Distribution of lignin in normal and tension wood

Summary The distribution of lignin in normal and tension wood of four hardwood species has been studied by examination in the electron microscope of the lignin skeletons remaining after removal of the polysaccharides with hydrofluoric acid. In normal wood fibers, the S₁ had a higher lignin concentration than the S₂ layer, which was not as highly lignified as in conifer tracheids. Vessels had a high concentration of lignin in both normal and tension wood, while the extent of lignification of the parenchyma was variable.In tension wood fibers, the S₁ and S₂ layers were highly lignified. A thick, unlignified G-layer was often associated with an extremely thin S₂ layer with a high concentration of lignin. In both normal and tension wood, the lignin had the same orientation as the cellulose micro-fibrils in the different cell wall layers. The results confirm the earlier conclusion that, in the species investigated, the same amount of lignin is present in gelatinous as in normal fibers. Evidently, the lignification mechanism operates normally in the non-gelatinous layers of the fibers, as well as in the vessels and in the parenchyma of tension wood.

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Zusammenfassung Die Ligninverteilung im Normalholz und im Druckholz von vier Laubhölzern wurde untersucht. Die Ligningerüste, die nach der Entfernung der Polysaccharide durch Fluorwasser-stoffsäure übrigblieben, wurden im Elektronenmikroskop beobachtet. In den Normalholzfasern hatte die S₁-eine höhere Ligninkonzentration als die S₂-Schicht, die weniger lignifiziert war als in den Koniferentracheiden. Die Gefäße hatten eine hohe Ligninkonzentration in sowohl Normal-als in Zugholz, während der Lignifizierungsgrad der Parenchymzellen variierte.In den Zugholzfasern waren die S₁- und S₂-Schichten völlig lignifiziert. Eine dicke, unlignifizierte G-Schicht war oft mit einer außerordentlich dünnen S₂-Schicht, die eine hohe Ligninkonzentration zeigte, verbunden. Sowohl im Normal- wie auch im Zugholz besaß das Lignin dieselbe Orientierung wie die Cellulosemikrofibrillen in den verschiedenen Zellwandschichten. Die Ergebnisse bestätigen den früheren Schluß, daß in den hier untersuchten Laubhölzern in den gelatinösen und in den normalen Fasern dieselbe Ligninmenge vorliegt. Offenbar läuft der Mechanismus der Lignifizierung in den S₁- und S₂-Schichten der gelatinösen Fasern des Zugholzes normal ab.

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This investigation was supported by the United States Department of Agriculture, Forest Service, through Forest Service Research Grant No. 1, which is hereby gratefully acknowledged.     

Anatomy and lignin distribution of reaction wood in two Magnolia species

Summary Anatomical features of reaction wood formed in two Magnolia species, M. obovata Thunb. and M. kobus DC. which are considered to be among the primitive angiosperms, were observed. In addition, the distribution of guaiacyl and syringyl units of lignins in the cell walls of normal and reaction wood was examined using ultraviolet (UV)- and visible light (VL)- microspectrophotometry coupled with the Wiesner and M?ule reactions. The two Magnolia species formed a tension-like reaction wood without possessing the typical gelatinous layer (G-layer) on the upper side of the inclined stem or branch, in which a radial growth promotion occurred. Compared with the normal wood, the reaction wood had the following anatomical features: (1) the secondary walls of fiber tracheids lacked the S₃ layer, (2) the innermost layer of fiber-tracheid walls showed a small microfibril angle, a fact being similar to the orientation of the microfibril angle of the G-layer in tension wood, and (3) the amounts of lignin decreased in the cell walls of fiber tracheids, especially with great decrease in proportion of guaiacyl units in lignins. In addition, VL-microspectrophotometry coupled with the Wiesner and M?ule reactions adopted in the present study showed potential to estimate the lignin contents in the cell walls and the proportion of guaiacyl and syringyl units in lignins. Received: 15 July 1998     

Distribution of lignin in normal and compression wood of Pinus taeda L.

Summary The distribution of lignin in normal and compression wood of loblolly pine (Pinus taeda L.) has been studied by the technique of lignin skeletonizing. Hydrolysis of the wood carbohydrates with hydrofluoric acid left normal wood tracheids with a uniform distribution of lignin in the S1 and S2 cell wall layers. However, the S3 region of both earlywood and latewood tracheids consistently retained a dense network of unhydrolyzable material throughout, perhaps lignin.Lignin content in compression wood averaged about 7% more than in normal wood and appears to be concentrated in the outer zone of the S2 layer. The inner S2 region, despite helical checking, is also heavily lignified. The S1 layer, although thicker than normal in compression wood tracheids, contains relatively little lignin.Ray cells, at least in normal wood, appear to be lignified to the same extent, if not more so in certain cases, than the longitudinal tracheids. Other locations where lignin may be concentrated include initial pit border regions and the membranes of bordered pits.This report is a detailed excerpt from the Ph. D. dissertation of R. A. P. Financial support provided by the College of Forestry at Syracuse University and the National Defense Education Act is hereby gratefully acknowledged.     

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.     

Fluid permeability in poplar tension and normal wood in relation to ray and vessel properties

The impact of ray and vessel features on the radial air permeability and liquid penetration was compared between poplar (Populus nigra) tension and normal wood. Air permeability was measured by the falling-water volume-displacement method. To measure liquid penetration, specimens were saturated with safranin solution by the full-cell process at low pressure, and the pattern of red color penetration was then examined. Results revealed no significant difference in vessel frequency, intervessel and vessel-ray pit diameter between tension and normal wood, whereas porosity and average vessel lumen area in normal wood were significantly greater than those in tension wood. Regarding rays, their length was not different between normal and tension wood, but the latter had more frequent rays per millimeter. Since xylem rays are important flow conduits in lateral movement of fluids, it could be hypothesized that a larger number of rays in tension wood would lead to improved radial permeability. However, neither air permeability nor liquid penetration varied significantly in the studied specimens. Consequently, the results proved that ray frequency has no determining role in radial fluid flow in poplar tension and normal wood and that the share of intervessel and vessel-ray pits in radial permeability is more important.     

Enzymic isolation of lignin from wood and pulps

After enzymic hydrolysis of polysaccharides in milled wood or pulp the unhydrolysed lignin residue becomes soluble in certain polar solvents. Extensive disintegration of the wood is necessary to obtain a sufficient accessibility toward the enzyme. For milling a porcelain rotary ball mill is recommended. A relationship has been found between the milling energy, which is proportional to the size of the mill, the milling time, and the yield of ball-milled wood lignin (BMWL). Enzymatically isolated lignin (EIL) requires a critical milling time which is shorter than that for obtaining maximum yields of BMWL. A procedure for isolation of the total lignin content from wood and pulps in the form of three fractions has been developed, giving a water soluble, low molecular carbohydrate-lignin complex by water extraction of ball-milled wood, a BMWL-carbohydrate complex by subsequent extraction with dioxane, and a EIL-carbohydrate complex by dioxane extraction of the residue after enzymic hydrolysis.     

A kinetic study of the acetylation of cellulose, hemicellulose and lignin components in wood

The rates of acetylation of Deal, Larch, Southern Yellow Pine and Sitka Spruce using acetic anhydride in xylene have been measured and compared with the composition of the woods. Although these woods have similar macroscopic characteristics, the correlation between rate of acetylation and composition remains unclear, although the holocellulose may play a role in converting the hydrophilic hydroxyl groups to hydrophobic acetyl groups. The rate of acetylation of Larch at 373 K was insignificant but the other wood samples showed significant acetylation at this temperature. The activation energies for the acetylation process suggest that several routes may be involved.     

Condensation of lignin during heating of wood

Summary The structural change of lignin during heating of wood was investigated quantitatively by a method combining nucleus exchange and nitrobenzene oxidation. Lignin modification during heating was mainly a diphenylmethane type condensation. About 40 and 75% of noncondensed units in protolignins were converted to diphenylmethane type units by heating of dry and wet wood meals up to 220 °C, respectively. On the other hand, during heating of modified lignin (dioxane lignin) various types of modifications in addition to diphenylmethane type condensation occurred. Lignin modification via the diphenylmethane type condensation was proposed as a new route for its utilization.     

The application of ultraviolet microscopy to the distribution of lignin in wood description and validity of the technique

A method has been developed for the determination of lignin distribution in the wood cell wall by ultraviolet microscopy. The method incorporates some important advances on previus applications of UV microscopy to the study of lignin distribution. Ultrathin cross-sections of wood are obtained by the sample preparation and sectioning techniques of electron microscopy. The specimens are examined in monochromatic ultraviolet light using quartz reflection optics. The microscope image is photographically recorded and the negative is subsequently subjected to densitometric analysis. Each stage of the analytical procedure has been critically assessed to determine its validity and limitations. The method is ideally suited to the study of the removal of lignin from the wood cell wall during cooking and possesses other important applications in wood technology.     

Chemical composition of wood and its connection with wood anatomy in Betula pubescens

ABSTRACT

The connection between chemical composition and anatomy of wood is poorly studied. Abiotic and biotic growth conditions affect the synthesis of structural compounds and the anatomy of wood at the same time as they affect growth. In this study, the wood chemical composition, and connections between wood chemistry and anatomy were studied in downy birch (Betula pubescens Ehrh.) grown on four growth sites possessing mineral and peat soils. Lignin, holocellulose, extractive and ash contents, and effective heating value were analysed and compared with libriform fibre double wall thickness and lumen diameter, vessel size and number, and ray and axial parenchyma numbers. Measured lignin and extractive contents were exceptionally high and holocellulose content low. Correlations between wood anatomy and effective heating value were partly different on different soils. Correlations between holocellulose and anatomy were the opposite of the correlations between other chemical compounds and anatomy. The significant correlations between chemical composition and anatomy were commonly opposite in trees grown on peat than in trees grown on mineral soil. Particularly, vessel characteristics and fibre wall thickness correlated significantly with wood chemistry in trees grown on mineral soil. The connections between wood anatomy and chemistry proved to be soil-dependent.     

Ethylene and tension wood formation in Eucalyptus gomphocephala

Summary Eucalyptus gomphocephala A.DC seedlings grown horizontally for 103 days had less terminal shoot elongation and higher internal and emanated ethylene levels in the basal portion of the stem than seedlings grown vertically under otherwise identical conditions. Horizontal seedlings had greater radial growth in the upper stem half than in the lower half of the basal portion of the stem. Upper halves contained 60–80 percent tension wood by volume, lower halves 0–10 percent tension wood. Radial growth in vertical seedlings was symmetrical, and they contained negligible tension wood. Upper halves of the basal portion of the stem of horizontal seedlings had greater amounts of internal and emanated ethylene than lower halves and vertical seedling halves. Ethylene differences between random halves of vertical seedlings were smaller than differences between upper and lower halves of horizontal seedlings. The data suggest an association between increased ethylene levels and tension wood formation.This work was made possible through the award of a Fulbright Postdoctoral Fellowship and an Honorarium to N. D. Nelson by the Australian-American Educational Foundation and CSIRO Division of Building Research, respectively, and is part of a larger body of research by the authors on hormonal aspects of wood quality in rapidly grown Eucalyptus spp. Appreciation is experssed to Peter Fitzgibbon and Jugo Ilic for competent technical assistance.     

Comparative studies on lignin distribution by UV microscopy and bromination combined with EDXA

Summary In order to elucidate a previously reported discrepancy in the ratio of the lignin concentration in the middle lamella to that in the secondary wall as determined by ultraviolet (UV) microscopy and bromination combined with EDXA, the ultraviolet absorptivity of the lignin and the lignin reactivity towards bromination were compared for black spruce wood (Picea mariana Mill.). In addition, UV microscopy and EDXA techniques were applied to the determination of lignin distribution in the tracheids in order to establish the relationship between the two techniques. The results indicated that, although the ultraviolet absorptivity in different morphological regions is essentially the same, the secondary wall lignin was 1.70 times more reactive towards bromination than the middle lamella lignin. By applying the value of 1.70 as a correction to the EDXA results, the estimated lignin distribution by EDXA was in fairly good agreement with that from UV microscopy.The authors would like to thank Dr. J.-F. Revol and Dr. M. Tsuji for their assistance during this study     

Analysis of birch wood lignin by oxidative degradation

Summary The lignin in birch wood has been subjected to analysis by oxidative degradation after milling of wood samples in a Wiley mill and in a rotatory ball mill. For comparison milled wood lignin from birch has also been analysed. It was found that the type of milling affects both the total yield of degradation acids and their relative frequency of occurrence. These findings are interpreted as being due to a cleavage of aryl ether linkages during the milling procedure. The oxidative degradation analysis gave rise to a total of 30 different acids which were tentatively identified on the basis of their mass spectral fragmentation patterns. Among the acids some were found having either a phenoxyacetic acid or a phenoxypropionic acid structure. The possible origin of these is discussed. A grant to one of us (R.A.N.) from Jacob Wallenbergs Forskningsstiftelse is gratefully acknowledged. Thanks are due to Kristina Gustafsson for skilful experimental assistance     

Stiffness of normal, opposite, and tension poplar wood determined using micro-samples in the three material directions

Mechanical tests on micro-samples were performed in the three material directions in normal, opposite, and tension wood collected from a poplar tree. Two custom micro-devices were designed and built in the laboratory to test samples under pure tension in the transverse direction and under 4-point bending conditions in the longitudinal direction. Both devices were designed to handle samples with a small transverse section (a few square mm), which allowed to select zones with homogenous anatomical features. The results indicate a very high longitudinal stiffness in tension wood (up to 35 GPa compared to an average of 18 GPa for normal wood). Considering wood density, the value represents a specific modulus that is nearly 70 % crystalline cellulose. However, tension wood is slightly less stiff in the tangential and radial directions (1,150 vs. 1,500 MPa for normal wood in the radial direction and 430 vs. 530 MPa in the tangential direction).     

COMPARATIVE STUDY OF WOOD PROPERTIES BETWEENWHITE WOOD OF DAHURIAN LARCH AND MONGOLIANSCOTCH PINE

DahurianlarchandMongolianscotchpinearetwomajorconunerciaIconilbroustTeesinDaxing'anlingForesnyArea.Itisob-viousthattbcwoodproPertiesandworkability'ofthetWoplantsarecompletelydifferent.Butlnrecert'years,ltlsfoundthattherearetwodiffer':nttypesinparameterofwood'scolour.phy'sicalandmechanicalproPertiesandwork-ability'inDahurianlarch,namelyredwoodandx"hite..od.l']Andthepropertiesofwhite`voodaresligl1tlyyellow-white,medianweightandhardness,goodinworkability'andLard-ness,goodinwodability'anduneas…     

Chemical structural elucidation of total lignins in woods I: fractionation of the lignin in residual wood meal after extraction of milled wood lignin

Residual wood meal after extraction of milled wood lignin (WMEM) ofEucalyptus globulus was extracted with alkali and LiCl/N,N-Dimethylacetamide (DMAc). These agents dissolve mainly hemicellulose and cellulose, respectively. The extractability of WMEM in alkali solutions was influenced by the degree of swelling of the cellulose. Under good swelling conditions, considerable amounts of cellulose and lignin were extracted with the hemicellulose. Maximum extractability was about 60% of the WMEM under optimum conditions (3 M or 5 M LiOH or 3M NaOH solution). Some portion of cellulose was extracted with LiCl/DMAc at room temperature. Thus, lignin inE. globulus WMEM was divided into three fractions: hemicellulose-lignin fraction, cellulose-lignin fraction, and insoluble-lignin fraction.Part of this work was presented at the 49th annual meeting of the Japan Wood Research Society, Tokyo, April 1999; and at the 50th annual meeting of the Japan Wood Research Society, Kyoto, April 2000     

Fracturing of wood under superimposed tension and torsion

A testing method using circumferentially notched round bars for investigating mixed mode behaviour under loading in tension and torsion is applied to wood. The applicability of the method to anisotropic materials is investigated for two types of wood, beech and spruce, considering the longitudinal and radial orientation with respect to the stem axis of the tree. The strong anisotropy of wood requires different evaluation procedures for radial and longitudinal sample orientation. The K-concept of linear elastic fracture mechanics (LEFM) and concepts of non-linear elastic fracture mechanics (NLEFM) were used for the evaluation of radial and longitudinal samples, respectively. Differences between the investigated wood types under radial orientation, in their durability to withstand torsional loads, could be observed by examining ratios of the values of the fracture toughness in mode III against mode I. Micrographs of the fracture surfaces support the assumption that the higher amount of wood rays in beech is responsible for the higher toughness under torsion. In case of longitudinal specimen geometry it was found that at very high levels of torsional deformation beech and spruce reach similar values in their specific fracture energy in mode I.     

A comparison of static bending,compression and tension parallel to grain and toughness properties of compression wood and normal wood of a giant sequoia

Summary Compression wood (CW) of the giant sequoia studied had higher values than normal wood (NW) in crushing strength and ultimate stress in tension parallel to grain, in toughness, in modulus of rupture, and in work to maximum load and total work in static bending. In the green condition CW had higher values than NW in stress at the proportional limit and work to the proportional limit, and about the same modulus of elasticity in static bending. In the dry condition CW was about equivalent to NW in work to the proportional limit, but was slightly weaker in stress at proportional limit and modulus of elasticity in static bending. The compression wood of this giant sequoia, even though formed when the tree was suppressed and having relatively narrow rings, can therefore be said to be essentially equivalent to normal wood so far as the mechanical properties tested in this study are concerned.Given at FPRS meeting in Dallas, Texas, June 1972