Background and Objectives: It is well known, that uncritical use of the dynamic light scattering (DLS) method may give unacceptable results for the volume or number distributions of particles as compared with transmission electron microscopy (TEM) data. The purpose of this study is to investigate application of the DLS method for determining the size of colloidal silica and gold nanoparticles and to compare results of three methods: DLS, TEM, and absorption spectroscopy (see next paper).