Determination of high content indium in indium anode slime by butyl acetate extraction-EDTA titration
1.Institute of Application of Mineral Resources Guangdong Province,Shaoguan 512026,China; 2.Key Laboratory of Radioactive and Rare Scattered Minerals Comprehensive Utilization,Ministry of Land and Resources,Shaoguan 512026,China
Abstract：Apart from much indium, the indium anode slime also contains lead, zinc, copper, tin, bismuth and antimony. These impurity elements will cause interference when the content of indium in indium anode slime was directly determined by EDTA titration.The sample was decomposed by hydrochloric acid, nitric acid, hydrobromic acid-sulfuric acid. In3+ was then complexed with I－ in potassium iodide-sulfuric acid medium to form InI4－, which could be extracted with butyl acetate. After reextraction with 2% (V∶V) hydrochloric acid twice, the content of indium in indium anode slime was finally analyzed by EDTA titration. The experimental results under optimized conditions indicated that the extraction rate for 30 mg of indium by 20 mL of butyl acetate in 1.5 mol/L KI-2.0 mol/L H2SO4 medium was almost 100%. Then, 15.00 mL of 2 g/L indium standard solution was re-extracted by 50 mL of 2% hydrochloric acid and 20 mL of 2% hydrochloric acid, respectively, and the reextraction rate was almost 100%. The titration was conducted using EDTA standard solution at pH 2.5-3.0 and slight boiling state .The endpoint was clear and bright with obvious abrupt change. The determination results were smooth. The proposed method was applied to the determination of indium in indium anode slime. The recoveries of indium were between 99% and 101%. The relative standard deviation (RSD, n=6) was less than 1%.
徐红江,路斌,董巧龙,等.真空蒸馏脱除粗铟中镉的实验研究[J].有色矿冶,2007,23(5):31-33.XU Hong-jiang,LU Bin,DONG Qiao-long,et al.Study of removing cadmium from crude indium by vacuum process[J].Non-ferrous Mining and Metallurgy,2007,23(5):31-33.
[2]
史旭峰,赵星,宋江伟.火焰原子吸收光谱法测定烟尘中铟的含量[J].云南地质,2015,34(4):617-621. SHI Xu-feng,ZHAO Xing,SONG Jiang-wei.The application of flame atomic absorption spectrometry to analysis of the content of smoke dust[J].Yunnan Geology,2015,34(4):617-621.
[3]
孔凡丽.火焰原子吸收光谱法测定锡渣中的铟[J].中国无机分析化学,2015,5(2):70-72.KONG Fan-li.Determination of indium in tin slag by flame atomic absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2015,5(2):70-72.
[4]
Kye-Sung P,Wakao S,Guido G,et al.Recovery of indium from In2O3 and liquid crystal display powder via a chloride volatilization process using polyvinyl chloride[J].Thermochimica Acta,2009,493(1-2):105-108.
[5]
Terashima S.Determination of indium and tellurium in fifty nine geological reference materials by solvent extraction and graphite furnace atomic absorption spectrometry[J].Geostandards and Geoanalytical Research,2001,25(1):127-132.
[6]
梁信源,蔡卓,黎铉海,等.极谱法测定锌、锑渣氧粉中的铟[J].光谱实验室,2012,29(3):1311-1314.LIANG Xin-yuan,CAI Zhuo,LI Xuan-hai,et al.Determination of indium in zinc and antimony oxide flue dust samples by polarography[J].Chinese Journal of Spectroscopy Laboratory,2012,29(3):1311-1314.
[7]
Charalambous A,Economou A.A study on the utility of bismuth-film electrodes for the determination of In in the presence of Pb and Cd by square wave anodic stripping voltammetry[J].Anal.Chim.Acta.,2005,547:53-58.
[8]
刘淑香.罗丹明B光度法测定高温合金中的痕量铟[J].河北民族师范学院学报(Journal of Hebei Normal University for Nationalities),2012,32(3):136-138.
[9]
彭翠红,奚长生,龙来寿,等.In(Ⅲ)-5-Br-PADAP-OP分光光度法测定锌渣中微量铟[J].分析测试学报,2004,23(4):101-103.PENG Cui-hong,XI Chang-sheng,LONG Lai-shou,et al.Spectrophotometric determination of trace indium in zinc slag with 5-Br-PADAP-OP[J].Journal of Instrumental Analysis,2004,23(4):101-103.
许洁瑜,麦丽碧,陈晓东.EDTA络合滴定法测定锡铋铟合金中的铟[J].材料研究与应用,2010,4(3):231-234.XU Jie-yu,MAI Li-bi,CHEN Xiao-dong.Determination of indium content in Sn-Bi-In alloyby EDTA complexometric titration[J].Materials Research and Application,2010,4(3):231-234.
[12]
张红梅,陈锐.ITO粉及ITO靶材中铟的测定-EDTA容量法[J].稀有金属,2003,27(1):188-190. ZHANG Hong-mei,CHEN Rui.Determination of indium in ITO powder and ITO target by EDTA titration[J].Chinese Journal of Rare Metala,2003,27(1):188-190.
[13]
宋伟明,林枫,买小霞,等.ITO粉末材料中铟含量的测定[J].石油化工与应用,2008,27(1):43-45.SONG Wei-ming,LIN Feng,MAI Xiao-xia,et al.The measurement of tin content in the ITO powder material[J].Petrochemical Inoustry Application,2008,27(1):43-45.
[14]
李合庆.EDTA直接容量法测定海绵铟中铟量的研究[J].有色矿冶,2010,26(6):54-57.LI He-qing.Research on determination of indium in sponge indium by EDTA titration directly[J].Non-ferrous Mining and Metallurgy,2010,26(6):54-57.
高小飞,倪文山,孙晓燕,等.乙酸丁酯萃取-电感耦合等离子体原子发射光谱法测定钨矿石中铟[J].理化检验:化学分册,2012,48(10):1181-1183.GAO Xiao-fei,NI Wen-shan,SUN Xiao-yan,et al.ICP-AES determination of indium in tungsten ore after extraction with butyl acetate[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2012,48(10):1181-1183.
[17]
刘金巍,刘庆学,刘凡岩,等.萃取火焰原子吸收分光光度法测定土壤中的镉铊铟银[J].分析试验室(Chinese Journal of Analysis Laboratory),2008,27(5):362-364.
[18]
余煜棉,李少明,庄小洪.萃取反萃取原子吸收光谱法测定地质物料中的金、银、镓、铟、铊和碲[J].黄金,1991,12(5):46-51.YU Yu-mian,LI Shao-ming,ZHUANG Xiao-hong.Determination of gold,silver,gallium,indium,thallium and tellurium in sample digest of geological materials by atomic absorption spectroscopy after solvent extraction-anti-extraction[J].Gold,1991,12(5):46-51.
