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Background: As a renewable carbon source, biomass energy not only helps in resolving the management problems of lignocellulosic wastes, but also helps to alleviate the global climate change by controlling environmental pollution raised by their generation on a large scale. However, the bottleneck problem of extensive production of biofuels lies in the filamentous crystal structure of cellulose and the embedded connection with lignin in biomass that leads to poor accessibility, weak degradation and digestion by microorganisms. Some pretreatment methods have shown significant improvement of methane yield and production rate, but the promotion mechanism has not been thoroughly studied. Revealing the temporal and spatial effects of pretreatment on lignocellulose will greatly help deepen our understanding of the optimization mechanism of pretreatment, and promote efficient utilization of lignocellulosic biomass. Here, we propose an approach for qualitative, quantitative, and location analysis of subcellular lignocellulosic changes induced by alkali treatment based on label-free Raman microspectroscopy combined with chemometrics. Results: Firstly, the variations of rice straw induced by alkali treatment were characterized by the Raman spectra, and the Raman fingerprint characteristics for classification of rice straw were captured. Then, a label-free Raman chemical imaging strategy was executed to obtain subcellular distribution of the lignocellulose, in the strategy a serious interference of plant tissues' fluorescence background was effectively removed. Finally, the effects of alkali pretreatment on the subcellular spatial distribution of lignocellulose in different types of cells were discovered. Conclusions: The results demonstrated the mechanism of alkali treatment that promotes methane production in rice straw through anaerobic digestion by means of a systemic study of the evidence from the macroscopic measurement and Raman microscopic quantitative and localization two-angle views. Raman chemical imaging combined with chemometrics could nondestructively realize qualitative, quantitative, and location analysis of the lignocellulose of rice straw at a subcellular level in a label-free way, which was beneficial to optimize pretreatment for the improvement of biomass conversion efficiency and promote extensive utilization of biofuel. [ABSTRACT FROM AUTHOR]

Background Enzymatic hydrolysis is a crucial step of biomass conversion into biofuels and different pretreatments have been proposed to improve the process efficiency. Amongst the various factors affecting hydrolysis yields of biomass samples, porosity and water accessibility stand out due to their intimate relation with enzymes accessibility to the cellulose and hemicellulose fractions of the biomass. In this work, sugarcane bagasse was subjected to acid and alkali pretreatments. The changes in the total surface area, hydrophilicity, porosity and water accessibility of cellulose were investigated by scanning electron microscopy (SEM) and nuclear magnetic resonance (NMR). Results Changes in chemical and physical properties of the samples, caused by the partial removal of hemicellulose and lignin, led to the increase in porosity of the cell walls and unwinding of the cellulose bundles, as observed by SEM. 1H NMR relaxation data revealed the existence of water molecules occupying the cores of wide and narrow vessels as well as the cell wall internal structure. Upon drying, the water molecules associated with the structure of the cell wall did not undergo significant dynamical and partial moisture changes, while those located in the cores of wide and narrow vessels kept continuously evaporating until reaching approximately20% of relative humidity. This indicates that water is first removed from the cores of lumens and, in the dry sample, the only remaining water molecules are those bound to the cell walls. The stronger interaction of water with pretreated bagasse is consistent with better enzymes accessibility to cellulose and higher efficiency of the enzymatic hydrolysis. Conclusions We were able to identify that sugarcane bagasse modification under acid and basic pretreatments change the water accessibility to different sites of the sample, associated with both bagasse structure (lumens and cell walls) and hydrophilicity (lignin removal). Furthermore, we show that the substrates with increased water accessibility correspond to those with higher hydrolysis yields and that there is a correlation between experimentally NMR-measured transverse relaxation times and the efficiency of enzymatic hydrolysis. This might allow for semiquantitative estimates of the enzymatic hydrolysis efficiency of biomass samples using inexpensive and non-destructive low-field 1H NMR relaxometry methods. [ABSTRACT FROM AUTHOR]

The present investigation aims at studying the effectiveness of alkali-assisted ultrasonication on pretreatment of garden biomass (GB). Dry and powdered GB suspended in 1% NaOH was ultrasonicated for 15, 30 and 60 minutes at a frequency of 25 KHZ. The mode of action and effectiveness of alkali-assisted ultrasonication on GB was established through microscopic, scanning electron microscopic and X-ray diffraction studies. A perusal of results showed that alkali-assisted ultrasonication led to fibrillation of GB which ultimately facilitated enzymatic hydrolysis. The results also indicated that alkali-assisted ultrasonication is an efficient means of pretreatment of GB at moderate (45-50°C) working temperature and low (1%) concentration of alkali. The yield of reducing sugar after enzymatic hydrolysis increased almost six times as compared to control due to alkali-assisted ultrasonication. [ABSTRACT FROM AUTHOR]

Background: In recent years, the growing demand for biofuels has encouraged the search for different sources of underutilized lignocellulosic feedstocks that are available in sufficient abundance to be used for sustainable biofuel production. Much attention has been focused on biomass fromgrass. However, large amounts of timber residues such as eucalyptus bark are available and represent a potential source for conversion to bioethanol. In the present paper, we investigate the effects of a delignification process with increasing sodium hydroxide concentrations, preceded or not by diluted acid, on the bark of two eucalyptus clones: Eucalyptus grandis (EG) and the hybrid, E. grandis x urophylla (HGU). The enzymatic digestibility and total cellulose conversion were measured, along with the effect on the composition of the solid and the liquor fractions. Barks were also assessed using Fourier-transform infrared spectroscopy (FTIR), solid-state nuclear magnetic resonance (NMR), X-Ray diffraction, and scanning electron microscopy (SEM). Results: Compositional analysis revealed an increase in the cellulose content, reaching around 81% and 76% of glucose for HGU and EG, respectively, using a two-step treatment with HCl 1%, followed by 4% NaOH. Lignin removal was 84% (HGU) and 79% (EG), while the hemicellulose removal was 95% and 97% for HGU and EG, respectively. However, when we applied a one-step treatment, with 4% NaOH, higher hydrolysis efficiencies were found after 48 h for both clones, reaching almost 100% for HGU and 80% for EG, in spite of the lower lignin and hemicellulose removal. Total cellulose conversion increased from 5% and 7% to around 65% for HGU and 59% for EG. NMR and FTIR provided important insight into the lignin and hemicellulose removal and SEM studies shed light on the cell-wall unstructuring after pretreatment and lignin migration and precipitation on the fibers surface, which explain the different hydrolysis rates found for the clones. Conclusion: Our results show that the single step alkaline pretreatment improves the enzymatic digestibility of Eucalyptus bark. Furthermore, the chemical and physical methods combined in this study provide a better comprehension of the pretreatment effects on cell-wall and the factors that influence enzymatic digestibility of this forest residue. [ABSTRACT FROM AUTHOR]

Background: Enzymatic hydrolysis is a crucial step of biomass conversion into biofuels and different pretreatments have been proposed to improve the process efficiency. Amongst the various factors affecting hydrolysis yields of biomass samples, porosity and water accessibility stand out due to their intimate relation with enzymes accessibility to the cellulose and hemicellulose fractions of the biomass. In this work, sugarcane bagasse was subjected to acid and alkali pretreatments. The changes in the total surface area, hydrophilicity, porosity and water accessibility of cellulose were investigated by scanning electron microscopy (SEM) and nuclear magnetic resonance (NMR)., Results: Changes in chemical and physical properties of the samples, caused by the partial removal of hemicellulose and lignin, led to the increase in porosity of the cell walls and unwinding of the cellulose bundles, as observed by SEM. (1)H NMR relaxation data revealed the existence of water molecules occupying the cores of wide and narrow vessels as well as the cell wall internal structure. Upon drying, the water molecules associated with the structure of the cell wall did not undergo significant dynamical and partial moisture changes, while those located in the cores of wide and narrow vessels kept continuously evaporating until reaching approximately 20% of relative humidity. This indicates that water is first removed from the cores of lumens and, in the dry sample, the only remaining water molecules are those bound to the cell walls. The stronger interaction of water with pretreated bagasse is consistent with better enzymes accessibility to cellulose and higher efficiency of the enzymatic hydrolysis., Conclusions: We were able to identify that sugarcane bagasse modification under acid and basic pretreatments change the water accessibility to different sites of the sample, associated with both bagasse structure (lumens and cell walls) and hydrophilicity (lignin removal). Furthermore, we show that the substrates with increased water accessibility correspond to those with higher hydrolysis yields and that there is a correlation between experimentally NMR-measured transverse relaxation times and the efficiency of enzymatic hydrolysis. This might allow for semiquantitative estimates of the enzymatic hydrolysis efficiency of biomass samples using inexpensive and non-destructive low-field (1)H NMR relaxometry methods.