Lignin analysis with benchtop NMR spectroscopy

Jerk Rönnols 1 , Ernesto Danieli 2 , Hélène Freichels 2 , and Fredrik Aldaeus 1
  • 1 RISE, Box 5604, SE-114 86, Stockholm, Sweden
  • 2 Magritek GmbH, Philipsstraße 8, 52068 Aachen, Germany
Jerk Rönnols, Ernesto Danieli, Hélène Freichels and Fredrik Aldaeus

Abstract

Benchtop nuclear magnetic resonance (NMR) spectroscopy is an emerging field with an appealing profile for industrial applications. The instrumentation offers the possibility to measure NMR spectra in situations where high-field NMR spectroscopy is considered too expensive or complicated. In this study, we investigated the scope and limitations of 1H NMR measurements on kraft lignins and black liquors at low magnetic field strengths (1.0 and 1.5 T). The ability to quantify different classes of compounds was investigated and found to be promising. NMR-based diffusion measurements were performed, with the aim of gaining insight into the molar mass of the lignins at hand. These measurements were fast, repeatable and in good agreement with established methods.

  • Assemat, G., Gouilleux, B., Bouillaud, D., Farjon, J., Gilard, V., Giraudeau, P., Malet-Martino, M. (2018) Diffusion-ordered spectroscopy on a benchtop spectrometer for drug analysis. J. Pharm. Biomed. Anal. 160:268–275.

    • Crossref
    • PubMed
    • Export Citation
  • Bogun, B., Moore, S. (2017) 1H and 31P benchtop NMR of liquids and solids used in and/or produced during the manufacture of methamphetamine by the HI reduction of pseudoephedrine/ephedrine. Forensic Sci. Int. 278:68–77.

    • Crossref
    • PubMed
    • Export Citation
  • Garver, T.M., Callaghan, P.T. (1991) Hydrodynamics of kraft lignins. Macromolecules 24:420–430.

    • Crossref
    • Export Citation
  • Gouilleux, B., Marchand, J., Charrier, B., Remaud, G.S., Giraudeau, P. (2018) High-throughput authentication of edible oils with benchtop ultrafast 2D NMR. Food Chem. 244:153–158.

    • Crossref
    • PubMed
    • Export Citation
  • Höpfner, J., Ratzsch, K.-F., Botha, C., Wilhelm, M. (2018) Medium resolution 1H-NMR at 62 MHz as a new chemically sensitive online detector for size-exclusion chromatography (SEC-NMR). Macromol. Rapid Commun. 39:1700766.

    • Crossref
    • Export Citation
  • Johnson, C.S. Jr. (1999) Diffusion ordered nuclear magnetic resonance spectroscopy: principles and applications. Prog. Nucl. Magn. Reson. Spectrosc. 34:203–256.

    • Crossref
    • Export Citation
  • Killner, M.H.M., Garro Linck, Y., Danieli, E., Rohwedder, J.J.R., Blümich, B. (2015) Compact NMR spectroscopy for real-time monitoring of a biodiesel production. Fuel 139:240–247.

    • Crossref
    • Export Citation
  • Killner, M.H.M., Danieli, E., Casanova, F., Rohwedder, J.J.R., Blümich, B. (2017) Mobile compact 1H NMR spectrometer promises fast quality control of diesel fuel. Fuel 203:171–178.

    • Crossref
    • Export Citation
  • Li, W., Chung, H., Daeffler, C., Johnson, J.A., Grubbs, R.H. (2012) Application of 1H DOSY for facile measurement of polymer molecular weights. Macromolecules 45: 9595–9603.

    • Crossref
    • Export Citation
  • Meyer, K., Kern, S., Zientek, N., Guthausen, G., Maiwald, M. (2016) Process control with compact NMR. Trends Anal. Chem. 83:39–52.

    • Crossref
    • Export Citation
  • Montgomery, J.R.D., Bazley, P., Lebl, T., Westwood, N.J. (2019) Using fractionation and diffusion ordered spectroscopy to study lignin molecular weight. Chemistry Open 8:1–6.

  • Montgomery, J.R.D., Lancefield, C.S., Miles-Barrett, D.M., Ackermann, K., Bode, B.E., Westwood, N.J., Lebl, T. (2017) Fractionation and DOSY NMR as analytical tools: from model polymers to a technical lignin. ACS Omega 2:8466–8474.

    • Crossref
    • PubMed
    • Export Citation
  • Norgren, M., Lindström, B. (2000) Physico-chemical characterization of a fractionated kraft lignin. Holzforschung 54:528–534.

    • Crossref
    • Export Citation
  • Rönnols, J., Schweinebarth, H., Jacobs, A., Stevanic, J.S., Olsson, A.-M., Reimann, A., Aldaeus, F. (2015) Structural changes in softwood kraft lignin during nonoxidative thermal treatment. Nord. Pulp Pap. Res. J. 30:550–561.

    • Crossref
    • Export Citation
  • Rönnols, J., Jacobs, A., Aldaeus, F. (2017) Consecutive determination of softwood kraft lignin structure and molar mass from NMR measurements. Holzforschung 71: 563–570.

  • Sjöström, E. (1977) The behavior of wood polysaccharides during alkaline pulping processes. Tappi 60: 151–154.

  • Stejskal, E.O., Tanner, J.E. (1965) Spin diffusion measurements: spin echoes in the presence of a time dependent field gradient. J. Chem. Phys. 42:288–297.

    • Crossref
    • Export Citation
  • Weber, S., Schrag, K., Mildau, G., Kuballa, T., Walch, S.G., Lachenmeier, D.W. (2018) Analytical methods for the determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) – a short review. Anal. Chem. Insights 13:1–16.

  • Zinovyev, G., Sulaeva, I., Podzimek, S., Rössner, D., Kilpeläinen, I., Sumerskii, I., Rosenau, T., Potthast, A. (2018) Getting closer to absolute molar masses of technical lignins. ChemSusChem 11:3259–3268.

    • Crossref
    • PubMed
    • Export Citation
Purchase article
Get instant unlimited access to the article.
$42.00
Log in
Already have access? Please log in.


or
Log in with your institution

Journal + Issues

Search