Abstract: The electrochemical behaviour and the current property of antimony based on the formation of ion-associate complexes of Sb(Ⅲ) with iodide and rhodamine basic dyes are investigated in HAc-NaAc buffer solution (pH 5.6).The mechanism of related reactions is discussed.A new simple,sensitive and selective oscillopolarographic method is established for the determination of trace antimony. The detection limit was 0.33 ng/ml.