Many direct methods cannot easily be used to measure analytes such as Cd(II), Cu(II), Ni(II), Pb(II), and Zn(II) ions in sea and river water since these elements are present at very low concentration and the sample has a very complex matrix. In this study a method was developed to preconcentrate these ions by solid phase extraction within a column system using a newly synthesised 2,3-dihydroxy benzaldehyde modified silica gel (SGDHB). Different parameters, such as pH, resin amount, eluent type, eluent volume, sample flow rate, preconcentration factors, and resin capacity were determined for the preconcentration of metal ions with the resin. Samples (125-500 ml) containing metal ions were passed through the column filled with SGDHB resin so that metal ions were retained on the column. The preconcentrated analytes were then eluted with 15 mL of 0.1 M HCl. The metal concentrations in the eluate were measured by FAAS. A sample and eluent flow rate of 1.12 and 0.56 ml/min respectively was used. Estimates of accuracy, precision, and detection limits were determined. In addition, analysis of the CRM LGC 6156 harbor sediment was undertaken, using the resin to isolate the analytes from potential interferences. Good agreement with certified values was obtained, indicating that the method is equally applicable to the analysis of water samples and to digests of solid materials.