A new dispersive liquid-liquid microextraction (DLLME) preconcentration method was developed for the determination of palladium. In the proposed approach, 2,2'-furyldioxime was used as chelating agent, while chloroform and methanol were used as extraction and dispersive solvents, respectively. Several factors that influence the microextraction efficiency, such as type and amount of extraction and dispersive solvents, acidity of sample solution, concentration of the chelating agent, and centrifugation time were investigated and the optimized microextraction conditions were established. Under the optimum conditions, the preconcentration factor of this method for palladium was reached at 250. The limit of detection for palladium was 0.04 mu g L-1 (3 s), and the relative standard deviation (RSD) was 1.1% (n = 8) at 4 mu g L-1 level. The accuracy of the method was performed by analysis of the certified standard reference material (CDN-PGMS-10). The developed method was applied successfully to the determination of palladium in the catalytic converter, anode slime, road sediment and water samples.