Abstract.A mineralization method HCl-free for heavy metals analysis in sediments and soils by DRC-ICP-MS was developed. The procedure, which uses concentrated nitric, hydrofluoric acid and hydrogen peroxide, was applied for the analysis of arsenic, cadmium, chromium, nickel and vanadium. The same samples were then analyzed, as pressed pellets, by wavelength dispersive X ray fluorescence (WD-XRF) using the dedicated PANalytical Pro Trace solution for the determination of trace elements. Comparison of ICP and XRF data showed good agreement for the elements under investigation, unless for chromium in soils, which recovery was not complete.