Aerogels have been studied as potential insulating and conducting materials, but little research has been conducted characterizing organic molecules in aerogel matrices using surface-enhanced Raman spectroscopy (SERS). In this study, SiO2-Ag colloid aerogels were used as enhanced surfaces for SERS. SERS spectra of 4-mercaptobenzoic acid (4-MCBA) adsorbed to acid- and base-catalyzed SiO2-Ag colloid aerogels were obtained. It was observed that acid-catalyzed silver sol gels with 4-MCBA mixed within the matrix provided SERS spectra with sharper and more enhanced peaks than the base-catalyzed silver sol gels