A simple, rapid and inexpensive method for separation and pre-concentration of some traces of hazardous elements is presented prior to their flame atomic absorption spectrometric determinations. At pH 9.0±0.1; cadmium(II) and silver(I) were separated simultaneously with 2 - ( Phenyl ) 4 , 5 - Di Phenyl Imidazole ( PDPI) as a new complexing agent and floated after adding sodium dodecyl sulfate (SDS) as a foaming reagent. The floated layer was then eluted by concentrated nitric acid in methanol and introduced to the flame atomic absorption spectrometer (FAAS). These ions can be eluted quantitatively with 0.5 ml 1M HNO3 in methanol. The linear range of the determination is between 0.01-2.2 μg mL-1 for Cd2+and, 0.02-1.9 μg mL-1 for Ag+ with a detection limits for , Cd2+and Ag+ were 1.3 ng mL-1 and 1.4 ng mL-1, respectively. The method has been successfully applied for determination of trace amounts of ions in radiology wastewater, amalgam, natural water and blood samples.