Performance of three chemically modified silica materials for solid phase extraction of polar compounds from aqueous solutions Silica gel (320 m 2 g -1 , 10 nm) was chemically modified with 3-chloropropyltrimethoxysilane or 3-aminopropyltrimethoxysilane, followed by reaction with aniline, 3-phenylchloropropylamine, or benzylamine. The resulting silicas were characterized by elemental analysis and spectroscopic techniques, namely diffuse reflectance spectroscopy (DRS), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and 29 Si variable amplitude cross-polarization magic-angle spin nuclear magnetic resonance (VACP-MAS-NMR). The resulting solids were shown to be stable in aqueous and non-aqueous media and were tested as sorbents for pre-concentration of derivatized phenolic compounds (acetyl derivatives of: phenol, o-cresol, m-cresol, p-cresol, 2-ethylphenol, 3-ethylphenol, and 4-ethylphenol) and some organochlorine pesticides (endrin, pentachlorobenzene, heptachloro epoxide, hexachlorobenzene, and lindane) in aqueous media. Extraction experiments were undertaken using a precleaned cartridge (10 cm610 mm ID) packed with modified silica gel and with commercial C-18 in order to evaluate the influence of the nature of the functional group onretention of the compounds under study. Results showed that silica modified with aniline gave the highest retention for the studied acetylated phenolic compounds. Silica modified with 3-phenylchloropropyl groups exhibited the highest retention for hexachlorobenzene and aldrin, while that modified with benzylamine showed the highest retention for eldrin, pentachlorobenzene, and heptachloro epoxide. Lindane was not retained by any of the tested materials.