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Melamine-formaldehyde in the conservation of waterlogged archaeological wood: investigating the effect of the treatment on wood residual chemistry with FTIR, 13C NMR, Py(HMDS)-GC/MS and EGA-MS 三聚氰胺-甲醛在水渍考古木材保护中的应用:利用傅立叶变换红外光谱、13C NMR、Py(HMDS)-GC/MS 和 EGA-MS 研究处理对木材残留化学成分的影响
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-27 DOI: 10.1007/s00226-024-01610-w
Maria Vlata, Stavroula Rapti, Stamatis Boyatzis, Michel Bardet, Jeannette Jacqueline Lucejko, Anastasia Pournou

This work examined the chemical interrelations between melamine–formaldehyde (MF) and waterlogged archaeological wood to demonstrate the effect of the MFtreatment on cultural heritage objects. Samples from a Roman waterlogged trunk of Greek fir, were analyzed with Fourier Transform Infrared Spectroscopy (FTIR), solid-state 13C Nuclear Magnetic Resonance (NMR), analytical pyrolysis with in-situ silylation Py(HMDS) coupled with Gas Chromatography Mass Spectrometry (GC/MS) and Evolved Gas Analysis-Mass Spectrometry, (EGA-MS) before and after the MFtreatment. FTIR results showed the formation of amide functionalities due to melamine reactions and strong evidence of lignin modification, while the deteriorated cellulose fraction appeared to have undergone further depletion as a result of the MF treatment. The 13C NMR spectra of the MF-treated wood clearly demonstrated the presence of the resin within the wood and indicated that MF carbons were strongly interacting with lignin moieties. Spectra also revealed that the retention of the MF resin in the wood was positively correlated to the degree of wood degradation. Py(HMDS)-GC/MS of MF-treated wood provided few peaks attributed to holocellulose or lignin pyrolytic products, and it was not possible to detect any signs of non-MF-modified wood components, as the lignocellulosic wood matrix appeared to have been transformed into a new biopolymer. EGA-MS profiles of the MF-treated archaeological wood showed early evolution of volatiles due to free MF retained in the wood, while its thermal stability appeared increased in comparison to untreated material. Nonetheless, mass peaks indicated that the chemistry of MF-treated wood was completely different from both fresh and untreated deteriorated wood. Overall, results showed that the MF treatment irreversibly modified the residual chemistry of the archaeological material and failed to preserve its original physical and historical integrity. This permanent modification of unknown longevity is considered not in line with conservation ethics and, therefore, inappropriate for the long-term preservation of cultural heritage objects.

这项工作研究了三聚氰胺-甲醛(MF)与水渍考古木材之间的化学相互关系,以证明三聚氰胺-甲醛处理对文化遗产物品的影响。在 MF 处理前后,采用傅立叶变换红外光谱法 (FTIR)、固态 13C 核磁共振法 (NMR)、原位硅化 Py(HMDS) 分析热解结合气相色谱-质谱联用仪 (GC/MS) 和进化气体分析-质谱联用仪 (EGA-MS) 对希腊杉木的罗马水渍树干样本进行了分析。傅立叶变换红外光谱(FTIR)结果显示,三聚氰胺反应形成了酰胺官能团,木质素被改性的证据确凿,而经过中频处理后,变质的纤维素部分似乎发生了进一步的损耗。经过甲酸甲酯处理的木材的 13C NMR 光谱清楚地显示了木材中树脂的存在,并表明甲酸甲酯碳与木质素分子发生了强烈的相互作用。光谱还显示,MF 树脂在木材中的保留与木材降解程度呈正相关。经过 MF 处理的木材的 Py(HMDS)-GC/MS 几乎没有出现全纤维素或木质素热解产物的峰值,也无法检测到任何非 MF 改性木材成分的迹象,因为木质纤维素木材基质似乎已转化为一种新的生物聚合物。经过甲酸甲酯处理的考古木材的 EGA-MS 图谱显示,由于木材中保留了游离的甲酸甲酯,挥发性物质发生了早期演变,与未经处理的材料相比,其热稳定性似乎有所提高。然而,质量峰表明,经过甲酸甲酯处理的木材的化学性质与新鲜和未经处理的变质木材完全不同。总之,结果表明,甲酸甲酯处理不可逆地改变了考古材料的残余化学成分,未能保持其原有的物理和历史完整性。这种寿命未知的永久性改变被认为不符合保护伦理,因此不适于对文物进行长期保护。
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引用次数: 0
Production of activated biocarbons by microwave-assisted chemical activation of hardwood sawdust and their application in the simultaneous removal of polymers of different origins from aqueous systems 通过微波辅助化学活化硬木锯屑生产活性生物碳,并将其应用于同时去除水体系中不同来源的聚合物
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-23 DOI: 10.1007/s00226-024-01623-5
Małgorzata Wiśniewska, Karina Tokarska, Teresa Urban, Piotr Nowicki, Agnieszka Woszuk

Sawdust from deciduous trees was used as a raw material for the preparation of carbonaceous adsorbents. Microwave-assisted chemical activation with K2CO3 and H3PO4 was used to produce materials with a well-developed porous structure. The obtained activated biocarbons were characterized in terms of their porous structure, elemental composition, morphology, thermal stability, as well as surface and electrokinetic properties. The sorption abilities of both materials towards synthetic (poly(acrylic acid)) and natural (lysozyme) polymers in the process of their removal from aqueous systems were determined. Both single adsorbates and mixed solutions of two polymeric adsorbates were tested. The stability of aqueous suspensions containing activated biocarbons and one or two polymers was also determined. As a result of microwave-assisted chemical activation two carbonaceous adsorbents were obtained, characterized by a very well-developed specific surface area (1093–1777 m2/g), a completely different type of porous structure (mesoporous or microporous), and the acidic nature of the surface. The maximum adsorption of poly(acrylic acid) was obtained from a mixed solution of both polymers and it reached values of 379 mg/g (for the sample activated with H3PO4 with mean pore diameter 3.04 nm and minimal contribution of micropores—0.3%) and 259 mg/g (for K2CO3 activated material characterized by the mean pore diameter equal to 1.72 nm and large contribution of micropores—77.4%). In the case of lysozyme, the adsorption efficiency was two times lower (sorption capacity of 127–166 mg/g). Based on the collective data analysis, it can be stated that the most probable mechanisms of polymeric destabilization (highly desirable in separation from the multicomponent solutions) are surface charge neutralization at pH 3 and bridging flocculation at pH 11 (especially for the systems containing material activated with H3PO4 and poly(acrylic acid)).

以落叶树的锯屑为原料制备了碳质吸附剂。利用 K2CO3 和 H3PO4 进行微波辅助化学活化,制备出具有发达多孔结构的材料。所获得的活化生物碳在多孔结构、元素组成、形态、热稳定性以及表面和电动特性等方面都具有特征。在从水体系中去除合成聚合物(聚丙烯酸)和天然聚合物(溶菌酶)的过程中,测定了这两种材料对它们的吸附能力。测试了单一吸附剂和两种聚合物吸附剂的混合溶液。此外,还测定了含有活性生物碳和一种或两种聚合物的水悬浮液的稳定性。微波辅助化学活化的结果是得到了两种碳质吸附剂,其特点是比表面积非常发达(1093-1777 m2/g),具有完全不同类型的多孔结构(介孔或微孔),表面呈酸性。两种聚合物的混合溶液对聚(丙烯酸)的吸附量最大,达到 379 mg/g(用 H3PO4 活化的样品,平均孔径为 3.04 nm,微孔占比最小-0.3%)和 259 mg/g(用 K2CO3 活化的材料,平均孔径为 1.72 nm,微孔占比最大-77.4%)。溶菌酶的吸附效率则低两倍(吸附容量为 127-166 毫克/克)。根据综合数据分析,可以认为聚合物脱稳(从多组分溶液中分离时非常需要)的最可能机制是 pH 值为 3 时的表面电荷中和和 pH 值为 11 时的架桥絮凝(特别是对于含有用 H3PO4 和聚丙烯酸活化的材料的系统)。
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引用次数: 0
New ester-type chemical bonding wood adhesion with a dicarboxylic acid compound 二羧酸化合物的新型酯类化学键木材粘合剂
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-22 DOI: 10.1007/s00226-024-01621-7
Daisuke Ando, Kenji Umemura, Hidefumi Yamauchi

Wood adhesion is one of the fundamental joint technologies for wood-based materials. We focused on an unprecedented chemical bonding wood adhesion. With the final goal of water-resistant wood adhesion using dicarboxylic acid compounds with straight alkyl chains, this study clarified the difference of adhesiveness between glutaric acid (GA) and citric acid (CA) to explore the direct effects of chemical bonding type adhesion on physical properties. In the prepared wood-based moldings, the structural analysis with 2D-NMR of the interphase between GA or CA and wood surfaces revealed that GA adhesion is cleaner and more reactive than CA adhesion, without any side reactions. GA reacted with the wood powder surface. In addition, the water resistance treatments of the GA-type wood-based molding showed a thickness reversibility that is not observed with CA-adhesion. The results indicate that GA-adhesion is very likely a chemical bonding type of wood adhesion, considering the molding process under high temperature and pressure conditions. The physical properties of the molding were evaluated to determine the adhesion properties. GA-type wood-based molding was tougher and more water-resistant than CA-type wood-based molding. The physical properties were attributed to the side-chain structure of GA. The results indicate that dicarboxylic acid compounds could be superior wood adhesives, and other dicarboxylic acids could be used for wood adhesion and the expression of material properties owing to their various side chain structures. Furthermore, the material properties could be controlled by considering the chemical structure of adhesive compounds in the future.

木材粘合是人造板的基本接合技术之一。我们重点研究了一种前所未有的化学键合木材粘合剂。以使用直烷基链的二羧酸化合物实现防水木材粘合为最终目标,本研究明确了戊二酸(GA)和柠檬酸(CA)粘合性的差异,以探索化学键合型粘合对物理性质的直接影响。在制备的木基模塑中,利用 2D-NMR 对 GA 或 CA 与木材表面的相间结构进行分析,结果表明 GA 的粘合比 CA 的粘合更清洁、反应性更强,且无任何副反应。GA 与木粉表面发生了反应。此外,GA 型木基模塑的耐水性处理显示出厚度可逆性,而 CA 粘合则没有这种现象。结果表明,考虑到高温高压条件下的模塑过程,GA 吸附很可能是一种化学键型的木材粘合。对模塑物的物理性质进行了评估,以确定其粘合性能。GA 型木基模塑比 CA 型木基模塑更坚韧、更耐水。这些物理性能与 GA 的侧链结构有关。研究结果表明,二羧酸化合物可作为优质的木材粘合剂,其他二羧酸也可用于木材粘合,并因其不同的侧链结构而表现出不同的材料特性。此外,未来还可通过考虑胶粘剂化合物的化学结构来控制材料特性。
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引用次数: 0
Progressive degradation of acetylated wood by the brown rot fungi Coniophora puteana and Rhodonia placenta 褐腐真菌 Coniophora puteana 和 Rhodonia placenta 对乙酰化木材的逐步降解作用
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-19 DOI: 10.1007/s00226-024-01620-8
Tiina Belt, Muhammad Awais

Acetylation is a wood modification method that reduces the hygroscopicity of wood and increases its resistance to degradation by wood decaying fungi. Even though acetylated wood can have very high decay resistance, the wood material can be degraded and sometimes deacetylated by fungi. This study investigated the degradation and deacetylation of acetylated wood by Coniophora puteana and Rhodonia placenta to better understand the relationship between degradation and deacetylation in two different brown rot fungi. Wood samples were exposed to the fungi in a stacked-sample decay test, followed by acetyl content measurements and FTIR spectroscopy to investigate chemical changes in the samples. The results showed that both fungi could degrade acetylated wood to high mass loss despite a strong reduction in moisture content, but only R. placenta was found to cause preferential deacetylation. The deacetylation was slight and only observed in the early stages of decay in highly acetylated wood. Otherwise, acetyl groups were lost from the samples at the rate of mass loss. FTIR spectroscopy confirmed the loss of acetyl groups and revealed some chemical differences between unacetylated and acetylated wood. The spectral data indicated the loss of acetyl groups from lignin, which suggests that the loss of acetyl groups is not only due to the degradation of acetylated carbohydrates. The degradation of acetylated wood required further investigation, but it is clear that extensive deacetylation is not a requirement for brown rot degradation.

乙酰化是一种木材改性方法,可降低木材的吸湿性,提高其抗木材腐朽真菌降解的能力。尽管乙酰化木材具有很强的抗腐性,但这种木材材料也会被真菌降解,有时还会被脱乙酰化。本研究调查了褐腐真菌 Coniophora puteana 和 Rhodonia placenta 对乙酰化木材的降解和脱乙酰化作用,以更好地了解两种不同褐腐真菌降解和脱乙酰化之间的关系。在堆叠样品腐朽试验中,木材样品暴露于真菌,然后测量乙酰含量,并用傅立叶变换红外光谱法研究样品中的化学变化。结果表明,尽管木材含水率大幅降低,但两种真菌都能降解乙酰化木材,造成大量质量损失,但只有胎盘霉菌能优先导致脱乙酰化。这种脱乙酰作用很轻微,而且只有在高乙酰化木材腐烂的早期阶段才能观察到。否则,乙酰基就会以质量损失的速度从样品中消失。傅立叶变换红外光谱证实了乙酰基的损失,并揭示了未乙酰化木材和乙酰化木材之间的一些化学差异。光谱数据表明乙酰基从木质素中流失,这表明乙酰基的流失不仅仅是由于乙酰化碳水化合物的降解。乙酰化木材的降解需要进一步研究,但很明显,广泛的脱乙酰化并不是褐腐病降解的必要条件。
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引用次数: 0
Peltogynoids contributing to discoloration in Peltogyne mexicana heartwood 造成墨西哥盾叶朴树心材褪色的盾叶朴树素
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-15 DOI: 10.1007/s00226-024-01617-3
Yusuke Taga, Kosei Yamauchi, Tohru Mitsunaga

Four new peltogynoid monomers (3, 7, 10, 11) and a new peltogynoid dimer (9) were isolated from the heartwood of Peltogyne mexiacana, along with six known compounds (1, 2, 4, 5, 6, 8). Among the known compounds, the absolute configurations of two flavanones (5, 6) were determined. The structures of the isolated compounds were determined using NMR and MALDI-TOF MS analysis. The discoloration of the methanol solutions of the isolated peltogynoids and flavanones was examined by exposing them to room light in the air. The methanol solutions of (+)-peltogynol (1) and (+)-mopanol (4) discolored to reddish and bluish purple, respectively. After discoloration, the b* values of these compounds decreased significantly from 12.1 to 19.1 to -0.7 and − 1.8, respectively. These precursors of pigment compounds 1 and 4 have a catechol moiety in the B ring, and a hetero-six-membered ring (D ring) connecting the B and C ring of flavan-3,4-diol via an oxyethylene bridge, which is similar to the structure of leucoanthocyanidin. These results led to the hypothesis that the metabolized pigment compounds have anthocyanidin-like structures with peltogyne skeleton.

从 Peltogyne mexiacana 的心材中分离出了四种新的莕菜素单体(3、7、10、11)和一种新的莕菜素二聚体(9),以及六种已知化合物(1、2、4、5、6、8)。在已知化合物中,确定了两种黄酮(5、6)的绝对构型。利用核磁共振和 MALDI-TOF MS 分析法确定了分离化合物的结构。将分离出的盾形酮类化合物和黄烷酮类化合物的甲醇溶液暴露在室温下进行褪色检测。(+)-peltogynol (1) 和 (+)-mopanol (4) 的甲醇溶液分别褪色为淡红色和蓝紫色。褪色后,这些化合物的 b* 值分别从 12.1 到 19.1 显著下降到-0.7 和-1.8。这些色素化合物的前体 1 和 4 的 B 环上有一个儿茶酚分子,一个杂六元环(D 环)通过氧乙烯桥连接黄烷-3,4-二醇的 B 环和 C 环,这与白花青素的结构相似。这些结果导致了一种假设,即代谢后的色素化合物具有类似花青素的结构,其骨架为盾形花青素。
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引用次数: 0
Evaluation of the antifungal efficiency of coatings on wood 评估木材涂层的抗真菌效率
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-15 DOI: 10.1007/s00226-024-01614-6
Olena Myronycheva, Injeong Kim, Olov Karlsson, Liudmyla Kiurcheva, Peter Jacobsson, Dick Sandberg

Wood is an important construction material, but a significant problem hindering its widespread use is susceptibility to biodeterioration and biodegradation. To protect wood against degradation, a surface coating can be used, and it is important to be able to predict the ability of the coating to prevent fungal growth. The currently available standard method to determine the antifungal efficiency of a coating has two weaknesses, viz. no evaluation of the moisture content in the wood material, and no possibility to study antifungal effect of the coating towards an individual fungus. A new quantitative method of determining the antifungal efficiency of coatings is therefore proposed, where a coating is applied to wood and exposed to an individual fungus in a Petri dish. Six commercial water-based coatings containing synthetic biocides were studied on filter paper (EN 15457) and with the new test method on wood blocks. The results show the importance of studying the antifungal efficiency of a coating using individual fungi instead of a mixture of fungi, since individual fungi interact differently with a given biocide in the coating. The moisture content of the wood substrate during the test was affected by how the fungus was established on the coating. This new test approach shows promise in screening the antifungal efficiency of wood coatings containing preservative substances applied to wood material surfaces.

木材是一种重要的建筑材料,但妨碍其广泛使用的一个重要问题是容易发生生物退化和生物降解。为了防止木材降解,可以使用表面涂层,而预测涂层防止真菌生长的能力非常重要。目前可用来确定涂层抗真菌效率的标准方法有两个弱点,即无法评估木质材料中的含水量,也无法研究涂层对单个真菌的抗真菌效果。因此,我们提出了一种新的定量方法来确定涂层的抗真菌效率,即在木材上涂抹涂层,并在培养皿中接触单个真菌。我们在滤纸(EN 15457)上对六种含有合成杀菌剂的商用水基涂料进行了研究,并在木块上使用新的测试方法进行了研究。结果表明,使用单个真菌而不是真菌混合物来研究涂料的抗真菌效率非常重要,因为单个真菌与涂料中特定杀菌剂的相互作用是不同的。在测试过程中,木质基材的含水量会受到真菌在涂层上生长方式的影响。这种新的测试方法有望筛选出木质材料表面含有防腐剂的木质涂料的抗真菌效率。
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引用次数: 0
Determination of local mechanical properties of clear wood in relation to the local fiber deviation 根据局部纤维偏差确定清材的局部机械特性
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-13 DOI: 10.1007/s00226-024-01607-5
L. Demoulin, G. Pot, L. Denaud, S. Girardon, B. Marcon

Products made with veneers such as Laminated Veneer Lumber can reach higher properties than solid wood because the defects such as knots (but not only) are distributed among the various layers. Visual sorting, even using automatic grading, is only partially efficient for evaluating mechanical properties, which mainly depends on the fiber orientation and the density both at local scale. An experimental protocol has been established to correlate the nondestructive (fiber orientation and density) estimation and the destructive (tensile test) measurement of beech veneer wood. The aim is to understand the impact of the small imperfections on clear wood in fiber orientation on the mechanical properties. In the present study, wood veneer is assumed to be a transverse isotropic material due to the predominant wood fiber direction in the growth direction of the tree. Experimental measurements of modulus of elasticity are based on Digital Image Correlation (DIC) and virtual extensometer. The Young modulus model is based on a composite material model that considers fiber orientation and density. The Young modulus model is used to determine longitudinal, transverse, and shear moduli, for specimens with angles ranging from 0 to 45°. Mechanical properties are obtained by mathematical minimization between experimental and model data. The coefficient of determination obtained was 0.97. The measure of the fiber angle with a resolution of 1 × 1 mm2 and the tensile test with the DIC, both local, significantly improve Young modulus measurement compared to previous studies’ assessment accuracy and allow for a better understanding of the wood behavior.

用单板(如层压单板木材)制成的产品可以达到比实木更高的性能,因为缺陷(如节疤)分布在各层中。目视分选,即使使用自动分级,也只能部分有效地评估机械性能,而机械性能主要取决于局部范围内的纤维方向和密度。我们已经制定了一个实验方案,将榉木单板木材的非破坏性(纤维方向和密度)评估与破坏性(拉伸试验)测量联系起来。这样做的目的是为了了解清材纤维取向上的微小瑕疵对机械性能的影响。在本研究中,假定木皮是横向各向同性材料,因为木纤维方向主要在树木的生长方向上。弹性模量的实验测量基于数字图像相关(DIC)和虚拟拉伸计。杨氏模量模型基于复合材料模型,该模型考虑了纤维方向和密度。杨氏模量模型用于确定角度为 0 至 45°的试样的纵向、横向和剪切模量。力学性能是通过对实验数据和模型数据进行数学最小化处理而获得的。确定系数为 0.97。与以往研究的评估精度相比,以 1 × 1 mm2 的分辨率测量纤维角和使用 DIC 进行局部拉伸测试,大大提高了杨氏模量的测量精度,并能更好地了解木材的行为。
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引用次数: 0
Early detection of heartwood rot caused by Fistulina hepatica in Castanea sativa productive coppices through low-invasive resistance drilling 通过低侵入性抗性钻探,及早发现蓖麻高产灌木中由肝蓟马引起的心材腐烂病
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-13 DOI: 10.1007/s00226-024-01616-4
Andreu Meijer, E. Jordán Muñoz-Adalia, Eduard Correal-Mòdol, Carlos Colinas

Chestnut Red Stain (CRS) is a heartwood discoloration that widely affects Castanea sativa Mill. productive coppice stands in the northeast of Spain. At the early stages of infection, the structural properties of the wood are not affected, but still its economic value drops up to 70% due to the rejection of this wood. This disease is caused by the fungus Fistulina hepatica (Schaeff.) With. and causes uncertainty to forest managers since the fungal infection is virtually impossible to detect before felling. The objective of this work was to develop an efficient detection method to evaluate the presence of F. hepatica in early stages of productive periods. A total of 72 chestnuts were analyzed through molecular methods to determine the presence of F. hepatica and with an IML resistance drill to characterize their wood. Thirteen wood quality indices were calculated and their correlation with the presence of the pathogen was evaluated using linear mixed models. We found clear differences between healthy and infected trees in four indices. A new specific index (Chestnut Red Stain Danger index) was designed to estimate the probability of infection by F. hepatica. The results support the hypothesis that the early presence of F. hepatica is detectable through inexpensive and fast mechanical methods early in a rotation. The results of this work will help forest managers evaluate the incidence of CRS, as well as it establishes a novel methodology for further development of resistance drilling techniques for heartwood rot detection.

栗木红斑(CRS)是一种心材变色现象,广泛影响西班牙东北部的栗木(Castanea sativa Mill.在感染初期,木材的结构特性不会受到影响,但由于这种木材被拒收,其经济价值仍会下降高达 70%。这种疾病由真菌 Fistulina hepatica (Schaeff.) With.这项工作的目的是开发一种有效的检测方法,以评估在丰产期早期是否存在 F. hepatica。通过分子方法分析了总共 72 颗栗子,以确定是否存在肝包虫病,并使用 IML 抗性钻孔机分析了木材的特征。我们计算了 13 项木材质量指标,并使用线性混合模型评估了它们与病原体存在的相关性。我们发现健康树木和受感染树木在四项指数上存在明显差异。我们还设计了一个新的特定指数(栗红褐斑危险指数)来估算被肝蝇疫菌感染的概率。研究结果支持这样的假设,即在轮伐初期,可以通过廉价、快速的机械方法检测到肝包虫的早期存在。这项工作的结果将有助于森林管理者评估 CRS 的发生率,并为进一步开发用于心材腐烂病检测的抗性钻孔技术提供了一种新方法。
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引用次数: 0
Characterizing the chemistry of artificially degraded Scots pine wood serving as a model of naturally degraded waterlogged wood using1H–13C HSQC NMR 利用 1H-13C HSQC NMR 分析作为自然降解水渍木材模型的人工降解苏格兰松木的化学特征
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-13 DOI: 10.1007/s00226-024-01618-2
Daniel J. Yelle, Magdalena Broda

Chemically and biologically degraded Scots pine wood was prepared as a model material for the research on new conservation agents for waterlogged archeological wood. In this study, the model wood was characterized using a 2D1H–13C solution-state NMR technique without derivatization, isolation, or extraction to assess the effect of applied degradation processes on its chemical composition and structure. The results clearly show how the two artificially degraded model wood types are chemically different. Biological decay by the brown-rot fungus Coniophora puteana caused degradation of wood polysaccharides, with heavy depletion in arabinan, mannan, and galactan, along with an increase in the cellulose's reducing ends (i.e., lowering the degree of polymerization) and partial deacetylation of mannan. The fungus cleaved roughly one-fifth of the β-aryl ethers in lignin, leading to a broadening effect on the lignin aromatic unit contours; other lignin sidechains were left untouched. Chemical degradation by NaOH hydrolysis resulted in a depletion in mannan, galactan, and glucan, as well as efficient deacetylation of mannan. It also decreased lignin content, causing changes in its structure; minor β-aryl ether cleavage along with substantial phenylcoumaran cleavage were evident. Detailed knowledge about the chemical composition and structure of artificially degraded model pine wood obtained in this research is necessary to understand the reactivity of these wood types with chemicals used for their conservation. This research will help explain the differences in the stabilization effectiveness observed between these wood types treated during conservation and understand the stabilization mechanisms, thus contributing to developing new, more effective conservation agents for wooden artifacts of Cultural Heritage.

制备了化学和生物降解的苏格兰松木,作为研究水涝考古木材新保护剂的模型材料。在这项研究中,使用 2D1H-13C 溶液态核磁共振技术对模型木材进行了表征,没有进行衍生、分离或提取,以评估应用降解过程对其化学成分和结构的影响。结果清楚地表明了两种人工降解的模型木材在化学成分上的不同。褐腐真菌 Coniophora puteana 的生物降解作用导致木材多糖降解,阿拉伯聚糖、甘露聚糖和半乳聚糖大量减少,纤维素的还原端增加(即聚合度降低),甘露聚糖部分脱乙酰化。真菌裂解了木质素中大约五分之一的 β-芳基醚,导致木质素芳香单元轮廓变宽;其他木质素侧链未受影响。用 NaOH 水解法进行化学降解会导致甘露聚糖、半乳聚糖和葡聚糖的减少,并有效地使甘露聚糖脱乙酰基。它还降低了木质素的含量,使其结构发生了变化;明显可见轻微的β芳基醚裂解和大量的苯基香豆素裂解。要了解这些木材类型与用于保护它们的化学品之间的反应性,就必须详细了解本研究中获得的人工降解松木模型的化学成分和结构。这项研究将有助于解释在保护过程中观察到的这些木材类型在稳定效果上的差异,并了解其稳定机制,从而为开发新的、更有效的文化遗产木质文物保护剂做出贡献。
{"title":"Characterizing the chemistry of artificially degraded Scots pine wood serving as a model of naturally degraded waterlogged wood using1H–13C HSQC NMR","authors":"Daniel J. Yelle,&nbsp;Magdalena Broda","doi":"10.1007/s00226-024-01618-2","DOIUrl":"10.1007/s00226-024-01618-2","url":null,"abstract":"<div><p>Chemically and biologically degraded Scots pine wood was prepared as a model material for the research on new conservation agents for waterlogged archeological wood. In this study, the model wood was characterized using a 2D<sup>1</sup>H–<sup>13</sup>C solution-state NMR technique without derivatization, isolation, or extraction to assess the effect of applied degradation processes on its chemical composition and structure. The results clearly show how the two artificially degraded model wood types are chemically different. Biological decay by the brown-rot fungus <i>Coniophora puteana</i> caused degradation of wood polysaccharides, with heavy depletion in arabinan, mannan, and galactan, along with an increase in the cellulose's reducing ends (i.e., lowering the degree of polymerization) and partial deacetylation of mannan. The fungus cleaved roughly one-fifth of the β-aryl ethers in lignin, leading to a broadening effect on the lignin aromatic unit contours; other lignin sidechains were left untouched. Chemical degradation by NaOH hydrolysis resulted in a depletion in mannan, galactan, and glucan, as well as efficient deacetylation of mannan. It also decreased lignin content, causing changes in its structure; minor β-aryl ether cleavage along with substantial phenylcoumaran cleavage were evident. Detailed knowledge about the chemical composition and structure of artificially degraded model pine wood obtained in this research is necessary to understand the reactivity of these wood types with chemicals used for their conservation. This research will help explain the differences in the stabilization effectiveness observed between these wood types treated during conservation and understand the stabilization mechanisms, thus contributing to developing new, more effective conservation agents for wooden artifacts of Cultural Heritage.</p></div>","PeriodicalId":810,"journal":{"name":"Wood Science and Technology","volume":"59 1","pages":""},"PeriodicalIF":3.1,"publicationDate":"2024-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s00226-024-01618-2.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142600737","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Effects of plant source selection and chemi-mechanical treatment on the fiber microstructures and mechanical behaviors of nanocellulose films 植物来源选择和化学机械处理对纳米纤维素薄膜的纤维微结构和机械性能的影响
IF 3.1 2区 农林科学 Q1 FORESTRY Pub Date : 2024-11-09 DOI: 10.1007/s00226-024-01613-7
Yangyang Qian, Chunyu Wang, Yijun Liu, Bingfei Shi, Jianqiang Zhang, Yuan Wei, Gang Chen

Cellulose nanofibers (CNFs) were isolated and prepared from six different plant sources (Nordic pine, poplar, cotton, flax, bamboo, and pineapple leaf fibers) through a carboxymethylation-homogenization treatment. The surface morphologies, size distributions, and chemical structures of the CNFs and their microfibers were investigated in detail. Atomic force microscopy (AFM) analysis showed that all kinds of CNFs had uniform diameters of less than 10 nm. However, the length and aspect ratio of CNFs exhibited significant differences due to the differences of anatomical characteristics from pulp species. Among these six nanofibers, the pineapple leaf-based nanofibers had the highest length of ca. 2.21 μm and aspect ratio of ca. 1263. Meanwhile, the resulting pineapple leaf-based nanocellulose film possessed the strongest tensile strength (229.0 ± 9.8 MPa) and toughness (33.9 ± 2.9 MJ/m3). Interestingly, the aspect ratio of cotton nanofibers was only 556, lower than that of bamboo, Nordic pine, and flax nanofibers, but the tensile strength (210.6 ± 4.8 MPa) and toughness (22.4 ± 0.6 MJ/m3) of cotton-based nanocellulose film were second only to the pineapple leaf-based nanocellulose film. The critical reason is that the cotton-based nanocellulose exhibited the highest crystallinity index (76.6%), superior to the other source-based nanocellulose. These results suggested that the high aspect ratio or high crystallinity are responsible for the excellent mechanical strengths of the nanocellulose film. This work sheds light on the preparation and selection of highly spindly or crystalline nonwood nanofibrils, suggesting that the pineapple leaf or cotton nanofibers have great potential as strength additives for nanocomposites.

通过羧甲基化-均质化处理,从六种不同的植物(北欧松、杨树、棉花、亚麻、竹子和菠萝叶纤维)中分离制备了纤维素纳米纤维(CNFs)。详细研究了 CNFs 及其微纤维的表面形态、尺寸分布和化学结构。原子力显微镜(AFM)分析表明,各种 CNFs 的直径均小于 10 纳米。然而,由于不同纸浆品种的解剖特征不同,CNFs 的长度和长宽比表现出显著差异。在这六种纳米纤维中,菠萝叶基纳米纤维的长度最大,约为 2.21 μm,长宽比约为 1263。同时,菠萝叶基纳米纤维素薄膜具有最强的拉伸强度(229.0 ± 9.8 MPa)和韧性(33.9 ± 2.9 MJ/m3)。有趣的是,棉纳米纤维的长宽比仅为 556,低于竹纳米纤维、北欧松纳米纤维和亚麻纳米纤维,但棉基纳米纤维素薄膜的拉伸强度(210.6 ± 4.8 MPa)和韧性(22.4 ± 0.6 MJ/m3)仅次于菠萝叶基纳米纤维素薄膜。关键原因是棉基纳米纤维素的结晶度指数最高(76.6%),优于其他来源的纳米纤维素。这些结果表明,高纵横比或高结晶度是纳米纤维素薄膜具有优异机械强度的原因。这项研究揭示了如何制备和选择高刺或高结晶非木材纳米纤维,表明菠萝叶或棉纳米纤维作为纳米复合材料的强度添加剂具有巨大潜力。
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Wood Science and Technology
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