Rapid, accurate and precise determination of tributyltin in sediments and biological samples by species specific isotope dilution-microwave extraction-gas chromatography-ICP mass spectrometry

M Monperrus, O Zuloaga, Eva Maria Krupp, D Amouroux, R Wahlen, B Fairman, O F X Donard

Research output: Contribution to journalArticle

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Abstract

The rapid and precise determination of tributyltin (TBT) in sediments and biological tissues has been performed by species specific isotope dilution mass spectrometric analysis (IDMS) using an inductively coupled plasma mass spectrometer as detector after capillary gas chromatography (CGC-ICP-MS). A new labelled TBT standard ((TBTCl)-T-117 in methanolic solution) commercial isotope provided by LGC Limited (Teddington, UK) was used for these determinations. Parameters affecting the ICP-MS performances, such as correction for detector dead time and mass bias correction, were carefully studied. The mass bias was corrected using two different methods: the bracketing mode and an on-line mode based on a continuous nebulisation of an antimony solution (Sb-121 and Sb-123). The on-line mode has been successfully applied for mass bias corrections and allows simultaneous GC-ICP-MS analysis of organotins. Three spiking procedures were compared using isotopically enriched TBT ((TBT)-T-117) to compare the efficiency of the extraction procedures for the different samples studied. A rapid method was developed (2 min) giving yield to good precision (uncertainty range between 0.7 and 13.7%) using a simultaneous microwave extraction and spiking procedure. The accuracy and precision of the different protocols has been validated on certified reference materials, such as PACS 2 (980 ng Sn g(-1)) and CRM 462 (70 ng Sn g(-1)) for the sediments, CRM 477 (2200 ng TBT g(-1)) and CRM 710 (135.1 ng TBT g(-1)) for the biological tissues. The results obtained were in all cases in good agreement with the certified reference values.

Original languageEnglish
Pages (from-to)247-253
Number of pages7
JournalJournal of Analytical Atomic Spectrometry
Volume18
Issue number3
DOIs
Publication statusPublished - 2003

Keywords

  • ATOMIC-ABSORPTION SPECTROMETRY
  • ORGANOTIN COMPOUNDS
  • SPECIATION ANALYSIS
  • BUTYLTIN COMPOUNDS
  • ENVIRONMENTAL-SAMPLES
  • DERIVATIZATION METHODS
  • EMISSION-SPECTROMETRY
  • LIQUID-CHROMATOGRAPHY
  • MS
  • METHYLMERCURY

Cite this

Rapid, accurate and precise determination of tributyltin in sediments and biological samples by species specific isotope dilution-microwave extraction-gas chromatography-ICP mass spectrometry. / Monperrus, M ; Zuloaga, O ; Krupp, Eva Maria; Amouroux, D ; Wahlen, R ; Fairman, B ; Donard, O F X .

In: Journal of Analytical Atomic Spectrometry, Vol. 18, No. 3, 2003, p. 247-253.

Research output: Contribution to journalArticle

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title = "Rapid, accurate and precise determination of tributyltin in sediments and biological samples by species specific isotope dilution-microwave extraction-gas chromatography-ICP mass spectrometry",
abstract = "The rapid and precise determination of tributyltin (TBT) in sediments and biological tissues has been performed by species specific isotope dilution mass spectrometric analysis (IDMS) using an inductively coupled plasma mass spectrometer as detector after capillary gas chromatography (CGC-ICP-MS). A new labelled TBT standard ((TBTCl)-T-117 in methanolic solution) commercial isotope provided by LGC Limited (Teddington, UK) was used for these determinations. Parameters affecting the ICP-MS performances, such as correction for detector dead time and mass bias correction, were carefully studied. The mass bias was corrected using two different methods: the bracketing mode and an on-line mode based on a continuous nebulisation of an antimony solution (Sb-121 and Sb-123). The on-line mode has been successfully applied for mass bias corrections and allows simultaneous GC-ICP-MS analysis of organotins. Three spiking procedures were compared using isotopically enriched TBT ((TBT)-T-117) to compare the efficiency of the extraction procedures for the different samples studied. A rapid method was developed (2 min) giving yield to good precision (uncertainty range between 0.7 and 13.7{\%}) using a simultaneous microwave extraction and spiking procedure. The accuracy and precision of the different protocols has been validated on certified reference materials, such as PACS 2 (980 ng Sn g(-1)) and CRM 462 (70 ng Sn g(-1)) for the sediments, CRM 477 (2200 ng TBT g(-1)) and CRM 710 (135.1 ng TBT g(-1)) for the biological tissues. The results obtained were in all cases in good agreement with the certified reference values.",
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author = "M Monperrus and O Zuloaga and Krupp, {Eva Maria} and D Amouroux and R Wahlen and B Fairman and Donard, {O F X}",
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TY - JOUR

T1 - Rapid, accurate and precise determination of tributyltin in sediments and biological samples by species specific isotope dilution-microwave extraction-gas chromatography-ICP mass spectrometry

AU - Monperrus, M

AU - Zuloaga, O

AU - Krupp, Eva Maria

AU - Amouroux, D

AU - Wahlen, R

AU - Fairman, B

AU - Donard, O F X

PY - 2003

Y1 - 2003

N2 - The rapid and precise determination of tributyltin (TBT) in sediments and biological tissues has been performed by species specific isotope dilution mass spectrometric analysis (IDMS) using an inductively coupled plasma mass spectrometer as detector after capillary gas chromatography (CGC-ICP-MS). A new labelled TBT standard ((TBTCl)-T-117 in methanolic solution) commercial isotope provided by LGC Limited (Teddington, UK) was used for these determinations. Parameters affecting the ICP-MS performances, such as correction for detector dead time and mass bias correction, were carefully studied. The mass bias was corrected using two different methods: the bracketing mode and an on-line mode based on a continuous nebulisation of an antimony solution (Sb-121 and Sb-123). The on-line mode has been successfully applied for mass bias corrections and allows simultaneous GC-ICP-MS analysis of organotins. Three spiking procedures were compared using isotopically enriched TBT ((TBT)-T-117) to compare the efficiency of the extraction procedures for the different samples studied. A rapid method was developed (2 min) giving yield to good precision (uncertainty range between 0.7 and 13.7%) using a simultaneous microwave extraction and spiking procedure. The accuracy and precision of the different protocols has been validated on certified reference materials, such as PACS 2 (980 ng Sn g(-1)) and CRM 462 (70 ng Sn g(-1)) for the sediments, CRM 477 (2200 ng TBT g(-1)) and CRM 710 (135.1 ng TBT g(-1)) for the biological tissues. The results obtained were in all cases in good agreement with the certified reference values.

AB - The rapid and precise determination of tributyltin (TBT) in sediments and biological tissues has been performed by species specific isotope dilution mass spectrometric analysis (IDMS) using an inductively coupled plasma mass spectrometer as detector after capillary gas chromatography (CGC-ICP-MS). A new labelled TBT standard ((TBTCl)-T-117 in methanolic solution) commercial isotope provided by LGC Limited (Teddington, UK) was used for these determinations. Parameters affecting the ICP-MS performances, such as correction for detector dead time and mass bias correction, were carefully studied. The mass bias was corrected using two different methods: the bracketing mode and an on-line mode based on a continuous nebulisation of an antimony solution (Sb-121 and Sb-123). The on-line mode has been successfully applied for mass bias corrections and allows simultaneous GC-ICP-MS analysis of organotins. Three spiking procedures were compared using isotopically enriched TBT ((TBT)-T-117) to compare the efficiency of the extraction procedures for the different samples studied. A rapid method was developed (2 min) giving yield to good precision (uncertainty range between 0.7 and 13.7%) using a simultaneous microwave extraction and spiking procedure. The accuracy and precision of the different protocols has been validated on certified reference materials, such as PACS 2 (980 ng Sn g(-1)) and CRM 462 (70 ng Sn g(-1)) for the sediments, CRM 477 (2200 ng TBT g(-1)) and CRM 710 (135.1 ng TBT g(-1)) for the biological tissues. The results obtained were in all cases in good agreement with the certified reference values.

KW - ATOMIC-ABSORPTION SPECTROMETRY

KW - ORGANOTIN COMPOUNDS

KW - SPECIATION ANALYSIS

KW - BUTYLTIN COMPOUNDS

KW - ENVIRONMENTAL-SAMPLES

KW - DERIVATIZATION METHODS

KW - EMISSION-SPECTROMETRY

KW - LIQUID-CHROMATOGRAPHY

KW - MS

KW - METHYLMERCURY

U2 - 10.1039/b203242m

DO - 10.1039/b203242m

M3 - Article

VL - 18

SP - 247

EP - 253

JO - Journal of Analytical Atomic Spectrometry

JF - Journal of Analytical Atomic Spectrometry

SN - 0267-9477

IS - 3

ER -