AbstractA new procedure of powder sample preparation for x‐ray emission analysis by melting has been worked out in detail. The mixture sample‐flux was melted and cooled in graphite crucible. The resulting glass disk was ready for direct measurement. The re‐fused graphite electrode of an electric arc furnace was used as the material for the graphite crucible. The dimension and shape of the crucible bottom were determined on the basis of sample holder dimension and sample behaviour during the cooling step. The reproducibility of Kα line measurement was below 1%. Resistance of the crucible to handling and the influence of graphite on Fe Kα, Ca Kα, SKα, Si Kα and Mg Kα line intensities also were i