In the present work the effectiveness of different lignocellulosic biomass fractionation processes based on ultrasounds technology was evaluated. Organosolv (acetic acid 60% v/v), alkaline (sodium hydroxide 7.5% w/w) and autohydrolysis treatments were applied at low temperature and the fractionation effectiveness was measured at different sonication conditions of the raw material. The obtained solid fractions were characterized using TAPPI standard methods, and the liquid fractions main components were quantified with the purpose of studying the effect that the treatment conditions had on the obtained by-products quality. Therefore, obtained lignin samples were characterized by ATR-IR spectroscopy and their thermal behaviour by TGA technique. The results showed that ultrasounds application improved the yield and selectivity of the studied processes and that the obtained lignin did not suffer significant modifications in its physicochemical properties. (C) 2011 Elsevier Ltd. All rights reserved.