In situ ethylation-purge and programmed-temperature-vaporizer cold trapping-gas chromatography-mass spectrometry as an automated technique for the determination of methyl- and butyltin compounds in aqueous samples

A new method for the determination of methyl- and butyltin compounds in aqueous samples is presented. The organotin species are derivatized in situ with sodium tetraethylborate (NaBEt4) in an 800-ml sample, purged on-line with helium and cryofocused at −40°C in the Tenax-filled glass insert of a mod...

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Hauptverfasser: Eiden, Ralf (VerfasserIn) , Schöler, Heinz Friedrich (VerfasserIn) , Gastner, Manfred (VerfasserIn)
Dokumenttyp: Article (Journal)
Sprache:Englisch
Veröffentlicht: 25 June 1998
In: Journal of chromatography
Year: 1998, Jahrgang: 809, Heft: 1, Pages: 151-157
ISSN:1873-3778
DOI:10.1016/S0021-9673(98)00164-2
Online-Zugang:Verlag, lizenzpflichtig, Volltext: https://doi.org/10.1016/S0021-9673(98)00164-2
Verlag, lizenzpflichtig, Volltext: https://www.sciencedirect.com/science/article/pii/S0021967398001642
Volltext
Verfasserangaben:Ralf Eiden, Heinz Friedrich Schöler, Manfred Gastner

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520 |a A new method for the determination of methyl- and butyltin compounds in aqueous samples is presented. The organotin species are derivatized in situ with sodium tetraethylborate (NaBEt4) in an 800-ml sample, purged on-line with helium and cryofocused at −40°C in the Tenax-filled glass insert of a modified split/splitless injector. The injector is equipped with a liquid nitrogen cooling and a heating wire which serves for programmed-temperature vaporization. After thermal desorption the peralkylated tin species are refocussed on the capillary GC column at 10°C followed by GC separation and mass spectrometric detection in the full scan mode. All steps are computer-controlled so that once the derivatizing reagent is added, the analysis is performed automatically. The concentration of NaBEt4, the reaction time, the purge flow-rate and the purge time were optimized. The preconcentration of sample volumes of 800 ml led to detection limits in the range of 1-2 ng Sn/l. Due to the compound specific information of the full scan mass spectra, the presented method is a powerful tool for the speciation of alkyltin compounds in aqueous samples. 
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