In this paper an experimental study has been made of correlation between optical, morphological and electrophysical properties for CdS-gelatin nanocomposites prepared by Successive Ionic Layer Adsorption and Reaction (SILAR) method, using UV-Visible spectroscopy, scanning electron microscopy (SEM) and Hall measurement techniques. The analyses of results show that direct band gap for prepared CdS-gelatin nanocomposites, is found to decrease with increasing cycles of SILAR. The variation in band gap is due to the size effect and carriers confinement in CdS semiconductor nanoparticles. Here, a correlation has been established between the band broadening and the increase in conductivity due to the increase in carrier density. It was found that electrophysical parameters depend on the size of the formed particles. The variation in conductivity values dependent on the number of cycles is associated with the redistribution of nanoparticles over the cross section of the polymer matrix. For relatively big particles with large grains, prepared at large numbers of SILAR, the mobility and conductivity of the carriers are increased and the special resistivity is decreased.