title: Novel ethyl-derivatization approach for the determination of fluoride by headspace gas chromatography/mass spectrometry.
abstract: We report a novel derivatization chemistry for determination of fluoride based on the 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 matrixes, 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 fluoride-complexing agents, such as Al(III) and Fe(III). The effect of large amounts of these interferences was studied, and the adverse effect of these ions was eliminated by use of the method of standard additions.
authors.affiliation: National Research Council of Canada, 1200 Montreal Road, Ottawa, ON K1A 0R6, Canada. e.pagliano@sns.it
authors.forename: Enea
authors.initials: E
authors.lastname: Pagliano
authors.forename: Juris
authors.initials: J
authors.lastname: Meija
authors.forename: Jianfu
authors.initials: J
authors.lastname: Ding
authors.forename: Ralph E
authors.initials: RE
authors.lastname: Sturgeon
authors.forename: Alessandro
authors.initials: A
authors.lastname: D'Ulivo
authors.forename: Zoltán
authors.initials: Z
authors.lastname: Mester
mesh_terms: D005290:Ferric Compounds / Q000737:chemistry*; D005459:Fluorides / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry
chemical_list: D005290:Ferric Compounds; D005459:Fluorides