In this study, the phase-separation phenomenon of non-ionic surfactants was used for separation and preconcentration of Pd(II). The cloud point extraction (CPE) method is based on the formation of PdI2 which is then entrapped in the non-ionic surfactant Triton X-114. Ethanol acidified with 0.5 M HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry. The main factors affecting CPE efficiency, such as sample solution pH, concentration of iodide ion and Triton X-114, equilibration temperature and time, were all investigated and optimized. At optimum conditions, a calibration curve was constructed for the determination of palladium according to the ligandless CPE procedure. Linearity was maintained between 1.0 to 500.0 ng/mL. The LOD based on three times the SD of the blank divided by the slope of analytical curve, (3Sb/m) was 0.3 ng/mL. Seven replicate determinations of a solution containing of 4.0 μg palladium gave a mean absorbance of 0.359 with RSD±1.85%. The high efficiency of CPE to carry out the determination of palladium in complex matrixes was demonstrated. The proposed method has been applied to the determination of trace amounts of palladium in a platinum-iridium alloy, water, and dust samples, with satisfactory results.