Quantification of Volatiles from Technical Lignins by Multiple Headspace Sampling-Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

A1 Journal article (refereed)

Internal Authors/Editors

Publication Details

List of Authors: Matthias Guggenberger, Antje Potthast, Thomas Rosenau, Stefan Böhmdorfer
Publisher: American Chemical Society
Publication year: 2019
Journal: ACS Sustainable Chemistry and Engineering
Volume number: 7
Issue number: 11
Start page: 9896
End page: 9903
eISSN: 2168-0485


Industrial lignins comprise a mixture of substances, including volatile,
low-molecular weight compounds. In material applications of lignins,
these volatiles contribute to the malodor of the finished product. We
developed a method based on solid-phase microextraction-gas
chromatography-mass spectrometry (SPME-GC-MS) to assay qualitatively and
quantitatively the volatiles emitted from lignin samples. Substances
were identified by mass spectra and retention indices, while
quantitation was achieved by multiple headspace sampling (MHS). Guaiacol
and dimethyl disulfide were calibrated as representative compounds for
the most prominent substance classes. The method was validated and gave
good recovery, ranging from 89 to 123% for dimethyl disulfide and 90 to
105% for guaiacol, a measurement range of several dozen nanogram to a
few micrograms, which can be extended by adjusting the sample amount,
and limits of detection of 86 ng for dimethyl disulfide and 25 ng for
guaiacol. Sample preparation is limited to weighing of the sample into a
headspace vial and requires no consumables or auxiliaries. The entire
analytical workflow was automatized, including the necessary data
evaluation, which combines the outcome of repeated analyses of the same
sample. The concentrations of guaiacol in four representative lignin
samples ranged from 0.4 to 1200 ppm, while dimethyl disulfide was
detected only in a single sample.

Last updated on 2020-22-09 at 06:12