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Hydrogen peroxide combined with acid treatment demonstrates its respective characteristics for the separation of lignocellulosic biomass. Herein, holocellulose was extracted from Cattail leaves (CL) by a two-step treatment with alkali and hydrogen peroxide-acetic acid (HPAA). Then carboxylated nanocellulose was hydrolyzed with a mixed organic/inorganic acid. The chemical composition of the holocellulose and the physicochemical properties of the separated carboxylated nanocellulose were comparable. Carboxyl groups were introduced on the nanocellulose as a result of the esterification process with citric acid (CA), which endows the nanocellulose with high thermal stability (315-318 °C) and good light transmission (>80 %). Furthermore, morphological analyses revealed that nanocellulose had a spider-web-like structure with diameter between 5 and 20 nm., Competing Interests: Declaration of competing interest We declare that we have no financial and personal relationships with other people or organizations that can inappropriately influence our work, there is no professional or other personal interest of any nature or kind in any product, service and/or company that could be construed as influencing the position presented in, or the review of the manuscript entitled., (Copyright © 2023 Elsevier B.V. All rights reserved.)