In this paper, we compared atomic absorption spectroscopy (AAS), anodic stripping voltammetry (ASV), and UV-vis spectroscopy for the determination of the concentration of CdSe nanocrystal (NC) solutions. The experimental results were combined with crystallographic calculations of the NC size, which led to a very accurate determination of the nanocrystal concentration--a crucial parameter for bioanalytical applications. Furthermore, such a combined approach can be extended to the determination of shell thickness of core/shell materials (e.g., CdSe/ZnS).