An XRF method was developed for the determination of Mg and Si in aluminium alloys in the range from 0.1 to 0.7 wt%, using a Si(Li) semiconductor detector, a 3H/Ti ring‐shaped radioactive source and a microcomputer. The Mg Kα and Al Kα lines were separated both with the help of library spectra (deconvolution) and with an Se absorption edge filter. The optimum values of the geometrical parameters were determined. Two 3H/Ti sources, covered and not covered with Cr, were tested. The standard deviations of concentrations determined by different methods was compared.
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