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Study On Strong Base Ion Exchange Fiber Separation For Determination Of Iron?Ainc?Gold In Pure Copper And Copper Compounds By Atomic Spectrometry

Posted on:2013-05-03Degree:MasterType:Thesis
Country:ChinaCandidate:L ChenFull Text:PDF
GTID:2381330545967611Subject:Analytical Chemistry
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This paper reviewed the current situation and development of separation and determination of the trace elements in high purity at home and aboard.Combined ICP-AES and FAAS,using the strong base ion exchange fiber as the separating materials,the separation and analysis of iron?zine?gold in pure copper and copper compounds were investigated.1.The influence of concentration of chloride ions on the adsorption of Cu(?),Fe(?),Zn(?)and Au(?)by strong base ion exchange fiber,and the effect of temperature on the adsorption performance were discussed.The results showed that when the concentration of chloride ions was 1.0 mol·L-1,the strong base ion exchange fiber could absorb Zn(?)and Au(?)stably,and when the concentration of chloride ions was greater than 5.0 mol·L-1,the strong base ion exchange fiber could absorb Cu(?)and Fe(?)stably.With the temperature increases,the saturated adsorption capacity of each complex anions increased,and the absorption equilibrium time of complex anions decreased.2.A new method has been established for separation and analysis of Fe in pure copper and copper compounds based on solid phase extraction combined with inductive coupled plasma emission spectrometry(ICP-AES).The research indicated that when the amount of Cu was 100 times more than Fe,the interference of Cu on determination Fe using ICP-AES was obviously,therefore,before determination of Fe in copper and copper compounds,the step of separation Fe and Cu matrix was necessaiy.In this paper,in the 6.0 mol·L-1 HCl medium,Fe(?)was adsorped by the strong base ion exchange fiber completely,then the Fe(?)adsorpted on the SBIEF was eluted by the 1.0 mol·L-1 HCl,so the interferences of determination Fe(?)was removed.The recoveries of Fe were in the range of 96?103%,the RSD of Fe were 2.3?4.2%.The detection limit of the method was 0.011 ?g·mL-1.3.Combined with FAAS,the application of strong base ion exchange fiber for determination of Fe in copper and copper compounds was studied.The result showed that when the amount of Cu was 70 times more than Fe,the relative deviation of determining Fe was 5%beyond.Therefore,before determination of Fe the Cu must be removed.The strong base ion exchange fiber was used as separation media,the flow rate of sample liquid and 3.0 mol·L-1 HCl as eluent was 2.0 mL·min-1,Cu(?)was eluted first,and then the Fe(?)outflow liquid was collected.So the Interference of Cu(?)was removed.The effect of SO42-in solution was investigated.When the concentration of SO42-in solution was range from 0.2 to 1.0 mol·L-1,its no influence on the separation.After being separated by strong base ion exchange fiber,the detection limit of determining Fe by FAAS was 0.021 ?g·mL-1.The method was applied on determination of Fe in high pure eusO4·SH2O,the content of Fe was 7.35?g·g-1,the recoveries of standard addition were 95.9?103%,and the RSD(n=3)were 0.1?1.1%.4.Combined with ICP-AES,the method of separation and determination of Zn?Au in high pure CuSO4·5H2O based on the application of strong base ion exchange fiber was researched.The research showed that when the mass concentration ratio ?Cu2+:?zn2+>50,the relative deviation of determining Zn using ICP-AES was 5%beyond;when the mass concentration ratio ?cu2+:?Au3+>30,the relative deviation of determining Au using ICP-AES was 5%beyond.Therefore,the Cu has to be removed before determining Zn and Au.The strong base ion exchange fiber was used as separation media,the flow rate of sample liquid was 1.0mL·min-1,then the Cu(?)was eluted by 1.0mol·L-1 HCl with the same flow rate;after eluting the Cu(?),0.01 mol·L-1 HNO3 was used to elute the Zn(?);at last,the Au(?)was eluted with the mixed solution of 30mg·mL-1 thiourea and 0.lmol·L-1 sulfuric acid,so the interference was removed.The effect of SO42-in solution was investigated.When the concentration of SO42-in solution was range from 0.2 to 1.0 mol·L-1,its no influence on the separation.After the separation,the method limit detection of Zn by ICP-AES was 0.006?g·mL-1,the method limit detection of Au by ICP-AES was 0.018?g·mL-1.The method was applied on determination of Zn and.Au in CuSO4·5H2O.The result was that the content of Zn in CuSO·5H2O was 5.57?g·g-1,the recoveries of standard addition were 96.6?98.6%,and the RSD(n=5)were 1.6?2.3%.The content of Au in CuSo4·5H2O was 0.97?g·g-1,the recoveries of standard addition were 95.9?97.9%,and the RSD(n=5)were 0.8?1.9%.
Keywords/Search Tags:strong base ion exchange fiber, solid phase extraction, micro-column separation, iron, zinc, gold, inductive coupled plasma emission spectrometry(ICP-AES), Flame atomic absorption spectrometry(FAAS)
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