In this study, chitosan nanoparticles (NC) were synthesized using two different acidic routes acetic acid (AA) and methacrylic acid (MA) employed as solubilizing agents and pH controllers. The resulting NC were characterized by dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), atomic force microscopy (AFM), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FTIR) to evaluate the influence of acid type on nanoparticle formation, morphology, and colloidal stability. The AA route produced nanoparticles with an average hydrodynamic diameter of 166 ± 4 nm and zeta potential of 21 ± 1 mV, whereas MA-derived NC exhibited a core–shell-like morphology, larger particle size 178 ± 3 nm, and enhanced electrostatic stability. Accelerated stability assays, including temperature variation, UV-C irradiation, and long-term storage, demonstrated superior stability for MA-based NC over 90 days. Adsorption-desorption experiments using methylene blue, monitored by UV–Vis spectroscopy, revealed NC derived from MA a maximum adsorption capacity of 65 % (3.25 mg/L) of the dye in relation to the initial concentration (5 mg/L), with a regeneration efficiency of 81 % (2.63 mg/L), indicating the potential for reuse of NCMA. Overall, the results demonstrate that acid-controlled synthesis plays a key role in governing the physicochemical properties and interfacial electrostatic interactions of chitosan nanoparticles, directly impacting their adsorption performance and regeneration behavior. These findings highlight the potential of chitosan nanoparticles as efficient, stable, and regenerable nanoadsorbents for water treatment applications.
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