The present invention provides for Troika acids attached to a macroporous resin and Methods of preparing the same, including direct attachment of a Troika acid, and attachment of a Troika acid precursor followed by generation of the Troika acid in situ. Methods of functionalizing a resin to facilitate attachment are also described. Multiple Troika acids, comprising a pair of Troika acids joined together are described. Synthetic routes to both microporous and macroporous resins modified by introduction of a suitable Troika-type acid have been designed and validated. In a preferred embodiment, a macroporous Troika resin removes Cu.sup.2+ and Ni.sup.2+ from aqueous solution with high affinity, and is selective against Mg.sup.2+ or Ca.sup.2+. The materials of the present invention have advantages for metal removal from power plant waste water.