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

Abstract

Access and use of this website and the material on it are subject to the Terms and Conditions set forth at A comparison of alkyl derivatization methods for speciation of mercury based on solid phase microextraction gas chromatography with furnace atomization plasma spectrometry detection Grinberg, P.; Campos, R. C.; Mester, Z.; Sturgeon, R.http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/jsp/nparc_cp.jsp?lang=fr L'accès à ce site Web et l'utilisation de son contenu sont assujettis aux conditions présentées dans le site LISEZ CES CONDITIONS ATTENTIVEMENT AVANT D'UTILISER CE SITE WEB. NRC Publications Record / Notice d'Archives des publications de CNRC:http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?action=rtdoc&an=8896935&lang=en http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?action=rtdoc&an=8896935&lang=fr READ THESE TERMS AND CONDITIONS CAREFULLY BEFORE USING THIS WEBSITE.http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/jsp/nparc_cp.jsp?lang=en Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communiquez avec nous à PublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. Questions? Contact the NRC Publications Archive team atPublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. If you wish to email the authors directly, please see the first page of the publication for their contact information. NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. For the publisher's version, please access the DOI link below./ Pour consulter la version de l'éditeur, utilisez le lien DOI ci-dessous.http://doi.org/10.1039/b212545eJournal of Analytical Atomic Spectrometry, 18, 8, pp. 902-909, 2003 A comparison of alkyl derivatization methods for speciation of mercury based on solid phase microextraction gas chromatography with furnace atomization plasma emission spectrometry detection{ Several 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 mm 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 ...

Determination of methylmercury in fish tissues by isotope dilution SPME-GC-ICP-MS

“…47 More recently, SPME has been applied to the determination of MMHg as an elegant, solvent-free sample extraction technique. 6,27,33,41,[48][49][50] The precision of results obtained using this technique is typically in the range of 2 to 10% RSD for MMHg.…”

“…The most frequently used procedures for the extraction of mercury species from solid samples are based on alkaline [2][3][4][5][6] and acidic leaching, 7,8 aqueous distillation, [9][10][11][12][13] supercritical fluid extraction 14 and microwave-assisted extraction. [15][16][17] Grignard reagents, [18][19][20][21] sodium tetraethylborate (NaBEt 4 ), 17,[22][23][24][25][26] sodium tetrapropylborate (NaBPr 4 ) 18,27 and sodium tetraphenylborate (NaBPh 4 ) [28][29][30][31][32][33] have been used for efficient derivatization. Gas chromatography, capillary electrophoresis or liquid chromatography are commonly used separation techniques for MMHg speciation in combination with atomic fluorescence spectrometry (AFS), 3,[34][35][36] electron-capture detection (GC-ECD), 37 atomic absorption spectrometry (AAS), 16,22 ion trap mass spectrometry, 30,31 inductively coupled plasma and microwave-induced plasma atomic emission spectrometry (ICP-AES, MIP-AES) …”

In situ ethylation of organolead, organotin and organomercury species by bromomagnesium tetraethylborate prior to GC‐ICP‐MS analysis

“…The ethylation process was investigated by several authors and found to be most effective in conditions where pH ranged between 4 and 6 [26,27]. This range was chosen for pH optimisation of the ethylation reaction employing BrMgEt 4 B.…”

Speciation analysis of mercury in seawater from the lagoon of Venice by on-line pre-concentration HPLC–ICP-MS

“…However, the drawback of GC is that the species have to be rendered volatile and this requires a derivatisation step first with either Grignard reagents or more recently tetraalkyborate compounds [5] which can be time consuming and can sometimes result in species transformations [6], because of this another method for comparison is desirable. HPLC on the other hand requires no derivatisation step, as the species do not need to be volatile before injection 0003-2670/$ -see front matter © 2008 Elsevier B.V. All rights reserved.…”