Autoclave leaching of sulfide concentrates may produce various ferric secondary phases, depending on the arsenic content and temperature. Silver is converted to argentojarosite, from which it is not recoverable by standard cyanidation methods. To increase silver recovery, it is necessary to reduce the argentojarosite formation during autoclave leaching. This study was devoted to the influence of gypsum on the formation of secondary phases of ferric arsenate and the subsequent recovery of gold and silver by cyanidation. The addition of gypsum at a consumption of 0.1 g/g(concentrate) helped to increase silver extraction from 13.4 to 98% at cyanidation. Gold recovery was 99%. An increase in gypsum consumption contributed to the ferric arsenate sulfate formation with an increased sulfate sulfur content, and a decrease in the As/S(sulfate) molar ratio in the cake from 3.7 to 0.88 contributed to an increase in silver extraction at cyanidation of up to 98%. Basic ferric sulfate is not formed in this case, since according to EDS mapping, the distribution of arsenic and sulfur over ferric-containing particles is uniform. According to TCLP, stable, sparingly soluble ferric arsenate phases are formed and the cake obtained after cyanidation is stable and suitable for disposal, since the final arsenic concentration in the solution was 0.45 mg/dm3.