Soil and sediment reference materials were used to calibrate and evaluate an analytical method for the determination of major (Si, Al, Fe, Mg, Ca, Na, K, Mn, P, Ti) and trace elements (As, Ba, Cd, Co, Cr, Cu, Ga, Mo, Mb, Ni, Pb, Rb, S, Sb, Sn, Sr, Th, U, V, Y, Zn, Zr) by sequential wavelength X-ray fluorescence spectrometry. Samples were prepared as pressed pellets and analysis was done with a total measuring time of thirty minutes per sample. Special attention was given to the selection of the thirty reference materials used for calibration of the spectrometer. Another set of eleven RM (reference materials) was analyzed for the evaluation of accuracy. Detection limits for trace elements (1-2 mg kg-1) are adequate both for geochemical and environmental purposes, except for Cd and Sb. Accuracy for trace elements falls within the expected interval of certified or recommended values in most cases, but for some major elements, like SiO2, some results showed discrepancies, evidencing difficulties associated with the determination of light elements in complex matrices. But when quality criteria proposed by mapping programs are applied to the results, their requirements are fulfilled. 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