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Flow injection-liquid chromatography-cold vapour atomic absorption spectrometry for rapid determination of methyl- and inorganic mercury
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2000 (English)In: The Analyst, ISSN 0003-2654, E-ISSN 1364-5528, Vol. 125, no 6, 1193-1197 p.Article in journal (Refereed) Published
Abstract [en]

A previously described system for determining low concentrations of mercury species in environmental samples using flow injection high-performance liquid chromatography cold vapour atomic absorption spectrometry (FI-HPLC-CVAAS) has been further developed with respect to time of analysis, long term signal stability, memory effects, detection limits, and environmental friendliness. Methyl and inorganic mercury were determined without pre-treatment in brackish water and in digested biological certified reference materials, DOLT-2 and TORT-2. Results were compared with those obtained by gas chromatography microwave-induced plasma atomic emission spectroscopy (GC-MIP-AES) using either butylation with a Grignard reagent or ethylation with sodium tetraethylborate. With the FI-HPLC-CVAAS system, absolute detection limits are 1.7 pg and 3.4 pg for methyl and inorganic mercury, respectively. Mercury species in a sample can be determined at the 0.4 ng l−1 level within 5 min. For lower concentrations the time for analysis has to be increased.

Place, publisher, year, edition, pages
RSC Publishing, 2000. Vol. 125, no 6, 1193-1197 p.
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:umu:diva-2293DOI: 10.1039/B000933OOAI: oai:DiVA.org:umu-2293DiVA: diva2:140228
Available from: 2003-09-25 Created: 2003-09-25 Last updated: 2012-06-27Bibliographically approved
In thesis
1. On the reliability of methods for the speciation of mercury based on chromatographic separation coupled to atomic spectrometric detection
Open this publication in new window or tab >>On the reliability of methods for the speciation of mercury based on chromatographic separation coupled to atomic spectrometric detection
2003 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis deals with the reliability of methods for the speciation of mercury in environmental and biological samples. Problems with speciation methods that couple chromatography to atomic spectrometric detection and how to overcome the problems are discussed. Analytical techniques primarily studied and evaluated are high performance liquid chromatography-cold vapour-atomic absorption spectrometry (HPLC-CV-AAS), HPLC-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), capillary electrophoresis-ICP-MS (CE-ICP-MS) and gas chromatography-ICP-MS (GC-ICP-MS). Applying a multi-capillary approach increased the analyte amount injected into a CE-ICP-MS system and improved the overall sensitivity. A microconcentric nebulizer with a cyclone spray chamber was shown to improve the detection limits for mercury species 3-13 times in HPLC-ICP-MS and 11-19 times in CE-ICP-MS compared to a cross-flow nebulizer with a Scott spray chamber. To decrease the interference of water vapour in HPLC-CV-AAS a Nafion dryer tube was inserted between the CV-generation and the detector. Methyl mercury was however lost in the Nafion unless it was reduced to elemental mercury prior transport through the dryer tube.

During sample pre-treatment, incomplete extraction, losses and transformation (alkylation, dealkylation, oxidation and reduction) of mercury species can lead to significant errors (underestimation and overestimation) in the determination of the concentrations. Methods to detect and determine the degree of transformation as well as correct for errors caused by transformation are presented in the thesis. The preferable method use species-specific enriched stable isotope standards in combination with MS detection and a matrix based calculation scheme. This approach is very powerful as both the concentrations of the species as well as the degrees of transformation can be determined within each individual sample.

Publisher
35 p.
Keyword
Analytical chemistry, Mercury, speciation, hyphenated techniques, HPLC, CE, GC, CV-AAS, ICP-MS, species-specific enriched stable isotope, Analytisk kemi
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:umu:diva-111 (URN)91-7305-429-1 (ISBN)
Public defence
2003-05-23, Umeå, 13:00 (English)
Available from: 2003-09-25 Created: 2003-09-25 Last updated: 2009-05-25Bibliographically approved

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Frech, Wolfgang

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