The surface composition and near-surface depth profiles of annealed films of poly(amide urethane) block copolymers were measured using angle-dependent electron spectroscopy for chemical analysis (ESCA). Segregation of the fluorinated polyamide soft segment to the surface was detected and quantified. The poly(amide urethane)s were made from amine-terminated polyamides with N-alkylated fluorinated side chains as well as fluorinated backbones, methylenebis(cyclohexandiyl diisocyanate) (H-12-MDI), and butanediol.(1) The resulting copolymers display extremely low surface energy. A deconvolution program was utilized to obtain composition-depth profiles and to confirm phase segregation.