This paper examines Wavelengths Dispersive X-Ray Fluorescence (WD-XRF) and Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) as complementary techniques to analyse major and trace elements. A set of Geostandard samples were analyzed and statistical methods were applied to the results. In the second part of this paper, the concentrations of Al, Cr, Fe, Ni, Cu Zn and Pb in sediments of two Moroccan rivers, Oum Er Rbia and Boufekrane, were determined. This study shows that the metal distribution in Oum Rbia sediments is homogeneous throughout the studied area. Whereas in Boufekrane sediments, enrichment was observed downstream (for Al, Cr, Fe, Ni) and inside the city of Meknes (for Cu, Zn and Pb). The Oum Er Rbia river sediments show significantly higher concentrations of Al, Fe, Cr, Ni, Cu and Zn. These higher concentrations can be attributed to the geological features of this river. The Boufekrane river sediments show higher Pb concentrations probably due to the pottery industry activities in the watershed.