A method is proposed to estimate the size distribution of nearly spherical metallic nanoparticles (NPs) from optical extinction spectroscopy (OES) measurements based on Mie's theory and an optimization algorithm. The described method is compared against two of the most widely used techniques for the task: transmission electron microscopy (TEM) and small-angle x-ray scattering (SAXS). The size distribution of Au and Cu NPs, obtained by ion implantation in silica and a subsequent thermal annealing in air, was determined by TEM, grazing-incidence SAXS (GISAXS) geometry, and our method, and the average radius obtained by all the three techniques was almost the same for the two studied metals. Concerning the radius dispersion (RD), OES and GISAXS give very similar results, while TEM considerably underestimates the RD of the distribution.