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Combinational thin films of antimony sulphoselenide [Sb2(S1_x Sex)3 ] have been synthesized on a good quality glass substrates using newly developed arrested precipitation technique (APT) by us. Sb(III) ions were arrested using aqueous alkaline solution of organic complexing agent. Highly reflecting uniform and tightly adhesive thin films were formed by optimizing various preparative conditions such as concentration, temperature, pH and rate of agitation on to a amorphous glass substrates. For the first time antimony chalcogenide films were analysed using 4' bromo PTPT reagent by spectrophotometric and atomic absorption spectroscopic (AAS) technique. Statistical assessment of the results show the formation of combinatorial thin films of Sb2S3 with Sb2Se3 which confirm the general formula [Sb2(S1_x Sex)3 ]. A band gap of combinatorial phase of [Sb2(S0.5Se0.5)3| 1.65 eV is obtained from electrical and optical studies. From the electrical measurement an activation energy of 0.8 eV is obtained in the temperature range 273-475 K. Optical absorption studies show that transitions are direct and allowed ones.