Synthesis of cadmium sulphide nanoparticles has been carried out in aqueous solution precipitation. Starch added during the synthesis of the nanoparticles resulted in cadmium-rich nanoparticles forming a stable complex with starch. The morphology and crystalline structure of such structures were measured by high-resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD), respectively. The grain size of the nanoparticles determined by these techniques was of the order of 5 nm, which correlates well with measurements performed by Raman scattering and photoacoustic spectroscopy. (c) 2007 Elsevier B.V. All rights reserved.