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OLIVEIRA, M. M. Nanostructure variability of cellulose from plants and the impact on cellulose nanocrystals production. 2018. 113 p. Tese (Doutorado em Ciência e Engenharia de Materiais) – Escola de Engenharia de São Carlos, Universidade de São Paulo, 2018. This work investigates the compositional and nanostructural variability of celluloses isolated from plants and the impact of the variability in the production of cellulose nanocrystals. A variable set of cellulose isolated from plants were generated starting with a range of feedstocks (coconut fiber, sisal fiber, eucalyptus sawdust, pine sawdust, sugarcane rind and sugarcane pith), applying a range of cellulose isolation processes (acetossolv, liquid hot water, alkaline, and liquid hot water + alkaline) and adding commercial cellulose (eucalyptus kraft pulp, dissolving pulp, and microcrystalline cellulose) as reference materials. The nanostructural characteristics were evaluated by calorimetric thermoporometry, X-ray diffraction, and moisture sorption isotherms. Composition was evaluated by standard wet chemical analysis and insights on functional groups were obtained by infrared spectroscopy. The cellulose nanocrystals were produced by acid hydrolysis with sulfuric acid and characterized by atomic force microscopy and X-ray diffraction. The measured parameters of the isolated celluloses were spread, showing we could achieve a highly diverse set of substrates. Significant correlations between measured variables across the sample set, indicating possible unforeseen multivariate relations among cellulose features. For example, we could show that cellulose monolayer hydration is determined by both hemicelluloses content (compositional parameter) as well as cellulose crystal width (structural parameter). Cellulose nanocrystals were successfully produced, although in some cases such as for the acetossolv pulps the acid conditions were too aggressive and oxidized the substrates. Finally, some quantitative correlations were seen between the parameters of cellulose substrates and the resulting cellulose nanocrystals. These results supply the first hints about how the nanostructural variability of isolated cellulose can influence the cellulose nanocrystals produced from them.