Abstract：The bismuth-riched lead contains some interference elements such as antimony, tin, tellurium and silver. When lead bullion is dissolved according to the traditional method, antimony or tin is easily hydrolyzed in nitric medium to form insoluble substances, which influences on the determination of bismuth. On the other hand, when the content of bismuth is determined according to the traditional EDTA titration method, the existing tellurium or silver in bismuth-riched lead can cause darkening of sample solution, which influences on the color observation in titration. Due to the presence of tin, the color of sample solution will be back to the red after appearing brilliant yellow, and the determination of bismuth is severely affected. The bismuth-riched lead sample was dissolved with nitric acid-tartaric acid. The dosage and addition sequence of ascorbic acid were discussed. The influence of impurity elements (tin and silver) and other coexisting elements on the determination of bismuth was investigated. The results showed that 5.0000g of bismuth-riched lead sample could be fully dissolved with 40mL of tartaric acid (100g/L) and 80mL of nitric acid (1+1). The dosage of ascorbic acid was 0.2g and it was added after pH adjustment. When the content of tin was less than 0.4mg, it had no influence on the determination of bismuth. When the content of tin was higher than 0.4mg, it was removed at low temperature by adding hydrobromic acid to eliminate its influence on the determination of bismuth. The redox reaction would not occur under this experimental condition. Other coexisting elements had no influence on the determination of bismuth. The proposed method was applied for the determination of bismuth in five high-bismuth lead samples. The relative standard deviations (RSD, n=5) of determination results were between 0.038% and 1.3%. One bismuth-riched lead sample was dissolved according to the experimental method. The content of bismuth was determined by the proposed method and inductively coupled plasma atomic emission spectrometry (ICP-AES), and the results were consistent. Three high-bismuth lead samples were used for the spiked recovery tests according to the experimental method. The recoveries were between 99.8% and 101%.
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