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Development of rapid method of spectral analysis capable of accompanying all the stages of nickel superalloy production is a hot topic of the analytical control of nickel superalloys. To ensure high accuracy of the results obtained by the methods of optical emission spectrometry and X-ray fluorescence spectrometry, reference materials (RM) adequate in composition to the analyzed samples are to be used. The lack of RM for novel grades of modern nickel alloys, entails the necessity of their development and certification. A methodical approach to the development and production of RM of new grades of nickel superalloys is presented. It is shown that production of the corresponding RM for spectral analysis apart from obvious requirement regarding the absence of defects (shells, cracks, nonmetallic inclusions, isolated zones differing in the content of alloying elements and impurities) requires also elimination of the areas of increased microporosity. In this case, the samples are rejected and melted down, the smelting modes of the CO blanks being adjusted if necessary. We have studied the structure and homogeneity of the manufactured RM and determined the certified values of the reference materials for nickel superalloys of the type VZhM, VKNA, etc. The potentiality of using the developed RM for optical emission spectroscopy with spark excitation and X-ray fluorescence analysis are considered. It is shown that optical emission spectroscopic analysis with spark excitation requires RM sets most close in composition to the analyzed samples when plotting a calibration characteristic, whereas when using X-ray fluorescence analysis, combined sets of RM are appropriate for analysis of the alloy grades similar in composition. The metrological characteristics of the reference materials of approved types (certified reference materials) for the spectral analysis developed at FSUE VIAM for the last seven years are presented.

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The determination of the elements Cu, Ni, Sb, Bi, Pb, Zn and Fe in the tin-based solder VPr35, as well as the elements Sn, Ni, Sb, Bi and In in the lead-based VPr40 solder by the method of х-ray fluorescence spectroscopy has been carried out. The calibration dependences are corrected taking into account the superposition of signals from interfering elements on the analytical signal and changes in intensity caused by inter-element influences in the matrix. The analysis was carried out by the method of fundamental parameters without using standard samples. The correctness of the results obtained was confirmed by their comparative analysis by atomic emission spectroscopy and high-resolution mass spectrometry with a glow discharge.

In this work, Al, Cr, Cu, Fe, Ni, Si and Y were determined in SDP-6 cathodes based on cobalt and SDP-1 and AZh8 nickel-based cathodes by x-ray fluorescence spectroscopy. The calibration dependences are corrected taking into account the superposition of signals from interfering elements on the analytical signal and changes in intensity caused by inter-element influences in the matrix. A standard-free analysis was carried out using the method of fundamental parameters. The correctness of the results obtained was confirmed by a comparative analysis by atomic emission spectroscopy and high-resolution mass spectrometry with a glow discharge.