The invention discloses a method for performing chemical separation, analysis and test on gold in antimony electrolyte. The method comprises the following steps: adjusting H<+> of a sample solution to0.5 to 1 mol/L by diluted 4 mol/L of hydrochloric acid, precipitating antimony in the sample solution in a form of sulfide, in the process, reducing gold ions in the solution into elemental gold to be adsorbed and wrapped in precipitate of antimony sulfide to achieve separating and enriching aims, boiling the solution, performing flocculation and aggregation on the precipitate, and filtering andremoving impurities; putting the precipitate together with filter paper into an original flask, adding concentrated sulfuric acid to treat the precipitate without drying by distillation, cooling aftera sulfuric acid solution is clear, pouring a small amount of water to dilute the sulfuric acid, adding hydrochloric acid to dissolve salt and filtering to remove the antimony; and putting the filterpaper and the precipitate into the original flask to perform digestive treatment, dissolving the salt by aqua regia, determining the volume and performing measurement by ICP-AES.