[en] Comparative analysis of results of chemical, activation, microstructura, X-ray phase analyses and X-ray spectral microanalysis of Y- and Bi-high temperature superconductors was performed. It is shown that the accuracy of oxygen determination in these materials, achieved during activation analysis, is sufficient for evaluating optimization of studied processes, choice of treatment conditions and fabrication of high-quality speamens. Calcination of basis materials and drying of prepared powders and their mixtures before synthesis and measurements are the required technological operations when producing HTSC and analyzing chemical composition