The chromatographic properties of silica gels treated with hydroxides of lithium (Li), sodium (Na), potassium (K), and cesium (Cs) were compared for selected acidic compounds. Alkali metal hydroxide treated silica gels (AMSG) were evaluated for their ability to retain, separate, and enrich trace residues of acidic compounds. AMSG adsorbents interact with acidic organic compounds, retaining those with pKa <12 from moderately polar solvents. Compounds of widely varying acidities, including sulfa drugs, were applied to 1.0 cm i.d. × 8.5 cm AMSG columns in methylene chloride/cyclohexane 1:1 (v/v) and either eluted with this solvent or a gradient of 0 to 50% methanol mixed with this solvent. When this gradient was used, elution volumes of the solutes (relative to phenol) were determined for each AMSG and for silica gel treated with tetramethyl ammonium hydroxide. A sterically hindered phenol, 2,6-ditertlarybutyl-4-methylphenol (BHT), did not Interact with any AMSG, suggesting that a steric requirement existed for surface interaction. Strongly acidic compounds were recovered as their corresponding salts. Retention of acidic compounds increased with increasing ionic radius of the alkali metal. Of the AMSGs, CS-silicate most effectively retained the weakly acidic phenols. After extraction of water samples, short Cs-silicate columns, 1.0 cm i.d. × 2.0 cm, successfully replaced liquid-liquid partitioning used in the analysis of Environmental Protection Agency Consent Decree phenols.