Controlled-pore silica glass modified with N-propylsalicylaldimine (SCPSG) has been investigated as a surface-active matrix for the separation of some metal ions. The porous silica glass base was confirmed to have better stability towards hydrolysis in aqueous solution buffered at pH = 9 in comparison to silica gel, which showed twice the surface area of controlled-pore silica glass. The different analytical parameters affecting the batch mode separation and preconcentration of trace Al(III), Ag(I) and Hg(II) in environmental samples using SCPSG, prior to their determination using inductively coupled plasma mass spectrometry (ICP-MS), were studied. The optimum conditions are pH 9.0 ± 0.1, time of stirring 30 min and the eluent concentration 0.5 mol dm -3 HNO3. The ion-exchange capacity of SCPSG with respect to Al(III), Ag(I) and Hg(II) was 0.27, 0.18 and 0.23 mmol g -1 , respectively. The recovery values for the metal ions were 96.8 ± 0.86, 98.1 ± 0.60 and 96.2 ± 1.06%, and the analytical detection limits were 26.1, 1.49 and 0.44 pg cm -3 , respectively, for a preconcentration factor of 100. The method has been applied to the determination of the investigated metal ions in natural water samples as well as certified and reported samples and the results were found to be accurate.