<正> The structures of 2, 6- and 3,4-xylenols together with their iodine redox products Ⅰ-Ⅲwere studied and critically investigated. Characterization of these matrials involves elemental, the-rmogravimetric, differential thermogravimetric and differential thermal analyses. IR and NMRspectrometry were used for the study of structural formulae of the obtained redox products. Theidentification and characterization of these materials confirm the proposed schemes representingredox reactions of xylenols with iodine. It also explained the schemes representing fragmentationof the investigated compounds by thermal analyses. Thin layer chromatography was also used forseparation and identification of redox products obtained in the reaction media.