Applications of synchrotron radiation X-ray fluorescence (SR-XRF) microscopy combined with scanning electron microscopy (SEM) are reported. Electron beam excited and synchrotron radiation induced X-ray emission spectra of the same yellow sand single particles are reported and compared. The Ti-K edge absorption fine structure of single microparticles of TiO2 (rutile, anatase, and a photocatalyst aerosol) are recorded by using monochromatic synchrotron radiation of tunable energy. It is shown that the discrimination between rutile and anatase is possible. Based on the single particle speciation, the toxicity of photocatalyst aerosol powder is discussed. (c) 2007 Elsevier B.V. All rights reserved.