A method to prepare monodisperse and simultaneously NMR-visible and fluorescent colloidal particles is described, and a systematic approach to obtain spectrally resolved diffusion coefficient for every component in a monodisperse colloidal suspension is presented. We also prepared bidisperse colloidal suspensions, where each colloid component has a distinct NMR spectral signature, and obtained the diffusion coefficients of both colloid species Simultaneously in concentrated colloidal Suspensions, with volume fractions between 20 and 50%. The colloidal model system developed in this work enables the study of colloidal phase behavior in binary mixtures for different number and size ratios.