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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/ac2030128Analytical Chemistry, 84, 5, pp. 2592-2596, 2012-03-06 A BACBD EF D A
ABSTRACTThe alkylation of nitrite and nitrate by triethyloxonium tetrafluoroborate allows determination of their ethyl esters by headspace GC-MS. In the present study, significant improvement in analytical performance are achieved by using negative chemical ionization (CI-). Detection limits are improved for at least an order of magnitude than those achieved using electron impact ionization (EI). The derivatization procedure has been optimized and alkaline conditions are adopted to minimize the conversion of nitrite to nitrate (determined to be 0.07% at 100 mg/L NO 2 -) and to avoid the exchange of oxygen between the analytes and the solvent (water).Quantitation entails the use of isotopically enriched standards (N 18 O 2 -and 15 NO 3 -), which also permits monitoring of potential conversion from nitrite to nitrate during the analysis (double spike isotope dilution).