Abstract: There are reliable chemical analysis methods for determining high, low and trace amounts of antimony in gold-antimony ore and antimony ore. However, the volumetric method for low content antimony measurements has a low analysis efficiency and involves a complex process. Atomic Fluorescence Spectrometry has a strong memory effect for high and low content antimony samples, resulting in poor analytical precision and accuracy. By using Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), the disadvantages of Atomic Fluorescence Spectrometry, Atomic Absorption Spectrometry and the volumetric method can be overcome. In this article, a description of the method for adding hydrofluoric-nitric-perchloric acid to dissolve samples, and using sulfuric acid as the latent solvent is given. The antimony in 20% hydrochloric acid was determined by ICP-AES with a wavelength of 217.5 nm. The detection limit is 30 μg/g and precision is less than 5%. The results of the national standard materials agree well with certified values. The results for actual samples with different antimony content are consistent with the results by cerium sulfate volumetry and Atomic Fluorescence Spectrometry. This method is reliable for samples with antimony contents of 0.05%-5%.