Monodisperse core-shell latices were synthesized, differing in the acrylic acid (AA) content in the particle shell (1 or 4 wt%) and the T-g of the acrylic core (around -40 or 10degreesC). In a first step, the drying mechanisms of the dialyzed latices were studied by confocal Raman spectroscopy. It was shown that, besides some unexpected features (briefly described in the article), drying occurred in a rather classical way, i.e., simultaneously from top to bottom and from edge to center. Then, the distributions of sulfate ion (SO4) (from sodium sulfate) and sodium dodecyl sulfate (SDS) in the dry latex films were established by confocal Raman spectroscopy and attenuated total reflectance (ATR). The two techniques were complementary. SO4 and SDS distributions were quite different, although presenting some common characteristics. In both cases, repartition of the low-molecular-weight species in the film was even less homogeneous when the AA content was lower and the particle core softer. However, SO4 showed enrichment at the film-substrate interface and depletion at the air side, whereas SDS showed concentration maxima at both interfaces. Interpretations stress the importance of desorption from the particle-water interface, transport by water. size effects. and diffusion. (C) 2003 Elsevier Science (USA). All rights reserved.