Oligomers were obtained from polyester samples by solvent extraction and dissolution methods. Dioxane, chloroform, and chlorobenzene were used for the extraction method, whereas dimethyl formamide and phenol : tetrachloroethane (1 : 1 mixture) were used for the dissolution method. The oligomers were separated and analyzed by a thin-layer chromatographic technique. It was observed that extraction with chloroform and dissolution with phenol : tetrachloroethane gave higher oligomer contents. Also, the values were higher for as-spun fibers. Thin-layer chromatographic analysis showed that in all the cases lower oligomers were obtained with a maximum of the cyclic trimer, whereas the efficiencies of solvents varied for removal of higher oligomers.