研究了Ｂｉ（Ⅲ）－Ｐｈ（Ⅱ）与八种变色酸双偶氮型试剂的示波极谱行为。其中五种含多卤素取代基的不对称结构试剂与Ｂｉ（Ⅲ）－Ｐｈ（Ⅱ）生成异核络合物，用单扫示波极谱法得到灵敏的络合吸附波。测定了络合物的组成，研究了电极过程和提出了电极反应机理．用巯基棉吸附和分离，可消除共存离子的于扰，建立了测定痕量铋的方法，用于铜合金和人发的分析，结果满意． The oscillopolarographic behaviors of Bi (Ⅲ) -Ph (Ⅱ) and eight chromotropic acid disazo type reagents were studied. Among them, five asymmetric structural reagents with polyhalogen substituents formed heteronuclear complexes with Bi (Ⅲ) -Ph (Ⅱ), and the sensitive complexed adsorptive waves were obtained by single sweep oscillopolarography. The composition of the complex was measured, the electrode process was studied and the electrode reaction mechanism was proposed. With thiol cotton adsorption and separation, can eliminate interference of coexisting ions, the establishment of a method of determination of trace bismuth for copper alloy and human hair analysis, the results are satisfactory.