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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 ...