The desorption of heavy metals from the P(St-DVB)/CuNi BNC microsphere was carried out with 0.5 M concentrations of NaOH solution because this concentration of NaOH showed a good desorption efficiency of heavy metal ions in batch desorption experiments. Desorption studies were conducted for up to four successive adsorption–desorption cycles. From the adsorption–desorption data, it was indicated that the removal efficiency (%) decreased with each adsorption–desorption cycle in progress for all investigated metals. Total regeneration was not achieved due to incomplete desorption of metal ions from the adsorbent (Table 7). The removal efficiency decreased from 70 to 56%, 63 to 50%, and 73 to 59%, respectively, for Pb, Cd, and Zn from cycle 1 to cycle 4. This preliminary study suggests that the P(St-DVB)/CuNi BNC microsphere is a potential adsorbent for the removal of heavy metal ions in a fixed-bed column with repeated usage.