In immiscible blends of poly(2-ethylhexyl acrylate-co-acrylic acid-co-vinyl acetate) P(2EHA-AA-VAc) with poly(vinylidene fluoride-co-hexafluoroacetone) p(VDF-HFA), depth profiling was carried out by PAS-FTIR and ATR-FTIR analyses. Integrated surface excesses of P(VDF-HFA) component (phi(1)) in blends were plotted against depth for P(2EHA-AA-VAc)/ P(VDF-HFA) (50/50), (30/70), and (10/90) blends. In all blends, since phi(1) decreased with increasing depth, it was expected that P(2EHA-AA-VAc)/P(VDF-HFA) blends would be gradient materials (surface segregation structures). Furthermore, at a few nm depth from the surface, XPS analysis was done to get more detailed information of the surface. We point out that PAS-FTIR is very effective analysis to get depth profiling in such immiscible polymer blends as P(2EHA-AA-VAc)/ P(VDF-HFA).