<p>In this work, the aryldiazonium salts radical addition method has been used successfully to anchor 8-hydroxyquinoline (8-HQ) moieties onto the surface of Amberlite XAD-4 beads. The nitroaniline aryldiazonium salt was generated (in-situ) and covalently grafted onto Amberlite XAD-4 by aid of hypophosphorous acid as a catalyst to facilitate the anchorage of 8-HQ chelator making use of the conventional diazo coupling. The successfulness of the synthesized chelating resin was confirmed by (ATR-IR), (TGA) and (XPS). The risen was packed into cartridges and used with standard solid phase extraction (SPE) apparatus for the extraction of trace metals; Co (II), Ni (II) and Cu (II) from groundwater samples prior to their measurement by (ICP-MS). The resin exhibited more than 90% enhancement in capacity exchange relative to the plain Amberlite XAD-4. Under the optimum conditions the sorption capacity of the sorbent was 0.366, 0.265 and 0.328 (mM/g) for Co (II), Ni (II) and Cu (II) respectively. The sorbent showed efficient performance when applied for SPE of trace metals from groundwater real samples from AlMadinah AlMumnawarah, Saudi Arabia.</p>