PURPOSE: To separate Sb from Bi easily, to eliminate a complicated process, and to recover Sb and Bi efficiently and separately, by sulfurizing a solution containing Sb and Bi in acidity with hydrochloric acid, fixing and separating only Sb as a sulfide.

CONSTITUTION: In a treatment of a solution containing Sb and Bi, sulfurization treatment is carried out in acidity with 4W8N hydrochloric acid, only Sb is fixed and separated as a sulfide. A solution obtained by adsorbing Sb or Bi in an electrolytic solution in copper electrolysis on a chelate resin or an anion exchange resin, eluting it with a hydrochloric acid solution, or a solution obtained by treating precipitated copper of electrolysis to give a solution containing Sb or Bi, treating the solution with a chelate resin or an anion exchange resin, and eluting it with a hydrochloric solution may be used as the solution containing Sb or Bi. When the acid concentration is low and near 4N, only bismuth sulfide is dissolved, and when it is ≥8N, antimony sulfide is also dissolved, so separation of Bi and Sb by sulfurization treatment is not carried out with ease.