Reaction of aq. NH4SCN with 22 N H2SO4 was studied in order to estimate the yield of HCN from thiocyanate-fixers under strong acid conditions. Main gaseous products were identified to be HCN, CS, and COS by GC-MS. The amounts of HCN were measured by Pyridine-Pyrazolone method (JIS K 0102) and the maximum concentrations were ca. 1.2×10-2 mol/l and 1.4×10-2 mol/l for 2 mol/l and 4 mol/l NH4SCN respectively. Yellow solid was precipitated in the reaction and the molecular formula was determined to be C2H2N2S3 by elementary analysis.