Abstract: The flotation separation behavior of Pd(Ⅱ) with potassium bromide-tetrabutyl ammonium bromide system and the conditions for the separation of Pd(Ⅱ) from other metal ions were studied.The results showed that Pd(Ⅱ) could be quantiatively separated from Ir(Ⅳ)、Pt(Ⅳ)、Ru(Ⅲ)、 Rh(Ⅲ) and Ga(Ⅲ) by flotation when the concentrations of potassium bromide and tetrabutylammonium bromide in solution were 1.5×10-2 mol/L and 2.0×10-3 mol/L,pH=2.0,respectively.The method has been used for the separation and determination of Pd(Ⅱ) in the sample of synthetic water with satisfactory results.