AbstractNi2+‐imprinted monolithic column was prepared for the removal of nickel ions from aqueous solutions. N‐Methacryloyl‐L‐histidine was used as a complexing monomer for Ni2+ ions in the preparation of the Ni2+‐imprinted monolithic column. The Ni2+‐imprinted poly(hydroxyethyl methacrylate‐N‐methacryloyl‐L‐histidine) (PHEMAH) monolithic column was synthesized by bulk polymerization. The template ion (Ni2+) was removed with a 4‐(2‐pyridylazo) resorcinol (PAR):NH3NH4Cl solution. The water‐uptake ratio of the PHEMAH–Ni2+ monolith increased compared with PHEMAH because of the formation of nickel‐ion cavities in the polymer structure. The adsorption of Ni2+ ions on both the PHEMAH–Ni2+ and PHEMAH monoliths were studied. The maximum adsorption capacity was 0.211 mg/g for the PHEMAH–Ni2+ monolith. Fe3+, Cu2+, and Zn2+ ions were used as competitive species in the selectivity experiments. The PHEMAH–Ni2+ monolithic column was 268.8, 25.5, and 10.4 times more selective than the PHEMAH monolithic column for the Zn2+, Cu2+, and Fe3+ ions, respectively. The PHEMAH–Ni2+ monolithic column could be used repeatedly without a decrease in the Ni2+ adsorption capacity. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010