A new technique for the analysis of binary alloys by means of X-ray fluorescence is described, as applied to the system tin-lead. Surface determination is avoided making use of intensities ratio of intervening elements. This allows the direct analysis of turnings. The technique is compared with that using po1ishedplates. It has been found that dispersion parameters, on using the method described, are lower than those obtained with the conventional method; this is attributed to segregation.