This paper developed a spectrophotometric determination of micro amounts of Gallium with butylrhodamineB in lead-zinc mineral. Large amounts of interfering ions Zn 2+ ?Pb 2+ ?Al 3+ ?Ca 2+ can be separated by anion exchange resin. High bond ions can be eliminated by using 6 mol/L hydrochloric acid-ascorbic acid.Gallium remained in column can be eluted by 0.5 mol/L hydrochloric acid. In the presence of acidic and Titanium chloride, by means of benzene extracting,determined the ultraviolet-red complex combined GaCl - 4 with butylrhodamineB.The method has been applied to determination of micro amounts of Gallium in lead-zinc mineral satisfactorily.