A new, simple, and rapid method was developed for selective extraction and determination of trace levels of
Pd(II) by dispersive liquid‐liquid microextraction (DLLME) preconcentration and flame atomic absorption spectrometry
detection. In the developed method, 2-mercaptobenzimidazole (MBI) was used as a Pd(II) complexing
agent. Chloroformand acetonewere selected as the extraction and dispersive solvents, respectively. The effective
DLLME parameters such as pH, kinds of extraction and dispersive solvents and their volumes, concentration of
the complexing agent, and extraction time were studied and optimized. Under the optimum experimental conditions,
the calibration graph was linear over the range of 15‐1100 μg L−1 with a detection limit (3σ) of 8 μg L−1
for palladium(II). The relative standard deviations (RSDs, n=6) were lower than 4.8%. The enhancement factor
was obtained to be 20.7. This environmentally‐friendly method was successfully applied to the determination of
trace levels of palladium(II) in soil, food, and spikedwaterfall and tapwater samples. The accuracy the developed
method was also evaluated by the analysis of the certified reference material GPP-10.