A novel type of adsorbent, TiO₂ impregnated pomegranate peels (PP@TiO₂) was successfully synthesized and its efficacy was investigated based on the removal of As(III) from water. The adsorbent was characterized using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectrometer (EDS), X-ray Diffraction (XRD) analysis, and Fourier Transform Infrared (FTIR) Spectroscopy, to evaluate its morphology, elemental analysis, crystallinity, and functional groups, respectively. Batch experiments were conducted on PP@TiO₂ for As(III) adsorption to assess the adsorption isotherm, effect of pH, and adsorption kinetics. Characterization data suggested that TiO₂ was successfully impregnated on the biomass substrate. The equilibrium data better fitted to the Langmuir isotherm model having a maximum adsorption capacity of 76.92 mg/g and better distribution coefficients (K_D) in the order of ~10³ mL/g. The highest percentage of adsorption was found at neutral pH. The adsorption kinetics followed the pseudo-2nd-order model. X-ray Photoelectron Spectroscopy (XPS) of the adsorption product exhibited that arsenic was present as As(III) and partially oxidized to As(V). PP@TiO₂ can work effectively in the presence of coexisting anions and could be regenerated and reused. Overall, these findings suggested that the as-prepared PP@TiO₂ could provide a better and efficient alternative for the synergistic removal of As(III) from water.