首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >LIMITATIONS OF ION CHROMATOGRAPHY WITH POST-COLUMN REACTION FOR DETERMINATION OF HEAVY METALS IN WATERS CONTAINING STRONG CHELATING AGENTS
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LIMITATIONS OF ION CHROMATOGRAPHY WITH POST-COLUMN REACTION FOR DETERMINATION OF HEAVY METALS IN WATERS CONTAINING STRONG CHELATING AGENTS

机译:柱色谱后测定强螯合剂水中重金属的离子色谱法的局限性

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A published method for the determination of heavy metals was applied to the determination of Cu(II), Ni(II), Zn(II) and Mn(II) in synthetic solutions that contained one of the following ligands (L): citrate, nitrilotriacetate (NTA), ethylenediaminetetraacetate acid (EDTA) and cyclohexylenediaminetetraacetate (CDTA). The method involves on-column derivatization with 2,6-pyridinedicarboxylic acid (PDCA) and ion-exchange separation, followed by post-column reaction with 4-(2-pyridylazo)resorcinol (PAR) to form metal-PAR chelates, which can be sensitively monitored by spectrophotometric detection at 520 nm. Solutions with 12.6 mu mol/l of Cu(II), Ni(II), Zn(II) and Mn(II) and 12.6 or 25.2 mu mol/l of L were analysed. A 100% recovery was obtained for all metals with citrate or NTA, for Cu(II), Zn(II) and Mn(II) with EDTA and only for Mn(II) with CDTA. The recoveries in further cases were Ni(II)-EDTA less than or equal to 68%, NI-CDTA less than or equal to 80%, Cu(II)-CDTA less than or equal to 20% and Zn(II)-CDTA less than or equal to 87%. To interpret these results, simpler solutions with 12.6 or 6.3 mu mol/l Cu(II) and Cu:L ratios (R) in the range 4.2-0.26 were analysed. For both citrate and NTA an almost 100% recovery of Cu(II) was found for all values of R. For EDTA, 100% recovery was only observed for R greater than or equal to 1.0. For CDTA the recoveries were between 76% (R = 4.2) and 0% (R less than or equal to 0.52). Speciation calculations showed that only kinetic factors were responsible for the inefficiency of both the on-column and the post-column derivatizations. Analytical implications of the results are discussed. [References: 17]
机译:已发布的测定重金属的方法用于测定含有以下配体(L)之一的合成溶液中的Cu(II),Ni(II),Zn(II)和Mn(II)。亚硝基三乙酸酯(NTA),乙二胺四乙酸(EDTA)和环己二胺四乙酸(CDTA)。该方法涉及用2,6-吡啶二甲酸(PDCA)进行柱上衍生化和离子交换分离,然后与4-(2-吡啶基偶氮)间苯二酚(PAR)进行柱后反应以形成金属PAR螯合物,通过分光光度法在520 nm处进行灵敏监测。分析了具有12.6 mol / l的Cu(II),Ni(II),Zn(II)和Mn(II)以及12.6或25.2 mol / l的L的溶液。对于使用柠檬酸盐或NTA的所有金属,使用EDTA的Cu(II),Zn(II)和Mn(II)以及仅使用CDTA的Mn(II),获得100%的回收率。在其他情况下,回收率分别为Ni(II)-EDTA小于或等于68%,NI-CDTA小于或等于80%,Cu(II)-CDTA小于或等于20%和Zn(II)- CDTA小于或等于87%。为了解释这些结果,分析了具有12.6或6.3μmol/ l的Cu(II)和Cu:L比率(R)在4.2-0.26范围内的简单溶液。对于柠檬酸盐和NTA,对于所有R值,Cu(II)的回收率均接近100%。对于EDTA,仅当R大于或等于1.0时,观察到100%的回收率。对于CDTA,回收率在76%(R = 4.2)和0%(R小于或等于0.52)之间。形态计算表明,仅动力学因素是造成柱上和柱后衍生化效率低下的原因。讨论了结果的分析意义。 [参考:17]

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