A flow injection (FI) kinetic spectrofluorimetric method was developed for the determination of palladium and the possible mechanism of catalytic reaction was discussed. Salicylaldehyde furfuralhydrazone (SAFH) was newly synthesized and its ionization, IR and elemental analysis were established. The methodwas based on the fluorescent enhancing reaction of SAFH with potassium bromate, whichwas catalysed by palladium in water medium at pH 7.30 and 30℃. Under these experimental conditions, the oxidized product of SAFH had excitation and emission wavelengths maxima at 370 and 460nm, respectively. The linear range of this method was 1.0-210ng/ml−1 with the R.S.D. of 1.3% from a series of 11 standards each containing 50ng/ml−1 of palladium. The detection limit was 0.30ng/ml−1 of palladium. A high analysis rate of 24 samples h−1 was obtained by the FI method. Sensitivity and selectivity were increased by a Pd2+preconcentration separation methodology. The proposed method was applied successfully to determine palladium in synthetic mixtures and mineral samples, the common interference ions were separated, and the results were agreeable with the standard values.