分光光度法和光度滴定法联合测定湿法炼锌流程中钴渣浸出液中锌钴镍
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摘要
湿法炼锌流程中钴渣浸出液中含有高浓度的Fe~(2+)和Mn~(2+),用分光光度法测定Co~(2+)和Ni~(2+)时,Fe~(2+)-EDTA会严重干扰Co~(2+)和Ni~(2+)的测定;在用光度滴定法测定Zn~(2+)和Co~(2+)合量时,Ni~(2+)对二甲酚橙指示剂具有封闭作用,Mn~(2+)亦与EDTA螯合,导致滴定结果偏高。为消除Fe~(2+)和Mn~(2+)对Zn~(2+)、Co~(2+)和Ni~(2+)测定的干扰,实验进行氧化分离Fe~(2+)和Mn~(2+)预处理,在NaAc/Hac缓冲体系下,以EDTA作显色剂用分光光度法测定Co~(2+)、Ni~(2+)。在波长466nm处,Co~(2+)的线性范围为50～500mg/L时与吸光度呈线性,相关系数R2为0.999 2;在384nm处,Ni~(2+)的线性范围为50～500mg/L时与吸光度呈线性,相关系数R2为0.999 8。根据分光光度法测出Ni~(2+)物质的量,加入1.1倍的丁二酮肟以除去Ni~(2+),用二甲酚橙为指示剂,EDTA鳌合-光度滴定法测定Zn~(2+)、Co~(2+)合量,扣减Co~(2+)含量得出Zn~(2+)含量。选取4个锌湿法炼锌流程中钴渣浸出液实际样品,按照实验方法中的分光光度法测定Co~(2+)和Ni~(2+),光度滴定法测定Zn~(2+)、Co~(2+)合量,Zn~(2+)、Co~(2+)和Ni~(2+)测定结果的相对标准偏差(RSD,n=6)均不大于0.70%,加标回收率分别为99.59%～100.41%、99.69%～100.64%、99.92%～100.08%。
The cobalt residue leaching solution in zinc hydrometallurgy contained high concentrations of Fe~(2+)and Mn~(2+).During the determination of Co~(2+)and Ni~(2+)by spectrophotometry,Fe~(2+)-EDTA had serious interference.On the other hand,when the total content of Zn~(2+)and Co~(2+)was determined by photometric titration,Ni~(2+)had blocking effect of xylenol orange indicator and Mn~(2+)could chelate with EDTA,resulting in higher titration results.In order to eliminate the interference of Fe~(2+)and Mn~(2+)on the determination of Zn~(2+),Co~(2+)and Ni~(2+),the pretreatment of Fe~(2+)and Mn~(2+)was conducted by oxidization separation in experiments.Co~(2+)and Ni~(2+)were determined by spectrophotometry using EDTA as coloring reagent in NaAc/HAc buffer solution.The concentration of Co~(2+)in range of 50-500 mg/L was linear to the absorbance at 466 nm and the correlation coefficient was R2=0.999 2.The concentration of Ni~(2+)in range of 50-500 mg/L was linear to the absorbance at 384 nm and the correlation coefficient was R2=0.999 8.The molar amount of Ni~(2+)was determined by spectrophotometry.Then Ni~(2+)was removed by adding 1.1 times of dimethylglyoxime.The total content of Zn~(2+)and Co~(2+)was determined by EDTA chelation-photometric titration using xylenol orange as indicator.The content of Zn~(2+)was calculated by deducting the content of Co~(2+).Four actual samples of cobalt residue leaching solution in zinc hydrometallurgy were selected.The content of Co~(2+)and Ni~(2+)was determined by spectrophotometry according to the experimental method.The total content of Zn~(2+)and Co~(2+)was determined by photometric titration.The relative standard deviations(RSD,n=6)of Zn~(2+),Co~(2+)and Ni~(2+)were all less than 0.70%.The spiked recoveries were 99.59%-100.41%,99.69%-100.64%and 99.92%-100.08%,respectively.
The cobalt residue leaching solution in zinc hydrometallurgy contained high concentrations of Fe~(2+)and Mn~(2+).During the determination of Co~(2+)and Ni~(2+)by spectrophotometry,Fe~(2+)-EDTA had serious interference.On the other hand,when the total content of Zn~(2+)and Co~(2+)was determined by photometric titration,Ni~(2+)had blocking effect of xylenol orange indicator and Mn~(2+)could chelate with EDTA,resulting in higher titration results.In order to eliminate the interference of Fe~(2+)and Mn~(2+)on the determination of Zn~(2+),Co~(2+)and Ni~(2+),the pretreatment of Fe~(2+)and Mn~(2+)was conducted by oxidization separation in experiments.Co~(2+)and Ni~(2+)were determined by spectrophotometry using EDTA as coloring reagent in NaAc/HAc buffer solution.The concentration of Co~(2+)in range of 50-500 mg/L was linear to the absorbance at 466 nm and the correlation coefficient was R2=0.999 2.The concentration of Ni~(2+)in range of 50-500 mg/L was linear to the absorbance at 384 nm and the correlation coefficient was R2=0.999 8.The molar amount of Ni~(2+)was determined by spectrophotometry.Then Ni~(2+)was removed by adding 1.1 times of dimethylglyoxime.The total content of Zn~(2+)and Co~(2+)was determined by EDTA chelation-photometric titration using xylenol orange as indicator.The content of Zn~(2+)was calculated by deducting the content of Co~(2+).Four actual samples of cobalt residue leaching solution in zinc hydrometallurgy were selected.The content of Co~(2+)and Ni~(2+)was determined by spectrophotometry according to the experimental method.The total content of Zn~(2+)and Co~(2+)was determined by photometric titration.The relative standard deviations(RSD,n=6)of Zn~(2+),Co~(2+)and Ni~(2+)were all less than 0.70%.The spiked recoveries were 99.59%-100.41%,99.69%-100.64%and 99.92%-100.08%,respectively.
引文
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[11]赵景波.浅议分析化学配位滴定法的教学要点[J].安徽化工(Anhui Chemical Industry),2018,44(4):119-120.
[12]中华人民共和国环境保护部.HJ168-2010环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.
[2]齐妍洁,张旭,沈庆峰,等.亚硝基R盐分光光度法测定硫酸锌溶液中的钴[J].矿冶,2014,23(4):97-100.QI Yan-jie,ZHANG Xu,SHEN Qing-feng,et al.Determination of cobalt in zinc sulfate solution by nitroso R salt spectrophotometry[J].Mining&Metallurgy,2014,23(4):97-100.
[3]刘和连,许方,黄海平.EDTA络合滴定法测定黄铜中铜和锌[J].冶金分析,2015,35(5):70-73.LIU He-lian,XU Fang,HUANG Hai-ping.Determination of copper and zinc in brass by EDTA complexometric titration[J].Metallurgical Analysis,2015,35(5):70-73.
[4]Sen R.Complexometric determination of zinc oxide in glass and ceramic materials[J].Taylor&Francis,2014,5(21):89-92.
[5]孙彬彬,童俊,鹿慧,等.EDTA滴定法结合酸碱滴定法用于碱液中锌、锡的联合测定以及游离碱的测定[J].冶金分析,2018,38(5):54-59.SUN Bin-bin,TONG Jun,LU Hui,et al.Application of EDTA titration combined with acid base titration in simultaneous determination of zinc and tin in alkaline solution as well as determination of free alkali[J].Metallurgical Analysis,2018,38(5):54-59.
[6]江荆,魏雅娟,邬景荣,等.丁二酮肟沉淀分离-EDTA滴定法测定含镍锌物料中的锌[J].冶金分析,2016,36(11):62-66.JIANG Jing,WEI Ya-juan,WU Jing-rong,et al.Determination of zinc in nickel-containing zinc materials by ED-TA titration[J].Metallurgical Analysis,2016,36(11):62-66.
[7]孙淑媛,孙龄高,殷齐西,等.矿石及有色金属分析手册[M].北京:冶金工业出版社,1990.
[8]Adela B B,Pilar B B,F B M.Simultaneous determination of copper and cobalt with EDTA using derivative spectrop hotometry[J].Talanta,1985,110(11):1313-1315.
[9]陈闽子,李阿丹,佟琦.镍铁合金镀液中Ni 2+含量的光度测定[J].冶金分析,2002,22(6):54-55.CHEN Min-zi,LI A-dan,TONG Qi.Photometric determination of Ni 2+content in nickel-iron alloy plating bath[J].Metallurgical Analysis,2002,22(6):54-55.
[10]Leo G,Peter A B,Marcus V K.Practical titration[EB/OL].28-29(2005-05)[2018-1-20].https://www.metrohm.com/en/documents/80295003.
[11]赵景波.浅议分析化学配位滴定法的教学要点[J].安徽化工(Anhui Chemical Industry),2018,44(4):119-120.
[12]中华人民共和国环境保护部.HJ168-2010环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.