The 2,4-Dihydroxy cinnamaldehyde thiosemicarbazide has been synthesized. Complex of 2,4-dihydroxy cinnamaldehyde thiosemicarbazide with transition metals, Vanadium (v) has been synthesized in methanol medium. The formation of the complex are endothermic processes. The ligand was characterized by melting point, elemental analysis, absorption spectra and antimicrobial activity while the complex was chara cterized by melting point, absorption spectra, A simple and sensitive spectrophotometric method was developed for transition metal complex of 2,4-dihydroxy cinnamaldehyde thiosemicarbazide. The optimum condition for complete colour development have been established. The stability constant, dissociation constant & change in free energy of vanadium (v) has been determined by Job's variation & mole ratio method indicate that the M:L is 2:1 . Tolerance limit of diverse ions in the determination of vanadium (v) with is investigated. Antimicrbial activity and antifungal activity have been studied.