The distribution of five metal ions (Mm+) including Fe(III), Co(II), Ni(II), Cu(II), and Zn(II) between dilute sulfate solutions and macrporous resins containing di(2-ethylhexyl)phosphoric acid (D2EHPA, HR) was investigated. Experiments were carried out as a function of aqueous pH, D2EHPA concentration in the resin phase, and temperature. The equilibrium data were numerically analyzed. It was shown that the sorption reaction could be described by assuming the formation of metal complexes with a general composition MRm(HRn) in the resin phase. For several systems a change of complex stoichiometry with temperature was observed and discussed. The apparent thermodynamic data for the formation of these complexes were also calculated.