研究目的
To study the roles of accessible and inaccessible cellulose in the load transfer of eucalyptus wood using deuterium exchange combined with near infrared spectroscopy.
研究成果
Polarized NIR spectroscopy of deuterated E. regnans wood confirmed that inaccessible hydroxyl groups were oriented more parallel to the grain compared to the accessible fraction. NIR spectroscopy also confirmed that tensile stress caused wood to adsorb moisture. The effect of mechanical strain on NIR spectra could be highlighted by removing desorption and re-protonation effects through averaging loading and unloading cycles. The prominent bands at 6420, 6240 and 4670 cm-1, assigned to hydroxyl groups, remained after deuteration, suggesting that the inaccessible fraction of cellulose was the major load-carrying structure. A small band responding to mechanical strain at around 4700 cm-1 in deuterated wood might indicate a contribution of accessible hydroxyls in load transfer.
研究不足
The study was limited by the effects of desorption and isotope re-exchange due to environmental fluctuations, which were compensated by averaging loading and unloading cycles. The risk of re-protonation during sample handling and spectra collection was also a limitation.
1:Experimental Design and Method Selection:
Deuterium exchange combined with near infrared spectroscopy was used to study the roles of accessible and inaccessible cellulose in the load transfer of eucalyptus wood. Monitoring the drying process helped to assign bands of deuterated wood samples. Polarized NIR spectra of protonated and deuterated samples confirmed that inaccessible hydroxyl groups in eucalyptus wood were preferably oriented in the longitudinal direction. The spectral changes on NIR spectra caused by mechanical strain could be highlighted by averaging loading and unloading cycles to compensate for effects of desorption and isotope re-exchange due to environmental fluctuations.
2:Sample Selection and Data Sources:
Five thin Eucalyptus regnans samples with a thickness of 0.5 to 1 mm in preferably radial direction were cut from sapwood of a quarter-sawn board with an air-dry density of 0.54 g/cm3 sourced from Canterbury, New Zealand.
3:5 to 1 mm in preferably radial direction were cut from sapwood of a quarter-sawn board with an air-dry density of 54 g/cm3 sourced from Canterbury, New Zealand.
List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Transmission NIR spectra were acquired using a Tensor 37 infrared spectrometer (Bruker, Germany) at a resolution of 8 cm-1 averaging 128 scans before and after deuteration. Deuterium oxide (99.9%, Sigma Aldrich, Australia) was used for deuteration.
4:9%, Sigma Aldrich, Australia) was used for deuteration.
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Samples were conditioned to constant weight in a sealed container over a saturated K2CO3 solution, equating to a relative humidity of 42.3%. Subsequently, four samples were oven dried at 103 °C before being immersed in a sealed container containing 25 mL deuterium oxide at room temperature for 7 days. One of the samples was dried in a container over phosphorus pentoxide (P2O5) to 0.8% while spectra were taken at different drying stages to monitor the drying process. The other three samples used to study the effect of polarization and mechanical stretching were dried over P2O5 close to FSP (monitored by sample mass) and then equilibrated over saturated K2CO3 solution in D2O.
5:3%. Subsequently, four samples were oven dried at 103 °C before being immersed in a sealed container containing 25 mL deuterium oxide at room temperature for 7 days. One of the samples was dried in a container over phosphorus pentoxide (P2O5) to 8% while spectra were taken at different drying stages to monitor the drying process. The other three samples used to study the effect of polarization and mechanical stretching were dried over P2O5 close to FSP (monitored by sample mass) and then equilibrated over saturated K2CO3 solution in D2O.
Data Analysis Methods:
5. Data Analysis Methods: NIR spectra were normalized using the “scale” function in R. “Slope” spectra were defined as the rate of change of the intensity with increasing tensile strain and calculated as the slope coefficient of the linear regression between normalized spectral intensity at each wavenumber and applied strain.
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