The various studies of nanoparticles are of great importance because of the wide application of nanotechnology. The shape and structure of the nanoparticles can be determined by transmission electron microscopy (TEM) and their chemistry by electron energy loss spectroscopy. TEM sample preparation is an expensive and difficult procedure, however. Surface sensitive, analytical techniques, such as Auger electron spectroscopy (AES) and x-ray photoelectron spectroscopy (XPS) are well applicable to detect the atoms that make up the nanoparticles, but cannot determine whether particle formation occurred. On the other hand, reflection electron energy loss spectroscopy (REELS) probes the electronic structures of atoms, which are strongly different for the atoms being in solution or in precipitated form. If the particle size is in the nm range, plasmon resonance can be excited in it, which appears as a loss feature in REELS spectrum. Thus, by measuring AES (XPS) spectra parallel with those of REELS, besides the atomic concentrations the presence of the nanoparticles can also be identified. As an example, the appearance of nanoparticles during ion beam induced mixing of C/Si layer will be shown