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Abstract.Polystyrene (PS) nanospheres were synthesized by emulsion polymerization using 2,2′-Azobis (2-methylpropionitrile) (AIBN) as initiator and Sodium dodecyl sulfate (SDS) act as surfactant. The size and distribution of the PS nanospheres were systematically investigated in terms of surfactant concentration. Effect of the surfactant towards to the particle size is study using SEM, FTIR and XRD. It is found that increase in Sodium dodecyl sulfate (SDS) concentration increase the reaction time thus longer time needed for the formation of the nanosphere. However their properties are comparable to the commercial Polystyrene PS nanosphere.