Abstract: Samples of aluminum or aluminum alloys in shapes of rods,lumps and pieces,were machined with lathe,saw or file to make a smooth surface suitable for XRFS analysis.In case of samples of filings,it was first pressed into the form of pieces by hydraulic press and then machined as required.Nine elements (i.e.Fe,Si,Cu,Ga,Mg,Mn,Zn,Ti,and Cr) were determined by the proposed method.In determination magnesium,which is not very sensitive in XRFS,a set of standard samples should be used for each determination,and the content should be calculated by peak values,so as to guarantee for accuracy.For samples having simple matrix components or having definite specification,contents of trace elements should be calculated by peak values without deduction of background values,in order to eliminate the error of background measurements.Results obtained by this method checked very well with those obtained by AES method.Values of RSD′s (n=7) for all the 9 elements were found to be less than 3%.