil conversion confirms that all catalysts have strong base sites.