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.