In this work, the adsorption behavior at the silver/toluene and alumina/ toluene interface of polystyrene-polyethylene oxide (PS-PEO) diblock copolymers of various molecular weights was investigated by implementation of the surface plasmon resonance (SPR) technique. This was accomplished under a careful choice of experimental setup and the use of a suitable physical model for the interpretation of the experimental data. Comparison between polystyrene homopolymer and PS-PEO diblock copolymer adsorption measurements indicate that PS-PEO is anchored on the alumina surface via the PEO block, while on silver the copolymer is attached by various chain segments. The measured final adsorption amounts on alumina are typical of end-attached polymeric brush formation while the dynamics of the adsorption process present two clearly different evolution regimes. This work provides insight into the many advantages of the use of the SPR technique as a valuable tool for similar surface studies. (c) 2006 Wiley Periodicals, Inc.