In ammonium sulfate-carboxy-2'-hydroxy-5'-sulfoformazylbenzene-Tween-80 system, the liquid-solid extration behaviour of the Cu(II), Co(II), NL(II), Zn(II), Cd(II) and Mn(II) was investigated. The results indicated that complexes of Cu(II), Co(II), Ni(II) with zincon were almost completely extracted in buffer solution (pH 6 similar to 9) by Tween-80 phase while Zn(II), Cd(II), Mn(II) were not. Quantitative separation and determination of Cu(II), Co(II), Ni(II) from mixed ions of Zn(II), Cd(II), Mn(II) in different pH buffer solutions were realized respectively.