Catalytic-Kinetic Potentiometric Determination of Trace Amount of Vanadium After Anion Exchange Separation
摘 要
研究了在稀硫酸介质中,以痕量钒(Ⅴ)催化溴酸钾氧化碘化钾的反应为指示反应,用碘离子选择电极跟踪I-,建立了催化动力学电位法测定钒的方法.在一定的条件下,该指示反应为一级反应,反应速度可用电位的变化ΔE表示.当时间固定,ΔE与钒(Ⅴ)浓度在0.015~0.1 mg·L-1范围内呈线性关系.方法的检出限为3.2×10-7g·L-1.该法可用于钢铁样品中钒的测定,试样溶液中钒(VO3-4)预先从弱碱性溶液中(pH 7.0~8.2)用强碱性阴离子交换树脂分离.用1.0 mol·L-1硫酸从树脂上将钒(Ⅴ)洗脱后按所述方法测定.测定结果与标准值相符,相对标准偏差小于5%.
Abstract
In a dil.H2SO4 medium,the oxidation of I- ion by KBrO3 was catalyzed by trace amount of vanadium(Ⅴ),and the potentiol change of I2/I-3 was detected by iodide ion selective electrode.It was found that the difference of potentials between the non-catalyzed reaction and catalyzed reaction (ΔE=E0-Et) was kept in linear relationship with the concentration of vanadium(Ⅴ) in the range from 0.015-0.10 mg of V(Ⅴ) per L,with a detection limit of 3.2×10-7g·L-1.It was also shown that the catalytic reaction was a 1st-order reaction,and its rate of reaction was expressed by ΔE.In its application to the determination of vanadium in steel samples,a preliminary anion ion-exchange separation of vanadium as VO3-4 on 717 strong-basic anion exchange resin from a slightly basic solution of pH 7.0-8.2.The vanadium (VO3-4) was eluted from the resin with 1.0 mol·L-1 H2SO4,and determined by the proposed method.The results obtained were checked quite well with the standard values,and values of RSD′s (n=9) were less than 5%.
中图分类号 O657.31
所属栏目 工作简报
基金项目 山东省博士基金(NO.2002BS0501)
收稿日期 2006/12/5
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备注李慧芝(1962-),女,吉林长春人,教授,主要从事分离富集及微量分析的研究.
引用该论文: LI Hui-zhi,FAN Rong,ZHAI Dian-tang,DU Xu. Catalytic-Kinetic Potentiometric Determination of Trace Amount of Vanadium After Anion Exchange Separation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(2): 131~133
李慧芝,范荣,翟殿棠,杜旭. 离子交换树脂分离富集催化动力学电位法测定痕量钒[J]. 理化检验-化学分册, 2008, 44(2): 131~133
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参考文献
【1】江天肃,翟庆洲.钒(Ⅴ)-三溴偶氮胂-溴酸钾催化动力学光度法测定钒[J].分析化学,2003,31(7):895.
【2】李志梅,陈国树.催化动力学光度法测定痕量钒(Ⅴ)[J].南昌大学学报:理科版,2003,27(2):144-1447.
【3】刘长增,韩长秀.钒(Ⅴ)催化氧化二甲基黄的反应及其应用[J].理化检验-化学分册,2002,38(11):558-560.
【4】孙炳耀,张欣欣.溴酸钾-碘离子体系催化动力学电位法测定痕量铜[J].分析化学,1997,25(6):696-699.
【5】程伟,孙炳耀.碘酸钾-碘离子体系催化动力学电位法测定痕量铜[J].郑州大学学报:自然科学版,2000,32(2):78-80.
【6】赖晓绮,薛君,黄承玲.催化动力学电位法测定痕量亚硝酸根[J].分析科学学报,2002,18(4):294-296.
【2】李志梅,陈国树.催化动力学光度法测定痕量钒(Ⅴ)[J].南昌大学学报:理科版,2003,27(2):144-1447.
【3】刘长增,韩长秀.钒(Ⅴ)催化氧化二甲基黄的反应及其应用[J].理化检验-化学分册,2002,38(11):558-560.
【4】孙炳耀,张欣欣.溴酸钾-碘离子体系催化动力学电位法测定痕量铜[J].分析化学,1997,25(6):696-699.
【5】程伟,孙炳耀.碘酸钾-碘离子体系催化动力学电位法测定痕量铜[J].郑州大学学报:自然科学版,2000,32(2):78-80.
【6】赖晓绮,薛君,黄承玲.催化动力学电位法测定痕量亚硝酸根[J].分析科学学报,2002,18(4):294-296.
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