It is studied the uptake of Zn(II) and Cu(II) from acid aqueous solutions using microcapsules containing 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester, a non-specific extractant, as an alternative method for metals separation in place of current techniques as ion-exchange solid resins or solvent extraction. The microcapsules employed in this study were prepared by an in situ radical polimerization method. The amount of extractant held within each microcapsule was determined by potentiometric titration. Many experimental tests were carried out to measure the hydrometallurgical capacity of the microcapsules to remove these metallic ions from the aqueous solutions.