Polymethyl methacrylate/CaSO4 (PMMA/CaSO4) and Polystyrene/CaSO4 (PS/CaSO4) nanocomposites were synthesized by deposition technique. Chemical structure and morphology of synthesized PMMA/CaSO4 and PS/CaSO4 nanocomposites were investigated using Fourier Transform Infrared (FTIR) and scanning electron microscope (SEM). SEM indicated that nano-CaSO4 particles present in nanosphere and have been homogeneously encapsulated in the PS matrix with irregular size. The FTIR shows characterized peaks in the region where from 400-700cm-1 which shows the probability of existence of bonding between CaSO4 nanoparticles and the polymer network in their respective polymer/CaSO4 nanocomposites. Thermal gravimetric analysis (TGA) shows that both PMMA/ CaSO4 and PS/CaSO4 nanocomposites have higher decomposition temperature in comparison with the purified polystyrene. Electrical conductivity measurement shows that PMMA/ CaSO4 and PS/CaSO4 nanocomposites show semiconducing in nature with conductivity lies between 10-7 to 10-5 S/cm.