Hydrous ferric oxide (HFO)-impregnated agarose beads were prepared as an adsorbent to reduce As(III) concentration in the pharmaceutical wastewater effluent generated from the manufacturing process of an arsenic-containing chemotherapeutic drug. The adsorbent was prepared by immersing wet agarose beads into FeCl<sub>3</sub> (aq), followed by another immersion into NaOH (aq), resulting in HFO precipitation directly within the agarose beads. The As(III) adsorption rate of HFO-impregnated agarose beads was determined to be external diffusion-limited, and having a Langmuir maximum adsorption capacity of 76.1 mg As(III)/g. Passing 6 L of the pharmaceutical wastewater through a packed column filled with the adsorbent in an upflow mode of 50 mL/min repeatedly for five times resulted in the reduction of As(III) concentration from 250 to 10 μg of As(III)/L of H<sub>2</sub>O. Column desorption was performed by passing 0.6 L of 0.1 M NaOH (aq) through the column in an upflow mode of 50 mL/min repeatedly for five times to regenerate the As(III)-adsorbed HFO-impregnated agarose beads. Chemical characterizations revealed that the As(III) species were adsorbed on HFO by the “inner-sphere” bidentate complexation via ligand exchange or “outer-sphere” association via electrostatic interaction, while the “outer-sphere”-associated As(III) species were most likely desorbed.