Novel Ethyl-Derivatization Approach for the Determination of Fluoride by Headspace Gas Chromatography/Mass Spectrometry

Abstract

Access and use of this website and the material on it are subject to the Terms and Conditions set forth at Novel ethyl-derivatization approach for the determination of fluoride by headspace gas chromatography/mass spectrometry Pagliano, Enea; Meija, Juris; Ding, Jianfu; Sturgeon, Ralph E.; D'Ulivo, Alessandro; Mester, Zoltán 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=21270353&lang=en http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?action=rtdoc&an=21270353&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/10.1021/ac302303rAnalytical Chemistry, 85, 2, pp. 877-881, 2012-12-10 Novel ethyl-derivatization approach for the determination of fluoride by headspace GC/MS ABSTRACTWe report a novel derivatization chemistry for determination of fluoride based on batch reaction of fluoride ions with triethyloxonium tetrachloroferrate(III) in a closed vessel to yield fluoroethane. Gaseous fluoroethane was readily separated from the matrix, sampled from the headspace and determined by gas chromatography/mass spectrometry. The method was validated using rainwater certified reference material (IRMM CA408) and subsequently applied to the determination of fluoride in various matrices, including tap water, seawater, and urine. An instrumental limit of detection of 3.2 µg/L with a linear range up to 50 mg/L was achieved. The proposed derivatization is a one-step reaction, requires no organic solvents and is safe, as the derivatizing agent is nonvolatile. Determination of fluoride is affected by common fluoridecomplexing agents, such as Al(III) and Fe(III). The effect of large ...

Determination of thiocyanate in saliva by headspace gas chromatography-mass spectrometry, following a single-step aqueous derivatization with triethyloxonium tetrafluoroborate

“…Triethyloxonium tetrafluoroborate has been recently introduced in the field of analytical chemistry as derivatizing agent for several inorganic anions of environmental and biomedical interest [21][22]. These inorganic anions -that cannot be analyzed directly by gas chromatography -are converted into volatile − is being typically used within 10 minutes from its preparation.…”

Analytical methods for the determination of halogens in bioanalytical sciences: a review

“…A promising derivatization procedure was proposed by D'Ulivo et al [178] and Pagliano et al [179]. This approach allows the use of GC to separate halogen ions (as well as other anions) using an aqueous phase reaction for further determination of halogens.…”

“…The sample with the derivatizing agent was left to react at room temperature for 3 h, and 250 μL of the headspace was injected (200°C, transfer line at 260°C). Quantitative alkylation of iodide, bromide, and chloride was obtained using trialkyloxonium tetrafluoroborates as the derivatizant agent [178], whereas for fluoride it was necessary to use triethyloxonium tetrachloroferrate(III) as the derivatizant agent in order to convert fluoride to fluoroethane [179]. In addition to the possibility of determining halogens in organic samples, this procedure was applied only for a CRM of water (BCR 612 groundwater) because the respective reagent used as the derivatizing agent had a high degree of reactivity with many inorganic and organic materials, which requires an efficient sample preparation procedure, besides avoiding the use of organic solvents.…”

Simple determination of fluoride in biological samples by headspace solid-phase microextraction and gas chromatography–tandem mass spectrometry

“…GC-mass spectrometry (MS) methods were published for the determination of fluoride in human whole blood and urine after derivatization with pentafluorobenzyl bromide [18] and pentafluorobenzyl p-toluenesulphonate [19], but these methods do not have a sufficient detection limit to detect fluoride in real samples. Headspace (HS) GC-MS following ethylation with triethyloxoniumtetrachloroferrate (III) was recently developed for the sensitive analysis of fluoride in tap water, seawater and urine [20]. The derivatization reagent, however, cannot be obtained commercially, and it takes a long time to synthesize the reagent.…”