A comparison of alkyl derivatization methods for speciation of mercury based on solid phase microextraction gas chromatography with furnace atomization plasma spectrometry detection

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DOIResolve DOI: http://doi.org/10.1039/b212545e
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TypeArticle
Journal titleJournal of Analytical Atomic Spectrometry
ISSN0267-9477
Volume18
Issue8
Pages902909; # of pages: 8
AbstractSeveral derivatizing agents were evaluated for use in speciating mercury in biological samples using solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES). Following digestion with methanolic potassium hydroxide, the pH of the samples was adjusted and NaCl added when necessary. The mercury species were then derivatized with sodium tetraphenylborate or sodium tetrapropylborate and extracted by SPME using a 100 µm PDMS coated fiber. The derivatized species were then separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. Propylation proved to be more sensitive, robust and faster than ethylation or phenylation, leading to procedural detection limits of 0.55 ng g−1 for methylmercury, 0.34 ng g−1 for ethylmercury and 0.23 ng g−1 for inorganic mercury. An intra-day and intra-fiber precision of typically 2.2% was achieved whereas long-term (4 months) and inter-fiber reproducibility precision was typically 4.4%. The accuracy of the method was validated by the analysis of Certified Reference Materials (DORM-2, DOLT-2 and TORT-2) from the National Research Council of Canada.
Publication date
LanguageEnglish
AffiliationNRC Institute for National Measurement Standards; National Research Council Canada
Peer reviewedNo
Identifier10391186
NRC number85
NPARC number8896935
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Record identifier8d7075fe-6524-42b9-a989-9adf85c54717
Record created2009-04-22
Record modified2016-05-09
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