Abstract: The acetylene produced in reaction of the sample of combined desulphurizing agent to water is burned in oxygen gas. The amount of CO₂ formed is determined in soda asbestos absorption gravimetric method so as to calculate CaC₂ content. The free CaO and CaC₂ in the sample are leached in glycerol-glycol-sucrose-water mixed leaching liquor. The total amount of Cao and CaC₂ is determined in EGTA complexometric titration at pH> 12. The amount of CaC₂ subtracted from the total amount of CaC₂ and CaO leaves the amount of free CaO. The CaCO₃ in residue after leaching is leached in acetic acid. The calcium acetate is determined in EGTA complexometric titration so as to calculate CaCO₃ content. The CaF₂ in the final residue leached in sulphuric acid chlorhydric acid-boracic acid-water is analyzed.