We performed particle size and particle size distribution measurements for L-cysteine-stabilized ZnS/Mn nanoparticles in the size region below 10 nm. For this we applied transmission electron microscopy (TEM), analytical ultracentrifugation (AUC), dynamic light scattering (DLS), and asymmetric ﬂow ﬁeld ﬂow fractionation (aF-FFF) measurements, and we calculated particle sizes with the help of X-ray diffraction (XRD) patterns and the shift of the band gap absorption in the UV-vis spectrum. The different methods are explained, and their limitations are discussed, with the conclusion that only a combination of different techniques can yield a realistic and complete picture about the size distribution of the sample. From these methods TEM, AUC, DLS, and aF-FFF measure the actual particle size distribution either in dispersion or after drying of the sample, whereas the particle size obtained from XRD patterns and with the help of the band gap widening corresponds to the average size of the crystal domains within the particles. We obtained particle size distributions with their maximum between 3 and 7 nm and a mean crystallite size of 3.5-4 nm.