Abstract：During the determination of Ag in tin-lead solder by flame atomic absorption spectrometry (FAAS), the presence of Sn would cause interference. The interference of Sn with Ag in determination by FAAS was discussed. The results showed that the maximum tolerant amount of Sn was 5 mg/mL during determination of Ag not higher than 2 μg/mL. As a result, a determination method of Ag in tin-lead solder was established by FAAS in 1.8 mol/L HCl medium, and whether the separation of Sn was required or not according to the content of Ag in sample. Take advantage of the characteristic of Ag+ which could react with excessive Cl－ to form soluble complex of [AgCl4]3－, the sample solution could be directly determined by FAAS after dissolution with HCl (3+1)-H2O2 or dissolution with HCl-HBr-H2O2 followed by removing Br when the mass fraction of Ag in sample was higher than 0.02%. However, when the mass fraction of Ag in sample was not higher than 0.02%, the volatilization and separation of Br and Sn should be conducted after dissolving sample with HCl-HBr-H2O2 then followed by the determination of test solution by FAAS. The results showed that the mass concentration of As in range of 0.2-2.5 μg/mL had linear relationship with correlation coefficient of 0.999 96. The detection limit was 0.004 μg/mL. The interference tests indicated that the splashing of Pb precipitate could be prevented by removing Br and Sn with HCl-H2O2 at 70-100 ℃. About 70%-90% Pb matrix could be precipitated to PbCl2 in HCl medium. At this time, the solution should be placed to clear before determination in order to prevent the influence of Pb precipitate on suction filtration of testing solution. The proposed method was applied to the determination of Ag (0.002 3%-1.1%) in representative samples and certifeid reference material of tin-lead solder. The results were basically consistent with those obtained by other methods (extraction spectrophotometry or potentiometric titration) or the certified values. The relative standard deviations (RSD, n=9-11) were between 0.88% and 4.8%. The actual samples were analyzed by this proposed method, and the recoveries were between 95% and 106%.
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