Determination of antimony in bismuth-rich lead by cerium sulfate titration method
XIE Lei1,2, YANG Tian-zu*2, YANG Hua-dong1, ZHANG Zhuo-jia1
1. National Quality Supervision and Inspection Center of Precious Metal and Heavy Nonferrous Products (Hunan), Chenzhou 423000, China; 2. School of Metallurgy and Environment, Central South University, Changsha 410083, China
Abstract：The accurate determination of impurity elements in bismuth-rich lead was of great significance to the control of production technological conditions for electrolytic refining. The determination of antimony in bismuth-rich lead was discussed. The sample was dissolved with nitric acid-tartaric acid mixture. Then the tartaric acid was carbonated with sulfuric acid followed by removing carbon with nitric acid. The hydrazine sulfate was used as reducing agent to reduce antimony (V) to antimony (III). In the medium of hydrochloric acid, the phosphoric acid was added to mask high-valence iron ions. The solution was heated to 80-90℃ and then titrated with cerium sulfate standard solution with methyl orange and methylene blue as the indicators. Thus, a determination method of antimony in bismuth-rich lead by cerium sulfate titration was established. The results of interference experiments showed that the coexisting elements (Pb, Bi, Cu, Ag, Sn, Fe, As and Au) in bismuth-rich lead had no influence on the determination of antimony. The proposed method was applied for the precision and recovery tests of actual samples of bismuth-rich lead. The relative standard deviations (RSD, n=9) were between 1.0% and 1.2%, and the recoveries were between 99% and 102%. After the sample was treated with tartaric acid-nitric acid mixture, the content of antimony was determined by cerium sulfate titration method and flame atomic absorption spectrometry (FAAS). The determination results of the above two methods were consistent. The experimental method was applied to the determination of antimony in actual sample of bismuth-rich lead, and the results were satisfactory by interlaboratory comparison test
李建红.高铋铅电解精炼回收Ag、Bi的实践[J].株冶科技(Science & Technology of Zhuzhou Smelter),2003,31(2):4-7,13.
[2]
刘金铭,粟明辉,刘可人,等.高铋粗铅电解精炼生产实践[J].湖南有色金属,2015,31(3):42-44,77.LIU Jin-ming,SU Ming-hui,LIU Ke-ren,et al.Practice of electrolytic refining for lead with high bismuth[J].Hunan Nonferrous Metals,2015,31(3):42-44,77.
[3]
袁培新.水口山高铋粗铅电解精炼的改进与实践[J].有色金属工程,2013,5(5):42-45.YUAN Pei-xin.Improvement and practice of electrolysis refining of crude lead with high bismuth in shuikoushan[J].Nonferrous Metals Engineering,2013,5(5):42-45.
[4]
何启贤,韦文宾.高铜、高铋粗铅的精炼实践[J].湖南有色金属,2008,24(2):22-24.HE Qi-xian,WEI Wen-bin,GAO Tong.Practice for refining crudelead with high copper and bismuth[J].Hunan Nonferrous Metals,2008,24(2):22-24.
[5]
高云,宋召霞.硫化钠还原-硫酸铈滴定法测定含锑金精矿中锑[J].冶金分析,2017,37(3):39-43.GAO Yun,SONG Zhao-xia.Determination of antimony in gold concentrate containing antimony by cerium sulfate titrimetry with sodium sulfide reduction[J].Metallurgical Analysis,2017,37(3):39-43.
[6]
石文莹.硫酸铈滴定法测定湿法炼锑电解液中锑的含量[J].湖南有色金属,2017,37(3):76-77,80.SHI Wen-ying.Determination of antimony content in wet antimony smelting electrolyte by cerium sulfate titration[J].Hunan Nonferrous Metals,2017,37(3):76-77,80.
[7]
冯丽琼,金晓峰,陈兵,等.硫酸铈容量法测定矿渣中锑含量[J].云南冶金,2011,40(3):66-67.FENG Li-qiong,JIN Xiao-feng,CHEN Bing,et al.Determination of antimony content in slag by cerium sulfate volumetric method[J].Yunnan Metallurgy,2011,40(3):66-67.
[8]
王凯.孔雀绿分光光度法测定粗铟中锑[J].冶金分析,2004,24(2):66-67.WANG Kai.Spectrophotometric determination of antimony in crude indium with malachite green[J].Metallurgical Analysis,2017,37(3):39-43.
[9]
许瑞波,马卫兴,许兴友,等.锑(III)-铍试剂III-TritonX-100三元体系分光光度法测定锑[J].冶金分析,2008,28(10):61-63.XU Rui-bo,MA Wei-xing,XU Xing-you,et al.Spectrophotometric determination of stibium with Sb(III)-beryllon III-TritonX-100 ternary system[J].Metallurgical Analysis,2008,28(10):61-63.
[10]
陈丽梅,谢明丽,罗正波,等.ICP-AES直接测定粗铅中锑、铜、铋[J].湖南有色金属,2016,32(2):74-76.CHEN Li-mei,XIE Ming-li,LUO Zheng-bo,et al.Determination method of antimony,copper and bismuth in crude lead by ICP-AES[J].Hunan Nonferrous Metals,2016,32(2):74-76.
[11]
张元,赵文志,杜少文,等.氢化物发生-电感耦合等离子体质谱法(HG-ICP-MS)测定地质样品中的砷锑[J].化学工程师,2018,32(1):31-33,37.ZHANG Yuan,ZHAO Wen-zhi,DU Shao-wen,et al.Determination of arsenic and antimony in geological samples by hydride generation inductively coupled plasma mass spectrometry (HG-ICP-MS)[J].Chemical Engineer,2018,32(1):31-33,37.
[12]
庞振兴,王贵玉,金伟,等.电感耦合等离子体质谱法测定硅铁中痕量铌、砷、锑[J].中国测试,2018,44(5):49-52.PANG Zhen-xing,WANG Gui-yu,JIN Wei,et al.Determination of trace niobium, arsenic and stibonium in ferrosilicon by ICP-MS[J].China Measurement & Testing Technology,2018,44(5):49-52.
李颜君,杨占菊,董更福,等.氢化物发生-原子荧光光谱法同时测定铅锭中砷锑[J].冶金分析,2017,37(11):75-79.LI Yan-jun,YANG Zhan-ju,DONG Geng-fu,et al.Simultaneous determination of arsenic and antimony in lead ingot by hydride generation-atomic fluorescence spectrometry[J].Metallurgical Analysis,2017,37(11):75-79.
[15]
刘君侠,葛小燕,李先和,等.EDTA滴定法连续测定粗铅铋合金中的铅铋[J].山东化工,2016,45(1):59-61.LIU Jun-xia,GE Xiao-yan,LI Xian-he,et al.Determine continuously lead and bismuth ions in lead-bismuth alloy by EDTA titration[J].Shandong Chemical Industry,2016,45(1):59-61.
[16]
章连香,王红霞,尚丽远,等.铅铋合金中铅的测定方法研究[J].矿冶,2006,15(2):91-93.ZHANG Lian-xiang,WANG Hong-xia,SHANG Li-yuan,et al.Study on the determination of lead in lead-bismuth alloy[J].Mining and Metallurgy,2006,15(2):91-93.
胡长春,王沿方,陈作王.电感耦合等离子体原子发射光谱法测定锡铅合金中的锡[J].化学分析计量, 2018,27(5):72-75.HU Chang-chun,WANG Yan-fang,CHEN Zuo-wang.Determination of tin in tin-lead alloy by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage, 2018,27(5):72-75.
