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The aim of the work was the assessment of capability for the change control in the structure of a compact material of pelletized heatproof nickel alloy grade EP741NP using the atomic emission method. The proposed method of evaluation is based on the statistical significance of the analytical response differences during atomic emission spectroscopy of solid specimens taken from one sample before and after heat treatment using the instruments AtomComp 81 and ARL 4460 with a high-voltage spark excitation. For calculations, the ratio of the line intensity of the analyzed element to the line intensity of the main sample component (in our case Ni 2254 ) was used. The difference confidence estimation was made by the averages comparison method in a variance analysis. The study results are presented on the effect of material structure on analytical response during atomic emission spectroscopy of solid specimens. It was proved that the samples before and after heat treatment give statistically differing results while analyzed.