A one-step method for priority compounds of concern in tar from former industrial sites: trimethylsilyl derivatisation with comprehensive two-dimensional gas chromatography

C. Gauchotte-Lindsay, P. Richards, L. A. McGregor, R. Thomas, R. M. Kalin

Research output: Contribution to journalArticle

11 Citations (Scopus)

Abstract

A dense non-aqueous phase liquid sample formed by release of coal tar into the environment was derivatised by trimethylsilylation using the reagent N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and extracted in hexane using accelerated solvent extraction. This procedure enables comprehensive extraction of an extensive suite of organic compounds from tar, which has not previously been described. Comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (GC×GC-TOFMS) was used for the analysis of the sample for concurrent evaluation of -OH functional group-containing compounds along with aliphatics, polycyclic aromatic hydrocarbons and other typical tar compounds normally determined via classic gas chromatography. Using statistically designed experiments, a range of conditions were tested for complete recovery of four different surrogates. The robustness and repeatability of the optimised derivatisation/extraction method was demonstrated. Finally, more than a hundred and fifty derivatised compounds were identified using mass spectra elucidation and GC×GC logical order of elution.

LanguageEnglish
Pages154-163
Number of pages10
JournalJournal of Chromatography A
Volume1253
Early online date5 Jul 2012
DOIs
Publication statusPublished - 31 Aug 2012

Fingerprint

Tars
Gas chromatography
Gas Chromatography
Coal Tar
Polycyclic Aromatic Hydrocarbons
Hexanes
Solvent extraction
Organic compounds
Functional groups
Mass spectrometry
Mass Spectrometry
Recovery
Liquids
Experiments
N,O-bis(trimethylsilyl)trifluoroacetamide

Keywords

  • coal tar phenols
  • comprehensive two-dimensional gas chromatography
  • environmental forensics
  • manufactured gas plant
  • oxygenated species
  • trimethylsilyl derivatisation

Cite this

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abstract = "A dense non-aqueous phase liquid sample formed by release of coal tar into the environment was derivatised by trimethylsilylation using the reagent N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and extracted in hexane using accelerated solvent extraction. This procedure enables comprehensive extraction of an extensive suite of organic compounds from tar, which has not previously been described. Comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (GC×GC-TOFMS) was used for the analysis of the sample for concurrent evaluation of -OH functional group-containing compounds along with aliphatics, polycyclic aromatic hydrocarbons and other typical tar compounds normally determined via classic gas chromatography. Using statistically designed experiments, a range of conditions were tested for complete recovery of four different surrogates. The robustness and repeatability of the optimised derivatisation/extraction method was demonstrated. Finally, more than a hundred and fifty derivatised compounds were identified using mass spectra elucidation and GC×GC logical order of elution.",
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A one-step method for priority compounds of concern in tar from former industrial sites : trimethylsilyl derivatisation with comprehensive two-dimensional gas chromatography. / Gauchotte-Lindsay, C.; Richards, P.; McGregor, L. A.; Thomas, R.; Kalin, R. M.

In: Journal of Chromatography A, Vol. 1253, 31.08.2012, p. 154-163.

Research output: Contribution to journalArticle

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