Determination of arsenic and antimony in copper electrolyte by hydrogen peroxide pretreatment-continuous titration method
XIAO Faxin 1, 2, CAO Dao 1, MAO Jianwei 1, SHEN Xiaoni 1, YANG Dixin 1
1 School of Materials Science and Engineering, Henan University of Science and Technology, Luoyang 471003, China; 2 Henan Key Laboratory of Advanced Nonferrous Metal Materials, Henan 471003, China
Abstract：In order to reduce analytical error resulted from the complicated chemical reaction among arsenic, antimony and bismuth in copper electrolyte, the environment of arsenic and antimony in copper electrolyte was simulated based on the continuous titration method of arsenic and antimony in arsenicantimony ore，and a method for determination of arsenic and antimony in copper electrolyte was developed by hydrogen peroxide pretreatmentcontinuous titration method. Firstly, the influences of As and Sb on analysis result of arsenic and antimony were eliminated by addtion of hydrogen peroxide. Then, sulfuric acid and hydrazine sulfate were added separately until the smoke emit to the bottle neck. After cooling down, Sb was titrated by ceric sulfate and As was titrated by potassium bromate in hydrochloric acid medium with methylene bluemethyl orange as indicator. The results showed that the optimal conditions in continuous titration were as follows: sulfuric acid dosage was 20 mL; smoking time was 5 min; the concentration of hydrochloric acid were 4.3 mol/L and temperature was 70 ℃ for determination of antimony; the concentration of hydrochloric acid were 1.8 mol/L and temperature was 80 ℃ for determination of arsenic. The proposed method was applied to the determination of synthetic copper electrolyte. The recoveries for arsenic and antimony were 96% and 104%, respectively. Moreover, this method was also used to the determination of copper electrolyte on copper electrolysis production line. The results were consistent with those obtained by atomic absorption spectrometry, and the relative standard deviation (n=6) was less than 1.2%.
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