Abstract:Accurate determination of arsenic in copper flash smelting dust is of great significance for the calculation of matter burdening and production control. The sample was dissolved with nitric acid-potassium chlorate saturated solution, ammonium fluoride solution and perchloric acid. After removing nitric acid with sulfuric acid (1+1), the arsenic ions in the solution were reduced to elemental arsenic with sodium hypophosphite in hydrochloric acid medium using copper sulfate as the catalyst. Other impurities were separated by filtration. The elemental arsenic was dissolved with excessive potassium dichromate standard titration solution. The excessive potassium dichromate standard titration solution was titrated with ferrous ammonium sulfate standard titration solution using N-phenylanthranilic acid as the indicator. The method for determination of arsenic in copper flash smelting dust by ferrous ammonium sulfate back titration was established. During the reduction of arsenic ions into elemental arsenic with sodium hypophosphite, some arsenic ions were possibly not reduced and then filtrated into the solution. The influence of residual arsenic in filtrate on the determination results was investigated. The results showed that the influence of arsenic in sample could be ignored because the mass fraction of arsenic in filtrate was less than 0.01%. The interference tests of coexisting elements showed that the influence of coexisting copper, lead, iron and zinc in sample on determination of arsenic could be ignored. The proposed method was applied for the determination of arsenic in three copper flash smelting dust samples. Meanwhile, the recovery tests of standard addition were conducted. The relative standard deviation (RSD, n=11) of determination results were between 0.35% and 2.6%. The recoveries were between 99% and 101%. The contents of arsenic in two copper flash smelting dust samples were determined according to the experimental method. The found results were consistent with those obtained by microwave digestion-inductively coupled plasma atomic emission spectrometry.
[1] 张荣良,丘克强,谢永金,等.铜冶炼闪速炉烟尘氧化浸出与中和脱砷[J].中南大学学报(自然科学版),2006,37(1):73-78. ZHANG Rongliang,QIU Keqiang,XIE Yongjin,et al.Treatment process of dust from flash smelting furnace at copper smelter by oxidative leaching and dearsenifying process from leaching solution[J].Journal of Central South University (Science and Technology),2006,37(1):73-78. [2] 范丽新,汤淑芳.Na2EDTA返滴定法测定铜冶炼烟尘中镉[J].冶金分析,2021,41(11):63-70. FAN Lixin,TANG Shufang.Determination of cadmium in copper smelting dust by Na2EDTA back titration[J].Metallurgical Analysis,2021,41(11):63-70. [3] 中华人民共和国工业和信息化部.YS/T 519.1—2009 砷化学分析方法 第1部分:砷量的测定 溴酸钾滴定法[S].北京:中国标准出版社,2010. [4] 陈娅陶,李艳萍,袁梦梅,等.溴酸钾滴定法测定铜冶炼烟尘中的砷含量[J].中国无机分析化学,2020,10(5):6-10. CHEN Yatao,LI Yanping,YUAN Mengmei,et al.Determination of arsenic in copper smelting smoke by potassium bromate titration[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(5):6-10. [5] 段萍.重铬酸钾容量法测定铅锌矿石中砷含量[J].世界有色金属,2017(22):205-206. DUAN Ping.Determination of arsenic content in lead-zinc ore by potassium dichromate volumetric method[J].World Nonferrous Metals,2017(22):205-206. [6] 中华人民共和国国家质量监督检验检疫总局.GB/T 23513.2—2009 锗精矿化学分析方法 第2部分:砷量的测定 硫酸亚铁铵滴定法[S].北京:中国标准出版社,2009. [7] 徐道军.火焰原子吸收法快速测定烟尘中的砷[J].科技展望,2015,25(22):157. XU Daojun.Rapid determination of arsenic in smoke and dust by flame atomic absorption spectrometry[J].Sci-ence and Technology,2015,25(22):157. [8] 乔柱,庄梅,张萍萍,等.氢化物发生-原子荧光光谱法测定铬矿中砷[J].冶金分析,2022,42(4):28-33. QIAO Zhu,ZHUANG Mei,ZHANG Pingping,et al.Determination of arsenic in chromium ore by hydride generation-atomic fluorescence spectrometry[J].Metallurgical Analysis,2022,42(4):28-33. [9] 邹雯雯,管嵩,孙博,等.微波消解-电感耦合等离子体原子发射光谱法测定铜精矿中银、铅、镉、汞和砷的含量[J].理化检验(化学分册),2021,57(12):1099-1103. ZOU Wenwen,GUAN Song,SUN Bo,et al.Determination of silver,lead,cadmium,mercury and arsenic in copper concentrate by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2021,57(12):1099-1103. [10] 万双,李先和,赵九轲.X射线荧光光谱法快速测定黑铜中的铜,砷,锑,铋,铅,镍,锌和锡[J].化学分析计量,2017,26(5):93-96. WAN Shuang,LI Xianhe,ZHAO Jiuke.Rapid determination of copper,arsenic,antimony,bismuth,lead,nickel,zinc and tin in black copper by X-ray fluorescence spectrometry[J].Chemical Analysis and Meterage,2017,26(5):93-96. [11] 李先和,万双.硫酸铅分离-EDTA滴定法测定铜闪速冶炼烟尘中的铅[J].中国无机分析化学,2020,10(2):15-19. LI Xianhe,WAN Shuang.Rapid determination of lead in copper flash smelting dust by lead sulfate separation-EDTA titration[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(2):15-19. [12] 戚月花,张淑玲,李先和,等.铜精矿中二氧化硅含量的快速测定[J].化学分析计量,2016,25(6):91-94. QI Yuehua,ZHANG Shuling,LI Xianhe,et al.Rapid determination of silicon dioxide content in copper concentrate[J].Chemical Analysis and Meterage,2016,25(6):91-94.