In decontamination process to remove radioactive materials of reactor cooling system, the metal ions dissolved by organic acids in decontamination solution are separated by use of ion exchange resin in the column. However, organic acids in decontamination solution decrease the apparent affinity of the resin to metal ions. In light of this, some experiments were carried out on the Amberlite IRN-77 cation resin with cobalt and iron to gain a better understanding of the complexation effects on the ion exchange process. Experimental results showed that EDTA among organic acids used as chemical decontaminants predominantly caused reduction of ion exchange capacity of cobaltous ion to resin since this reagent formed the complex with the cobaltous ion stronger than that with the ferrous ion. In contrast, the effects of oxalic acid and citric acid were found to be negligible. And, single and two-component nonlinear equilibrium relationships of the metal ions were established using experimental data.