FIELD: pharmaceutics. SUBSTANCE: invention refers to pharmaceutical and analytical chemistry and can be used in pharmaceutical industry for control of technological processes and quality of pharmaceutical preparations, as well as waste water and air zone of chemical-pharmaceutical enterprises. Substance of the method is based on ability of triazide to be recovered on various types of graphite electrodes and consists in conversion of triazide from sample into water solution and in direct (without preliminary accumulation on electrode) voltammetric determination of triazide in background of Britton-Robinson buffer mixture pH=7 in presence of 0.01 M sodium sulfite by recording cathode peaks in the square-wave mode of capturing voltammograms in the range from (-0.4) to (-1.4) V at potential scanning rate of 150 mV/s, pulse amplitude of 50 mV. Triazide concentration is determined from the height of the peak in the range of potentials from (-0.60) to (-1.0) V relative to the silver chloride electrode by adding a standard solution of triazide. EFFECT: sensitivity and rapidness of analysis is achieved.