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This work deals with the characterization of ZnS NanoParticles (NP), prepared by precipitation employing thioacetamide as sulfur source at different reaction time length. The attention is focused on the modification induced on structural, surface and electronic properties of ZnS NP by post-synthesis treatments. These were aimed at removing from the samples surface adsorbed reactants, by washing or thermal treatments, both in air or vacuum. The effect of these parameters is followed by X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Fourier Transform InfraRed (FTIR), gas-volumetric and ThermoGravimetric Analysis (TGA). Moreover, the effect of nanostructuration on the semiconducting material band gap is evaluated by Diffuse Reflectance UV-Vis (DR UV-Vis) spectroscopy. Density Functional Theory (DFT) calculations have been employed to clarify the role of the adsorbed reactants on the surface stability and to assess the relationship between particle size and band gap value.