This paper dedicated to the further development of the novel aqua-impregnated-resin (AIR) technique reports the results obtained by studying the column separation of equimolar mixtures of Cu(2+), Al(3+), and Zn(2+) on iminodiacetic (IDA) and polyacrylic (PAR) resins by using 0.2 M heptane solutions of either bis(2-ethylhexyl) phosphoric acid (DEHPA) or bis(2-ethyhexyl) dithiophosphoric acid (DEHDTPA) as selective eluents for extractive desorption of metal ions from the resin phase. The quantitative separation of Cu(2+)-Al(3+) mixtures has been achieved by sequential elution of metals from PAR with DEHDTPA and H(2)SO(4) solutions. Purification of Cu(2+) from Al(3+) and/or Zn(2+) and Al(3+) from Cu(2+) and Zn(2+) is achieved by extractive elution of metal mixtures from IDAR or PAR with DEHPA or DEHDTPA solutions, respectively, followed by stripping of the purified metals with 1.1 M H(2)SO(4). The resulting purity of metals obtained with the yield of >96% exceed 95%.