Determination of lead and cadmium in zinc chloride-ammonium chloride electrolyte system by anodic stripping voltammetry
MU Peng-tao1,SHEN Qing-feng2,YU Xiao-hua2,XU Shuang-quan2,LIU Chun-xia*1
1.Research Center for Analysis and Measurement, Kunming University of Science and Technology, Kunming 650093, China; 2.Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming 650093, China
Abstract:The simultaneous determination of Pb2+ and Cd2+ in ZnCl2-NH4Cl system by anodic stripping voltammetry was established without pre-separation. The influence of Cu2+ on the determination of Pb2+ was eliminated using ethylene diamine tetraacetic acid (EDTA) and sulfosalicylic acid as masking agent. The optimal determination conditions were as follows: the scanning potential was -0.80~-0.30 V, the enrichment potential was -0.85 V, the enrichment time was 100 s, and the scanning rate was 0.015 V/s. Pb2+ and Cd2+ showed sensitive stripping peaks at -0.48 V and -0.68 V, respectively. The common ions in solution had no interference with the determination. The concentration of Pb2+ and Cd2+ in range of 9.7×10-9-2.4×10-4 and 1.8×10-8-8.9×10-5 mol/L showed good linearity to the peak current. The correlation coefficient was 0.995 and 0.998, respectively. The detection limit of Pb2+ and Cd2+ was 3.9×10-9 and 1.9×10-9 mol/L, respectively. The content of Pb2+ and Cd2+ in ZnSO4 electrolyte and ZnCl2-NH4Cl electrolyte was determined by the proposed method. The relative standard deviation (RSD, n=6) was 0.83%-2.1% and 0.56%-0.75%, and the recoveries were 89%-108% and 92%-104%, respectively.
慕鹏涛,沈庆峰,俞小花,徐双全,刘春侠. 阳极溶出伏安法测定氯化锌-氯化铵电解制锌体系中铅和镉[J]. 冶金分析, 2016, 36(4): 17-22.
MU Peng-tao,SHEN Qing-feng,YU Xiao-hua,XU Shuang-quan,LIU Chun-xia. Determination of lead and cadmium in zinc chloride-ammonium chloride electrolyte system by anodic stripping voltammetry. , 2016, 36(4): 17-22.
Saba A E,Elsherief A E.Continuous electrowinning of zinc[J].Hydrometallurgy,2000(54):91-106.
[2]
尚美洁.可提高热镀锌产品质量的助镀剂改善工艺[J].表面工程资讯,2014(4):10-11.SHANG Mei-jie.The quality of products galvanized fluxing agent to improve the process[J].Information of Surface Engineering,2014(4):10-11.
[3]
戴桂元,胡涛,王玉成.2-甲基-3-羟基吡啶的合成研究[J].化学试剂,2001,23(6):370-371.DAI Gui-yuan,HU Tao,WANG Yu-cheng.Synthesis of 2-methyl-3-hydroxylpyridine[J].Chemical Reagents,2001,23(6):370-371.
[4]
徐维普,吴毅雄,刘秀忠,等.锌铝合金的钎焊研究[J].机械工程材料,2004,28(7):32-34.XU Wei-pu,WU Yi-xiong,LIU Xiu-zhong,et al.Zn-Al alloy soldering[J].Materials for Mechanical Engineering,2004,28(7):32-34.
[5]
邓良勋,吴保庆.氯化锌氨络合物制锌新工艺的工业化实践[J].有色金属:冶炼部分,2011(4):14-15.DENG Liang-xun,WU Bao-qing.Industrialization of new process to electrolysis zinc from zinc chloride and ammonia complex[J].Nonferrous Metals:Extractive Metallurgy,2011(4):14-15.
裴如俊,郭玉敏,张丽.氢化物发生-原子荧光光谱法测定废水中痕量铅[J].中国环境监测,2000,16(3):30-31.PEI Ru-jun,GUO Yu-min,ZHANG Li.Determination of trace lead in wastewater sample by hydride generation-atomic fluorescence spectrometry[J]. Environmental Monitoring in China,2000,16(3):30-31.
[9]
杨国武,王明海,李杰,等.氢化物发生-原子荧光光谱法测定镀锌板镀层中痕量镉[J].冶金分析,2009,29(10):32-35.YANG Guo-wu,WANG Ming-hai,LI Jie,et al. Determination of trace cadmium in the coating of galvanized plate by hydride generation atomic fluorescence spectrometry[J].Metallurgical Analysis,2009,29(10):32-35.
[10]
张宁,郭秀平,李星,等.巯基棉分离富集ICP-AES法测定高盐冶金废水中痕量铅镉铜银[J].岩矿测试,2014,33(4):551-555.ZHANG Ning,GUO Xiu-ping,LI Xing,et al.Determination of trace amounts of Pb,Cd,Cu and Ag in high salinity water by ICP-AES with sulfhydryl cotton separation and preconcentration[J].Rock and Mineral Analysis,2014,33(4):551-555.
[11]
姚春毅,马育松,贾海涛,等.微波消解-电感耦合等离子体质谱法测定煤炭中铅镉铬砷汞铍[J].冶金分析,2014,34(8):22-26.YAO Chun-yi,MA Yu-song,JIA Hai-tao,et al.Determination of lead,cadmium,chromium,arsenic,mercury and beryllium in coals by inductively coupled plasma mass spectrometry with microwave digestion[J].Metallurgical Analysis,2014,34(8):22-26.
[12]
朱正鑫,张宗才,张志华,等.阳极溶出伏安极谱法测定皮革中铅含量的研究[J].皮革科学与工程,2011,21(5):51-55.ZHU Zheng-xin,ZHANG Zong-cai,ZHANG Zhi-hua,et al.Study on determination of lead content in leather with anodic dissolution current-voltage polarography[J].Leather Science and Engineering,2011,21(5):51-55.
[13]
王燕凤,张旭,梁龙伟,等.阳极溶出伏安法同时测定锌电解液中微量镉和铅[J].矿冶,2012,21(2):111-114.WANG Yan-feng,ZHANG Xu,LIANG Long-wei,et al.Simultaneous determination of trace Cd and Pb in zinc electrolyte by anodic stripping voltammetry[J].Mining and Metallurgy,2012,21(2):111-114.
[14]
邓克.硫酸锌中微量铅镉的极谱法连续测定[J].科技创新导报,2008(34):4-5.DENG Ke.Successive determination of trace lead and cadmium in zinc sulfate by polarography[J].Science and Technology Innovation Herald,2008(34):4-5.
[15]
Ensafi A A,Khayamian T,Benvidi A,et al. Simultaneous determination of copper, lead and cadmium by cathodic adsorptive stripping voltammetry using artificial neural network[J].Analytica Chimica Acta,2006(1):225-232.