AbstractUltrasonic irradiation with organic solvents and alkaline extractions were carried out on a fast-growing poplar wood, triploid of Populus tomentosa Carr., in an attempt to develop efficient lignin isolation procedures. Four organosolv and three alkaline lignin fractions were successively isolated and comparatively characterized by sugar analysis, alkaline nitrobenzene oxidation, gel permeation chromatography (GPC), Fourier transform infra-red spectroscopy (FT-IR), quantitative 13C, and 2D HSQC nuclear magnetic resonance (NMR) spectroscopy, as well as thermogravimetric analysis (TGA). The results showed that the ultrasonic treatments and sequential extractions with three different concentrations of NaOH led to a release of 90.9% of the original lignin. The four organosolv lignin preparations obtained under the ultrasound-assisted extractions were degraded significantly and contained more carbohydrate and non-condensed syringyl units when compared to the three alkaline lignin preparations. Furthermore, the analyses confirmed that L5, the lignin preparation with the highest yield (44.6% of the original lignin), was partially acylated at the γ-carbon of the side-chain preferentially over syringyl units. The percentage of lignin acylation of β-O-4’ linkages was about 14%. The amount of β-O-4’, β-β’, and –OCH3 were estimated to be about 0.31/Ar, 0.06/Ar, and 1.73/Ar, respectively. The ratio of S/G was calculated to be 2.0.