Determination of lead in crude tin by EDTA titration method
FAN Li-xin1,2,LU Qing3,4
1.Beijing General Research Institute of Mining and Metallurgy,Beijing 102628,China; 2.Beijing Key Laboratory for Evaluation and Testing of Metallic Mineral Resources,Beijing 102628,China; 3.Central Iron & Steel Research Institute,Beijing 100081,China; 4.NCS Testing Technology Co.,Ltd.,Beijing 100094,China
Abstract:The high content lead in sample is usually determined by EDTA titration after lead sulfate precipitate separation. However, the interference of tin and bismuth cannot be ignored when the method is applied for the determination of lead content in crude tin. The sample was dissolved in PTFE beaker with hydrochloric acid-nitric acid-perchloric acid and hydrochloric acid-nitric acid-hydrobromic acid. Under the experimental conditions, the tin in sample could react with hydrobromic acid to form stannic bromide, which would be removed through volatilization. After treatment by lead sulfate precipitate separation, the mercaptoacetic acid was added into solution before titration to mask bismuth. The determination method of lead in crude tin by EDTA titration was established in HAc-NaAc buffer solution using xylenol orange as the indicator. The experimental conditions were further optimized, including the ageing time of precipitate, the dosage of HAc-NaAc buffer solution and the slight boiling time. The optimum conditions were finally obtained as follows: the ageing time was 2 h, the dosage of HAc-NaAc buffer solution at pH 5.5-6.0 was 30 mL, and the slight boiling time was 10 min. The proposed method was applied for the determination of lead in crude tin, and the found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The relative standard deviation (RSD, n=11) was 0.68% and 0.38%, respectively. The recoveries of standard addition were between 98% and 102%.
范丽新,陆青. EDTA滴定法测定粗锡中铅[J]. 冶金分析, 2017, 37(5): 68-72.
FAN Li-xin,LU Qing. Determination of lead in crude tin by EDTA titration method. , 2017, 37(5): 68-72.
邓正平,温青.锡及锡合金可焊性镀层电镀工艺[J].电镀与精饰,2006,28(5): 33-38.DENG Zheng-ping,WEN Qing.Electrolating technology for tin and tin alloy solderable coating[J].Plating and Finishing,2006,28(5):33-38.
[2]
李振昊,李文乐,孔繁华,等.掺杂二氧化锡的应用研究进展[J].化工进展,2010,29(12):2324-2340.LI Zhen-hao,LI Wen-le,KONG Fan-hua,et al.Advances in applied research of doped SnO2[J].Chemical Industry and Engineering Progress,2010,29(12):2324-2340.
[3]
邓兆磊,杨亚峰.我国粗锡冶炼技术现状及发展前景[J].中国有色冶金,2015,44(2):34-38.DENG Zhao-lei,YANG Ya-feng.Status and development prospects of crude tin smelting process in China[J].China Nonferrous Metallurgy,2015,44(2):34-38.
[4]
赵树宝.EDTA络合滴定法连续测定铁矿石中铝铅锌[J].冶金分析,2011,31(11):66-69.ZHAO Shu-bao.Continuous determination of aluminum,lead and zinc in iron ore by EDTA complexometric titration[J].Metallurgical Analysis,2011,31(11):66-69.
[5]
武明丽.快速EDTA滴定法测定高铅渣料中的铅[J].现代化工,2015,35(7):171-174.WU Ming-li.Quick determination of lead in high lead slag with EDTA titrimetry[J].Modern Chemical Industry,2015,35(7):171-174.
[6]
方文韬,史旭峰,朱克聪.铋矿石中高含量铅的测定方法[J].云南地质,2015,34(3):480-483.FANG Wen-tao,SHI Xu-feng,ZHU Ke-cong.The determination method of high Pb in Bi ore[J].Yunnan Geology,2015,34(3):480-483.
[7]
Chulsung Kim,Say-Kee Ong.Recycling of lead-contaminated EDTA wastewater[J].Journal of Hazardous Materials,1999,69:273-286.
[8]
Chulsung Kim,Yongwoo Lee,Say-Kee Ong.Factors affecting EDTA extraction of lead from lead-contaminated soils[J].Chemosphere,2003,51(9):845-853.
[9]
黄葡英,谢辉.EDTA滴定法测定铅锡合金[J].冶金分析,2013,33(3):77-79.HUANG Pu-ying,XIE Hui.Determination of lead in lead-tin alloy by EDTA titration method[J].Metallurgical Analysis,2013,33(3):77-79.
[10]
向德磊.EDTA滴定法测定铅冶炼原料中铅含量结果正确度的探讨[J].冶金分析,2016,36(8):35-40.XIANG De-lei.Discussion on the determination accuracy of lead content in smelting raw materials by EDTA titration method[J].Metallurgical Analysis,2016,36(8):35-40.
[11]
段旭川.同时溶解和ICP-AES同时测定焊锡材料中的铅、锡和银[J].分析测试学报,2006,25(1):122-124.DUAN Xu-chuan.Simultaneous dissolution of tin,silver and lead in tin-lead solder alloy and their determination by ICP-AES[J].Journal of Instrumental Analysis,2006,25(1):122-124.