Tert-butyldimethylsilyl chitosan synthesis and characterization by analytical ultracentrifugation, for archaeological wood conservation

Wakefield, Jennifer M. K.; Braovac, Susan; Kutzke, Hartmut; Stockman, Robert A.; Harding, Stephen E.

Abstract

The Oseberg ship is one of the most important archaeological testimonies of the Vikings. After excavation in 1904, the wooden gravegoods were conserved using alum salts. This resulted in extreme degradation of a number of the objects a hundred years later through acid depolymerisation of cellulose and lignin. The fragile condition of the artefacts requires a reconsolidation which has to be done avoiding water as solvent. We synthesized tert-butyldimethylsilyl (TBDMS) chitosan which is soluble in a 50:50 solution of ethyl acetate and toluene. Measurement of its molecular weight, to anticipate its penetration, provided a challenge as the density difference of the polymer and solvent was too small to provide adequate solute redistribution under a centrifugal field, so a two-stage process was implemented (i) determination of the weight-average molar mass of the aqueous soluble activated precursor, chitosan mesylate, Mw,mc using sedimentation equilibrium with the SEDFIT-MSTAR algorithm, and determination of the degree of polymerisation DP; (ii) measurement of the average degree of substitution DSTBDMS of the TBDMS group on each chitosan monosaccharide monomer unit using NMR, to augment the Mw,mc value to give the molar mass of the TBDMS-chitosan. For the preparation, we find Mw = 9.8 kg·mol−1, which is within the acceptable limit for penetration and consolidation of degraded wood. Future work will test this on archaeological wood from different sources.

Citation

Wakefield, J. M. K., Braovac, S., Kutzke, H., Stockman, R. A., & Harding, S. E. (2020). Tert-butyldimethylsilyl chitosan synthesis and characterization by analytical ultracentrifugation, for archaeological wood conservation. European Biophysics Journal, 49, 781-789. https://doi.org/10.1007/s00249-020-01450-z

• Journal Article Type: Article
• Acceptance Date: Jul 17, 2020
• Online Publication Date: Aug 26, 2020
• Publication Date: Dec 1, 2020
• Deposit Date: Apr 21, 2021
• Publicly Available Date: Apr 23, 2021
• Journal: European Biophysics Journal
• Print ISSN: 0175-7571
• Electronic ISSN: 1432-1017
• Publisher: Springer Verlag
• Peer Reviewed: Peer Reviewed
• Volume: 49
• Pages: 781-789
• DOI: https://doi.org/10.1007/s00249-020-01450-z
• Keywords: Biophysics; General Medicine
• Public URL: https://nottingham-repository.worktribe.com/output/4869593
• Publisher URL: https://link.springer.com/article/10.1007/s00249-020-01450-z
• Additional Information: Received: 2 March 2020; Revised: 10 July 2020; Accepted: 17 July 2020; First Online: 26 August 2020; : ; : There are no conflicts of interest to declare.