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This work is a part of a study on the development of a technology for immobilizing mercury in waste based on the principles of converting mercury and its compounds in waste to mercury sulfide. The purpose of this work is to analyze existing methods for determining mercury in solid samples and develop a rapid assessment methodology for routine monitoring of the residual mercury content in the final product. This powder is a mixture of glass, sulfur, mercury sulfide, bentonite, and mercury residue. Methods for determining mercury were analyzed in order to select a method for rapid analysis of the residual mercury content in complex powders formed as a final product after immobilization of mercury and mercury oxide in waste. A modification of known methods was proposed, and specific conditions were developed for correctly determining the concentration of metallic mercury in the range of less than 2 mg/kg of powder. Titration of neutralized samples (pH value of the sample in the range of 2.3±0.2) performed with a solution of ammonium thiocyanate in the presence of an indicator – diphenylcarbazone. For expert verification of the results of waste demercurization, the method of x-ray fluorescence analysis was proposed. Preliminary experiments have shown the prospects of using this technique for expert control