This paper reports on preconcentration and separation of trace Pd(II) and Pt(IV) with silica gel bonded by aminopropyl-benzoylazo-1-(2-pyridylazo)-2-naphthol (ABPN . SG). ABPN . SG is stable in solution between 6 mol/liter HCl and pH 9.0. The maximum adsorptive capacity of Pd(II) on ABPN . SG is 96 mu mol/g. After preconcentration and separation using an ABPN . SG column, Pd(II) and Pt(IV) of ppb level in artificial water samples can be measured by spectrophotometry. (C) 1995 Academic Press, Inc.