Access and use of this website and the material on it are subject to the Terms and Conditions set forth at Reduction of measurement uncertainty by experimental design in highorder (double, triple, and quadruple) isotope dilution mass spectrometry: application to GC-MS measurement of bromide Pagliano, Enea; Mester, Zoltán; Meija, Juris 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=21270351&lang=en http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?action=rtdoc&an=21270351&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/10.1007/s00216-013-6724-5Analytical and Bioanalytical Chemistry, pp. 1-9, 2013-03

Aqueous phase reaction of trialkyloxonium tetrafluoroborates, R 3 O + BF 4 -(RdMe, Et) has been tested in the alkylation of simple inorganic anionic substrates such as halogen ions, cyanide, thiocyanate, sulphide and several oxoanions or their corresponding oxoacids. Gaseous products were separated and identified by gas chromatography mass spectrometry (GC-MS). Alkylated derivatives RI, RBr, RCl were obtained for iodide, bromide, and chloride, respectively, while for fluoride its conversion efficiency to RF is very poor. RCN and R 2 S were obtained for cyanide and sulphide, while thiocyanate gives RSCN as a main reaction product with a minor amount of alkylisothiocyanate, RNCS (<7%). Among tested oxoanions only nitrites and nitrates give volatile derivatives under the form of RsOsNO and RsOsNO 2 , respectively. Reaction performed by adding Et 3 O + BF 4 -in CH 2 Cl 2 to aqueous sample with extraction in the organic phase of reaction products, failed to identify other less volatile reaction products. Using 2 mL sample in 4 mL reaction vial (T ) 25°C), 100 µL of 2 M Et 3 O + BF 4 -and injecting 250 µL of headspace into GC-MS, detection limits (3 s) are in the range of 1-280 ng mL -1 . Application to determination of bromide in groundwater certified reference material (BCR-612, 252 ( 10 µg kg -1 of bromide) gave results in excellent agreement with certified values. The method, being not responsive to iodate, allows the selective determination of iodide in the presence of iodate. Total iodine can be determined after reduction of iodate to iodide by NaBH 4 . Application of the method to iodide-iodate speciation in table salt gave results in excellent agreement with parallel analysis performed by ion chromatography as a reference method.

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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 ...