Zn(II), Cd(II), and Hg(II) complexes of N-alkyl-N-phenyl dithiocarbamates were used as single-source precursors to synthesized ZnS, CdS, and HgS nanoparticles. The nanoparticles were characterized by XRD, SEM, TEM, UV-Vis, and photoluminescence spectroscopy. SEM images revealed that the morphology of the nanoparticles shift toward a ball-like shape with increase in the alkyl chain. The absorption and emission spectroscopy show quantum confinement effect. Application of EMA to the absorption spectra show an average particle size of 4.21 for ZnS1, 4.40 for ZnS2, 6.6 for CdS1, and 5.2 nm for CdS, respectively.