Amberlite XAD-2, a polystyrene-divinylbenzene copolymer, and XAD-7, a methacrylate type copolymer, were evaluated as stationary phases in TLC. Several different binders and plate preparation procedures were evaluated. Rf data were collected for aniline and phenol derivatives, for ampholytes such as ami no acids, dipeptides, and sulfas, and for nonelectrolytes such as benzaldehyde and acetophenone derivatives. Eluting conditions examined included effect of pH (for the acids and bases), effect of solvent composition, and type of organic solvent in the eluting mixture. The influence of the structure of the model compounds and of the stationary phase on retention was considered. The XAD copolymers acted as reversed stationary phases, and retention on the XAD thin layer corresponded to retention data observed in HPLC studies employing XAD copolymer columns. Numerous separations were possible on the XAD thin layers.