Abastract: Simultaneous extraction and preconcentration of Pd(II) and Pt(II) from alkaline cyanide solution using hexadecylpyridinium bromide (HPB) as extractant were investigated. The factors affecting extraction and preconcentration efficiency, including diluent type, concentration of hexadecylpyridinium bromide, content of modifier, phase ratio (O/A), contact time of aqueous and organic phase, concentrations of Pd(II) and Pt(II) and pH value of solution, were studied. The results indicate that, at concentration of hexadecylpyridinium bromide (HPB) 0.05 mol/L, content of n-octyl alcohol 30% (volume fraction), phase ratio (O/A)=1:5, pH values 10.5 contact time of 5 min, Pd(II) ( © 2016, Science Press. All right reserved.