The spectroscopy of the adsorbed silane coupling agent on micro-sized silica particles was observed by H-1 solid state NMR (SSNMR) under fast magic angle spinning (MAS). We found that this is a fast and effective way to characterize the structure and dynamics of the thin layer of coupling agent on the surface of micro-sized silica. Compared with conventional Si-29 NMR spectroscopy and other methods, the present proton solid state NMR is a promising method to characterize the adsorbed layer on micro-sized silica. (C) 2008 Elsevier B. V. All rights reserved.