The incorporation of plant materials is an effective method to improve the stability of chitosan beads, as it further increases the adsorption of toxic dyes and metals from aqueous systems. In the present study, chitosan gels were impregnated with a novel type of powder as the groundnut hull powder in order to form composite beads by using a simple droplet-based microfluidic system. The beads were then characterised through various techniques such as SEM, TGA, FTIR, and XRD. Microscopic imaging revealed a change in the surface morphology of the composite beads, which became rough and wrinkled with more valley-like features and irregular cracks. FTIR data suggest that the impregnation of groundnut hull powder led to an increase in functional groups. The thermal analysis allowed for the assessment of composite bead hydration contents and indicated the presence of groundnut hull entrapped in the loaded beads, which was corroborated by vibrational spectroscopy. XRD analysis allows us to conclude that there is an involvement of groundnut hull in the chitosan gels, and the consequence of that is the formation of amorphous beads, which would make them suitable for the adsorption of toxic dyes and metals from water systems.