The treatment of 4-amino-3,5-diphenyl-4H-1,2,4-triazole 3 with various bis-aldehydes resulted in the formation of bis-4-arylidenamino-3,5-diphenyl-4H-1,2,4triazoles (4a-d) derivatives. NaBH 4 reduction of 4-arylidenamino derivatives of 1,2,4-triazoles afforded 4-arylamino-3,5-diphenyl-4H-1,2,4-triazoles (5a-d). The synthesized all new triazole derivatives of the Schiff base and corresponding bis amino compounds 4a,d-5a,d were characterized by IR, 1 H-NMR, 13 C-NMR spectral data. In order to investigate the relative effects of the differences between the structures of the synthesized triazole derivatives on their extractionabilities and-selectivities for different metal cations, constants of oveall extraction (logK ex ) of 1:1 (M:L) complexes, the extractions (logK ex ) for CHCl 3 /H 2 O systems have been determined with ICP-AES spectroscopy at 25 ± 0.1°C. Remarkable complexation properties are found towards some transition metal cations. The stability sequences of the triazole derivatives in CHCl 3 for the metal cations generally found in order: (II). The synthesized all compounds were tested for antimicrobial activity against 11 bacteria.