Change search
ReferencesLink to record
Permanent link

Direct link
Preparation, preservation and application of pure isotope-enriched phenyltin species.
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.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2006 (English)In: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 386, no 5, 1505-1513 p.Article in journal (Refereed) Published
Abstract [en]

A method combining liquid/liquid extraction and chromatographic fractionation has been developed for the preparation of pure monophenyltin (MPhT), diphenyltin (DPhT), and triphenyltin (TPhT), synthesized from isotope-enriched Sn metal using phenylation of SnI(4) in diethylether (DEE) followed by quenching with HBr and water. After two successive extractions of the aqueous HBr phase with DEE, >99% of both DPhT and TPhT was recovered in the combined DEE phase and 94% of the MPhT remained in the aqueous phase. The MPhT in the aqueous phase was extracted into dichloromethane. The organic phases were vaporized and the PhTs were redissolved in MeOH/water/acetic acid/sodium acetate (59/30/6/8, v/v/v/w), which was also used as storing solution. Aliquots of the two solutions containing either DPhT and TPhT or MPhT were injected into a silica-based C(18) column for isolating and purifying single species. The yields of pure MPhT, DPhT, and TPhT, each synthesized from isotope-enriched (118)Sn metal, (122)Sn metal, and (124)Sn metal, were better than 99%. After chromatographic separation, the single phenyltin compounds were mixed to prepare a spike for multiple-isotope species-specific isotope dilution (MI-SSID). MI-SSID was successfully used to determine phenyltin compounds in the certified reference material, mussel tissue BCR CRM-477. At -20 degrees C, all of the fractionated phenyltin species were stable in the storage solution for at least 197 days. When these standards were stored at 4 degrees C or 22 degrees C, 4-6% of the DPhT and TPhT degraded within 27 days. The degradation of DPhT and TPhT increased with the ionic strength and acidity of the storage solution.

Place, publisher, year, edition, pages
Berlin: Springer , 2006. Vol. 386, no 5, 1505-1513 p.
Keyword [en]
Chemical Fractionation/methods, Chromatography; Gas/methods, Chromatography; High Pressure Liquid/methods, Gas Chromatography-Mass Spectrometry/methods, Isotopes, Organotin Compounds/analysis/chemical synthesis, Reproducibility of Results, Sensitivity and Specificity, Time Factors
URN: urn:nbn:se:umu:diva-11788DOI: 10.1007/s00216-006-0695-8PubMedID: 16937090OAI: diva2:151459
Available from: 2007-03-09 Created: 2007-03-09 Last updated: 2011-03-14Bibliographically approved
In thesis
1. Speciation analysis of butyl- and phenyltin compounds in environmental samples by GC separation and atomic spectrometric detection
Open this publication in new window or tab >>Speciation analysis of butyl- and phenyltin compounds in environmental samples by GC separation and atomic spectrometric detection
2006 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The main goal of the work presented in this thesis is to improve the reliability of existing methods for speciation analysis of organotin compounds

Species-specific isotope dilution (SSID) calibration in combination with gas chromatography – inductively coupled plasma mass spectrometry was used to investigate the transformation of phenyltin species during sample preparation. Isotope-enriched phenyltin species were synthesized from corresponding isotope-enriched tin metals. SSID with a mixture of phenyltin species (PhTs) from one isotope was used to evaluate different extraction procedures for the determination of PhTs in fresh water sediment. Preparative liquid chromatography was used to produce single isotope-enriched phenyltin species making a multi-isotope spike (MI) SSID calibration possible. Different extraction procedures for the analysis of phenyltin species in biological samples were evaluated by applying MI-SSID. Degradation of TPhT and DPhT during sample extraction was observed and quantified. Accurate results were therefore obtained. A sample preparation procedure using mild extraction conditions with reasonable recoveries is described.

The stability of organotin standards was investigated under different storage conditions. Mono- and diphenyltin were found to be redistributed and degraded during storage in methanol but were stabilized in sodium acetate/ acetic acid. A fast redistribution between monobutyl- and diphenyl tin has been observed and therefore it is therefore recommended that standards be derivatized as soon as possible after butyl- and phenyltin standards are mixed.

Included in the thesis is also an investigation of the analytical potential of using instrumentation based on atomic absorption spectrometry (AAS) for speciation analysis of organotin compounds. The method was based on gas chromatographic separation, atomization in a quartz tube and detection by line source (LS) AAS and for comparison, by state of the art continuum source (CS) AAS. Analytical performances of CSAAS system were found to be better compared to LSAAS.

Place, publisher, year, edition, pages
Umeå: Kemi, 2006. 35 p.
Organotin speciation analysis, species-specific isotope dilution, inductively coupled plasma mass spectrometry, single isotope spike, multi-isotope spike, redistribution, species transformation, preparative liquid chromatography, gas chromatography, line source atomic absorption spectrometry, continuum source atomic absorption spectrometry
National Category
Analytical Chemistry
urn:nbn:se:umu:diva-892 (URN)91-7264-187-8 (ISBN)
Public defence
2006-11-03, KBC3A9, KBC, Department of Chemistry, Analytical Chemistry, 90187 Umeå, 10:00 (English)
Available from: 2006-10-11 Created: 2006-10-11 Last updated: 2011-04-06Bibliographically approved

Open Access in DiVA

No full text

Other links

Publisher's full textPubMed

Search in DiVA

By author/editor
Tesfalidet, Solomon
By organisation
Department of Chemistry
In the same journal
Analytical and Bioanalytical Chemistry

Search outside of DiVA

GoogleGoogle Scholar
The number of downloads is the sum of all downloads of full texts. It may include eg previous versions that are now no longer available

Altmetric score

Total: 139 hits
ReferencesLink to record
Permanent link

Direct link