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This paper reports the synthesis and analysis of the characterization results of PbS and PbS/ZnO core/shell nanoparticles embedded in Polyvinyl Alcohol (PVA) matrix. The technique adopted in this work is wet chemical synthesis of PVA/PbS and PVA/PbS/ZnO core/shell nanoparticles. In total, two different sets of samples comprising of nine samples have been synthesized by altering parameters like PVA concentration and shell thickness for the PVA/PbS and PVA/PbS/ZnO samples, respectively. Various characterization techniques are used to analyze the influence of alteration of matrix concentration and shell thickness upon the as-synthesized nanoparticles. The techniques include UV-Vis Spectroscopy (UV-vis), Photoluminescence (PL) Spectroscopy, X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Analysis of X-Rays (EDAX) and Transmission Electron Microscopy (TEM). Results of the characterization techniques confirm the formation of nanoparticles of PbS and PbS/ZnO, respectively.