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Preparation and certification of ERM-AE670, a 202Hg enriched methylmercury isotopic reference material
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
Umeå University, Faculty of Science and Technology, Chemistry.
2004 (English)In: JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, ISSN 0267-9477, Vol. 19, no 10, 1315-24 p.Article in journal (Refereed) Published
Abstract [en]

The need for comparability of methylmercury, noted MeHg, measurement results and for the reduction of their associated uncertainties is hampered by the lack of suitable calibration materials. An isotopic certified reference material, ICRM, of MeHg containing isotopically enriched Hg has the potential to answer these problems, in combination with the isotope dilution mass spectrometry, IDMS, strategy. The objective of this work was to produce such a material, of demonstrated stability and carrying certified values traceable to the SI accompanied by combined uncertainty statements. Mercury oxide enriched in 202Hg was used for the preparation of a solution of 202Hg enriched CH3HgCl. The starting material had previously been employed for the preparation of ERM-AE640; a 202Hg enriched inorganic mercury ICRM. The CH3HgCl was synthesised by reaction with a Grignard reagent and a subsequent comproportionation reaction between (CH3)2Hg and HgCl2. The process was optimised to give a high yield of the product, minimise contamination with naturalHg and additional steps were applied to purify the material from other Hg species and by-products of the synthesis reaction. Aliquots of 5 g of the solution were sealed in quartz ampoules for later distribution as a reference material, named ERM-AE670. Using gas chromatography inductively coupled plasma mass spectrometry, only MeHg and inorganic Hg was detectable in the finished reference material with inorganic Hg in <2% of the total amount. The isotopic composition of Hg in the form of MeHg was confirmed to be identical to that of ERM-AE640, within enlarged uncertainty statements. The Hg amount content in the form of MeHg was obtained by subtraction of the inorganic Hg amount content from the total Hg amount content (determined by IDMS in the digested material). The final uncertainty on the Hg amount content in the form of MeHg (3.5% relative, k= 2) included a contribution covering for potential changes over 2 years of shelf-life. This contribution was estimated from the results of a 1 year isochronous stability study.

Place, publisher, year, edition, pages
2004. Vol. 19, no 10, 1315-24 p.
URN: urn:nbn:se:umu:diva-14247DOI: doi:10.1039/b407368aOAI: diva2:153918
Available from: 2007-05-25 Created: 2007-05-25 Last updated: 2011-01-12Bibliographically approved
In thesis
1. Mercury species transformations in marine and biological systems studied by isotope dilution mass spectrometry and stable isotope tracers
Open this publication in new window or tab >>Mercury species transformations in marine and biological systems studied by isotope dilution mass spectrometry and stable isotope tracers
2005 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis focuses on the implementation of species-specific isotope dilution (SSID) methodology and stable isotope tracers to determine mercury species occurrence and transformation processes in-situ and during sample treatment. Isotope enriched tracers of methyl-, ethyl- and inorganic mercury were synthesised and applied in different combinations to marine and biological samples. Experimental results were obtained using gas chromatography-inductively coupled plasma-mass spectrometry (GC-ICP-MS).

Mercury methylation and methylmercury demethylation processes in surface sediments were studied in the brackish Öre River estuary, Bothnian Bay. Uni- and multivariate data evaluation identified the organic material content and mercury methylation potential in the sediments as important factors controlling incipient methylmercury levels. Mercury species distribution in mice treated with the pharmaceutical preservative Thimerosal (ethylmercurithiosalicylate) was studied. The ethylmercury moiety of Thimerosal was observed to rapidly convert to inorganic mercury in the mice during the treatment period as well as during sample treatment, hence necessitating SSID methodology for accurate ethylmercury determinations in biological samples.

To facilitate the introduction of SSID as a routine quantitative method in mercury speciation, a methylmercury isotopic certified reference material (ICRM) was produced. Prior to certification, the stability of the material was examined in conventional and isochronous stability studies spanning 12 months, which permitted uncertainty estimation of the methylmercury amount content for two years of shelf-life.

Finally, a field-adapted SSID method for methylmercury determinations in natural water samples was developed. The proposed analytical protocol significantly simplified sample storage- and treatment procedures without sacrifices in analytical accuracy.

Place, publisher, year, edition, pages
Umeå: Kemi, 2005. 38 p.
Analytical chemistry, Mercury, methylmercury, ethylmercury, Thimerosal, speciation, methylation, demethylation, brackish water sediment, natural waters, GC-ICP-MS, species-specific isotope dilution, isotope enriched tracers, Analytisk kemi
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
urn:nbn:se:umu:diva-467 (URN)91-7305-838-6 (ISBN)
Public defence
2005-04-01, KB3A9, Kemiskt Biologiskt Centrum (KBC), Umeå Universitet 90187, Umeå, 10:00 (English)
Available from: 2005-03-09 Created: 2005-03-09 Last updated: 2009-05-25Bibliographically approved

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