Amino derivative of chloromethylated polystyrene resin was synthesized and functionalized by 1,10-phenanthroline (1,10-Phen) to yield a novel adsorbent, namely 4-methylamino-[N,N-bis(2,2 0 )-1,10-phenanthroline] polystyrene (4-MABPPS). The complete development of novel adsorbent along with its characterization is described in detail. The adsorption ability and selectivity of 4-MABPPS were investigated for cobalt and zirconium ions so as to efficiently separate cobalt ion impurities from zircalloy cladding material of nuclear reactors. The experimental results showed selective uptake of cobalt by the adsorbent in the presence of zirconium.