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NMR determination of sorption isotherms in earlywood and latewood of Douglas fir. Identification of bound water components related to their local environment

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Published/Copyright: March 28, 2017
Holzforschung
From the journal Holzforschung Volume 71 Issue 6

Abstract

Earlywood (EW) and latewood (LW) have different hygromechanical behaviors, if subjected to relative humidity (RH) variations. To understand this effect better, the adsorption mechanisms of EW and LW of Douglas fir were studied by 2D 1H NMR relaxometry under conditions of equilibrium moisture content (EMC) at 20°C. Two bound water components were detected with relaxation times T1 and T2 indicating that they are located in distinct environments but these are similar in EW and LW. Sorption isotherms were calculated and analyzed based on the sorption model of Dent. A difference of sorption energy between the two water components is in agreement with their mobility difference observed on T1−T2 correlation spectra. Moreover, for the two bound water components, EW and LW exhibit different sorption isotherms at high RH. This may be attributed to a difference of adsorption capacity. Based on the macrofibril models provided by the literature, the following hypothesis is proposed: bound water components are located in lamellar and lenticular areas, both leading to possible deformations.

Keywords: 2D NMR relaxometry; 2D T1−T2 correlation spectra; earlywood; hemicelluloses; latewood; macrofibril; sorption isotherms

Acknowledgments

The Douglas supply by INRA Nancy (France) is acknowledged, in particular Julien Ruelle (LERFoB) for fruitful discussions. The manuscript was improved by the insightful comments of reviewers from Holzforshung.

References

Abragam, A. The Principles of Nuclear Magnetism. Clarendon Press, Oxford, 1961.10.1063/1.3057238Search in Google Scholar

Almeida, G., Gagné, S., Hernandez, R.E. (2007) A NMR study of water distribution in hardwoods at several equilibrium moisture contents. Wood Sci. Technol. 41:293–307.10.1007/s00226-006-0116-3Search in Google Scholar

Almeida, G., Huber, F., Perré, P. (2014) Free shrinkage of wood determined at the cellular level using an environmental scanning electron microscope. Maderas-Cienc. Tecnol. 16:187–198.10.4067/S0718-221X2014005000015Search in Google Scholar

Araujo, C.D., MacKay, A.L., Hailey, J.R.T., Whittall, K.P., Le, H. (1992) Proton magnetic resonance techniques for characterization of water in wood: application to white spruce. Wood Sci. Technol. 26:101–113.10.1007/BF00194466Search in Google Scholar

Araujo, C.D., Avramidis, S., MacKay, A.L. (1994) Behaviour of solid wood and bound water as a function of moisture content: a proton magnetic resonance study. Holzforschung 48:69–74.10.1515/hfsg.1994.48.1.69Search in Google Scholar

Boyd, J.D. (1982) An anatomical explanation for visco-elastic and mechano-sorptive creep in wood, and effects of loading rate on stregth. In: New Perspectives in Wood Anatomy, Eds. Martinus Nijhoff. Dr. W. Junk Publishers, La Hague. pp. 171–222.10.1007/978-94-017-2418-0_8Search in Google Scholar

Brown, R.J.S. (1989) Information available and unavailable from multiexponential relaxation data. J. Magn. Reson. 82:539–561.10.1016/0022-2364(89)90217-5Search in Google Scholar

Brunauer, S., Emmett, P.H., Teller, E. (1938) Adsorption of gases in multimolecular layers. J. Am. Chem. Soc. 60:309–319.10.1021/ja01269a023Search in Google Scholar

Brunauer, S., Deming, L.S., Deming, W.E., Teller, E. (1940) On a theory of the Van der Waals adsorption of gases. J. Am. Chem. Soc. 62:1723–1732.10.1021/ja01864a025Search in Google Scholar

Butler, J.P., Reeds, J.A., Dawson, S.V. (1981) Estimating solutions of first kind integral equations with nonnegative constraints and optimal smoothing. SIAM J. Numer. Anal. 18:381–397.10.1137/0718025Search in Google Scholar

Bytchenkoff, D., Rodts, S. (2011) Structure of the two-dimensional relaxation spectra seen within the eigenmode perturbation theory and the two-site exchange model. J. Magn. Reson. 208:4–19.10.1016/j.jmr.2010.09.007Search in Google Scholar PubMed

Care, S., Lenoir, N., Bertrand, F., Bornert, M. (2013) Microstructural and multiscale characterization of wood subjected to humidity by X-ray microtomography and magnetic resonance imaging. ICTMS Conference, Ghent, Belgium, p. 4.Search in Google Scholar

Carr, H.Y., Purcell, E.M. (1954) Effects of diffusion on free precession in nuclear magnetic resonance experiments. Phys. Rev. 94:630–638.10.1103/PhysRev.94.630Search in Google Scholar

Cox, J., McDonald, P.J., Gardiner, B.A. (2010) A study of water exchange in wood by means of 2D NMR relaxation correlation and exchange. Holzforschung 64:259–266.10.1515/hf.2010.036Search in Google Scholar

Dent, R.W. (1977) A multilayer theory for gas sorption. Part I: sorption of a single gas. Text. Res. J. 47:145–152.10.1177/004051757704700213Search in Google Scholar

Donaldson, L. (2007) Cellulose microfibril aggregates and their size variation with cell wall type. Wood Sci. Technol. 41:443–460.10.1007/s00226-006-0121-6Search in Google Scholar

D’Orazio, F., Bhattacharja, S., Halperin, W., Gerhardt, R. (1989) Enhanced self-diffusion of water in restricted geometry. Phys. Rev. Lett. 63:43–46.10.1103/PhysRevLett.63.43Search in Google Scholar PubMed

D’Orazio, F., Bhattacharja, S., Halperin, W.P., Eguchi, K., Mizusaki, T. (1990) Molecular diffusion and nuclear-magnetic-resonance relaxation of water in unsaturated porous silica glass. Phys. Rev. B 42:9810–9818.10.1103/PhysRevB.42.9810Search in Google Scholar PubMed

Engelund, E.T., Thygesen, L.G., Svensson, S., Hill, C.A.S. (2013) A critical discussion of the physics of wood-water interactions. Wood Sci. Technol. 47:141–161.10.1007/s00226-012-0514-7Search in Google Scholar

English, A.E., Whittall, K.P., Joy, M.L.G., Henkelman, R. (1991) Quantitative two-dimensional time correlation relaxometry. Magn. Reson. Med. 22:425–434.10.1002/mrm.1910220250Search in Google Scholar PubMed

Faure, P., Rodts, S. (2008) Proton NMR relaxation as a probe for setting cement pastes. Magn. Reson. Imaging 26:1183–1196.10.1016/j.mri.2008.01.026Search in Google Scholar PubMed

Faure, P., Caré, S., Po, C., Rodts, S. (2005) An MRI-SPI and NMR relaxation study of drying-hydration coupling effect on microstructure of cement-based materials at early age. Magn. Reson. Imaging 23:311–314.10.1016/j.mri.2004.11.034Search in Google Scholar PubMed

Faure, P., Peter, U., Lesueur, D., Coussot, P. (2012) Water transfers within hemp lime concrete followed by NMR. Cement Concrete Res. 42:1468–1474.10.1016/j.cemconres.2012.07.007Search in Google Scholar

Fourmentin, M. (2015) Impact de la répartition et des transferts d’eau sur les propriétés des matériaux de construction à base de chaux formulées. PhD thesis: Université Paris-Est, France.Search in Google Scholar

Greenspan, L. (1977) Humidity fixed points of binary saturated aqueous solutions. J. Res. Nbs. A Phys. Ch. 81A:89–96.10.6028/jres.081A.011Search in Google Scholar

Gril, J. (1988) Une modélisation du comportement hydro-rhéologique du bois à partir de sa microstructure. PhD thesis: Université Pierre et Marie Curie (Paris 6), France.Search in Google Scholar

Hahn, E.L. (1949) An accurate nuclear magnetic resonance method for measuring spin-lattice relaxation times. Phys. Rev. 76:145–147.10.1103/PhysRev.76.145Search in Google Scholar

Hailwood, A.J., Horrobin, S. (1946) Absorption of water by polymers. Analysis in terms of a simple model. Trans. Far. Soc. 42B:84–102.10.1039/tf946420b084Search in Google Scholar

Hill, C.A.S., Ramsay, J., Gardiner, B. (2015) Variability in water vapour sorption isotherm in Japanese Larch (Larix kaempferi Lamb.) – earlywood and latewood influences. Int. Wood Prod. J. 6:53–59.10.1179/2042645314Y.0000000090Search in Google Scholar

Hunt, D.G. (1990) Longitudinal shrinkage-moisture relations in softwood. J. Mater. Sci. 25:3671–3676.10.1007/BF00575403Search in Google Scholar

Javed, M.A., Kekkonen, P.M., Ahola, S., Telkki, V.-V. (2015) Magnetic resonance imaging study of water absorption in thermally modified pine wood. Holzforschung 69:899–907.10.1515/hf-2014-0183Search in Google Scholar

Kulasinski, K., Guyer, R., Derome, D., Carmeliet, J. (2015) Water adsorption in wood microfibril-hemicellulose system: role of the crystalline-amorphous surface. Biomacromolecules 16:2972–2978.10.1021/acs.biomac.5b00878Search in Google Scholar PubMed

Labbé, N., De Jéso, B.D., Lartigue, J.-C., Daudé, G., Pétraud, M., Ratier, M. (2002) Moisture content and extractive materials in maritime pine wood by low field 1H NMR. Holzforschung 56:25–31.10.1515/HF.2002.005Search in Google Scholar

Meiboom, S., Gill, D. (1958) Modified spin-echo method for measuring nuclear relaxation times. Rev. Sci. Instrum. 29:688–691.10.1063/1.1716296Search in Google Scholar

Meier, H., Wilkie, K.C.B. (1959) The distribution of polysaccharides in the cell-wall of tracheids of pine (Pinus silvestris L.). Holzforschung 13:177–182.10.1515/hfsg.1959.13.6.177Search in Google Scholar

Menon, R.S., MacKay, A.L., Hailey, J.R.T., Bloom, M., Burgess, A.E., Swanson, J.S. (1987) An NMR determination of the physiological water distribution in wood during drying. J. Appl. Polym. Sci. 33:1141–1155.10.1002/app.1987.070330408Search in Google Scholar

Porion, P., Faugère, A.M., Levitz, P., Van Damme, H., Raoof, A., Guilbaud, J.-P., Chevoir, F. (1998) A NMR investigation of adsorption/desorption hysteresis in porous silica gels. Magn. Reson. Imaging 16:679–682.10.1016/S0730-725X(98)00024-1Search in Google Scholar

Rodts, S., Bytchenkoff, D. (2010) Structural properties of 2D NMR relaxation spectra of diffusive systems. J. Magn. Reson. 205:315–318.10.1016/j.jmr.2010.04.021Search in Google Scholar PubMed

Salmén, L. (2015) Wood morphology and properties from molecular perspectives. Ann. For. Sci. 72:679–684.10.1007/s13595-014-0403-3Search in Google Scholar

Salmén, L., Burgert I. (2009) Cell wall features with regard to mechanical performance. A review. Holzforschung 63:121–129.10.1515/HF.2009.011Search in Google Scholar

Sasaki, M., Kawai, T., Hirai, A., Hashi, T., Odajima, A. (1960) A study of sorbed water on cellulose by pulsed NMR technique. J. Phys. Soc. Jpn. 15:1652–1657.10.1143/JPSJ.15.1652Search in Google Scholar

Sharp, A.R., Riggin, M.T., Kaiser, R, Schneider, M.H.. (1978) Determination of moisture content of wood by pulsed nuclear magnetic resonance. Wood Fiber Sci. 10:74–81.Search in Google Scholar

Sing, K.S.W., Everett, D.H., Haul, R.A.W., Moscou, L., Pierotti, R.A., Rouquerol, J., Siemeneawska, T. (1985) Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity. Pure Appl. Chem. 57:603–619.10.1351/pac198254112201Search in Google Scholar

Skaar, C. Wood-Water Relations. Springer-Verlag, Berlin, 1988.10.1007/978-3-642-73683-4Search in Google Scholar

Song, Y.Q., Venkataramanan, L., Hürlimann, M.D., Flaum, M., Frulla, P., Straley, C. (2002) T1-T2 correlation spectra obtained using a fast two-dimensional Laplace inversion. J. Magn. Reson. 154:261–268.10.1006/jmre.2001.2474Search in Google Scholar PubMed

Telkki, V.-V., Yliniemi, M., Jokisaari, J. (2013) Moisture in softwoods: fiber saturation point, hydroxyl site content, and the amount of micropores as determined from NMR relaxation time distributions. Holzforschung 67:291–300.10.1515/hf-2012-0057Search in Google Scholar

Vittadini, E., Dickinson, L.C., Chinachoti, P. (2001) 1H and 2H NMR mobility in cellulose. Carbohyd. Polym. 46:49–57.10.1016/S0144-8617(00)00282-4Search in Google Scholar

Whittall, K.P., MacKay, A.L. (1989) Quantitative interpretation of NMR relaxation data. J. Magn. Reson. 84:134–152.10.1016/0022-2364(89)90011-5Search in Google Scholar

Willems, W. (2015) A critical review of the multilayer sorption models and comparison with the sorption site occupancy (SSO) model for wood moisture sorption isotherm analysis. Holzforschung 69:67–75.10.1515/hf-2014-0069Search in Google Scholar

Winston, P.W., Bates, D.H. (1960) Saturated solutions for the control of humidity in biological research. Ecology 41:232–237.10.2307/1931961Search in Google Scholar

Received: 2016-9-15
Accepted: 2017-2-15
Published Online: 2017-3-28
Published in Print: 2017-6-27

©2017 Walter de Gruyter GmbH, Berlin/Boston

Articles in the same Issue

  1. Frontmatter
  2. Effects of thermo-hygro-mechanical (THM) treatment on the viscoelasticity of in-situ lignin
  3. 2D NMR characterization of wheat straw residual lignin after dilute acid pretreatment with different severities
  4. Determination of inorganic element distribution in the freeze-fixed stem of Al2(SO4)3-treated Hydrangea macrophylla by TOF-SIMS and ICP-AES
  5. NMR determination of sorption isotherms in earlywood and latewood of Douglas fir. Identification of bound water components related to their local environment
  6. The combined effects of initial microfibrillar angle and moisture contents on the tensile mechanical properties and angle alteration of wood foils during tension
  7. Fatigue behavior of Japanese cypress (Chamaecyparis obtusa) under repeated compression loading tests perpendicular to the grain
  8. Influence of strain rate, temperature and fatigue on the radial compression behaviour of Norway spruce
  9. Effect of conditioning history on the characterization of hardness of thermo-mechanical densified and heat treated poplar wood
  10. An innovative composite plywood for the acoustic improvement of small closed spaces
  11. Antioxidant activity of Scots pine heartwood and knot extractives and implications for resistance to brown rot
  12. Quantitative observation of the foraging tunnels in Sitka spruce and Japanese cypress caused by the drywood termite Incisitermes minor (Hagen) by 2D and 3D X-ray computer tomography (CT)
https://doi.org/10.1515/hf-2016-0152
Keywords for this article
2D NMR relaxometry; 2D T1−T2 correlation spectra; earlywood; hemicelluloses; latewood; macrofibril; sorption isotherms

Articles in the same Issue

  1. Frontmatter
  2. Effects of thermo-hygro-mechanical (THM) treatment on the viscoelasticity of in-situ lignin
  3. 2D NMR characterization of wheat straw residual lignin after dilute acid pretreatment with different severities
  4. Determination of inorganic element distribution in the freeze-fixed stem of Al2(SO4)3-treated Hydrangea macrophylla by TOF-SIMS and ICP-AES
  5. NMR determination of sorption isotherms in earlywood and latewood of Douglas fir. Identification of bound water components related to their local environment
  6. The combined effects of initial microfibrillar angle and moisture contents on the tensile mechanical properties and angle alteration of wood foils during tension
  7. Fatigue behavior of Japanese cypress (Chamaecyparis obtusa) under repeated compression loading tests perpendicular to the grain
  8. Influence of strain rate, temperature and fatigue on the radial compression behaviour of Norway spruce
  9. Effect of conditioning history on the characterization of hardness of thermo-mechanical densified and heat treated poplar wood
  10. An innovative composite plywood for the acoustic improvement of small closed spaces
  11. Antioxidant activity of Scots pine heartwood and knot extractives and implications for resistance to brown rot
  12. Quantitative observation of the foraging tunnels in Sitka spruce and Japanese cypress caused by the drywood termite Incisitermes minor (Hagen) by 2D and 3D X-ray computer tomography (CT)
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