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The interaction of bilirubin (BR) with europium ions was studied at mercury electrode by cyclic voltammetric and chronocoulometric methods in Tris buffer solution (pH 8.0). Bilirubin was strongly adsorbed at the mercury electrode with a two-electron irreversible reduction peak at about À1.30 V (vs. AgaAgCl). After adding europium ions into the bilirubin solution, the reduction peak current of BR decreased proportionally to the concentration of the europium ions. A complex such as Eu 3 -BR which could not be reduced before À1.5 V (vs. AgaAgCl) would be formed. With the help of IR and UV-visible spectral experiments, the structural formula of the complex has been proposed.