Matrix absorption effects have been examined with scattered X-rays by using WDXRF system for Fe-Ca and Fe-Ti binary compounds. Fe as analyte and elements which some of them the K absorption edge just below the characteristic K X-ray energies of the analyte (Fe) as matrix have been chosen. Pure and binary with Fe ratio ranging from 10% to 90% samples were prepared with these elements. These samples have been analyzed in WDXRF system. At the end of measurement, the coherent and Compton scattering X-rays data of Rh K alpha X-rays from these samples have been obtained. Matrix absorption effects have been examined by calculating coherent / Compton scattered X-rays intensity ratio.