Untreated (CS) and ozone-treated (OCS) cotton stalks sere studied to determine the effects of ozonation on the content of water-soluble phenolics, on the chemical features of cell wall (CW) matrix complexes (MC), and on in situ structural and chemical properties as reflected in solid-state cross-polarization/ magic angle spinning (CP/MAS) 13 C NMR spectroscopy. The concentrations of water-soluble total monomeric phenolics sere 20.1 and 48.2 mg/100 g of dry matter in the CS and OCS materials, respectively