Abstract：The sample was decomposed with nitric acid, hydrochloric acid and perchloric acid. Hydrochloric acid was added to react with silver ions to form silver chloride precipitate. After filtration, the content of silver in precipitate was determined by lead fire assaying gravimetry. The interference of palladium was eliminated. Meanwhile, the content of silver in filtrate was determined by atomic absorption spectrometry (AAS). Thus the content of silver in sample could be obtained by summing the silver content in precipitate and filtrate. Therefore, the determination of silver in silver-palladium concentrate by lead fire assaying gravimetry combined with AAS was realized. Since the silver chloride precipitate had serious adsorption effect on platinum and palladium in precipitate formation process, the influence of platinum and palladium in precipitate on the determination of silver content was investigated. The results showed that after capture of precious metals in precipitate by lead fire assaying, the interference of platinum in precious metal particles could be ignored. However, the influence of palladium on the determination of silver could not be ignored. The precious metal particles was dissolved with 10mL of nitric acid (1+1) at low temperature. The content of platinum in precious metal particles was determined by AAS. The interference of palladium in precipitate could be eliminated by deducting the amount of palladium in precious metal particles from the results of lead fire assaying method. The interference tests indicated that the interference of coexisting elements in filtrate including palladium, copper, bismuth, gold and platinum could be ignored. The silver-palladium concentrate sample was determined according to the experimental method, and the relative standard deviations (RSD, n=11) were between 0.028% and 0.059%. High-purity silver nitrate was added for recovery test, and the recoveries were between 98% and 102%. The proposed method was applied for the determination of silver in silver-palladium concentrate sample, and the found results were basically consistent with those obtained by potassium iodide potentiometric titration.
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