Determination of lead and bismuth in arsenic-antimony soot by inductively coupled plasma atomic emission spectrometry after matrix separation with hydrobromic acid
Besides of As and Sb,the arsenic-antimony soot also contains some other valuable elements such as Pb and Bi.As a kind of secondary resource,the arsenic-antimony soot has attracted more and more at-tention in recent years.The analysis and testing of valuable elements in arsenic-antimony soot can provide quantitative basis for the recycle and trade of such secondary resource.Since the contents of As and Sb in arsenic-antimony soot are relatively high,if the sample is decomposed by the traditional HNO3-HCl-HClO4 system,Sb will be partially hydrolyzed after leaching with HCl,resulting in the turbidity of solution due to the formation of antimony oxychloride precipitate.In this study,the sample was dissolved with HNO3-HCl-HClO4 system.Then As and Sb were removed with hydrobromic acid(HBr).The method for the de-termination of Pb and Bi contents in arsenic-antimony soot by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The mass concentration of Pb and Bi in range of 1.00-30.00 μg/mL showed linear relationship with the corresponding emission intensity,and the correlation coefficients were 0.999 9.The limits of detection for Pb and Bi in the method were 0.000 6％and 0.006％.The con-tents of Pb and Bi in five typical arsenic-antimony soot samples were determined according to the experi-mental method.The relative standard deviations(RSD,n=11)of determination results were less than 2％.The Grubbs test results indicated that there was no abnormal value in 11 measurements.The spiked recoveries were between 94.0％and 102.3％.The determination results were consistent with those ob-tained by flame atomic absorption spectrometry(FAAS)and EDTA titration method.The proposed meth-od effectively solved the turbidity problem of solution due to the hydrolysis of Sb after dissolution of arse-nic-antimony soot,thus solving the problem of inaccurate determination results of Pb and Bi.It could be applied for the determination of Pb and Bi contents in arsenic-antimony soot samples.
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