The material composition of the sublimates from dust chambers in titanium chlorinators has been studied by chemical, X-ray and microprobe analysis methods. Studies of the phase composition of dust chamber sublimates have shown that the object consists of aqueous and anhydrous chloride phases to a greater extent. Two forms of niobium present, such as oxychloride and oxide niobium were found. The presence of zirconium in sublimates has a chloride and oxychloride nature. Experiments for the aqueous leaching of dust chamber sublimates were conducted to determine the optimal process conditions: S:L ratio = 1:8, leaching time = 1 hour, temperature = 25℃. Studies were conducted to choose an acidic reagent for cake leaching followed by the conversion of niobium and zirconium into a solution. A solution consisting of HF+H2SO4 was selected as an acidic reagent for cake leaching. Optimal conditions for the extraction of niobium and zirconium into solution were established, such as 25% [18M HF] +75% [7M H2SO4], S:L ratio = 1:3, temperature = 90 °C, duration of the leaching process = 120 minutes. Under these leaching conditions, the extraction of niobium, zirconium, and titanium into solution was 94.06%, 84.95% and 32.35%, respectively. The elemental and phase composition of the residue from acid leaching of cake were determined.