The aim of this study is to investigate the effect of particle size on the non-isothermal pyrolysis of almond shells (AS) and olive stones (OS) and to show possible differences in the composition of the different fractions obtained after milling and sieving. The results obtained from the study of different particle size of AS and OS samples show significant differences in the solid residue obtained and in the shape and overlapping degree of the peaks, especially with the smaller particle size. These differences can be due to different factors: (a) the amount of inorganic matter, which increases as particle size decreases, (b) heat and mass transfer processes, (c) different sample composition as a consequence of the milling process which may provoke changes in the structure and the segregation of the components (in addition to the ashes) increasingly changes the composition of the sample as the particle size decreases. (C) 2013 Elsevier B.V. All rights reserved.