In this work, we report that the adsorption and aggregation processes of Au nanoparticles on a polymer surface can be monitored by means Of surface-enhanced Raman scattering (SERS) spectroscopy. Specifically, we were able to analyze the adsorption process of citrate-stabilized Au nanoparticles onto a film of poly(4-vinylpyridine) (P4VP) by taking a series of SERS spectra, during the self-assembly of Au nanoparticles onto the polymer film. in order to better analyze the SERS spectra, we separately conducted quartz crystal microbalance (QCM), UV/vis spectroscopy, and atomic force microscope (AFM) measurements. The adsorption kinetics revealed by QCM under the in situ conditions was in fair agreement with that determined by the ex situ AFM measurement. The number of Au nanoparticles adsorbed oil P4VP increased almost linearly with time: 265 Au nanoparticles per 1 mu m(2) were adsorbed on the P4VP film after 6 h of immersion. The SERS signal measured in the ex situ condition showed a More rapid increase than that of QCM; however, its increasing pattern was quite similar to that of UV/vis absorbance at longer wavelengths, Suggesting that Au nanoparticles actually became agglornerated on P4VP, (C) 2009 Elsevier Inc. All rights reserved.