Abstract：Bismuth concentrate could be dissolved with hydrochloric acid,nitric acid and perchloric acid. However, the antimony-bismuth concentrate with similar composition could not be dissolved with the same acid dissolution method. The reason for this phenomenon was discussed. The phase analysis of bismuth concentrate and antimony-bismuth concentrate were respectively performed with X-ray diffractometer (XRD). The results showed that the incomplete dissolution of antimony-bismuth paragenetic minerals was possibly the reason for the incomplete dissolution of antimony-bismuth concentrate. Based on this, the original sample dissolution method was improved. The sample was pre-dissolved with hydrochloric acid, nitric acid and perchloric acid. After perchloric acid fume, the hydrochloric acid and hydrobromic acid were supplemented for three times to further dissolve the sample. When the improved dissolution method was conducted for antimony-bismuth concentrate, there was few gray insoluble residues existed in sample solution, but no black insoluble substances. The gray insoluble residues were treated by potassium pyrosulfate fusion-acid dissolution method, and then the content of bismuth in it was determined by atomic absorption spectrometry (AAS). The calculation results indicated that the ratio of bismuth content in gray insoluble residue to sample was not more than 0.2%. In other words,the content of bismuth in gray insoluble residues could be ignored. Consequently, the determination of bismuth in antimony-bismuth concentrate was realized by EDTA titration after the sample was treated with the improved dissolution method. The sample amount was optimized and 0.3g was finally selected. The interference of high-content antimony in antimony-bismuth concentrate sample on the determination was discussed. The results indicated that most antimony in sample had been volatilized in sample dissolution process, and the residual antimony in sample solution had no interference with the determination. The experimental method was applied for the determination of bismuth in antimony-bismuth concentrate sample. The relative standard deviations (RSD, n=8) were between 0.22% and 0.47%. The recoveries of standard addition were between 99% and 101%. The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).
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