umu.sePublications
Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
A simple method for synthesis of organotin species to investigate extraction procedures in sediments by isotope dilution-gas chromatography-inductively coupled plasma mass spectrometry: Part 2. 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.
Show others and affiliations
2004 (English)In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 19, no 3, 368-372 p.Article in journal (Refereed) Published
Abstract [en]

A rapid method for the synthesis of phenyltin species based on the phenylation of tin iodide was developed and a standard of 124Sn, enriched monophenyltin (MPhT), diphenyltin (DPhT) and triphenyltin (TPhT) was produced. Isotope enriched species were added to and equilibrated with the certified reference material BCR 646 to evaluate different extraction procedures currently in use for the determination of organic tin species in sediments. Samples were measured by gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) with species specific isotope dilution (SSID) calibration. For TPhT measurement results agreed with the certified values for extraction methods using tropolone in diethyl ether alone or in the presence of NaCl and HCl as well as with 50% HBr. However, with 50% HBr, concentrations obtained for DPhT and MPhT were above the upper limit (2) of the certification. The stability of phenyltin species was studied by comparing their signal magnitudes in spike solutions generated directly after derivatisation with those obtained after applying the extraction–derivatisation procedures. Degradation of phenyltin species was matrix dependent and appeared for most of the extraction methods investigated. For water standards and BCR 646, extraction with methanol combined with dichloromethane or methanol combined with acetic acid gave no degradation when applied with less than 20 min ultrasonication. Extraction efficiencies for these two methods were however low for the BCR 646 matrix, in particular for DPhT and MPhT.

Place, publisher, year, edition, pages
London: Royal Society of Chemistry , 2004. Vol. 19, no 3, 368-372 p.
Identifiers
URN: urn:nbn:se:umu:diva-14325DOI: 10.1039/b313787bOAI: oai:DiVA.org:umu-14325DiVA: diva2:153996
Available from: 2007-06-15 Created: 2007-06-15 Last updated: 2017-12-14Bibliographically 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.
Keyword
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
Identifiers
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)
Opponent
Supervisors
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 text

Search in DiVA

By author/editor
Kumar, Sunil J.Tesfalidet, SolomonSnell, James PNguyen Van, DongFrech, Wolfgang
By organisation
Department of Chemistry
In the same journal
Journal of Analytical Atomic Spectrometry

Search outside of DiVA

GoogleGoogle Scholar

doi
urn-nbn

Altmetric score

doi
urn-nbn
Total: 130 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf