Micro-pyrolysis of technical lignins in a new modular rig and product analysis by GC–MS/FID and GC × GC–TOFMS/FID
✍ Scribed by Michael Windt; Dietrich Meier; Jan Henk Marsman; Hero Jan Heeres; Sjaak de Koning
- Publisher
- Elsevier Science
- Year
- 2009
- Tongue
- English
- Weight
- 948 KB
- Volume
- 85
- Category
- Article
- ISSN
- 0165-2370
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✦ Synopsis
A new offline-pyrolysis rig has been designed to allow multifunctional experiments for preparative and analytical purposes. The system conditions can be set and monitored, e.g. temperature, its gradients and heat flux. Some special features include (1) high heating rates up to 120 8C/s with pyrolysis temperatures up to 850 8C at variable pyrolysis times and (2) the selection of different atmospheres during pyrolysis. A complete mass balance of products and reactants (gas, liquids and solids) by gravimetric methods and sequential chromatographic analyses was obtained.
The pyrolytic behaviour and the decomposition products of lignin-related compounds were studied under different conditions: heating rates (from 2.6 8C/s up to 120 8C/s), pyrolysis temperatures at 500 8C and 800 8C in different atmospheres (N 2 , H 2 , and mixtures of N 2 and acetylene). Kraft lignin, soda lignin, organosolv lignin, pyrolytic lignin from pine bio-oil, residues from biomass hydrolysis and fermentation were studied.
The obtained pyrolysis products were classified into three general groups: coke, liquid phase and gas phase (volatile organic compounds (VOC) and permanent gases). The liquid fraction was analysed by GC-MS/FID. In addition, comprehensive two-dimensional GC was applied to further characterise the liquid fraction. VOCs were semi-quantified by a modified headspace technique using GC-MS/FID analysis. The micro-pyrolysis rig proved to be an efficient and useful device for complex pyrolysis applications.