A convenient organic solvent treatment method was developed for the determination of Cd, Cr, Hg, and Pb in polyethylene and polypropylene matrices by energy dispersive X-ray fluorescence spectrometry. The solvent treatment method had many advantages for the fast, simple, and accurate multi-element analysis of these materials. Calibration curves were prepared using organometallic compounds in xylene in the concentration range of 1-80 mg kg(-1). The prepared samples had a homogeneous elemental distribution and good durability. The trueness for the quantification of mentioned elements were checked by using a polyethylene certified reference material. The apparent recoveries of the elements with certified values were in the range of 0.81 (Hg) to 1.14 (Pb). The precision was normally better than 8% RSD, with the exception of Hg (10%). The method detection limits were found to be 12, 24, 12, and 12 mg kg(-1) for Cd, Cr, Hg, and Pb, respectively. Polyethylene and polypropylene samples were analyzed by both the XRF method and the reference technique for comparative purposes. Application of analysis of variance (ANOVA) showed no differences between the mean results. The proposed method could be also applied to several different xylene soluble plastics.