Comparative studies on microstructures and chemical compositions of cell walls of two solid wood floorings

Two common wood flooring materials, taun (Pometia spp.) and cumaru (Dipteryx odorata), were used as investigated objects and comparison was made between the two wood species for their density, microstructure, microfibril angle (MFA), cellulose crystallinity and the main chemical composition. Results showed that the density of cumaru was 0.941 g·cm^?3, significantly larger than that of taun, 0.737 g·cm^?3. The biggest difference of two wood species in microstructures was fiber cells. Fiber cells of cumaru had dense cell walls, almost no cell lumens; while fiber cells of taun had relatively thin cell walls, with apparent cell lumens. The thickness of fiber cell wall of cumaru and taun were 6.80 and 2.82 µm, respectively, and the former is about 2.5 times thicker than the latter. Measured data of MFA indicated that the average MFA of cumaru was 11.7°, smaller than that of taun, 13.4°. The relative crystallinity of cumaru and taun were 54.0 and 50.8%, respectively. The two wood species had the similar holocellulose contents, but the lignin content of cumaru was higher than that of taun, especially that the content of extractive of cumaru was as twice as that of taun.     

Dual-axis electron tomography: a new approach for investigating the spatial organization of wood cellulose microfibrils

We have employed dual-axis electron tomography to investigate the 3D organization of cellulose microfibrils in plastic resin-embedded, delignified cell walls of radiata pine early wood. The ∼ 1 nm thick tomographic slices produced in this study provided for a resolution of ∼ 2 nm in the cross-section of the slices throughout the 150 nm thick plastic sections. This resolution is sufficient to resolve individual cellulose microfibrils and to map the 3D organization of the cellulose microfibrils within the S2 layer of the secondary cell walls. The individual cellulose microfibrils measure ∼ 3.2 nm in diameter, and appear to consist of a ∼ 2.2 nm unstained core and a ∼ 0.5 nm thick surface layer that is lightly stained. Both individual and clustered cellulose microfibrils are seen surrounded by more heavily stained and irregularly shaped residual lignin and hemicellulose. The tightness of packing of the cellulose microfibrils in the cluster varies along the thickness of the section. These findings demonstrate that dual-axis electron tomography is a technique that can provide new insights into the 3D organization of cellulose microfibrils in plant cell walls.     

Nanostructural assembly of cellulose,hemicellulose, and lignin in the middle layer of secondary wall of ginkgo tracheid

Physical, chemical, and biological properties of wood depend largely on the properties of cellulose, noncellulosic polysaccharides, and lignin, and their assembly mode in the cell wall. Information on the assembly mode in the main part of the ginkgo tracheid wall (middle layer of secondary wall, S2) was drawn from the combined results obtained by physical and chemical analyses of the mechanically isolated S2 and by observation under scanning electron microscopy. A schematic model was tentatively proposed as a basic assembly mode of cell wall polymers in the softwood tracheid as follows: a bundle of cellulose microfibrils (CMFs) consisting of about 430 cellulose chains is surrounded by bead-like tubular hemicellulose-lignin modules (HLM), which keep the CMF bundles equidistant from each other. The length of one tubular module along the CMF bundle is about 16 ± 2 nm, and the thickness at its side is about 3–4 nm. In S2, hemicelluloses are distributed in a longitudinal direction along the CMF bundle and in tangential and radial directions perpendicular to the CMF bundle so that they are aligned in the lamellae of tangential and radial directions with regard to the cell wall. One HLM contains about 7000 C₆-C₃ units of lignin, and 4000 hexose and 2000 pentose units of hemicellulose.     

TEM/FE-SEM studies on tension wood fibres of Acer spp., Fagus sylvatica L. and Quercus robur L.

Tension wood (TW) fibres from maple, beech and oak were analysed with special emphasis on the cell wall fine structure and deposition of aromatic compounds within the gelatinous layer (GL). For this purpose, transmission electron microscopy (TEM) was applied after section staining with potassium permanganate. There was evidence for the occurrence of aromatic compounds in the GLs of fibres of all three species. Some GLs showed a concentric sub-layering. Hence, conclusions about the biosynthetic activities during cell wall formation in TW could be derived. Additional information about structural characteristics of TW fibres were obtained by means of field emission electron microscopy. High-resolution micrographs of cell walls were used for measurements of diameter and microfibril angle (MFA) of cellulose aggregates (CAG). CAG of 7 nm were observed although their diameter varied greatly in the GLs. MFA in the secondary wall of TW was slightly smaller than in opposite wood. The microscopic methods provided complementary ultrastructural and topochemical information on tension wood fibres. The subcellular localisation of aromatic compounds and the observations of the ultrastructural morphology will contribute to the understanding of origin and functionality of TW and its characteristic GL.     

An investigation on the transition characteristics of the wood cell walls during carbonization

The structural changes of the cell wall and crystalline cellulose of Quercus variabilis wood in a pyrolysis system at several temperatures ranging from 250 to 500°C were investigated to examine the wood carbonization characteristics. The volume of the wood sample was decreased and the weight loss was increased by increasing the carbonization temperature. Vessels collapsed severely in tangential direction during the charring process above 350°C. SEM observation indicated that the layering structure of the walls in wood fibers and parenchyma cells were retained below 300°C. However, the cell walls above 350°C changed to an amorphous-like structure without cell wall layering. X-ray diffraction confirmed that the cellulose crystalline substance was still remained at the carbonization temperature of 300°C but was not detected above 350°C. It can be concluded that the transition from Q. variabilis wood to charcoal might occur at approximately 350°C.     

Modulus of elasticity in scarf-jointed wooden beams: a case study with polyvinyl acetate and isocyanate adhesives

In the present study, elastic properties of scarf-jointed oak (Quercus castaneifolia) timbers with the application of two different types of adhesives (polyvinyl acetate and isocyanate) were evaluated using free flexural vibration of free–free beam method in different flexural directions of vibration, i.e., tangential and redial directions. Samples were taken from trees of Hyrcanian forests in Iran with nominal dimensions of 20 × 20 × 360 mm³. Comparing the results of elastic properties of clear oak wood beams with scarf-jointed samples wood showed that scarf joints with the bonding angles of 70° and 75°, covered by polyvinyl acetate adhesive, did not demonstrate any significant effect on modules of elasticity. Scarf-jointed beams with smaller joint angles (60° and 65°) were considerably weaker or totally unreliable in their moduli of elasticity. It is also shown that the magnitude of effect gets worst by using isocyanate rather than polyvinyl acetate adhesive.     

火炬松不同种源纸浆材材性的变异

1983年火炬松31个种源引种栽培在浙江富阳中国林业科学研究院亚热带林业研究所实验林场,研究表明该批种源间10年生树木生长量和纸浆材材性因子如晚材率、管胞形态特征值(管胞长度、宽度、腔径、壁厚、长宽比、腔径比、壁腔比)、管胞S2层微纤丝角和木材基本密度存在着显著差异,木材主要化学成分中纤维素和木素含量种源间存在着显著差异,而戊聚糖和苯醇浸提物含量种源间差异不显著.这些材性特征除了木材化学性状因子外,均受中等以上程度遗传控制.木材纤维素、木素、戊聚糖和苯醇浸提物含量的广义遗传力分别为0.088、0.003、0.340和0.307,其余性状广义遗传力均大于0.50.引种地栽培环境对木材性状有显著影响.种源原产地纬度与树木生长量、管胞宽度、管胞直径和管胞微纤丝角呈负相关,与晚材率、木材密度呈正相关.31个种源树木胸高直径与管胞长宽比、管胞壁腔比、木材密度呈显著负相关,与管胞宽度、管胞直径、管胞腔径比呈正相关.     

Reaction wood anatomy and lignin distribution in <Emphasis Type="Italic">Gnetum gnemon</Emphasis> branches

This study investigated the anatomical and chemical characteristics of the reaction wood of a gymnpsperm species, Gnetum gnemon, and discussed on contributing factor for the type of reaction wood in this species. Cell morphology, microfibril angle (MFA) of the S₂ layer and lignin distribution in secondary walls of tracheary elements, and lignin content were examined on three branches. Observations included no G-layer formation, significant decreases in vessel frequency, and altered MFA, and visible-light absorbance after lignin colour reactions in tracheid and fiber tracheid walls on the upper side in almost all samples. These results suggest that reaction wood in G. gnemon was similar to that in ‘tension-wood-like-reaction wood’ in angiosperms. On the other hand, reaction wood showed decrease in the lignin concentration in the fiber tracheid walls compared to the tracheid walls. In addition, the lignin in the tracheid and fiber tracheid walls was originally rich in syringyl units, suggesting that changes in the anatomical and chemical characteristics of secondary xylem due to reaction wood formation might relate to the ratio of the syringyl to guaiacyl units in lignin in the cell walls which function for mechanical support.     

Enzymatic hydrolysis of wood with alkaline treatment

Pulverized samples of wood, cedar and eucalyptus were treated with 5 N NaOH solutions at 25–150 °C. Hemicellulose and lignin content in the samples decreased with increasing treatment temperatures, while the recovery of glucose was maintained at nearly 90 %. X-ray diffraction analysis showed that the content of the original cellulose I structure in the samples decreased with increasing temperature, and most of the cellulose in the sample treated at 150 °C was converted to cellulose II by mercerization. Enzymatic hydrolysis of the alkaline-treated samples was carried out at 37 °C using solutions comprising a mixture of cellulase and β-glucosidase. The samples treated at higher temperatures showed better enzymatic degradability. Treatment with an alkaline solution of lower concentration (1 N NaOH) at 150 °C was also used. Despite significant quantities of hemicellulose and lignin being removed, mercerization was not induced. The enzymatic degradability was much lower than that of the sample treated with a 5 N NaOH solution at 150 °C. Thus, treatment with concentrated alkaline solution at high temperature led to not only the removal of hemicellulose and lignin, but also to modification of the cellulose structure, which resulted in high efficiency of enzymatic saccharification of the wood samples.     

Creep and stress relaxation behavior for natural cellulose crystal of wood cell wall under uniaxial tensile stress in the fiber direction

We investigated the temporal changes in creep and stress relaxation behavior in both microscopic crystalline cellulose and macroscopic strain of wood specimen using Japanese cypress (Chamaecyparis obtusa Endl.) to understand the viscoelastic properties of wood cell walls. Specimens 600 µm in thickness were observed by the X-ray diffraction and submitted to tensile load. The crystal lattice strain of (004) plane and macroscopic strain of specimen were continuously detected during creep and stress relaxation tests. It was found that the creep compliance based on macroscopic strain showed a gradual increase after instantaneous deformation due to loading and then the parts of creep deformation remained as permanent strain after unloading. On the other hand, crystal lattice strain showed a different behavior for macroscopic strain; it kept a constant value after instantaneous deformation due to loading and then increased gradually after a certain period of time. These differences between macroscopic and microscopic levels were never found in the stress relaxation tests in this study. Relaxation modulus at the macroscopic level only showed a decreasing trend throughout the relaxation process. However crystal lattice strain kept a constant value during the macroscopic relaxation process. In addition, the microfibril angle (MFA) of wood cell wall has a role of mechanical behavior at microscopic level; crystal lattice strains were smaller with increasing MFA at both creep and relaxation processes. Creep compliance and stress relaxation modulus at the macroscopic level decreased and increased with increasing MFA, respectively. Our results on the viscoelastic behavior at microscopic level evidenced its dependency on MFA.     

Characterization of lignin-derived products from Japanese beech wood as treated by two-step semi-flow hot-compressed water

Japanese beech (Fagus crenata) wood was treated by two-step semi-flow hot-compressed water (the first stage: 230 °C/10 MPa/15 min, the second stage: 270 °C/10 MPa/15 min), and produced lignin-derived products in the hot-compressed water-soluble portions at the first and second stages, and the final residue of the second stage was characterized with alkaline nitrobenzene oxidation method and gel permeation chromatographic analysis. As a result, the lignin-derived products at the first stage, where hemicellulose was also decomposed, consisted of lignin-based monomers and dimers and oligomers/polymers in the water-soluble portion. A large part of the oligomers/polymers was, however, recovered as the precipitate during 12 h setting after hot-compressed water treatment. By the analysis of nitrobenzene oxidation products, there were relatively higher contents of ether-type lignin in the precipitate at the first stage than in original beech wood. Since the ether linkages of lignin are more preferentially cleaved by this hot-compressed water, lignin-based polymeric fractions were flowed out from the porous cell walls from which hemicellulose was removed. On the other hand, at the second stage condensed-type lignin remained in the precipitate and residue. Based on these results, decomposition behavior of lignin in Japanese beech wood as treated by the two-step semi-flow hot-compressed water was discussed regarding the topochemistry of lignin structure.     

The influence of acetosolv pulping conditions on the enzymatic hydrolysis of Eucalyptus pulps

Eucalyptus globulus wood was subjected first to HCl–catalysed delignification with 70% acetic acid under conditions realizing an incomplete 3 × 3 × 3 factorial design (HCl concentration 0, 0.025 or 0.05%; temperature 120, 140 or 160 °C; reaction time 1, 2.5 or 4 h), and then to enzymatic hydrolysis. The hydrolysis kinetics conformed to both Ghose's empirical model and a biexponential equation. The biexponential fit implies the presence of both readily and reluctantly hydrolysed cellulose fractions, and the fitted coefficients show hydrolysis yield to depend largely on the digestibility of the latter. Multiple regression of performance variables on pulping conditions showed that neither the rate nor the extent of hydrolysis is greatest for pulps with minimum lignin or xylose contents; we attribute this circumstance to the condensation and precipitation of lignin under severe pulping conditions, which protects the cellulose of the pulp from enzymatic attack. Received 20 June 1998     

Provenance variation in growth and wood properties of juvenile Cyclocarya paliurus

Cyclocarya paliurus is a highly valued and multiple function tree species. There has been increasing interest in planting and managing C. paliurus for timber production and medical use owing to loss of harvestable acreage. Seed from six provenances was collected from the main natural range of this species. Significant variation in growth and wood properties was measured among the six provenances at age 7 years. Provenance mean height and DBH varied significantly from 730–991 and 6.7–10.0 cm, whereas provenance means of wood basic density and crystallinity ranged from 463–554 kg m^?3 and 51.4–74.1 %, respectively. Mean provenance microfibril angle (MFA) at breast height ranged from 18.1° to 23.2°, while MFA at breast height varied from 11.0° to 34.5° among growth rings which showed a consistent pith-to-bark trend of declining angles. There was no significant relationship of growth rate with latitude or longitude of seed sources, however, provenances from low latitude and longitude grew faster at the trial site. Wood quality was significantly related to latitude of seed sources, showing a positive correlation for both wood basic density and wood crystallinity, but a highly negative association with MFA. Significant correlations between wood properties measured indicated that there exists a great opportunity to improve wood quality of C. paliurus through selection of juvenile trees with low MFA.     

Recycled ionic liquid 1-ethyl-3-methylimidazolium acetate pretreatment for enhancing enzymatic saccharification of softwood without cellulose regeneration

In this work, pretreatment of wood meals using a recycled ionic liquid (IL), 1-ethyl-3-methylimidazolium acetate ([Emim]Ac), enhanced glucose liberation by enzymatic saccharification, without dissolution of cellulose and lignin. In contrast, previous studies on IL pretreatment have mostly focused on lignocellulosic dissolution to regenerate cellulose and removing lignin. Softwood (Cryptomeria japonica) was pretreated with [Emim]Ac at 60–100 °C for 2–8 h without collecting regenerated cellulose. The pretreatment did not have a strong effect on wood component dissolution (weight of residues: 91.7–98.8%). The residues contained relatively high amounts of lignin (26.6–32.6%) with low adsorption of [Emim]Ac (0.9–2.7%). Meanwhile, the crystallinity index (C _r I) of cellulose in the wood was significantly reduced by pretreatment, from 50.9% to 28.4–37.1%. In spite of the high lignin contents in the residues, their glucose liberation values by enzymatic saccharification using a cellulase mixture were 3–16 times greater than that of untreated wood. A good correlation was found between the saccharification effectiveness of pretreated samples and the C _r I. Although lignin dissolved in [Emim]Ac continued to accumulate after repeated use of [Emim]Ac, the pretreatment was found to be effective for three consecutive cycles without the need to remove the dissolved materials.     

Quantifying lignin and holocellulose content in coniferous decayed wood using near-infrared reflectance spectroscopy

To determine the independent decomposition rates of lignin and cellulose of decayed woody debris, a technique for the rapid analysis of lignin and cellulose is required. We applied a near-infrared spectroscopy (NIRS) technique to measure the lignin and holocellulose content in decayed wood. We succeeded in creating partial least-squares (PLS) models to estimate the lignin and holocellulose content in the decayed wood of five species using NIR spectra. Although the accuracy was acceptable for the estimation of a five-species mixed model (R ² = 0.970 for lignin and R ² = 0.962 for holocellulose), it was further improved when the model was applied to each species independently. This combination of NIRS and a PLS model is a valuable tool for the determination of the lignin and holocellulose content in decayed wood. The technique is time efficient (3 min per sample) and non-hazardous (no acid treatment is required).     

Influence of initial planting spacing and genotype on microfibril angle,wood density,fibre properties and modulus of elasticity in Pinus radiata D. Don corewood

Pinus radiata D. Don trees from six clones, grown at initial spacings of 2500 stems ha⁻¹ and 833 stems ha⁻¹ were destructively harvested. For these trees wood properties were measured on radial slices sampled at a height of 1.4 m above the ground. Relative to wide spacing, close initial stand spacing significantly reduced microfibril angle (MFA) and ring width and significantly increased dynamic modulus of elasticity (MOE), fibre length, latewood percentage and cell wall thickness. Density and fibre width were not significantly different between spacing treatments. Examination of the influence of genetic population on wood properties indicated that genotype significantly influenced MFA, MOE and ring width. The key wood properties MFA, MOE and fibre length were regressed against tree diameter, height and stem slenderness. All three wood properties were most strongly correlated with stem slenderness. Multiple regression models developed for MFA, MOE and ring width accounted for respectively 62%, 81% and 58% of the variation in these variables. The following changes occurred in sampled properties with increasing ring number: MFA and ring width declined markedly; MOE and fibre length increased markedly; latewood percentage and cell wall thickness increased slightly; and density and fibre width did not show any radial trend.     

Histological changes in the cell wall structure during wood decay by Trametes hirsuta and Trametes versicolor in neem (Azadirachta Indica A. Juss)

ABSTRACT

Structural alterations in the wood cell walls of neem inoculated with by Trametes hirsuta and T. versicolor were studied by microscopic methods. In vitro decayed wood showed extensive weight loss of test blocks (26.7 and 41.38% by T. versicolor and T. hirsuta, respectively) at the end of 3 months. Selective delignification in the initial phase followed by simultaneous removal of lignin was evident in test blocks inoculated with both the species. The separation of middle lamellae and patches of cellulosic polysaccharides stained blue with Astra blue in the delignified region of the fiber wall during early stages indicates selective mode of decay. In contrast, the occurrence of erosion troughs with characteristic U-notch in tangential sections is a characteristic feature of simultaneous rot that was apparent after 3 months of incubation. The decay pattern occurred concomitantly in all the xylem elements irrespective of general resistance pattern shown by vessel and axial parenchyma cells. At an advance stage, both species of Trametes showed formation of erosion channels along the microfibrils angle of cellulose which is considered as characteristics of soft rot decay type. The sharing of white rot and soft rot decay pattern by both the fungi suggest a phylogenetic link between both groups of fungi.     

A review of wood thermal pretreatments to improve wood composite properties

The objective of this paper is to review the published literature on improving properties of wood composites through thermal pretreatment of wood. Thermal pretreatment has been conducted in moist environments using hot water or steam at temperatures up to 180 and 230 °C, respectively, or in dry environments using inert gases at temperatures up to 240 °C. In these conditions, hemicelluloses are removed, crystallinity index of cellulose is increased, and cellulose degree of polymerization is reduced, while lignin is not considerably affected. Thermally modified wood has been used to manufacture wood–plastic composites, particleboard, oriented strand board, binderless panels, fiberboard, waferboard, and flakeboard. Thermal pretreatment considerably reduced water absorption and thickness swelling of wood composites, which has been attributed mainly to the removal of hemicelluloses. Mechanical properties have been increased or sometimes reduced, depending on the product and the conditions of the pretreatment. Thermal pretreatment has also shown to improve the resistance of composites to decay.     

Distribution of structure and lignin within growth rings of Norway spruce

A radial core from a Norway spruce (Picea abies (L.) Karst.) estimated to be about 107 years old was cut from a board and was analyzed for density and microfibril angle (MFA). Furthermore, cell geometry, wall thickness and lignin distribution were analyzed on three selected growth rings in detail. Intra-ring differences in the density profiles are also true for cell wall thicknesses as well as radial and tangential lumen diameters. A higher MFA was found for earlywood with a slow decrease toward the latewood region. The lignin was found to remain rather constant throughout the growth rings, which suggests a constant chemical composition of the cell wall material within the growth ring. From the recorded datasets on a cellular level, it can be concluded that the main adaptation regarding structure–property relationships toward the optimization of water transport and mechanical stability is mainly achieved at the cell level.