A simple, rapid and selective method has been developed for the extractive spectrophotometric determination of palladium(II) using 4-(4'-fluorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole, (FBIMMT). In hydrochloric acid medium palladium(II) instantly forms stable yellow colored 1:1 complex with FBIMMT at room temperature, which was well extracted in chloroform. The extracted palladium(II)-FBIMMT species showed absorption maximum at 390 nm against reagent blank. The molar absorptivity

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... nd Sandell's sensitivity of palladium(II)-FBIMMT in chloroform were found to be 5.404 × 10 3 L mol -1 cm -1 and 0.0196 µg cm -2 respectively. The Beer's law was obeyed up to 17.5 µg mL -1 of palladium(II). The optimal concentration range for maximum precision was evaluated from Ringbom's plot and was found to be 5 to 17.5 µg mL -1 . To establish the optimum extraction conditions; various experimental parameters such as acidity, reagent concentration, solvents, shaking time, interference of cations and anions have been studied. To determine accuracy and precision of proposed method, determinations were carried out at five identical aliquots. The selectivity of the method was enhanced by the use of masking agents. The stoichiometry of the extracted species was assessed by Job's method, mole ratio method and verified by log-log plot. The present method was successfully applied for the separation and determination of palladium(II) from binary mixtures, multi component synthetic mixtures, synthetic mixtures corresponding to alloys and catalyst.