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Fe(III)–chitosan microbeads (Fe–CTB) were prepared using a chemical coprecipitation method. SEM–EDX, FTIR, XRD, TGA, BET, and pH _pzc were performed for the characterization of the adsorbent. Various parameters were optimized as pH, adsorption time, adsorbent dose, initial Cr(VI), and PO₄³⁻ ion concentration and the effect of assorted ions for adsorption studies. Fe–CTB microbeads revealed more than 80% detoxification for a 100 mg L⁻¹ initial concentration at pH 3 with 60 min stirring of Cr(VI) and PO₄³⁻ ion having adsorption capacities of 34.15 and 32.27 mg g⁻¹, respectively. The adsorption process for Cr(VI) and PO₄³⁻ ion followed the monolayer adsorption as they favored the Langmuir isotherm model. Kinetic and thermodynamic studies’ emphasis on the adsorption process was spontaneous and exothermic with pseudo-second-order kinetics for both adsorbates. The microbeads were found to be reusable in multiple cycles.