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Titel |
Technical Note: In-situ derivatization thermal desorption GC-TOFMS for direct analysis of particle-bound non-polar and polar organic species |
VerfasserIn |
J. Orasche, J. Schnelle-Kreis, G. Abbaszade, R. Zimmermann |
Medientyp |
Artikel
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Sprache |
Englisch
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ISSN |
1680-7316
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Digitales Dokument |
URL |
Erschienen |
In: Atmospheric Chemistry and Physics ; 11, no. 17 ; Nr. 11, no. 17 (2011-09-02), S.8977-8993 |
Datensatznummer |
250010049
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Publikation (Nr.) |
copernicus.org/acp-11-8977-2011.pdf |
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Zusammenfassung |
An in-situ derivatization thermal desorption method followed by gas
chromatography and time-of-flight mass spectrometry (IDTD-GC-TOFMS) was
developed for determination of polar organic compounds together with
non-polar compounds in one measurement. Hydroxyl and carboxyl groups of
compounds such as anhydrous sugars, alcohols and phenols, fatty acids and
resin acids are targets of the derivatization procedure. Derivatization is
based on silylation with N-Methyl-N-trimethylsilyl-trifluoroacetamide
(MSTFA) during the step of thermal desorption. The high temperature of
300 °C during desorption is utilized for the in-situ derivatization on the
collection substrate (quartz fibre filters) accelerating the reaction rate.
Thereby, the analysis time is as short as without derivatization. At first
the filter surface is dampened with derivatization reagent before insertion
of the sample into the thermal desorption unit. To ensure ongoing
derivatization during thermal desorption the carrier gas is enriched with
MSTFA until the desorption procedure is finished. The precisions of all
studied analytes were below 17 % within a calibration range from 22 pg
(abietic acid) up to 342 ng (levoglucosan). Limits of quantification (LOQ)
for polycyclic aromatic hydrocarbons (PAH) were between 1 pg (fluoranthene)
and 8 pg (indeno[1,2,3-cd]pyrene), for resin acids 37–102 pg and for
studied phenols 4–144 pg. LOQ for levoglucosan was 17 pg. |
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