Abstract: An ion exchange separation, recovery and regeneration process for the control of iron is disclosed that can replace the conventional bleed stream process used in copper electrowinning. The disclosed process minimizes the loss of cobalt from the electrowinning circuit and can effect a lowering of the total iron concentration in the electrolyte circuit with an associated increase in current efficiency. The process captures the iron as iron(III) on an ion exchange medium containing a plurality of --CH(PO.sub.3 R.sub.2).sub.2 or --C(PO.sub.3 R.sub.2).sub.2 -- groups through which the divalvent metal ions pass. The iron(III) is then reduced with copper(I) to form iron(II) that is freed from the exchange medium, thereby permitting regeneration of the medium.