Radial depth profiling of microbial degradation in waterlogged archaeological wood using maximum water content, X-ray diffraction, infrared spectroscopy, and light microscopy
Source abstract
Abstract
Abstract This study investigated depth-dependent microbial degradation in waterlogged archaeological wood using an integrated analytical approach combining maximum water content (MWC), X-ray diffraction (XRD), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), and light microscopy. These methods were systematically applied to increment cores extracted from three hull logs (left bottom log 3-3, right bottom log 1-1, and right bottom log 2-1) recovered from the Mado shipwreck No. 2 (AD 1151–1224) in the Yellow Sea, Republic of Korea. Logs 3-3 and 1-1 were normal wood, whereas log 2-1 was identified as compression wood. Each core was sectioned at approximately 1 cm intervals from the surface inward, and all analyses were conducted on the same depth-resolved sections, enabling direct comparison among physical, chemical, and anatomical indicators. This approach successfully delineated degraded zones, revealing consistent relationships among elevated MWC values, reduced crystallinity, ATR-FTIR evidence of polysaccharide loss and lignin enrichment, and microscopic signs of microbial attack. Degradation depths varied markedly among logs (approximately 4–5 cm in log 3-3, 9–9.5 cm in log 1-1, and ∼1 cm in log 2-1), underscoring the need for log-specific evaluation, even within a single shipwreck, for accurate assessment of preservation states and effective conservation planning.
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Research context
OpenAlex topics: Wood Treatment and Properties · Wood and Agarwood Research · Building materials and conservation
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
Department of Wood Science and Engineering , Chonnam National University , Gwangju 61186 , Republic of Korea
West Sea Cultural Heritage Division , National Research Institute of Maritime Heritage , Taean-gun, Chungcheongnam-do 32132 , Republic of Korea
Funding
National Research Foundation of Korea
References (62)
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1. Ahvenainen, P., Kontro, I., and Svedström, K. (2016). Comparision of sample crystallinity determination methods by X-ray diffraction for challenging cellulose I materials. Cellulose 23: 1073–1086.10.1007/s10570-016-0881-6 ↗
2. Åkerholm, M. and Salmén, L. (2001). Interactions between wood polymers studied by dynamic FT-IR spectroscopy. Polymer 42: 963–969.10.1016/S0032-3861(00)00434-1 ↗
3. Almkvist, G., Norbakhsh, S., Bjurhager, I., and Varmuza, K. (2016). Prediction of tensile strength in iron-contaminated archaeological wood by FT-IR spectroscopy – a study of degradation in recent oak and Vasa oak. Holzforschung 70: 855–865, https://doi.org/10.1515/hf-2015-0223.10.1515/hf-2015-0223 ↗
4. Balzano, A., Merela, M., and Čufar, K. (2022). Scanning electron microscopy protocol for studying anatomy of highly degraded waterlogged archaeological wood. Forests 13: 161, https://doi.org/10.3390/f13020161.10.3390/f13020161 ↗
5. Bardet, M., Gerbaud, G., Giffard, M., Doan, C., Hediger, S., and Le Pape, L. (2009). 13C high-resolution solid-state NMR for structural elucidation of archaeological woods. Prog. Nucl. Magn. Reson. Spectrosc. 55: 199–214, https://doi.org/10.1016/j.pnmrs.2009.02.001.10.1016/j.pnmrs.2009.02.001 ↗
6. Björdal, C.G. (2012). Evaluation of microbial degradation of shipwrecks in the Baltic sea. Int. Biodeterior. Biodegrad. 70: 126–140.10.1016/j.ibiod.2012.01.012 ↗
7. Björdal, C.G. and Dayton, P.K. (2020). First evidence of microbial wood degradation in the coastal waters of the Antarctic. Sci. Rep. 10: 12774.10.1038/s41598-020-68613-y ↗
8. Björdal, C.G., Daniel, G., and Nilsson, T. (1999). Microbial decay of waterlogged archaeological wood found in Sweden - applicable to archaeology and conservation. Int. Biodeterior. Biodegrad. 43: 63–73.10.1016/S0964-8305(98)00070-5 ↗
9. Blanchette, R.A. (2000). A review of microbial deterioration found in archaeological wood from different environments. Int. Biodeterior. Biodegrad. 46: 189–204, https://doi.org/10.1016/s0964-8305(00)00077-9.10.1016/S0964-8305(00)00077-9 ↗
10. Blanchette, R.A., Obst, J., and Timell, T. (1994). Biodegradation of compression wood and tension wood by white and brown rot fungi. Holzforschung 48: 34–42, https://doi.org/10.1515/hfsg.1994.48.s1.34.10.1515/hfsg.1994.48.s1.34 ↗
11. Bouramdane, Y., Fellak, S., El Mansouri, F., and Boukir, A. (2022). Impact of natural degradation on the aged lignocellulose fibers of Moroccan cedar softwood: structural elucidation by infrared spectroscopy (ATR-FTIR) and X-ray diffraction (XRD). Fermentation 8: 698, https://doi.org/10.3390/fermentation8120698.10.3390/fermentation8120698 ↗
12. Broda, M. and Hill, C.A.S. (2021). Conservation of waterlogged wood: past, present and future perspectives. Forests 12: 1193, https://doi.org/10.3390/f12091193.10.3390/f12091193 ↗
13. Cao, H., Gao, X., Chen, J., Xi, G., Yin, Y., and Guo, J. (2023). Changes in moisture characteristics of waterlogged archaeological wood owing to microbial degradation. Forests 14: 9–18, https://doi.org/10.3390/f14010009.10.3390/f14010009 ↗
14. Cha, M.Y., Lee, K.H., Kim, J.S., and Kim, Y.S. (2021). Variations in bacterial decay between cell types and between cell wall regions in waterlogged archaeological wood excavated in the intertidal zone. IAWA J. 42: 457–474, https://doi.org/10.1163/22941932-bja10068.10.1163/22941932-bja10068 ↗
15. Chen, Q.M., Hu, Z., Chang, H.M., and Li, B. (2007). Micro analytical methods for determination of compression wood content in loblolly pine. J. Wood Chem. Technol. 27: 169–178, https://doi.org/10.1080/02773810701700810.10.1080/02773810701700810 ↗
16. Čufar, K., Gričar, J., Zupančič, M., Koch, G., and Schmitt, U. (2008). Anatomy, cell wall structure and topochemistry of waterlogged archaeological wood aged 5200 and 4500. IAWA J. 29: 55–68, https://doi.org/10.1163/22941932-90000170.10.1163/22941932-90000170 ↗
17. De Jong, J. (1977). Conservation techniques for old waterlogged wood from shipwrecks found in the Netherlands. In: Walters, A.H. (Ed.), Biodeterioration investigation techniques. Applied Science Publishers, London, pp. 295–338.
18. Donaldson, L.A. and Singh, A.P. (2013). Formation and structure of compression wood. In: Fromm, J. (Ed.), Cellular aspects of wood formation. Springer, Berlin, pp. 225–256.10.1007/978-3-642-36491-4_9 ↗
19. Emmanuel, V., Odile, B., and Céline, R. (2015). FTIR spectroscopy of woods: a new approach to study the weathering of the carving face of a sculpture. Spectrochim. Acta, Part A 136: 1255–1259, https://doi.org/10.1016/j.saa.2014.10.011.10.1016/j.saa.2014.10.011 ↗
20. Gelbrich, J., Mai, C., and Militz, H. (2008). Chemical changes in wood degraded by bacteria. Int. Biodeterior. Biodegrad. 61: 24–32, https://doi.org/10.1016/j.ibiod.2007.06.007.10.1016/j.ibiod.2007.06.007 ↗
21. Guo, J., Chen, J., Meng, Q., Ploszczanski, L., Liu, J., Luo, R., Jin, T., Siedlaczek, P., Lichtenegger, H.C., Yin, Y., et al.. (2022). Molecular and crystal structures of cellulose in severely deteriorated archaeological wood. Cellulose 29: 9549–9568, https://doi.org/10.1007/s10570-022-04856-4.10.1007/s10570-022-04856-4 ↗
22. Hastrup, A.C.S., Howell, C., Larsen, F.H., Sathitsuksanoh, N., Goodell, B., and Jellison, J. (2012). Differences in crystalline cellulose modification due to degradation by brown and white rot fungi. Fungal Biol. 116: 1052–1063, https://doi.org/10.1016/j.funbio.2012.07.009.10.1016/j.funbio.2012.07.009 ↗
23. High, K.E. and Penkman, K.E.H. (2020). A review of analytical methods for assessing preservation in waterlogged archaeological wood and their application in practice. Heritage Sci. 8: 83, https://doi.org/10.1186/s40494-020-00422-y.10.1186/s40494-020-00422-y ↗
24. Hoffmann, P. (1986). On the stabilization of waterlogged oakwood with PEG. II. Designing a two-step treatment for multi-quality timbers. Stud. Conserv. 31: 103–113, https://doi.org/10.1179/sic.1986.31.3.103.10.1179/sic.1986.31.3.103 ↗
25. Hoffmann, P. (2013). Conservation of archaeological ships and boats – personal experiences. Archetype Publications, London.
26. Hoffmann, P., Singh, A., Kim, Y.S., Wi, S.G., Kim, I.-J., and Schmitt, U. (2004). The Bremen Cog of 1380 – an electron microscopic study of its degraded wood before and after stabilization with PEG. Holzforschung 58: 211–218, https://doi.org/10.1515/hf.2004.033.10.1515/HF.2004.033 ↗
27. Huisman, D.J., Manders, M.R., Kretschmar, E.I., Klaassen, R.K.W.M., and Lamersdorf, N. (2008). Burial conditions and wood degradation at archaeological sites in the Netherlands. Int. Biodeterior. Biodegrad. 61: 33–44, https://doi.org/10.1016/j.ibiod.2007.06.008.10.1016/j.ibiod.2007.06.008 ↗
28. Kiliç, N. (2025). Determining the condition of waterlogged archaeological woods and iron nails from the Yenikapı 17 shipwreck using multiple analytical techniques. Heritage Sci. 13: 64.10.1038/s40494-025-01604-2 ↗
29. Kim, Y.S. (1990). Chemical characteristics of waterlogged archaeological wood. Holzforschung 44: 169–172.10.1515/hfsg.1990.44.3.169 ↗
30. Kim, Y.S. and Singh, A.P. (1999). Micromorphological characteristics of compression wood degradation in waterlogged archaeological pine wood. Holzforschung 53: 381–385, https://doi.org/10.1515/hf.1999.063.10.1515/HF.1999.063 ↗
31. Kim, Y.S. and Singh, A.P. (2000). Micromorphological characteristics of wood biodegradation in wet environments: a review. IAWA J. 21: 135–155, https://doi.org/10.1163/22941932-90000241.10.1163/22941932-90000241 ↗
32. Kim, Y.S. and Singh, A.P. (2016). Wood as cultural heritage material and its deterioration by biotic and abiotic agents. In: Kim, Y.S., Funada, R., and Singh, A.P. (Eds.), Secondary xylem. Academic Press, London, pp. 169–190.10.1016/B978-0-12-802185-9.00012-7 ↗
33. Kim, Y.S., Singh, A.P., and Nilsson, T. (1996). Bacteria as important degraders in waterlogged archaeological woods. Holzforschung 50: 389–392, https://doi.org/10.1515/hfsg.1996.50.5.389.10.1515/hfsg.1996.50.5.389 ↗
34. Kim, J.S., Cha, M.Y., Lee, K.H., and Kim, Y.S. (2022). Bacterial decay in waterlogged archaeological compression wood varies with severity of compression wood. Holzforschung 76: 622–636, https://doi.org/10.1515/hf-2022-0005.10.1515/hf-2022-0005 ↗
35. Klaassen, R.K.W.M. (2008). Bacterial decay in wooden foundation piles: patterns and causes. A study of historical pile foundations in the Netherlands. Int. Biodeterior. Biodegrad. 61: 45–60, https://doi.org/10.1016/j.ibiod.2007.07.006.10.1016/j.ibiod.2007.07.006 ↗
36. Li, R., Zhang, Z., Jiao, L., Yin, Y., Tie, F., and Sun, M. (2024). Combining microscale ATR-FTIR and chemometrics to interpret degradation characteristics of earlywood, latewood, and compression wood in waterlogged archaeological pine wood. Heritage Sci. 12: 387, https://doi.org/10.1186/s40494-024-01510-z.10.1186/s40494-024-01510-z ↗
37. Macchioni, N., Pizzo, B., Bernabei, M., and Visintin, G. (2000). Dating trials of wooden historic artefacts through FT-IR spectroscopy. J. Cult. Heritage 43: 303–310, https://doi.org/10.1016/j.culher.2019.10.011.10.1016/j.culher.2019.10.011 ↗
38. Macchioni, N., Pizzo, B., Capretti, C., and Giachi, G. (2012). How an integrated diagnostic approach can help in a correct evaluation of the state of preservation of waterlogged archaeological wooden artefacts. J. Archaeol. Sci. 39: 3255–3263, https://doi.org/10.1016/j.jas.2012.05.008.10.1016/j.jas.2012.05.008 ↗
39. Macchioni, N., Capretti, C., Sozzi, L., and Pizzo, B. (2013). Grading the decay of waterlogged archaeological wood according to anatomical characterization. The case of the Fiavé site (N-E Italy). Int. Biodeterior. Biodegrad. 84: 54–64, https://doi.org/10.1016/j.ibiod.2013.05.028.10.1016/j.ibiod.2013.05.028 ↗
40. Macchioni, N., Pecoraro, E., and Pizzo, B. (2018). The measurement of maximum water content (MWC) on waterlogged archaeological wood: a comparison between three different methodologies. J. Cult. Heritage 30: 51–56, https://doi.org/10.1016/j.culher.2017.10.005.10.1016/j.culher.2017.10.005 ↗
41. McConnachie, G., Eaton, R., and Jones, M. (2008). A re-evaluation of the use of maximum moisture content data for assessing the condition of waterlogged archaeological wood. e-PS 3: 29–35.
42. McLean, J.P., Jin, G., Brennan, M., Nieuwoudt, M.K., and Harris, P.J. (2014). Using NIR and ATR-FTIR spectroscopy to rapidly detect compression woo in Pinus radiate. Can. J. Res. 44: 820–830, https://doi.org/10.1139/cjfr-2013-0329.10.1139/cjfr-2013-0329 ↗
43. National Research Institute of Maritime Cultural Heritage (2011). Taean Mado Shipwreck No. 2 - Underwater Excavation (Government Publications Registration No. 11-1550197-000012-14), Mokpo, Republic of Korea. (Text in Korean)
44. Nindiyasari, F., Erika, G., Zimmermann, T., Manian, A., Randow, C., Zehbe, R., Fernández-Díaz, L., Ziegler, A., Fleck, C., and Schmahl, W. (2015). Characterization and mechanical properties investigation of the cellulose/gypsum composite. J. Compos. Mater. 50: 657–672.10.1177/0021998315580826 ↗
45. Nishiyama, Y., Langan, P., and Chanzy, H. (2002). Crystal structure and hydrogen-bonding system in cellulose Iβ from synchrotron X-ray and neutron fiber diffraction. J. Am. Chem. Soc. 124: 9074–9082, https://doi.org/10.1021/ja0257319.10.1021/ja0257319 ↗
46. Pandey, K.K. and Pitman, A.J. (2003). FTIR studies of the changes in wood chemistry following decay by brown-rot and white-rot fungi. Int. Biodeterior. Biodegrad. 52: 151–160, https://doi.org/10.1016/s0964-8305(03)00052-0.10.1016/S0964-8305(03)00052-0 ↗
47. Park, S., Baker, J.O., Himmel, M.E., Parilla, P.A., and Johnson, D.K. (2010). Cellulose crystallinity index: measurement techniques and their impact on interpreting cellulase performance. Biotechnol. Biofuels Bioprod. 3: 10, https://doi.org/10.1186/1754-6834-3-10.10.1186/1754-6834-3-10 ↗
48. Pedersen, N.B., Gierlinger, N., and Thygesen, L.G. (2015). Bacterial and abiotic decay in waterlogged archaeological Picea abies (L.) Karst studied by confocal Raman imaging and ATR-FTIR spectroscopy. Holzforschung 69: 103–112, https://doi.org/10.1515/hf-2014-0024.10.1515/hf-2014-0024 ↗
49. Pizzo, B., Pecoraro, E., and Macchioni, N. (2013). A new method to quantitatively evaluate the chemical composition of waterlogged wood by means of attenuated total reflectance Fourier transform infrared (ATR FT-IR) measurements carried out on wet material. Appl. Spectrosc. 67: 553–562, https://doi.org/10.1366/12-06819.10.1366/12-06819 ↗
50. Pizzo, B., Pecoraro, E., Alves, A., Macchioni, N., and Rodrigues, J.C. (2015). Quantitative evaluation by attenuated total reflectance infrared (ATR-FTIR) spectroscopy of the chemical composition of decayed wood preserved in waterlogged conditions. Talanta 131: 14–20, https://doi.org/10.1016/j.talanta.2014.07.062.10.1016/j.talanta.2014.07.062 ↗
51. Purusatama, B.D. and Kim, N.H. (2018). Quantitative anatomical characteristics of compression wood, lateral wood, and opposite wood in the stem wood of Ginkgo biloba L. BioResources 13: 8076–8088, https://doi.org/10.15376/biores.13.4.8076-8088.10.15376/biores.13.4.8076-8088 ↗
52. Purusatama, B.D., Choi, J.K., Lee, S.H., and Kim, N.H. (2020). Microfibril angle, crystalline characteristics, and chemical compounds of reaction wood in stem wood of Pinus densiflora. Wood Sci. Technol. 54: 123–137, https://doi.org/10.1007/s00226-019-01140-w.10.1007/s00226-019-01140-w ↗
53. Rowell, R.M., Pettersen, R., Han, J.S., Rowell, J.S., and Tshabalala, M.A. (2012). Cell wall chemistry. In: Rowell, R.M. (Ed.), Handbook of wood chemistry and wood composites. CRC Press, Boca Raton, pp. 169–190.10.1201/b12487 ↗
54. Schwanninger, M., Rodrigues, J.C., Pereira, H., and Hinterstoisser, B. (2004). Effects of short-time vibratory ball milling on the shape of FT-IR spectra of wood and cellulose. Vib. Spectrosc. 36: 23–40, https://doi.org/10.1016/j.vibspec.2004.02.003.10.1016/j.vibspec.2004.02.003 ↗
55. Segal, L., Creely, J.J., Martin, A.E., and Conrad, C.M. (1959). An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Text. Res. J. 29: 786–794, https://doi.org/10.1177/004051755902901003.10.1177/004051755902901003 ↗
56. Shen, D., Li, N., Fu, Y., Macchioni, N., Sozzi, L., Tian, X., and Liu, J. (2018). Study on wood preservation state of Chinese ancient shipwreck Huaguangjiao I. J. Cult. Heritage 32: 53–59, https://doi.org/10.1016/j.culher.2018.01.009.10.1016/j.culher.2018.01.009 ↗
57. Singh, A.P. (1997). The ultrastructure of the attack of Pinus radiata mild compression wood by erosion and tunneling bacteria. Can. J. Bot. 75: 1095–1102, https://doi.org/10.1139/b97-120.10.1139/b97-120 ↗
58. Singh, A.P., Kim, Y.S., and Singh, T. (2016). Bacterial degradation of wood. In: Kim, Y.S., Funada, R., and Singh, A.P. (Eds.), Secondary xylem. Academic Press, London, pp. 169–190.10.1016/B978-0-12-802185-9.00009-7 ↗
59. Singh, A.P., Kim, J.S., Möller, R., Chavan, R.R., and Kim, Y.S. (2024). The pivotal role of microscopy in unravelling the nature of microbial deterioration of waterlogged wood: a review. Forests 15: 889, https://doi.org/10.3390/f15050889.10.3390/f15050889 ↗
60. Tanaka, F., Koshijima, T., and Okamura, K. (1981). Characterization of cellulose in compression and opposite woods of a Pinus densiflora tree grown under the influence of strong wind. Wood Sci. Technol. 15: 265–273, https://doi.org/10.1007/bf00350944.10.1007/BF00350944 ↗
61. Wang, X., Chen, W., Liang, Y., and Li, N. (2025). Physical and chemical degradation characteristics of waterlogged archaeological wood from the Wenzhou no. 1 shipwreck. Heritage Sci. 13: 520, https://doi.org/10.1038/s40494-025-02034-w.10.1038/s40494-025-02034-w ↗
62. Zhang, H., Shen, D., Zhang, Z., and Ma, Q. (2022). Characterization of degradation and iron deposits of the wood of Nanhai I shipwreck. Heritage Sci. 10: 202, https://doi.org/10.1186/s40494-022-00845-9.10.1186/s40494-022-00845-9 ↗