The anodic oxidation of reductant H2PO2- related to electroless nickel plating was studied at various pH, reductant concentrations, temperatures, and additives using electrochemical methods. The oxidation rate of H2PO2- decreases with the decrease in pH and, when pH is in the range of 4-6, the oxidation rate can be increased by adding malic acid. Malic acid decreases the reaction order of H2PO2- from 0.54 to 0.19. The existence of free Ni2+ in the solution decreases the H2PO2- oxidation rate because insoluble materials are formed between free Ni2+ and HPO32+ coming from the oxidation product of H2PO2-. The detrimental effect of free Ni2+ can be eliminated by the addition of malic acid through the complex reaction between free Ni2+ and malic acid. Experimental results are better explained by the electroless reaction presented by Van Der Meerakker.