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10 pages, 898 KiB  
Article
Is There a Relationship Between Helicobacter pylori Infection and Anthropometric Status?
by Lilian Camaño Carballo, Alejandro Ernesto Lorenzo Hidalgo, Paola Andrea Romero Riaño, Alejandro Martínez-Rodríguez and Daniela Alejandra Loaiza Martínez
Gastrointest. Disord. 2025, 7(1), 21; https://doi.org/10.3390/gidisord7010021 (registering DOI) - 6 Mar 2025
Abstract
Background: Helicobacter pylori infection, overweight, and obesity are global health concerns. This bacterium is involved in the pathophysiology of chronic gastritis and gastric cancer. Additionally, overweight and obesity, associated with unhealthy eating habits and sedentary lifestyles, cause alterations in the gut microbiota [...] Read more.
Background: Helicobacter pylori infection, overweight, and obesity are global health concerns. This bacterium is involved in the pathophysiology of chronic gastritis and gastric cancer. Additionally, overweight and obesity, associated with unhealthy eating habits and sedentary lifestyles, cause alterations in the gut microbiota that facilitate gastric colonization by Helicobacter pylori. Moreover, individuals with obesity tend to consume low-quality foods due to episodes of anxiety and exhibit elevated insulin levels, which may promote the development of gastric neoplasms. Studies conducted in Latin America have found that over 50% of participants are infected with Helicobacter pylori, a situation similar to that reported in Ecuador, where the prevalence of overweight and obesity in individuals aged 19 to 59 years reached 64.58% in 2018. Both health issues are influenced by the high consumption of processed foods or those prepared under inadequate hygiene conditions. Methods: In this context, this research aimed to correlate the body composition of university students with the prevalence of Helicobacter pylori. An observational, cross-sectional, and descriptive study was conducted with 57 Nursing, Medicine, and Psychology students from Universidad Indoamérica, Ambato campus, during 2024. Fecal samples were analyzed to detect the presence of the bacterium, and anthropometric measurements were taken to establish a possible relationship between these parameters. Results: Of the 57 students who participated, 54.39% tested positive for Helicobacter pylori. However, the presence of the bacteria did not show any relationship with body composition parameters such as fat mass, lean mass, BMI, weight, height, or age. Conclusions: The study found no evidence of a connection between Helicobacter pylori infection and anthropometric parameters in this university population. However, the high incidence of infections highlights the importance of promoting the consumption of safe food and ensuring timely diagnosis and treatment. Full article
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<p>Patients’ test results for <span class="html-italic">Helicobacter pylori.</span></p>
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<p>Test results for <span class="html-italic">Helicobacter pylori</span> antigen detection in stool samples divided by patient gender.</p>
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40 pages, 4884 KiB  
Article
Impacts of Mechanical Injury on Volatile Emission Rate and Composition in 45 Subtropical Woody Broad-Leaved Storage and Non-Storage Emitters
by Yali Yuan, Yimiao Mao, Hao Yuan, Ming Guo, Guomo Zhou, Ülo Niinemets and Zhihong Sun
Plants 2025, 14(5), 821; https://doi.org/10.3390/plants14050821 (registering DOI) - 6 Mar 2025
Abstract
Biogenic volatile organic compounds (BVOCs) significantly impact air quality and climate. Mechanical injury is a common stressor affecting plants in both natural and urban environments, and it has potentially large influences on BVOC emissions. However, the interspecific variability in wounding-induced BVOC emissions remains [...] Read more.
Biogenic volatile organic compounds (BVOCs) significantly impact air quality and climate. Mechanical injury is a common stressor affecting plants in both natural and urban environments, and it has potentially large influences on BVOC emissions. However, the interspecific variability in wounding-induced BVOC emissions remains poorly understood, particularly for subtropical trees and shrubs. In this study, we investigated the effects of controlled mechanical injury on isoprenoid and aromatic compound emissions in a taxonomically diverse set of 45 subtropical broad-leaved woody species, 26 species without and in 19 species with BVOC storage structures (oil glands, resin ducts and glandular trichomes for volatile compound storage). Emissions of light-weight non-stored isoprene and monoterpenes and aromatic compounds in non-storage species showed moderate and variable emission increases after mechanical injury, likely reflecting the wounding impacts on leaf physiology. In storage species, mechanical injury triggered a substantial release of monoterpenes and aromatic compounds due to the rupture of storage structures. Across species, the proportion of monoterpenes in total emissions increased from 40.9% to 85.4% after mechanical injury, with 32.2% of this increase attributed to newly released compounds not detected in emissions from intact leaves. Sesquiterpene emissions, in contrast, were generally low and decreased after mechanical injury. Furthermore, wounding responses varied among plant functional groups, with evergreen species and those adapted to high temperatures and shade exhibiting stronger damage-induced BVOC emissions than deciduous species and those adapted to dry or cold environments. These findings suggest that mechanical disturbances such as pruning can significantly enhance BVOC emissions in subtropical urban forests and should be considered when modeling BVOC fluxes in both natural and managed ecosystems. Further research is needed to elucidate the relationship between storage structure characteristics and BVOC emissions, as well as their broader ecological and atmospheric implications. Full article
(This article belongs to the Section Plant Physiology and Metabolism)
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Figure 1
<p>Emission rates of isoprene (<b>A</b>,<b>B</b>), monoterpenes (<b>C</b>,<b>D</b>), sesquiterpenes (<b>E</b>,<b>F</b>) and aromatic compounds (<b>G</b>,<b>H</b>) from intact and mechanically injured leaves of 45 subtropical tree species (<a href="#plants-14-00821-t001" class="html-table">Table 1</a>) classified among deciduous and evergreen species and species having or lacking specialized volatile-storing structures (resin ducts, glandular trichomes, oil cells and oil glands). (<b>A</b>,<b>C</b>,<b>E</b>,<b>G</b>) are the species actual average (±SE) emission rates, and (<b>B</b>,<b>D</b>,<b>F</b>,<b>H</b>) are the mean emission rates for intact and damaged leaves. Three replicate trees were sampled for each species, and from each tree, two leaves were measured. The values for two replicate leaves per plant were averaged and then the average for three replicate plants was calculated. * denotes significant differences between intact and injured leaf blade emission rates according to paired-samples <span class="html-italic">t</span>-tests (<span class="html-italic">p</span> &lt; 0.05). “ns” denotes no significant difference between the emission rates of intact and injured leaf blade.</p>
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<p>The proportions of compounds (monoterpenes, sesquiterpenes and aromatic compounds) in intact (<b>A</b>) and damaged (<b>B</b>) leaves in species with and without volatile storage structures and group-average share of BVOC classes for intact (<b>C</b>) and damaged (<b>D</b>) leaves in species without storage structures and for intact (<b>E</b>) and damaged (<b>F</b>) leaves in storage species. “New” represents the share of compounds not observed in the emissions of intact leaves and emitted after the leaves were injured.</p>
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<p>Comparison of average ± SE monoterpene and aromatic compound emission rates among intact and mechanically injured evergreen and deciduous leaves with (19 species) and without (26 species) specialized storage for 45 subtropical woody species. The number of species for each group is shown within each bar. Different letters denote significant differences (<span class="html-italic">p</span> &lt; 0.05) between intact and injured leaf blades among the groups according to ANOVA followed by Duncan tests. The comparisons for isoprene and sesquiterpenes were not informative due to too few species for presence of storage/leaf duration combinations (<span class="html-italic">n</span> = 19). The abbreviations are Deci—deciduous species; Eve—evergreen species.</p>
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<p>Comparison of average ± SE monoterpene and aromatic compound emission rates among intact and mechanically injured leaves of species with varying stress resistance, tolerant to high and low temperatures (<b>A</b>,<b>B</b>) and to high light and shade (<b>C</b>,<b>D</b>) among the 45 subtropical woody species studied. The number of species for each group is shown within each bar. Different letters denote significant differences (<span class="html-italic">p</span> &lt; 0.05) between intact and injured leaves among the groups according to ANOVA followed by Duncan tests. Too few combinations of stress tolerance/presence of storage structure were available for isoprene and sesquiterpenes. Species ecological potentials are HT—high temperature resistant (thermophilus, <span class="html-italic">n</span> = 28); CT—cold tolerant (<span class="html-italic">n</span> = 16); LT—high-light resistant (<span class="html-italic">n</span> = 33); ST—shade tolerant (<span class="html-italic">n</span> = 11).</p>
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<p>Schematic overview of emission characteristics of volatile isoprenoids and aromatics, the wounding responses of emissions, and volatile functions as associated with presence of leaf storage structures and ecological adaptations. The direction from the base to the vertex of the isosceles triangles indicates the change in the expression of the given trait.</p>
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20 pages, 3813 KiB  
Article
Extraction of Curcuminoids and Carvacrol with Biobased Ionic Liquids—Evaluation of Anti-Cancer Properties of Curcuminoid Extracts
by Chefikou Salami, Jean-Pierre Mbakidi, Sandra Audonnet, Sylvie Brassart-Pasco and Sandrine Bouquillon
Molecules 2025, 30(5), 1180; https://doi.org/10.3390/molecules30051180 (registering DOI) - 6 Mar 2025
Abstract
Six biobased ionic liquids were prepared from saturated fatty acids (octanoic, decanoic and dodecanoic acids) and choline with yields up to 90% following procedures respecting green chemistry principles. These ionic liquids were fully characterized (NMR, IR, elemental analysis, viscosimetry and TGA) and used [...] Read more.
Six biobased ionic liquids were prepared from saturated fatty acids (octanoic, decanoic and dodecanoic acids) and choline with yields up to 90% following procedures respecting green chemistry principles. These ionic liquids were fully characterized (NMR, IR, elemental analysis, viscosimetry and TGA) and used as extraction solvents for bioactive compounds (curcuminoids and carvacrol) using classical conditions, and the ionic liquids were able to be recovered after five runs without loss of activity. The ionic liquid containing a C12 carbon chain was the best extracting solvent, extracting 95% of the total curcuminoids contained in turmeric and 69% of the total carvacrol contained in oregano, which are higher yields compared to the extraction procedures described in the literature. As C12 ionic liquids were more cytotoxic than C8 ones, the biological activity of the curcuminoids extracted with C8 ionic liquids was evaluated on a MIAPaCa-2, a pancreatic adenocarcinoma cell line for which antitumor activity of curcuminoids had previously been reported. Compared to the cytotoxicity of the commercially available extract, the cytotoxic activity of the extracts was slightly weaker. Full article
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<p>Curcumin structures.</p>
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<p>Cytotoxicity of <b>7a</b>, <b>9a</b> and <b>9b</b> ILs on MiaPaca-2 cells evaluated using the WST-1 assay. Results are expressed as means ± SD. Statistical significance was studied using <span class="html-italic">t</span>-tests. NS: not significant; ***: <span class="html-italic">p</span> &lt; 0.001; ****: <span class="html-italic">p</span> &lt; 0.0001. <span class="html-italic">n</span> = 7.</p>
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<p>Cytotoxicity of <b>7a</b>, <b>9a</b> and <b>9b</b> ILs on MiaPaca-2 cells evaluated using crystal violet staining. Results are expressed as means ± SD. Statistical significance was studied using <span class="html-italic">t</span>-test. NS: not significant; ***: <span class="html-italic">p</span> &lt; 0.001; ****: <span class="html-italic">p</span> &lt; 0.0001. <span class="html-italic">n</span> = 7.</p>
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<p>MiaPaca-2 cell toxicity of curcuminoid extract analyzed using WST-1 (<b>a</b>) and crystal violet (<b>b</b>) assay compared to commercial curcuminoid analyzed using WST-1 (<b>c</b>) and crystal violet (<b>d</b>), Results are expressed as means +/− SD. Statistical significance was studied using <span class="html-italic">t</span>-tests. NS: not significant; *: <span class="html-italic">p</span> &lt; 0.05; **: <span class="html-italic">p</span> &lt; 0.01; ***: <span class="html-italic">p</span> &lt; 0.001; ****: <span class="html-italic">p</span> &lt; 0.0001. <span class="html-italic">n</span> = 7; N = 2.</p>
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<p>MiaPaca-2 cell growth analyzed using the Incucyte S3 v2024A software. (<b>a</b>) Liquid ionic extracted curcuminoids. (<b>b</b>) Commercial curcuminoids. Results are expressed as means ± SD. <span class="html-italic">n</span> = 3; N = 3.</p>
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<p>MiaPaca-2 cell migration analyzed using Incucyte Scratch wound analysis software v2024A. (<b>a</b>) Liquid ionic extracted curcuminoids. (<b>b</b>) Commercial curcuminoids. Results are expressed as means ± SD. <span class="html-italic">n</span> = 6; N = 3.</p>
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<p>Synthesis of cholinium lactate and levulinate.</p>
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25 pages, 10057 KiB  
Article
Machine Learning Analysis of Hydrological and Hydrochemical Data from the Abelar Pilot Basin in Abegondo (Coruña, Spain)
by Javier Samper-Pilar, Javier Samper-Calvete, Alba Mon, Bruno Pisani and Antonio Paz-González
Hydrology 2025, 12(3), 49; https://doi.org/10.3390/hydrology12030049 (registering DOI) - 6 Mar 2025
Abstract
The Abelar pilot basin in Coruña (northwestern Spain) has been monitored for hydrological and hydrochemical data to assess the effects of eucalyptus plantation and manure applications on water resources, water quality, and nitrate contamination. Here, we report the machine learning analysis of hydrological [...] Read more.
The Abelar pilot basin in Coruña (northwestern Spain) has been monitored for hydrological and hydrochemical data to assess the effects of eucalyptus plantation and manure applications on water resources, water quality, and nitrate contamination. Here, we report the machine learning analysis of hydrological and hydrochemical data from the Abelar basin. K-means cluster analysis (CA) is used to relate nitrate concentrations at the outlet of the basin with daily interflows and groundwater flows calculated with a hydrological balance. CA identifies three linearly separable clusters. Times series Gaussian process regression (TS-GPR) is employed to predict surface water nitrate concentration by incorporating hydrological variables as additional input parameters using a time series shifting. TS-GPR allows modelling nitrate concentrations based on shifted interflows and groundwater flows and chemical concentrations with R2 = 0.82 and 0.80 for training and testing, respectively. Groundwater flow from five days prior to the current date, Qg5, is the most important input parameter of the TS-GPR model. Interaction effects between the variables are found. TS-GPR validation with recent data provides results consistent with those of testing (R2 = 0.85). Model inspection by permutation feature importance and partial dependence plots shows interactions between Qg5 and Cl, and between Ca and Mg. Full article
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Graphical abstract

Graphical abstract
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<p>Location of the Abelar pilot basin south of A Coruña city in northwestern Spain. The coordinate system is ETRS89/UTM zone 29N (EPSG 25,829). Ground elevation contour lines are spaced 2 m. The elevation of the gauging station is 394 m a.s.l.</p>
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<p>Stacked area chart displaying daily values of precipitation and streamflow components.</p>
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<p>Time evolution of daily streamflows calculated with the hydrological water balance model (lines) and measured chemical data of chloride and nitrate (<b>a</b>) and Ca, Mg, and K data (<b>b</b>).</p>
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<p>Flowchart of the methodology of CA modelling in this study.</p>
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<p>Flowchart of the methodology for the TS-GPR modelling in this study.</p>
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<p>Plot of inertia versus number of clusters for 20 K-means models fitted on <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>Q</mi> </mrow> <mrow> <mn>1</mn> </mrow> </msub> </mrow> </semantics></math>, <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>Q</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msub> </mrow> </semantics></math>, and nitrate data. The optimal number of clusters (three) corresponds to the elbow of the curve where the slope of the curve visibly bends from the high to low slope.</p>
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<p>(<b>a</b>) Pair plot of nitrate concentration (mg/L) versus groundwater flow fraction <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>Q</mi> </mrow> <mrow> <mn>2</mn> </mrow> </msub> </mrow> </semantics></math>. (<b>b</b>) Time series plot of nitrate concentration (mg/L) clustered data. The plot shows the three clusters identified by K-means.</p>
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<p>Scatter plots of predicted versus tested nitrate concentrations on the training (left plots) and testing sets (right plots) for (<b>a</b>) the baseline model, and (<b>b</b>) the model with the best correlated hydrological variables. The training results are based on k-fold cross-validation of the training set with 10 folds and 10 repeats.</p>
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<p>Scatter plots of predicted versus tested nitrate concentrations on the training (left plots) and testing sets (right plots) for (<b>a</b>) the model with the best correlated hydrological variables and shifting (10 days), and (<b>b</b>) the model with the best correlated hydrological variables, shifting (10 days) and chemical variables. The training results are based on k-fold cross-validation of the training set with 10 folds and 10 repeats.</p>
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<p>Time series plot of predicted versus tested nitrate concentrations. The plot illustrates the close alignment between observed and predicted nitrate concentrations over time, along with moderately narrow confidence intervals.</p>
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<p>Boxplot of permutation features importance on the testing set. The plot shows the relevance of the time series approach with groundwater flow five days before the current date (<math display="inline"><semantics> <mrow> <msub> <mrow> <mi>Q</mi> </mrow> <mrow> <mi>g</mi> <mn>5</mn> </mrow> </msub> </mrow> </semantics></math>) as the most important variable. The concentrations of Cl, Ca, and Mg are also relevant as they cause great decreases in the R<sup>2</sup> score when shuffled.</p>
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<p>PDP plots of variables <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>Q</mi> </mrow> <mrow> <mi>g</mi> <mn>5</mn> </mrow> </msub> </mrow> </semantics></math> and Cl (<b>a</b>), and Ca and Mg (<b>b</b>). The rightmost plots show an interaction effect between each pair of variables. All variables are unitless after scaling.</p>
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<p>ICE plots of variables <math display="inline"><semantics> <mrow> <msub> <mrow> <mi>Q</mi> </mrow> <mrow> <mi>g</mi> <mn>5</mn> </mrow> </msub> </mrow> </semantics></math> and Cl (<b>a</b>), and Ca and Mg (<b>b</b>). Both pairs of variables have a positive effect on the model’s predictions. The dashed orange lines indicate that on average, increases in each pair of variables lead to higher nitrate concentrations.</p>
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<p>Scatter plot of predicted versus tested nitrate concentrations for the TS-GPR model of step 4 (with shifting of the best correlated hydrological variables and chemical variables) on the validation set.</p>
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<p>Time series plot of predicted versus tested nitrate concentrations on the validation set. The plot illustrates the close alignment between observed and predicted nitrate concentrations over time, along with moderately narrow confidence intervals.</p>
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16 pages, 1739 KiB  
Article
Dietary Behavioural Preferences of Spanish and German Adults and Their Translation to the Dietary Recommendations of a Personalised Nutrition App in the Framework of the Stance4Health Project
by Daniel Hinojosa-Nogueira, Beatriz Navajas-Porras, Silvia Pastoriza, Adriana Delgado-Osorio, Ángela Toledano-Marín, Sascha Rohn, José Ángel Rufián-Henares and José Javier Quesada-Granados
Nutrients 2025, 17(5), 912; https://doi.org/10.3390/nu17050912 (registering DOI) - 6 Mar 2025
Abstract
Background/Objectives: The influence of individual differences in the selection of food portions can have a deep effect on recommendations for personalised nutrition. In addition to typical aspects such us energy density and nutrient composition, portion size is important for dietary recommendations. This [...] Read more.
Background/Objectives: The influence of individual differences in the selection of food portions can have a deep effect on recommendations for personalised nutrition. In addition to typical aspects such us energy density and nutrient composition, portion size is important for dietary recommendations. This study examined the dietary behaviours and portion size selection of 224 subjects in Spain and Germany to use such information to improve dietary adherence to a personalised nutrition app. Methods: An online questionnaire administered to adults in Spain and Germany collected sociodemographic data and dietary habits. The measurement of portion sizes was derived from a classification ranging from XXS to XL across 22 food groups, with assistance from a photographic atlas. Results: Significant differences across dimensions were found. Dietary habits showed that omnivores were the majority in both countries, with significant differences in the consumption of bread, desserts, and beverages. The Mediterranean diet was significantly followed by the Spanish group, reflecting cultural differences. Body mass index (BMI) was slightly higher among Germans, although both populations fell within the normal ranges. Portion size comparisons revealed statistically significant differences in the consumption of various food items between the two countries. Spaniards consumed higher amounts of rice, meat, and legumes, while Germans consumed larger portions of stews, lasagne, and pizza. These variations highlight differing dietary habits influenced by cultural preferences and dietary guidelines. Conclusions: The findings support the development of novel personalised nutrition apps that consider user preferences and enhance dietary adherence, thereby contributing to improved dietary recommendations and health outcomes. Full article
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Graphical abstract
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<p>Adherence to the Mediterranean diet (AMD) by country. A score of 8 or higher indicates high AMD. Differences between Spanish and German samples. ** Significant at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>Heat map showing significant Spearman correlations between BMI, age, and adherence to the Mediterranean diet (AMD). ** Correlation significant at <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>Differences in food size choices by gender and most preferred sizes. Circle size is proportional to frequency. Differences between gender. ** Significant at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>Differences in food size choices by country. Circle size is proportional to frequency. Differences between country. ** Significant at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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19 pages, 4183 KiB  
Article
Scaling Up Red Ginger Kombucha Fermentation: Insights into Its Chemical Profile and Health-Promoting Properties
by Hani Mulyani, Nina Artanti, Ratna Yuniati and Yasman Yasman
Fermentation 2025, 11(3), 128; https://doi.org/10.3390/fermentation11030128 (registering DOI) - 6 Mar 2025
Abstract
Red ginger, a plant widely available in Indonesia, is known for its rich content of bioactive compounds, including flavonoids and phenolics, which are known for their strong antioxidant properties. This study explored the fermentation of red ginger extract with kombucha inoculum (SCOBY), aiming [...] Read more.
Red ginger, a plant widely available in Indonesia, is known for its rich content of bioactive compounds, including flavonoids and phenolics, which are known for their strong antioxidant properties. This study explored the fermentation of red ginger extract with kombucha inoculum (SCOBY), aiming to evaluate its potential as a health-enhancing herb with antioxidant and antidiabetic properties by neutralizing free radicals and inhibiting α-glucosidase activity. This study included laboratory-scale (100 mL) and large-scale (10 L) fermentation using 10% red ginger concentration and 15% red ginger kombucha SCOBY for fermentation periods of 0, 7, and 14 days at room temperature. The analysis included sugar content (glucose, fructose, and maltose), organic acids (acetic acid, lactic acid, and gluconic acid), pH, total titrated acids, total polyphenols (Folin–Ciocalteu), and total flavonoids (AlCl3). Fermented red ginger kombucha showed high levels of acetic, lactic, and gluconic acids, along with minor components such as phenolic acids, indicating its potential health benefits as a natural antioxidant. Red ginger kombucha showed significant antioxidant and antidiabetic activity, indicating its potential in managing conditions such as prediabetes and type 2 diabetes. The results of the fermented ginger study showed potential as a health drink with antioxidant and antidiabetic properties given its ability to reduce free radicals and inhibit the activity of the enzyme α-glucosidase. Full article
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<p>Red ginger. Source: Personal documentation.</p>
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<p>GC chromatogram of the n-hexane fraction of red ginger before fermentation.</p>
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<p>HPLC chromatogram of sugar content (glucose and fructose) in red ginger kombucha after 12 days of fermentation.</p>
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<p>Effect of process scale and fermentation time on the glucose and fructose content of red ginger kombucha. Lowercase letters indicate the interaction between scale and fermentation time (a, b, c, d, e, f), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>HPLC chromatogram of organic acid content (acetic acid, lactic acid, and gluconic acid) of red ginger kombucha after 12 days of fermentation.</p>
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<p>Effect of process scale and fermentation time on the acetic acid, lactic acid, and gluconic acid contents of red ginger kombucha. Lowercase letters indicate the interaction between scale and fermentation time (a, b, c), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>pH of red ginger kombucha resulting from various fermentation times. Values for both laboratory scale and larger production scale are presented. Lowercase letters indicate the interaction between scale and fermentation time (a, b), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>Total acid content of red ginger kombucha resulting from various fermentation times. Values for both the laboratory scale and larger production scale are presented. Lowercase letters indicate the interaction between scale and fermentation time (a, b,c), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>The total polyphenol content in of red ginger kombucha resulting from various fermentation times at both the laboratory and production scales is presented. Lowercase letters indicate the interaction between scale and fermentation time (a, b), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>The total flavonoid content in red ginger kombucha, as a function of fermentation time, at both laboratory and production scales, is presented. Lowercase letters indicate the interaction between scale and fermentation time (a), showing that the values are not significant at the <span class="html-italic">p</span> &gt; 0.05 level.</p>
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<p>Inhibition of the free radical DPPH in red ginger kombucha resulting from fermentation time at both laboratory scales and larger production scales are presented. Lowercase letters indicate the interaction between scale and fermentation time (a, b), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.05 level.</p>
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<p>α-Glucosidase inhibition in red ginger kombucha resulting from various fermentation times at both the laboratory scale and larger production scale. Lowercase letters indicate the interaction between scale and fermentation time (a, b, c), showing significantly different values at the <span class="html-italic">p</span> &lt; 0.01 level.</p>
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16 pages, 2811 KiB  
Article
Extraction and Analysis of Phenolic Compounds from Rocket: Development of a Green and Innovative DES-Based Extraction Method
by Vittoria Terrigno, Susanna Della Posta, Giorgia Pietrangeli, Teodora Chiara Tonto, Vittoria Locato, Laura De Gara and Chiara Fanali
Molecules 2025, 30(5), 1177; https://doi.org/10.3390/molecules30051177 (registering DOI) - 6 Mar 2025
Abstract
Eruca sativa Mill. is an annual plant belonging to the Cruciferous family that is characterized by the presence of antioxidant bioactive molecules such as phenolic compounds. Their extraction is usually performed through solid–liquid extraction based on the use of organic solvent. Deep eutectic [...] Read more.
Eruca sativa Mill. is an annual plant belonging to the Cruciferous family that is characterized by the presence of antioxidant bioactive molecules such as phenolic compounds. Their extraction is usually performed through solid–liquid extraction based on the use of organic solvent. Deep eutectic solvents (DESs) are new green solvents capable of increasing bioactive molecules yield if replaced with organic solvents. The aim of this work was to develop a green analytical method based on the use of DESs for the determination of phenolic compounds in rocket plants. The extraction optimization involved the selection of the best extraction solvent among different selected DESs and the study of the parameters that mainly affect the extraction yield: the quantity of water to add to the selected DES to reduce its viscosity, the matrix-to-solvent ratio, and the time and temperature of the extraction. ChCl-glucose (1:2 molar ratio) DES was selected as the extraction solvent under the following optimized conditions: 1:50 (w/v) as the matrix-to-solvent ratio; 30% of water was added to the DES; extraction time of 30 min; and extraction temperature of 50 °C. The rocket phenolic compounds profile was determined through a high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) analysis. The innovative green method was applied to real plant samples to determine the growth conditions that favored the accumulation of bioactive molecules. Full article
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<p>TPC of rocket extracts obtained with different DESs and traditional solvents. A one-way analysis of variance (ANOVA) followed by Tukey’s test was performed to define statistically significant differences. Different letters indicate statistically significant differences among results.</p>
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<p>FTIR spectra of glucose (<b>a</b>), ChCl-glucose DES (<b>b</b>) and ChCl (<b>c</b>), respectively.</p>
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<p>Concentration (mg GAE/g) of phenolic compounds extracted from rocket varying the percentage of water added to the selected DES. A one-way analysis of variance (ANOVA) followed by Tukey’s test was performed to define statistically significant differences. Different letters indicate statistically significant differences among results.</p>
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<p>Concentration (mg GAE/g) of phenolic compounds obtained considering different quantities of the matrix-to-solvent ratio. A one-way analysis of variance (ANOVA) followed by Tukey’s test was performed to define statistically significant differences. Different letters indicate statistically significant differences among results.</p>
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<p>Concentration (mg GAE/g) of phenolic compounds obtained by testing different extraction times. A one-way analysis of variance (ANOVA) followed by Tukey’s test was performed to define statistically significant differences. Different letters indicate statistically significant differences among results.</p>
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<p>Concentration (mg GAE/g) of phenolic compounds obtained testing different extraction temperatures. A one-way analysis of variance (ANOVA) followed by Tukey’s test was performed to define statistically significant differences. Different letters indicate statistically significant differences among results.</p>
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<p>Complex GAPI analysis. Collection (1); preservation (2); transport (3); storage (4); type of method (5); scale of extraction (6); solvents/reagents used (7); additional treatments (8); amount (9); health hazard (10); safety hazard (11); energy (12); occupational hazard (13); waste (14); waste treatment (15); type of analysis (16).</p>
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<p>HPLC-PDA chromatogram (λ = 280 nm) of rocket extract obtained using optimized conditions and the phenolic compounds putatively identified: isorhamnetin (1); quercitin-3-O-galactoside (2); roseoside (3); quercitin (4); ferulic acid (5); chlorogenic acid (6).</p>
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12 pages, 5153 KiB  
Article
Preparation of CL-20 with Controllable Particle Size Using Microfluidic Technology
by Zihao Zhang, Jin Yu, Yujia Wen, Hanyu Jiang, Siyu Xu, Yubao Shao, Ergang Yao, Heng Li and Fengqi Zhao
Molecules 2025, 30(5), 1176; https://doi.org/10.3390/molecules30051176 (registering DOI) - 6 Mar 2025
Abstract
As a typical high-energy-density material, the sensitivity of CL-20 severely limits its application in explosives and propellants. Adjusting its structure at the microscopic level can effectively solve such problems. In this study, a microfluidic recrystallization technique was used to prepare ε-CL-20 with three [...] Read more.
As a typical high-energy-density material, the sensitivity of CL-20 severely limits its application in explosives and propellants. Adjusting its structure at the microscopic level can effectively solve such problems. In this study, a microfluidic recrystallization technique was used to prepare ε-CL-20 with three different particle sizes, with narrow particle size distributions (D50 = 2.77 μm, 17.22 μm and 50.35 μm). The prepared samples had fewer surface defects compared to the raw material. As the particle size decreased, the density of CL-20 increased and its impact sensitivity was significantly reduced. The activation energy of the CL-20 prepared using microfluidic technology increased with increases in particle size. Laser ignition experiments revealed that smaller CL-20 particles had the highest energy release efficiency, while larger particles exhibited a higher energy density and more stable energy release. The combustion performance and safety of CL-20 can be effectively improved by improving the crystal size distribution and surface morphology. Controllable preparation of multiple particle sizes of CL-20 was achieved using microfluidic recrystallization technology, which provides a reference for the preparation of multiple particle sizes of other energetic materials. Full article
(This article belongs to the Section Materials Chemistry)
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<p>SEM and statistical plots of particle size. (<b>a</b>) Raw CL-20, (<b>b</b>) S1, (<b>c</b>) S2, (<b>d</b>) S3. (<b>a1</b>,<b>a2</b>) SEM and particle size distribution of Raw CL-20; (<b>b1</b>,<b>b2</b>) SEM and particle size distribution of S1; (<b>c1</b>,<b>c2</b>) SEM and particle size distribution of S2; (<b>d1</b>,<b>d2</b>) SEM and particle size distribution of S3.</p>
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<p>Axial concentration distribution of solute on the (0 0 1) crystal face (<b>a</b>) before adsorption; (<b>b</b>) after adsorption [<a href="#B21-molecules-30-01176" class="html-bibr">21</a>]. (The black dashed box indicates that the axial concentration distribution curve of the ε-CL-20 molecule intersects the concentration curve of the crystal surface, indicating that some solutes have entered the groove area of the crystal face).</p>
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<p>XRD of raw CL-20, S1, S2, and S3.</p>
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<p>The angle of repose and density of raw CL-20, S1, S2 and S3.</p>
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<p>DSC curves of raw CL-20, S1, S2, and S3. (<b>a</b>) Raw CL-20, (<b>b</b>) S1, (<b>c</b>) S2, (<b>d</b>) S3.</p>
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<p>Images of flame propagation at 192 W/cm<sup>2</sup> for (<b>a</b>) raw CL-20, (<b>b</b>) S1, (<b>c</b>) S2, (<b>d</b>) S3.</p>
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<p>Ignition delay time of raw CL-20, S1, S2, and S3.</p>
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<p>Impact sensitivity and electrostatic spark sensitivity of raw CL-20, S1, S2, and S3.</p>
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<p>The microfluidic system.</p>
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17 pages, 2564 KiB  
Article
Comparative Analysis of Amorphous and Biodegradable Copolymers: A Molecular Dynamics Study Using a Multi-Technique Approach
by Alovidin Nazirov, Jacek Klinowski and John Nobleman
Molecules 2025, 30(5), 1175; https://doi.org/10.3390/molecules30051175 (registering DOI) - 6 Mar 2025
Abstract
We investigate the molecular dynamics of glycolide/lactide/caprolactone (Gly/Lac/Cap) copolymers using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), 1H second-moment, 1H spin-lattice relaxation time (T1) analysis, and 13C solid-state NMR over a temperature range of 100–413 K. [...] Read more.
We investigate the molecular dynamics of glycolide/lactide/caprolactone (Gly/Lac/Cap) copolymers using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), 1H second-moment, 1H spin-lattice relaxation time (T1) analysis, and 13C solid-state NMR over a temperature range of 100–413 K. Activation energies and correlation times of the biopolymer chains were determined. At low temperatures, relaxation is governed by the anisotropic threefold reorientation of methyl (-CH3) groups in lactide. A notable change in T1 at ~270 K and 294 K suggests a transition in amorphous phase mobility due to translational diffusion, while a second relaxation minimum (222–312 K) is linked to CH2 group dynamics influenced by caprolactone. The activation energy increases from 5.9 kJ/mol (methyl motion) to 22–33 kJ/mol (segmental motion) as the caprolactone content rises, enhancing the molecular mobility. Conversely, lactide restricts motion by limiting rotational freedom, thereby slowing global dynamics. DSC confirms that increasing ε-caprolactone lowers the glass transition temperature, whereas higher glycolide and lactide content raises it. The onset temperature of main-chain molecular motion varies with the composition, with greater ε-caprolactone content enhancing flexibility. These findings highlight the role of composition in tuning relaxation behavior and molecular mobility in copolymers. Full article
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<p>DSC thermograms of copolymers 0.5Gly/0.2Lac/0.3Cap and 0.5Gly/0.4Lac/0.1Cap, where heating (1⟶) and cooling (⟵2) are indicated. The dashed vertical lines represent a phase transition temperature (T<sub>g</sub>).</p>
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<p>Solution-state <sup>13</sup>C NMR spectra (75 MHz) of copolymers 0.5Gly/0.2Lac/0.3Cap and 0.5Gly/0.4Lac/0.1Cap recorded at 313 K. Letters (A–G) indicate the assignment of molecular groups. The samples were dissolved in CDCl<sub>3</sub> (chloroform-d, 77.2 ppm, triplet due to deuterium coupling), with TMS (0 ppm) as the internal reference.</p>
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<p>Derivatives of <sup>1</sup>H NMR absorption spectra of (<b>a</b>) 0.5Gly/0.2Lac/0.3Cap and (<b>b</b>) 0.5Gly/0.4Lac/0.1Cap at different temperatures. The proton derivative spectra at 273 K are highly sensitive compared to the broad DSC lines (c.f. <a href="#molecules-30-01175-f001" class="html-fig">Figure 1</a>) for both polymers, indicating the early onset of chain molecular dynamics motion in preparation for the phase transition.</p>
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<p>Second moments of the <sup>1</sup>H NMR lines of 0.5Gly/0.2Lac/0.3Cap and 0.5Gly/0.4Lac/0.1Cap versus temperature. The glass phase transition temperatures, T<sub>g</sub> indicated by the vertical lines (according to DSC, c.f. <a href="#molecules-30-01175-f001" class="html-fig">Figure 1</a>).</p>
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<p>Arrhenius plots of <sup>1</sup>H spin-lattice relaxation times measurements at 200 MHz and 9 MHz for 0.5Gly/0.2Lac/0.3Cap and 0.5Gly/0.4Lac/0.1Cap. <sup>1</sup>H experimental data fitted using the BPP model as indicated by solid lines. The experiments conducted from the low to high temperatures and the glass phase transition T<sub>g</sub> indicated by the vertical dashed lines (according to DSC, c.f. <a href="#molecules-30-01175-f001" class="html-fig">Figure 1</a>).</p>
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<p>The resonance frequency of 75.56 MHz <sup>13</sup>C solid-state NMR of copolymers 0.5Gly/0.2Lac/0.3Cap and 0.5Gly/0.4Lac/0.1Cap at different temperatures. The molecular groups are indicated by letters corresponding to the structure of copolymer chains. Solid-state NMR technology is still under development compared to its solution-state counterpart. One of the key technical challenges is the difficulty of spinning amorphous materials at high speeds. Due to their unique behavioral properties, such as superfluid-like elasticity, these materials tend to lose centrifugal axis stability during rotation. The magnitude of <sup>13</sup>C hydrocarbon signals effectively increases with rising temperature, corresponding to an increase in intensity due to fast trans-gauche isomerization and translational diffusion motion.</p>
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<p>FTIR spectra of copolymers (<b>a</b>) 0.5Gly/0.2Lac/0.3Cap and (<b>b</b>) 0.5Gly/0.4Lac/0.1Cap at different temperatures. The band assignments correspond to hydroxyl end-groups (-OH), carbonyl (C=O), methyl (-CH<sub>3</sub>), methylene (-CH<sub>2</sub>-), and methide (-CH-) vibrational motions. The spectra clearly indicate differences in the vibrational motions of the modulated chains.</p>
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28 pages, 12048 KiB  
Article
Exploring Thermal Runaway: Role of Battery Chemistry and Testing Methodology
by Sébastien Sallard, Oliver Nolte, Lorenz von Roemer, Brahim Soltani, Alexander Fandakov, Karsten Mueller, Maria Kalogirou and Marc Sens
World Electr. Veh. J. 2025, 16(3), 153; https://doi.org/10.3390/wevj16030153 (registering DOI) - 6 Mar 2025
Abstract
One of the major concerns for battery electric vehicles (BEVs) is the occurrence of thermal runaway (TR), usually of a single cell, and its propagation to adjacent cells in a battery pack. To guarantee sufficient safety for the vehicle occupants, the TR mechanisms [...] Read more.
One of the major concerns for battery electric vehicles (BEVs) is the occurrence of thermal runaway (TR), usually of a single cell, and its propagation to adjacent cells in a battery pack. To guarantee sufficient safety for the vehicle occupants, the TR mechanisms must be known and predictable. In this work, we compare thermal runaway scenarios using different initiation protocols (heat–wait–seek, constant heating, nail penetration) and battery chemistries (nickel manganese cobalt oxide, NMC; lithium iron phosphate, LFP; and sodium-ion batteries, SIB) with the cells in a fully charged state. Our goal is to specifically trigger a variety of different possible TR scenarios (internal failure, external hotspot, mechanical damage) with different types of chemistries to obtain reliable data that are subsequently employed for modeling and prediction of the phenomenon. The safety of the tested cells depending on their chemistry can be summarized as LFP > SIB >> NMC. The data of the TR experiments were used as the basis for high-fidelity modeling and predicting of TR phenomena in 3D. The models simulated reaction rates, represented by the typically employed Arrhenius approach. The effects of the investigated TR triggering methods and cell chemistries were represented with sufficient accuracy, enabling the application of the models for the simulation of thermal propagation in battery packs. Full article
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<p>Overview of the relationships between causes and the thermal runaway and propagation mechanisms of a Li-ion battery (SEI = Solid Electrolyte Interphase, T = Temperature).</p>
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<p>Overview of the relationships between NMC aging and degradation mechanisms in a Li-ion cell.</p>
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<p>Position of the seven thermocouples (TCs) on an 18,650 cell. The yellow area represents the heating pad.</p>
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<p>Geometry of single cell with clamps as employed in the 3D CFD simulation environment.</p>
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<p>Temperature evolution during the CH experiments of (<b>a</b>) the LFP, (<b>b</b>) the SIB (<b>b</b>,<b>c</b>) the NMC811 cell, photo of (<b>d</b>) the LFP cell at 540 s, limited fuming, (<b>e</b>) the SIB cell at the thermal runaway at 460 s, and, (<b>f</b>) the NMC811 cell at the thermal runaway at 720 s. Note the fume was so dense for the SIB that rapidly nothing else was visible with the camera.</p>
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<p>Temperature evolution during the HWS experiment of (<b>a</b>) the LFP, (<b>b</b>) the SIB cell and (<b>c</b>) the NMC811 cell.</p>
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<p>Temperature evolution during nail penetration test of (<b>a</b>) the SIB and (<b>b</b>) the NMC811 cells. Photos of the cells when visual change are recorded attributed to the TR event, i.e., (<b>c</b>) visible smoke for the SIB (from the top only) or (<b>d</b>) visible smoke (bottom left) and sparks for the NMC811.</p>
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<p>Temperature rise rates at the lateral surface depending on the cell chemistry (LFP, SIB and NMC) during a thermal runaway for each trigger method ((<b>a</b>) constant heating, (<b>b</b>) heat-wait-seek, (<b>c</b>) nail penetration). Note the logarithmic scaling of the temperature gradient as well as the different scaling of the temperature gradient in diagram °C.</p>
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<p>Temperature rise rates at different side surface locations during a thermal runaway depending on the trigger method for each cell chemistry ((<b>a</b>) LFP, (<b>b</b>) SIB, (<b>c</b>) NMC). Note the logarithmic scaling of the temperature gradient as well as the different scaling of the temperature gradient in diagram °C.</p>
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<p>Cell energy density (red dots) in Wh/kg for the LFP, SIB and NMC811 cells as well as the capacity-normalized gas volume in L/Ah emitted during thermal runaway tests using different trigger methods.</p>
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<p>MC811 (<b>a</b>) constant heating, used for NMC model calibration, and (<b>b</b>) heat–wait–seek comparison between measurement and CFD.</p>
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<p>Nail penetration comparison for NMC811 (<b>a</b>) and SIB (<b>b</b>) between measurement and CFD.</p>
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<p>NMC811 heat–wait–seek comparison between different thermocouples in measurement (<b>a</b>) and CFD simulation (<b>b</b>).</p>
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<p>Health state evolution of the NMC811 cell CH thermal runaway reaction progress described with the calibrated Ren mechanism; 100% = pristine state material, 0% = wrecked material.</p>
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<p>LFP constant heating ((<b>a</b>), used for LFP model calibration) and heat–wait–seek (<b>b</b>) comparison between measurement and CFD.</p>
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<p>SIB constant heating ((<b>a</b>), used for SIB model calibration) and heat–wait–seek (<b>b</b>) comparison between measurement and CFD.</p>
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<p>NMC811 cell located in the autoclave and with a specific cell holder for the nail penetration test.</p>
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<p>NMC811 cell with temperature sensors and one heating pad located in the autoclave before the thermal runaway experiment.</p>
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<p>LFP cell during CH experiment at ca. 928 s after beginning of the experiment.</p>
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<p>Overview of important sensor traces during the SIB nail penetration test. The top panel shows cell voltage and nail penetration depth, while the bottom panel shows the temperature at the cell bottom and the autoclave pressure, all as a function of time. The first detection of cell voltage deviations as well as the point of maximum temperature on the lateral cell surface are indicated by dashed lines.</p>
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<p>Overview of important sensor traces during the NMC nail penetration test. The top panel shows cell voltage and nail penetration depth, while the bottom panel shows the temperature at the cell bottom and the autoclave pressure, all as a function of time. The first detection of cell voltage deviations as well as the point of maximum temperature on the lateral cell surface are indicated by dashed lines.</p>
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<p>SIB cell during nail penetration test, ca. 1 s after <a href="#wevj-16-00153-f007" class="html-fig">Figure 7</a>c. A small but dense white smoke emission is visible on the bottom left of the cell.</p>
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<p>NMC811 cell during nail penetration test, ca. 1.5 s after <a href="#wevj-16-00153-f007" class="html-fig">Figure 7</a>d. Flames become visible on the top of the cell holder and last for 2 more seconds. A tenuous smoke, emitted from the cell since the start of the TR, explains the blurry nature of the recording.</p>
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16 pages, 7861 KiB  
Article
Preparation and Performance Evaluation of Environmentally Friendly Foam Hydrogel Based on Polyvinyl Alcohol/Organic Titanium Crosslinking Agent
by Ru Ma, Gaoshen Su, Ya Nie, Huan Yang and Xiaorong Yu
Gels 2025, 11(3), 181; https://doi.org/10.3390/gels11030181 (registering DOI) - 6 Mar 2025
Abstract
Foam and hydrogel profile control are commonly utilized water-blocking and profile modification techniques in oil fields. This study integrates a foam system with a gel system, employing an organic titanium crosslinking agent to crosslink polyvinyl alcohol, thereby forming a gel system. Concurrently, a [...] Read more.
Foam and hydrogel profile control are commonly utilized water-blocking and profile modification techniques in oil fields. This study integrates a foam system with a gel system, employing an organic titanium crosslinking agent to crosslink polyvinyl alcohol, thereby forming a gel system. Concurrently, a gas-evolving agent is incorporated into the system to induce in situ foaming, thereby creating an environmentally benign foam gel system. The fundamental constituents of this system comprise 2 wt% to 5 wt% polyvinyl alcohol, 2 wt% to 4 wt% crosslinker, and 0.3 wt% to 0.9 wt% gas-generating agent. By varying the amounts of each component, the strength grade, gelation time, and foaming volume of the foam gel can be effectively adjusted. The results of the temperature resistance performance evaluation indicate that within the temperature range of 80 °C to 130 °C, the gelation performance of the foam gel is stable and good. At 90 °C, the foam gel can remain stable for 340 days with minimal strength variation. The plugging experiments indicate that the formulated foam gel system exhibits superior injectability and can effectively seal the sand-filled tube model, achieving a blocking efficiency of up to 96.36%. Full article
(This article belongs to the Special Issue Gels in the Oil Field)
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<p>Effect of the synergistic effect of polyvinyl alcohol and crosslinker concentration on the gelatinization grade of foam gel.</p>
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<p>Effect of the synergistic effect of polyvinyl alcohol and crosslinker concentration on the gelatinization volume of foam gel.</p>
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<p>Effect of the synergistic effect of polyvinyl alcohol and crosslinker concentration on the gelatinization time of foam gel.</p>
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<p>Experimental phenomena of gelatinization of 5 wt% polyvinyl alcohol concentration under different crosslinker concentrations.</p>
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<p>The effect of gas-generating agent concentration on the gel strength, gelation time, and gel volume of foam gels.</p>
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<p>Experimental phenomena of foam gel formation under different gas-generating agent concentrations.</p>
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<p>FTIR analysis of PVA foam gel.</p>
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<p>SEM: foam gel microstructure. (<b>a</b>) Internal structure of the gel; (<b>b</b>) Gel surface structure.</p>
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<p>Morphological characteristics of foam gels at 4× magnification. (<b>a</b>) Initial state of polyvinyl alcohol foam gel; (<b>b</b>) State of polyvinyl alcohol foam gel after 100 days at 90 °C; (<b>c</b>) State of polyvinyl alcohol foam gel after 200 days at 90 °C; (<b>d</b>) State of polyvinyl alcohol foam gel after 362 days at 90 °C.</p>
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<p>Weight loss rate–temperature variation of polyvinyl alcohol gel/foam gel.</p>
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<p>Effect of salt concentration on the properties of foam gels.</p>
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<p>Effect of temperature on the properties of foam gels.</p>
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<p>Viscoelastic analysis of gels.</p>
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<p>Relationship between volume retention rate and defoaming rate with time.</p>
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<p>Schematic diagram of the displacement experimental setup.</p>
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27 pages, 5195 KiB  
Article
Enhanced Adsorption of Methylene Blue in Wastewater Using Natural Zeolite Impregnated with Graphene Oxide
by Gabriela Tubon-Usca, Cyntia Centeno, Shirley Pomasqui, Amerigo Beneduci and Fabian Arias Arias
Appl. Sci. 2025, 15(5), 2824; https://doi.org/10.3390/app15052824 (registering DOI) - 5 Mar 2025
Abstract
The use of graphene oxide (GO) in combination with mesoporous materials has gained interest in the development of adsorbents. In this study, GO was impregnated into zeolite at three concentrations (ZGO2.5, ZGO5, and ZGO10) through a simple thermal process to enhance the adsorption [...] Read more.
The use of graphene oxide (GO) in combination with mesoporous materials has gained interest in the development of adsorbents. In this study, GO was impregnated into zeolite at three concentrations (ZGO2.5, ZGO5, and ZGO10) through a simple thermal process to enhance the adsorption of methylene blue (MB). Characterization of the resulting materials was performed using spectroscopic techniques such as UV-Vis and FT-IR spectroscopy, SEM, and EDS, confirming the presence of GO on zeolite. Batch experiments were conducted to evaluate their performance, analyzing contact time, pH effect, and adsorption kinetics. Pseudo-first-order, pseudo-second-order, and Elovich kinetic models were applied, and the adsorption mechanism was studied using Langmuir, Freundlich, Temkin II, and Dubinin–Radushkevich (D-R) isotherms at different temperatures. Optimal adsorption was achieved at 273 K, 100 mg L−1 of MB, adsorbent mass of 100 mg, 250 rpm, and pH 5–9, with 90% removal efficiency after 70 min. The pseudo-second-order, Freundlich, and D-R models best described the process (R2 > 0.98), suggesting a mixed physisorption–chemisorption mechanism. The maximum adsorption capacity from the D-R isotherm reached 119 mg g−1 at 333 K. Thermodynamic studies showed that adsorption was a spontaneous and endothermic process. These findings highlight the potential of GO-impregnated zeolite as an effective adsorbent for MB. Full article
(This article belongs to the Section Materials Science and Engineering)
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<p>(<b>a</b>) Uv–visible spectrum of graphene oxide; (<b>b</b>) Uv–visible spectrum of natural zeolite; (<b>c</b>) spectra of natural zeolite impregnated with GO at a concentration of 10 mg mL<sup>−1</sup> (ZGO10), 5 mg mL<sup>−1</sup> (ZGO5), and 2.5 mg mL<sup>−1</sup> (ZGO2.5); all spectra were recorded in aqueous solution.</p>
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<p>FTIR spectra of GO, zeolite, and the ZGO2.5, ZGO5, and ZGO10 nanocomposites.</p>
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<p>(<b>a</b>) Graphene oxide (GO) morphology; bar, <math display="inline"><semantics> <mrow> <mn>10</mn> <mo> </mo> <mi mathvariant="normal">μ</mi> <mi mathvariant="normal">m</mi> </mrow> </semantics></math>; (<b>b</b>) natural zeolite; bar, <math display="inline"><semantics> <mrow> <mn>20</mn> <mo> </mo> <mi mathvariant="normal">μ</mi> <mi mathvariant="normal">m</mi> </mrow> </semantics></math>; (<b>c</b>) nanocomposite of zeolite and graphene oxide, bar, <math display="inline"><semantics> <mrow> <mn>10</mn> <mo> </mo> <mi mathvariant="normal">μ</mi> <mi mathvariant="normal">m</mi> </mrow> </semantics></math>.</p>
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<p>(<b>a</b>) Electron-dispersive spectroscopy (EDS) spectrum of graphene oxide; (<b>b</b>) EDS spectrum of natural zeolite (bar, <math display="inline"><semantics> <mrow> <mn>100</mn> <mo> </mo> <mi mathvariant="normal">μ</mi> <mi mathvariant="normal">m</mi> </mrow> </semantics></math>) (<b>c</b>) EDS spectrum of nanocomposite formed of natural zeolite and graphene oxide (ZOG).</p>
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<p>(<b>a</b>) Point of zero charge of ZGO10; (<b>b</b>) effect of pH on the equilibrium adsorption capacity of the composite ZGO10 towards MB.</p>
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<p>Contact time dependence of (<b>a</b>) MB concentration (Ct) and (<b>b</b>) adsorption capacity (qt) for pristine zeolite and GO; (<b>c</b>) MB removal efficiency (RE%) vs. contact time for the composite adsorbents.</p>
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<p>Adsorption kinetics of MB on ZGO2.5, ZGO5, and ZGO10 as a function of contact time (up to 120 min). (<b>a</b>) Pseudo-first- and -second order models; (<b>b</b>) Elovich model.</p>
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<p>Intraparticle diffusion plot showing three regions of linearity (C<sub>0</sub> = 100 mg L<sup>−1</sup>, T = 298 K).</p>
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<p>Fitting of the experimental isotherm data at different temperatures using the isotherm models of (<b>a</b>) Langmuir; (<b>b</b>) Freundlich; (<b>c</b>) Temkin; (<b>d</b>) Dubinin–Radushkevich.</p>
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<p>Illustrative diagram of the adsorption mechanisms of MB<sup>+</sup> onto ZGO including arrows identifying distinct material regions (surface and pores).</p>
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<p>van’t Hoff regression for determining the thermodynamic parameters of MB adsorption onto ZOG10.</p>
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28 pages, 4600 KiB  
Article
Utilization of Coniferous and Deciduous Tree and Paper Ashes as Fillers of Rigid Polyurethane/Polyisocyanurate (PU/PIR) Foams
by Joanna Liszkowska, Magdalena Stepczyńska, Andrzej Trafarski, Justyna Miłek and Tomasz Karasiewicz
Materials 2025, 18(5), 1165; https://doi.org/10.3390/ma18051165 - 5 Mar 2025
Abstract
Five series of rigid polyurethane–polyisocyanurate (RPU/PIR) foams were obtained. They were modified by ashes from burning paper (P) and wood: conifers (pine—S, spruce—S’) and deciduous trees (oak—D, birch—B). The ash was added to rigid polyurethane–polyisocyanurate foams (PU/PIR). In this way, five series of [...] Read more.
Five series of rigid polyurethane–polyisocyanurate (RPU/PIR) foams were obtained. They were modified by ashes from burning paper (P) and wood: conifers (pine—S, spruce—S’) and deciduous trees (oak—D, birch—B). The ash was added to rigid polyurethane–polyisocyanurate foams (PU/PIR). In this way, five series of foams with different ash contents (from 1 to 9% wt.) were obtained: PP, PS, PD, PS’, PB. The model foam (reference—W) was obtained without filler. The basic properties, physico-mechanical, and thermal properties of the ashes and obtained foams were examined. It was specified, among other things, the cellular structure by scanning electron microscopy (SEM), and changes in chemical structure by Fourier-transform infrared spectroscopy (FTIR) were compared. The obtained foams were also subjected to thermostating in a circulating air dryer in increased temperature (120 °C) for 48 h. Ash tests showed that their skeletal density is about 2.9 g/cm3, and the pH of their solutions ranges from 9 to 13. The varied color of the ashes affected the color of the foams. SEM-EDS tests showed the presence of magnesium, calcium, silicon, potassium, aluminum, phosphorus, sodium, and sulfur in the ashes. Foam tests showed that pine ash is the most beneficial for foams, because it increases their compressive strength three times compared to W foam and improves their thermal stability. All ashes cause the residue after combustion of the foams (retention) to increase and the range of combustion of the samples to decrease. Full article
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<p>Ashes used for foams: (<b>a</b>) pine, (<b>b</b>) spruce, (<b>c</b>) birch, (<b>d</b>) paper, (<b>e</b>) oak.</p>
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<p>Ashes in resin for SEM-EDS.</p>
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<p>SEM images of ashes.</p>
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<p>DSC–EDS of ashes: (<b>a</b>) paper—P; (<b>b</b>) pine—S; (<b>c</b>) spruce—S’; (<b>d</b>) birch—B; (<b>e</b>) oak—D.</p>
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<p>DSC–EDS of ashes: (<b>a</b>) paper—P; (<b>b</b>) pine—S; (<b>c</b>) spruce—S’; (<b>d</b>) birch—B; (<b>e</b>) oak—D.</p>
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<p>FTIR of ashes.</p>
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<p>DSC of ashes.</p>
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<p>TGA and DTG of ashes.</p>
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<p>FTIR of foams with ashes: W—reference; PB9—with birch; PD7—witch oak; PS’9—with spruce; PS7—with pine; PP9—with paper.</p>
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<p>TGA and DTG of foams.</p>
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<p>Retention of foam content ashes.</p>
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<p>Dependence of flame range on ash content in foams.</p>
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<p>Dependence of water absorption on the content of ash in foam.</p>
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<p>Dependence of absorbability on the content of ash in foam.</p>
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<p>Dependence of compressive strength on ash content in foams.</p>
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<p>Foam structure.</p>
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22 pages, 12118 KiB  
Article
Modern Comprehensive Metabolomic Profiling of Pollen Using Various Analytical Techniques
by Petra Krejčí, Zbyněk Žingor, Jana Balarynová, Andrea Čevelová, Matěj Tesárek, Petr Smýkal and Petr Bednář
Molecules 2025, 30(5), 1172; https://doi.org/10.3390/molecules30051172 - 5 Mar 2025
Abstract
Pollen is a cornerstone of life for plants. Its durability, adaptability, and complex design are the key factors to successful plant reproduction, genetic diversity, and the maintenance of ecosystems. A detailed study of its chemical composition is important to understand the mechanism of [...] Read more.
Pollen is a cornerstone of life for plants. Its durability, adaptability, and complex design are the key factors to successful plant reproduction, genetic diversity, and the maintenance of ecosystems. A detailed study of its chemical composition is important to understand the mechanism of pollen–pollinator interactions, pollination processes, and allergic reactions. In this study, a multimodal approach involving Fourier transform infrared spectrometry (FTIR), direct mass spectrometry with an atmospheric solids analysis probe (ASAP), matrix-assisted laser desorption/ionization (MALDI) and ultra-high-performance liquid chromatography–mass spectrometry (UHPLC-MS) was applied for metabolite profiling. ATR-FTIR provided an initial overview of the present metabolite classes. Phenylpropanoid, lipidic, and carbohydrate structures were revealed. The hydrophobic outer layer of pollen was characterized in detail by ASAP-MS profiling, and esters, phytosterols, and terpenoids were observed. Diacyl- and triacylglycerols and carbohydrate structures were identified in MALDI-MS spectra. The MALDI-MS imaging of lipids proved to be helpful during the microscopic characterization of pollen species in their mixture. Polyphenol profiling and the quantification of important secondary metabolites were performed by UHPLC-MS in context with pollen coloration and their antioxidant and antimicrobial properties. The obtained results revealed significant chemical differences among Magnoliophyta and Pinophyta pollen. Additionally, some variations within Magnoliophyta species were observed. The obtained metabolomics data were utilized for pollen differentiation at the taxonomic scale and provided valuable information in relation to pollen interactions during reproduction and its related applications. Full article
(This article belongs to the Special Issue Applied Analytical Chemistry: Second Edition)
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<p>ATR-FTIR spectra of conifer, monocot, and dicot representatives. (<b>A</b>)—Pine (<span class="html-italic">Pinus nigra</span>). (<b>B</b>)—Spruce (<span class="html-italic">Picea abies</span>). (<b>C</b>)—Tulip (<span class="html-italic">Tulipa x gesneriana</span>). (<b>D</b>)—King cup (<span class="html-italic">Caltha palustrir</span>).</p>
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<p>PCA score plot from ASAP-MS analysis in positive ionization mode of studied pollen species. (<b>A</b>)—All studied species. (<b>B</b>)—Magnoliophyta species.</p>
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<p>ASAP-MS spectra of conifer, monocot, and dicot representatives. (<b>A</b>)—Pine (<span class="html-italic">Pinus nigra</span>). (<b>B</b>)—Spruce (<span class="html-italic">Picea abies</span>). (<b>C</b>)—Tulip (<span class="html-italic">Tulipa x gesneriana</span>). (<b>D</b>)—King cup (<span class="html-italic">Caltha palustrir</span>). The intensity number in each panel is referred to as the most intense peak in the spectrum (100%). Identified signals are given in bold.</p>
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<p>Boxplots of normalized intensities of selected signals in studied pollen species measured by ASAP-MS. (<b>A</b>)—Dehydroabietic acid (<span class="html-italic">m</span>/<span class="html-italic">z</span> 301.2162). (<b>B</b>)—Ester of linolenic acid and methyloxooctadecanoate (<span class="html-italic">m</span>/<span class="html-italic">z</span> 575.5053). (<b>C</b>)—β-sitosterol (<span class="html-italic">m</span>/<span class="html-italic">z</span> 397.3810). (<b>D</b>)—Octadecatetraendiol (<span class="html-italic">m</span>/<span class="html-italic">z</span> 279.2334).</p>
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<p>LDI-MS spectra of conifer, monocot, and dicot representatives. (<b>A</b>)—Pine (<span class="html-italic">Pinus nigra</span>), (<b>B</b>)—Tulip (<span class="html-italic">Tulipa x gesneriana</span>), (<b>C</b>)—King cup (<span class="html-italic">Caltha palustrir</span>). The intensity number in each panel refers to the most intense peak in the spectrum (100%). Identified signals are given in bold.</p>
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<p>MALDI-MS imaging analysis of selected pollens attached to double-sided tape on the MALDI imaging plate. (<b>A</b>)—Photo of the studied pollen mixture. (<b>B</b>)—Dehydroabietol cinnamate (<span class="html-italic">m</span>/<span class="html-italic">z</span> 455.2228). (<b>C</b>)—Linolenoyl–linoleoyl–palmitoyl–glycerol (<span class="html-italic">m</span>/<span class="html-italic">z</span> 891.6803). (<b>D</b>)—Trilinolenoyl–glycerol (<span class="html-italic">m</span>/<span class="html-italic">z</span> 911.6513).</p>
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<p>Quantity of selected phenolic acids (<b>A</b>) and flavonoids (<b>B</b>) in all studied pollen species.</p>
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<p>Quantity of selected anthocyanins in studied pollens.</p>
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<p>UHPLC-MS analysis of pollen extracts. (<b>A</b>)—King cup (<span class="html-italic">Caltha palustrir</span>). (<b>B</b>)—Pine (<span class="html-italic">Pinus nigra</span>). (<b>C</b>)—Tulip (<span class="html-italic">Tulipa x gesneriana</span>). Chromatograms are reconstructed for <span class="html-italic">m</span>/<span class="html-italic">z</span> 301.0357 (which represents parent ion of quercetin or aglycone arising during fragmentation of its glycosylated forms). Retention time of peaks of following identified compounds are denoted in bold: quercetin (<span class="html-italic">m</span>/<span class="html-italic">z</span> 301.0357, Rt 8.10 min), quercetin dihexoside (<span class="html-italic">m</span>/<span class="html-italic">z</span> 625.1423, Rt 6.40 min), quercetin hexoside (<span class="html-italic">m</span>/<span class="html-italic">z</span> 463.0886, Rt 7.12 min), and its modified form (<span class="html-italic">m</span>/<span class="html-italic">z</span> 447.0967, Rt 7.92 min). Intensity is related to most intensive peak in chromatograms (100%). Identified signals are given in bold.</p>
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<p>Scheme of another collection and pollen isolation process.</p>
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<p>Scheme of taxonomical classification of studied pollen species. Magnoliophyta are currently divided into Liliopsida (monocots), Magnoliopsida (magnoliids), and Rosopsida (eudicots). The latter two involved former dicots.</p>
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<p>FTIR-ATR spectra of all studied pollen species. (<b>A</b>)—Wavenumbers 4000−2200 cm<sup>−1</sup>. (<b>B</b>)—Wavenumbers 2200–400 cm<sup>−1</sup>. The top green line represents pine pollen, and the bottom green line represents spruce pollen. The top purple line represents rose pollen, and the bottom purple line represents snowflake pollen. The top dark green line represents magnolia pollen, and the bottom dark green line represents beech pollen. The top dark purple line represents geranium pollen, and the bottom dark purple line represents scilla pollen.</p>
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<p>Peak area of cyanidin, cyanidin hexoside, and cyanidin dihexoside in different coloured tulip pollens.</p>
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<p>PCA score plot from UHPLC-MS analysis of studied pollen species in negative ionization mode.</p>
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<p>Application of capillary tube for direct pollen analysis using ASAP-MS technique. Arrow shows capillary modification and pollen insertion.</p>
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15 pages, 7435 KiB  
Article
Solvent Regulation in Layered Zn-MOFs for C2H2/CO2 and CO2/CH4 Separation
by Xingyao Zhao, Xiaotong Chang, Caixian Qin, Xiaokang Wang, Mingming Xu, Weidong Fan, Qingguo Meng and Daofeng Sun
Molecules 2025, 30(5), 1171; https://doi.org/10.3390/molecules30051171 - 5 Mar 2025
Abstract
The development of alternative adsorptive separation technologies is extremely significant for the separation of C2H2/CO2 and CO2/CH4 in the chemical industry. Emerging metal–organic frameworks (MOFs) have shown great potential as adsorbents for gas adsorption and [...] Read more.
The development of alternative adsorptive separation technologies is extremely significant for the separation of C2H2/CO2 and CO2/CH4 in the chemical industry. Emerging metal–organic frameworks (MOFs) have shown great potential as adsorbents for gas adsorption and separation. Herein, we synthesized two layered Zn-MOFs, UPC-96 and UPC-97, with 1,2,4,5-tetrakis(4-carboxyphenyl)-3,6-dimethylbenzene (TCPB-Me) as a ligand via the solvent regulation of the pH values. UPC-96 with a completely deprotonated ligand was obtained without the addition of acid, exhibiting two different channels with cross-sectional sizes of 11.6 × 7.1 and 8.3 × 5.2 Å2. In contrast, the addition of acid led to the partial deprotonation of the ligand and afforded UPC-97 two types of channels with cross-sectional sizes of 11.5 × 5.7 and 7.4 × 3.9 Å2. Reversible N2 adsorption isotherms at 77 K confirmed their permanent porosity, and the differentiated single-component C2H2, CO2, and CH4 adsorption isotherms indicated their potential in C2H2/CO2 and CO2/CH4 separation. Full article
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<p>Crystal structure of UPC-96: (<b>a</b>) Coordination mode of Zn<sup>2+</sup> and ligand; (<b>b</b>) Single layered framework with <span class="html-italic">sql</span> topology; (<b>c</b>) 2D layered unit with three layers; (<b>d</b>) 3D framework with two channels. Zn, sky-blue; C, gray; N, green; O, red; and H, pale.</p>
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<p>Crystal structure of UPC-97: (<b>a</b>) Coordination mode of Zn<sup>2+</sup> and ligand; (<b>b</b>) Infinite S-shaped chain; (<b>c</b>) Parallel layered unit of chains in opposite directions; (<b>d</b>) 3D framework with two channels. Zn, sky-blue; C, gray; N, green; O, red; and H, pale.</p>
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<p>PXRD patterns of (<b>a</b>) UPC-96 and (<b>b</b>) UPC-97.</p>
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<p>SEM images of (<b>a</b>) UPC-96 and (<b>b</b>) UPC-97.</p>
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<p>TGA curves of UPC-96 and UPC-97 (<b>a</b>) before and (<b>b</b>) after activation.</p>
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<p>FT-IR spectra of (<b>a</b>) UPC-96 and (<b>b</b>) UPC-97.</p>
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<p>(<b>a</b>) N<sub>2</sub> adsorption/desorption isotherms and (<b>b</b>) pore size distribution of UPC-96 and UPC-97.</p>
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<p>Single-component adsorption/desorption isotherms of C<sub>2</sub>H<sub>2</sub>, CO<sub>2</sub>, and CH<sub>4</sub>: UPC-96 at (<b>a</b>) 273 and (<b>b</b>) 298 K; UPC-97 at (<b>c</b>) 273 and (<b>d</b>) 298 K.</p>
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<p>Cycling adsorption/desorption isotherms at 298 K: UPC-96 for (<b>a</b>) C<sub>2</sub>H<sub>2</sub>, (<b>b</b>) CO<sub>2</sub>, and (<b>c</b>) CH<sub>4</sub>; UPC-97 for (<b>d</b>) C<sub>2</sub>H<sub>2</sub>, (<b>e</b>) CO<sub>2</sub>, and (<b>f</b>) CH<sub>4</sub>.</p>
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<p>Adsorption enthalpy of (<b>a</b>) UPC-96 and (<b>b</b>) UPC-97 for C<sub>2</sub>H<sub>2</sub>, CO<sub>2</sub>, and CH<sub>4</sub>.</p>
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<p>IAST selectivity of (<b>a</b>) UPC-96 and (<b>b</b>) UPC-97 for equimolar C<sub>2</sub>H<sub>2</sub>/CO<sub>2</sub> and CO<sub>2</sub>/CH<sub>4</sub> mixtures at 298 K.</p>
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<p><sup>1</sup>H NMR spectrum of TCPB-Me.</p>
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