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The present paper describes the synthesis of four azo-Schiff base named (1a-4a) by diazotization reaction of the synthesized Schiff bases with sulfonamide compound. All new synthesized derivatives were identified by melting points, CHNS, FT-IR and 1H-NMR spectra. All compounds were tested for their antibacterial activity that showed good activity. The synthesized compounds were used as sensitive and selective analytical reagent for the spectrophotometric determination of cadmium (II). The calibration curve is linear between 0.05 and 30 μ g.ml-1 and limit of quantification, LOQ of (1.203, 1.078, 1.443 and 0.875) μ g.ml-1 with molar absorptivity and Sandal's sensitivity values of ligands 2.4778x104, 1.6740x104, 1.70019x104, 1.9002 x104 L mol-1 cm-1 (0.049x10-4, 0.169x10-4, 0.132x10-4, 0.110 x10-4 μ g.cm-2, for 1a, 2a, 3a and 4a, respectively. The composition of the Cd (II) - (1a, 2a, 3a and 4a) complex is established as 1:2 by molar ratio and job methods. An excellent linearity with a correlation coefficient value of (0.9997, 0.9996, 0.9974 and 0.9985) is obtained for the complexes. [ABSTRACT FROM AUTHOR]