Abstract：The determination method of arsenic and antimony in tin ore usually adopts spectrophotometry. A new determination method of arsenic and antimony in tin ore by hydride generation-atomic fluorescence spectrometry was established after the sample was dissolved in hydrochloric acid-nitric acid by microwave digestion. The results showed that the sample could be dissolved by microwave digestion with 8 mL of mixed hydrochloric acid-nitric acid (5+3) as solvent. When the concentration of hydrochloric acid was about 0.96 mol/L, the mass concentration of both thiourea and ascorbic acid were 10 g/L, HCl (1+9) was used as carrier liquid, and 20 g/L potassium borohydride solution was used as reducing agent, the calibration curves were plotted based on the fluorescence intensity of arsenic and antimony against the corresponding mass concentration. The linear correlation coefficients were both not less than 0.999 8. The detection limit of arsenic and antimony was 0.044 2 μg/L and 0.020 4 μg/L, respectively. The interference test showed that the coexisting elements in tin ore sample did not interfere with the determination. The proposed method was applied to the determination of arsenic and antimony in tin ore actual samples. The relative standard deviation(RSD,n=6) was 1.1%-1.3% and 0.99%-1.4%, respectively. The recoveries were 99%-104% and 98%-104%, respectively. The certified reference materials of tin ore were determined by the experimental method. The results were basically consistent with the certified values.
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