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Confirmation of vanadium complex formation using electrospray mass spectrometry and determination of vanadium speciation by sample stacking capillary electrophoresis
Authors:Chen ZuLiang  Owens Gary  Naidu Ravendra
Institution:a Centre for Environmental Risk Assessment and Remediation, University of South Australia, Mawson Lakes, SA 5095, Australia
b CRC for Contamination Assessment and Remediation of Environments, Mawson Lakes Boulevard, Mawson Lakes, SA 5095, Australia
Abstract:Capillary zone electrophoresis (CZE) with UV detection was used to determine vanadium species. Nitrilotriacetic acid (NTA), hydroxyethylethylenediaminetriacetic acid (HEDTA), ethylenediaminetetraacetic acid (EDTA), diethylenetriaminepentaacetic acid (DTPA), ethylene glycol-bis(2-aminoethylether)-tetraacetic acid (EGTA) and 2,6-pyridinedicarboxylic acid (PDCA) were investigated to determine whether these ligands formed stable anionic complexes with vanadium. Of all the ligands studied HEDTA was the most suitable ligand because it gave the largest UV response with reasonable migration time. Electrospray mass spectrometry (ES-MS) was used to confirm the formation of VO2(HEDTA)]2− and VO(HEDTA)]1− in solution. An electrolyte containing 25 mM phosphate, 0.25 mM tetradecyltrimethylammonium bromide (TTAB) at pH 5.5 was optimum for the separation of these anionic vanadium complexes. Sample stacking techniques, including large-volume sample stacking (LVSS) and field-amplified sample injection (FASI), were tested to improve the sensitivity. Best sensitivity was obtained using FASI, with detection limits of 0.001 μM, equivalent to 0.4 μg L−1, for VO2(HEDTA)]2− and 0.01 μM, equivalent to 3.4 μg L−1 for VO(HEDTA)]1−. The utility of the method for the speciation of V(IV) and V(V) was demonstrated using ground water samples.
Keywords:Capillary zone electrophoresis  Vanadium speciation  Electrospray mass spectrometry  Sample stacking techniques
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