The transformation of lignocellulosic biomass (LB) to obtain chemicals, materials and biofuelsthrough the establishment of biorefineries is in full development. The difficulty in valuing this LB lies in itschemical and physical complexity, with cellulose, hemicelluloses and lignin forming a complex three-dimensional network. To facilitate the accessibility, progression and action of the catalysts in the lignocellulosicmatrix, a physico-chemical pretreatment step of the LB is necessary. Given the cost of pretreatment, it iscritical to understand and predict their effects on LB. In our project, we have designed one of the most comprehensive datasets to date on the chemical evolution ofpoplar wood polysaccharides and their degradation products during dilute acid pretreatment. Anunprecedented set of 38 conditions was generated using a design of experiment approach within the followingparameter ranges: 2-60 min, 120-190°C, 0-4%wt H2SO4. These conditions were applied to carefully selected poplar samples using an in-house fully instrumentedpretreatment device (schematic diagram below) designed to accurately apply the operating conditions(temperature and residence time). Solid poplar wood residues and pretreatment liquid were analyzed for 12wood-derived compounds (sugars, inhibitors, and lignin), but also for gravimetric and spectral evolution. Allthese data have been compiled in a fully available dataset of the evolution of poplar wood and provided with anadvanced description of the equipment and methods to encourage sharing and easy reuse.