The project focused on the isolation and detailed characterization of lignin and other biopolymers from three low‑input crops – Miscanthus × giganteus, Paulownia tomentosa and Silphium perfoliatum – cultivated on the University of Bonn campus. In the first work package, lignin was extracted by an organosolv process that employed an 80 % ethanol solution at a solid‑to‑liquid ratio of 1:8, heated to 170 °C for 90 minutes in a Parr reactor. After filtration and washing, the lignin was precipitated by acidification to pH 2, centrifuged, washed with distilled water and freeze‑dried for 72 hours. The procedure was repeated in triplicate for each biomass and particle size (1.6–2.0 mm, 0.5–1.0 mm, <0.25 mm) to confirm reproducibility. Chemical composition of the raw materials was determined according to NREL laboratory analytical procedures, and the resulting high‑purity lignins were compared with commercial references (Indulin AT and Kraft lignin). The work produced two peer‑reviewed papers in 2020, reporting on the extraction efficiency and the influence of harvest season on monolignol composition.
The second work package addressed the development of multivariate models for lignin molecular‑weight determination using 1H‑NMR spectroscopy on both benchtop and high‑field instruments. A partial least squares (PLS) regression model was calibrated on a high‑field spectrometer and then transferred to a benchtop device. The study, published in the Journal of Pharmaceutical and Biomedical Analysis in 2022, demonstrated that the benchtop instrument delivered comparable accuracy to the high‑field system, thereby validating a cost‑effective alternative for routine analysis. A subsequent article in Analytical Chemistry explored the feasibility of calibration transfer between the two instrument classes. By using a small set of transfer samples, the authors achieved a successful transfer that avoided the need for full re‑calibration, reducing time, energy and financial costs. These findings highlight the potential for rapid, reliable lignin characterization in industrial settings and suggest that the approach can be extended to other biopolymers and spectroscopic techniques such as 2D fluorescence and Raman.
Collaboration was organized around a consortium led by Prof. Schulze of the Helmholtz‑Bioscience Research Centre (HBRS) and supported by Spectral Service AG and the research group of Prof. Monakhova. Additional partners included Prof. Rehahn from TU Darmstadt and Dr. Keyzers from the University of Wellington. The project ran from 2020 until a flood in July 2021 temporarily halted experimental work at the Rheinbach campus. After rebuilding infrastructure, the team resumed data collection and extended the project timeline to April 2023. Funding totaled €774,650.77, with a 93.68 % grant rate; €272,757.01 was allocated to scientific staff, €42,709.65 to employment costs, €4,350 to teaching, €26,897 to administration, €5,078.43 to travel, and €428,208.68 to the purchase of a 2D‑GPC/MS system. Spectral Service AG contributed €45,000 over three years. The project’s outcomes demonstrate that benchtop 1H‑NMR, coupled with multivariate calibration transfer, can provide a rapid, low‑cost alternative to high‑field instruments for lignin molecular‑weight analysis, with broader implications for routine quality control of both bio‑ and fossil‑based polymers in the polymer and pharmaceutical industries.
