Abstract：When elements of high concentration in high-alloyed steel are determined by OES-Spark , X-ray fluorescence spectrometry (XRF) and inductively coupled plasma optical emission spectrometry (ICP-OES) , absorption enhancements, grain size effects, differences in metallurgical phases composition, inter-elemental interferences (OES-Spark and XRF) and poor precision (ICP-OES) affect the accuracy of the response. The preparation of samples as borate beads would lead to many advantages, i.e. elimination of phase composition and metallurgical grain-size effects, high homogeneity and dissolution of inclusions (oxides, nitrides, carbides) and treatment of any shape and amount of sample. In this work, a new method of preparation has been developed. The experimental trials have been conducted in determination of high-alloyed steel international certified materials by XRF.
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