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采用直接紫外检测的毛细管电泳法对钒(IV)和钒(V)进行柱上络合及同步分离。

On-column complexation and simultaneous separation of vanadium(IV) and vanadium(V) by capillary electrophoresis with direct UV detection.

作者信息

Chen ZuLiang, Naidu Ravendra

机构信息

CSIRO Land and Water, Adelaide Laboratory, PMB2, Glen Osmond SA 5064, Australia.

出版信息

Anal Bioanal Chem. 2002 Oct;374(3):520-5. doi: 10.1007/s00216-002-1456-y. Epub 2002 Sep 14.

Abstract

An on-column complexation method has been developed for the simultaneous determination of V(IV) and V(V). Vanadium species were chelated with aminopolycarboxylic acids to form anionic complexes which were separated by capillary zone electrophoresis (CZE) with direct UV detection. Ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentacetric acid (DTPA), nitrilotriacetic acid (NTA), and N-2-hydroxyethylethlendiaminetriacetric acid (HEDTA) were investigated as both ligand and running electrolyte. Of the ligands studied the complexes of EDTA with V(IV) and V(V) resulted in the highest selectivity and UV response. The conditions used for on-column complexation and separation, including pH, and electrolyte ligand concentration, were examined to achieve reasonable separation selectivity and detection sensitivity. The optimum separation of the anionic forms of V(IV) and V(V) was obtained by use of CZE with UV detection at 185 nm and an electrolyte containing 5 mmol L(-1) EDTA at pH 4.0. Linear calibration plots were obtained in the concentration range10-300 micro mol L(-1); detection limits were 3 micro mol L(-1) for V(IV) and 1 micro mol L(-1) for V(V). The proposed method was demonstrated for the determination of vanadium in groundwater spiked with V(IV) and V(V).

摘要

已开发出一种柱上络合方法用于同时测定V(IV)和V(V)。钒物种与氨基多羧酸螯合形成阴离子络合物,通过毛细管区带电泳(CZE)结合直接紫外检测进行分离。研究了乙二胺四乙酸(EDTA)、二乙烯三胺五乙酸(DTPA)、次氮基三乙酸(NTA)和N-(2-羟乙基)乙二胺三乙酸(HEDTA)作为配体和运行电解质的情况。在所研究的配体中,EDTA与V(IV)和V(V)的络合物具有最高的选择性和紫外响应。考察了用于柱上络合和分离的条件,包括pH值和电解质配体浓度,以实现合理的分离选择性和检测灵敏度。通过使用CZE在185 nm处进行紫外检测以及在pH 4.0下含有5 mmol L⁻¹ EDTA的电解质,实现了V(IV)和V(V)阴离子形式的最佳分离。在10 - 300 μmol L⁻¹浓度范围内获得了线性校准曲线;V(IV)的检测限为3 μmol L⁻¹,V(V)的检测限为1 μmol L⁻¹。该方法被用于测定添加了V(IV)和V(V)的地下水中的钒。

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