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A novel sorbent for simultaneous separation of cadmium and copper was prepared by functionalizing SBA-15 nanoporous silica with diphenylcarbazide. A solid-phase extraction method using the above sorbent has been developed to separate and concentrate trace amount of cadmium and copper ions from environmental samples by flame atomic absorption spectrophotometry measurements. The optimum experimental conditions such as pH, flow rates, type and the smallest amount of eluent for elution of cadmium and copper ions, break through volume and effect of coexisting ions on the separation and determination of cadmium and copper ions were evaluated. The extraction efficiency for cadmium and copper ions were greater than 98% and limit of detection (LOD) was 0.15 and 0.45ngmL⁻¹ for cadmium and copper, respectively. The preconcentration factor was 294 and 291 for cadmium and copper …