An alternative methodology based on the combination of microextraction with flame atomic absorption spectrometry (FAAS) is reported for the determination of Pd2+ in environmental samples. Cetyltrimethyl ammonium bromide (CTAB) was used as a cationic surfactant and a precipitating agent. The method involves the formation of a PdI42- complex with Pd2+ in the presence of iodide and CTAB causes PdI42- to precipitate. The method was performed using 0.01% (w/v) CTAB and 0.1% (w/v) KI in 35 mL 0.1% (v/v) nitric acid for the preconcentration of Pd2+. Under the optimized conditions, the calibration curve was linear between 20 and 170 mu g L-1 with a correlation coefficient of 0.9964. The limit of detection and preconcentration factor were 2.4 mu g L-1 and 35 for Pd2+. The results showed that this solvent-free microextraction is simple and sensitive for the preconcentration and determination of micrograms per liter of Pd2+ in seawater, stream water, and road dust with 94% to 103% spiked recoveries.