In the present article, a simple, rapid, selective, sensitive and economical method has been developed for the separation/preconcentration of the trace amounts of Pd(II) in different real samples using alumina coated magnetite nanoparticles modified by sodium dodecyl sulfate and its determination by flame atomic absorption spectrometry after eluting with 1.0 mol L -1 thiourea. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range and relative standard deviation of Pd(II) were 280 (for 700 mL of sample solution), 4.3 ng mL −1 , 6.0 -120.0 ng mL −1 and 4.6% (for 10 ng mL -1 , n=10), respectively.