Technical Note: In-situ derivatization thermal desorption GC-TOFMS for direct analysis of particle-bound non-polar and polar organic species
Orasche, J.
Schnelle-Kreis, J.
Abbaszade, G.
Zimmermann, R.
11, 17: 8977 - 8993
DOI: https://doi.org/10.5194/acp-11-8977-2011
Persistent URL: http://resolver.sub.uni-goettingen.de/purl?gldocs-11858/7053
Persistent URL: http://resolver.sub.uni-goettingen.de/purl?gldocs-11858/7053
Orasche, J.; Schnelle-Kreis, J.; Abbaszade, G.; Zimmermann, R., 2011: Technical Note: In-situ derivatization thermal desorption GC-TOFMS for direct analysis of particle-bound non-polar and polar organic species. In: Atmospheric Chemistry and Physics, Band 11, 17: 8977 - 8993, DOI: 10.5194/acp-11-8977-2011.
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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-trimethylsilyltrifluoroacetamide
(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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