Search Results (54)

Water vapor sorption in porous activated carbons (PACs) is governed by a complex interplay of pore architecture and surface functionality and often exhibits pronounced adsorption–desorption hysteresis. In this work, chestnut-shell-derived carbons were synthesized via a two-step thermal route—pyrolysis at 550 °C for 120 min followed by KOH activation at either 600 °C or 800 °C for 240 min—and evaluated using a dynamic vapor sorption analyzer to quantify water uptake, hysteresis, and temperature-dependent energetics. Both materials exhibit sigmoidal Type V isotherms, characteristic of cooperative water clustering on hydrophobic carbon surfaces with localized polar sites. At 25 °C, The PAC sample prepared at 800 °C shows a sharper uptake transition and higher total capacity (~0.45 g/g at 90% RH), compared to the broader, more gradual isotherm of the 600 °C sample (~0.17 g/g). Temperature-dependent isotherms collected between 25 °C and 45 °C were fit using the Dubinin–Serpinsky (DS-4) model, yielding good agreement (R² ≈ 0.997) and enabling mechanistic interpretation of primary site adsorption and cooperative cluster growth. Clausius–Clapeyron analysis of ln P versus 1/T at fixed loadings yielded isosteric heats of adsorption (ΔH) decreasing from approximately 45.4 kJ mol⁻¹ at low uptake (0.02 g g⁻¹) to ~43.8 kJ mol⁻¹ at intermediate loading, followed by a slight increase to ~44.2 kJ mol⁻¹ at higher coverage (0.35 g g⁻¹). This trend reflects the transition from strong adsorption at high-energy surface sites to cooperative water clustering and confinement effects within the pore network. These findings highlight the role of activation temperature in modulating sorption mechanisms and energetics, offering practical guidance for tuning biomass-derived carbons for atmospheric water harvesting applications. Full article

This paper presents a new study and analysis of the thermo-hygroscopic behavior of Arthrospira platensis using dynamic vapor sorption (DVS) system. Thermo-hygroscopic characterization is essential for optimizing the drying process and enhancing storage conditions. Therefore, the objective of this work was to investigate the thermo-hygroscopic properties of Arthrospira (Spirulina) platensis using a dynamic vapor sorption (DVS) system. This thermo-hygroscopic analysis focused on three fundamental parameters, namely: the desorption isotherms, the net isosteric heat of water desorption, and the moisture diffusivity. Desorption isotherms were measured at five different temperatures (25 °C, 40 °C, 50 °C, 60 °C and 80 °C) over a relative humidity range of 10–80%. The desorption isotherm data were fitted to five semi-empirical models: GAB, Oswin, Smith, Henderson, and Peleg. The results indicated that the GAB model provided the best fit for the experimental data. The net isosteric heat of desorption was determined using the Clausius–Clapeyron relation. It decreased from 21.3 to 4.29 KJ/mol as the equilibrium moisture content increased from 0.02 to 0.1 Kg/Kg (dry basis). Additionally, the moisture diffusivity of Arthrospira platensis was estimated based on Fick’s second law of diffusion and the desorption kinetics obtained from the DVS equipment. This parameter varied between 1.04 10⁻⁸ m²/s and 1.46 10⁻⁷ m²/s for average moisture contents ranging from 0.003 Kg/Kg to 0.191 Kg/Kg (dry basis). Furthermore, the activation energy for desorption was estimated to be approximately 33.7 KJ/mol. Full article

Objectives: Drug-drug cocrystals with improved properties can be used to facilitate the development of synergistic therapeutic combinations. The goal of the present study is to obtain novel drug-drug cocrystals involving two anti-glioma agents, temozolomide (TMZ) and myricetin (MYR). Methods: The novel TMZ-MYR cocrystal was prepared via slurry and solvent evaporation techniques and characterized by X-ray diffraction, thermal analysis, infrared spectroscopy, and dynamic vapor sorption measurements. The stability, compaction, and dissolution properties were also evaluated. Results: Crystal structure analysis revealed that the cocrystal lattice contains two TMZ molecules, one MYR molecule, and four water molecules, which are linked by hydrogen bonding interactions to produce a three-dimensional network. The cocrystal hydrate exhibited favorable stability and tabletability compared to pure TMZ. A dissolution study showed that the maximum solubility of MYR in the cocrystal (176.4 μg/mL) was approximately 6.6 times higher than that of pure MYR·H₂O (26.9 μg/mL), while the solubility of TMZ from the cocrystal (786.7 µg/mL) was remarkably lower than that of pure TMZ (7519.8 µg/mL). The solubility difference between MYR and TMZ was diminished from ~280-fold to ~4.5-fold. Conclusions: Overall, the TMZ-MYR cocrystal optimizes the stability and tabletability of TMZ and the dissolution behavior of both drugs, offering a promising approach for synergistic anti-glioma therapy with improved clinical potential. Full article

Brine purification is an important process unit in chlor-alkali industrial plants for the production of sodium hydroxide, chlorine, and hydrogen. The membrane cell process requires ultrapure brine, which is obtained through mechanical filtration, chemical precipitation and fine polishing, and ion exchange using polymer resins. Temperature variations can lead to the degradation of the exchange properties of these resins, primarily causing a decrease in their exchange capacity, which negatively impacts the efficiency of the brine purification. After multiple ion exchange regeneration cycles, significant quantities of spent resins may be generated. These must be managed in accordance with resource efficiency and hazardous waste management to ensure the sustainability of the industrial process. In this paper, a comparative study is conducted to characterize the long-term stability of a new commercial chelating resin used in the industrial electrolysis process. The spectroscopic methods of physicochemical characterization included: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) and attenuated total reflectance–Fourier transform infrared spectroscopy (ATR-FTIR). The thermal behavior of the polymer resins was evaluated using the following thermogravimetric methods: thermogravimetry (TG), derivative thermogravimetry (DTG), and differential thermal analysis (DTA), while the moisture behavior was studied using dynamic vapor sorption (DVS) analysis. To assess the energy potential, the polymer resins were analyzed to determine their calorific value and overall energy content. Full article

This study investigates the coupled hygrothermal behavior of mycelium-based composites (MBCs) as a function of their microstructural organization, governed by fungal species, substrate type, additive incorporation, and treatment method. Eleven composite formulations were selected and characterized using a multi-scale experimental approach, combining scanning electron microscopy, dynamic vapor sorption, vapor permeability tests, capillary uptake measurements, and transient thermal conductivity analysis. SEM analysis revealed that Ganoderma lucidum forms dense and interconnected hyphal networks, whereas Trametes versicolor generates looser, localized structures. These morphological differences directly influence water vapor transport and heat conduction. Additive-enriched composites exhibited up to 21.8% higher moisture uptake at 90% RH, while straw-based composites demonstrated higher capillary uptake and free water saturation (up to 704 kg/m³), indicating enhanced moisture sensitivity. In contrast, hemp-based formulations with Ganoderma lucidum showed reduced sorption and vapor permeability due to limited pore interconnectivity. Thermal conductivity varied nonlinearly with temperature and moisture content. Fitting the experimental data with an exponential model revealed a moisture sensitivity coefficient thirty times lower for GHOP compared to VHOP, highlighting the stabilizing effect of a compact microstructure. The distinction between total and effective porosity emerged as a key factor in explaining discrepancies between apparent and functional moisture behavior. These findings demonstrate that hygric and thermal properties in MBCs are governed not by porosity alone, but by the geometry and connectivity of the internal fungal network. Optimizing these structural features enables fine control overheat and mass transfer, laying the groundwork for the development of high-performance, bio-based insulation materials. Full article

Polymeric scaffolds are promising in tissue engineering due to their structural similarity to extracellular matrix components. This study aimed to design freeze-dried hydrogels based on chitosan (CHT) and hyaluronic acid (HA). Chitosan-based gels were crosslinked with oxidized maltodextrin (MDo) before the freeze-drying step, resulting in spongy porous scaffolds. Based on the state-of-the-art, our hypothesis was that crosslinking would increase scaffold stiffness and delay the degradation of the CHT:HA resorbable scaffolds swelled in a hydrated physiological environment. The physicochemical and mechanical properties of crosslinked CHT- and CHT:HA-based scaffolds were analyzed. Hygroscopic and swelling behavior were assessed using dynamic vapor sorption analysis and batch studies. Degradation was evaluated under different conditions, including in phosphate-buffered saline (PBS), PBS with lysozyme, and lactic acid solutions, to investigate scaffold resistance against enzymatic and acidic degradation. The porosity of the spongy materials was characterized using scanning electron microscopy, while dynamic mechanical analysis provided information on the mechanical properties. Crosslinked scaffolds showed reduced swelling, slower degradation rates, and increased stiffness, confirming MDo as an effective crosslinking agent. Scaffolds loaded with ciprofloxacin (CFX) demonstrated their ability to deliver therapeutic agents, as the CFX loading capacity was promoted by CHT–CFX interactions. Microbiologic investigation confirmed the results. Finally, cytotoxicity tests displayed no toxicity. In conclusion, MDo-crosslinked CHT and CHT:HA scaffolds exhibit enhanced stability, functionality, and mechanical performance, making them promising for cartilage tissue engineering. Full article

Concrete porosity is one of the fundamental properties for the structural characterization of cementitious materials. This study compares porosity data obtained with dynamic water vapor sorption (DWVS) with the more commonly used mercury intrusion porosimetry (MIP) method for a wide range of concrete samples made with basaltic aggregates, typical of the Canary Islands, which are porous. The objective was to propose an alternative method for routine concrete monitoring that avoids the use of a hazardous substance such as mercury. The results reveal fundamental differences between the MIP and water-accessible porosimetry (WAP) data, although a correlation between the methods was revealed where MIP = 1.18 × WAP. The study was completed by an analysis of the relationships between the porosity and the characteristics and properties of concrete (water/cement ratio and strength), as well as the calculation of the tortuosity factor and a frost durability factor. Full article

Atmospheric water harvesting (AWH) is a promising alternative to address immediate water needs. Desiccant-based AWH could compete effectively with other commercially available AWH technologies. One of the primary challenges facing desiccant-based AWH is the energy required to desorb the captured water vapor from the desiccant. This work presents a multi-faceted approach targeted explicitly at low-humidity and arid regions, aiming to overcome the limitations of the refrigerant-based AWH system. It includes assessing common desiccants (zeolite, activated alumina, and silica gel) and their forms (beads, powdered, or coated on a substrate). A bench-scale test rig was designed to evaluate different types and forms of desiccants for adsorption and desorption cycles and overall adsorption capacity (g/g), kinetic profiles, and rates. Experimental results indicate that beaded desiccants possess the highest adsorption capacity compared to powdered or coated forms. Furthermore, coated desiccants double the water uptake (1.12 vs. 0.56 g water/g desiccant) and improve adsorption/desorption cycling by 52% compared to beaded forms under the same conditions. Additionally, Brunauer–Emmett–Teller (BET), X-ray diffraction (XRD), and dynamic vapor sorption (DVS) analysis show the pore geometry, morphology, and sorption capacity. The goal is to integrate these performance improvements and propose a more effective, energy-efficient desiccant-based AWH system. Full article

Irbesartan (IRB) is a commonly used BCS Class II antihypertensive drug requiring dissolving capacity enhancement to address oral bioavailability limitations. In this work, seven new IRB salts were successfully synthesized, including one carboxylate (IRB-MAL) and six sulfonate salts (IRB-TOSA, IRB-BSA, IRB-4-CBSA, IRB-2, 5-CBSA, IRB-MSA, and IRB-CPSA). Their vitro dissolution, intrinsic dissolution rates (IDRs), thermal/hygroscopic stability (via thermal analysis, dynamic vapor sorption, and accelerated stability tests), and phase transition process (monitored by in situ Raman spectroscopy) were evaluated. The results revealed that IRB-TOSA, IRB-MAL, IRB-BSA, IRB-4-CBSA, and IRB-MSA salts exhibited IDRs of 0.3194–0.7383 mg/(cm²·min), all significantly higher than IRB, with dissolution concentrations increased by 14.9–113.6%. IRB-TOSA and IRB-4-CBSA salts demonstrated excellent hydrothermal stability. Single crystal structure analysis confirmed proton transfer from coformers’ sulfonic/carboxylic acids (deprotonation site, H-out) to IRB’s diazaheterocycles (protonation site, H-in) in IRB salts. Six sulfonate salts exhibited N_H-in–H···O_H-out and N_non-H-in–H···O_H-out hydrogen bonds, with the former absent in IRB-MAL. Furthermore, supramolecular synthon studies revealed distinct hydrogen-bonding patterns (e.g., bifurcated bonds in 2,5-CBSA and CPSA salts) that correlate with moisture resistance. Quantitative analysis of IRB salts suggested hydrogen bond strengths may influence their melting points (decomposition temperatures). This study demonstrates that IRB salts hold promise for advanced pharmaceutical applications. Full article

Adsorption chillers are distinguished by their low electricity consumption, lack of moving parts and exceptional reliability. However, their considerable weight, due to the low sorption capacity of conventional adsorbents, remains a key limitation. This study investigates the effect of introducing thermally conductive additives—aluminium powder, copper powder and graphite flakes—at 5, 15 and 25 wt.% to silica-gel-based adsorbent beds on the enhancement of heat transfer. In contrast to other works, this study also includes a novel analysis of the thermal properties of dry sorbents, since the moisture content affects the thermal conductivity. Additives improve the thermal conductivity, as measured by the laser flash method (LFA), of the bed by up to 20.7% while maintaining a reasonable sorption capacity, as measured by the dynamic vapor sorption (DVS). Additions of copper at 5–15 wt.% and graphite flakes at 15–25 wt.% provide an optimal compromise between thermal conductivity and sorption capacity. Aluminium powder, on the other hand, offers flexibility over a wider range (5–25 wt.%). The increased thermal conductivity of these modified materials is expected to lead to more efficient heat transport, which suggests the hypothesis that it could reduce the cycle time and increase the efficiency of adsorption chillers. Full article

The morphology of wheat starch granules with different damaged starch (DS) content was analyzed using a particle size analyzer and scanning electron microscopy (SEM); the granular structure was studied using FT-IR spectroscopy and X-ray diffraction (XRD); and the granule–water interaction was evaluated by thermogravimetric analysis (TGA) and dynamic vapor sorption (DVS). The increase in the level of DS shifted the population of B-type granules towards larger particle diameters and shifted the population of A-type granules towards smaller particle diameters. The appearance of the surface of the starch-damaged granules was rough and flaky (SEM images). Crystallinity reductions were related to higher mechanical damage levels of the granular structure (FT-IR and XRD). Higher DS increased the liquid-water absorption capacity of the granules. Higher DS was associated with increments in less-bound water proportions and reductions in more strongly bound water proportions and related to reductions in the evaporation temperature of these water populations (TGA analyses). Concerning DVS data, the results suggested that the driving force for water–monolayer attachment to the starch granules decreased as DS increased. Therefore, it was suggested that the changes in granule structure led to a weaker water–starch polymer chain interactions due to the increase in DS. The results contribute to a better understanding of the influence of mechanical damage on the starch granular structure, which could be related to the rheological and thermal behavior of starch-based systems with different DS. Full article

This study investigates the use of Brewers’ Spent Grains (BSGs) as a sustainable biocomposite building materials, using cornstarch as a biopolymer binder. BSG aggregates are compared with hemp shives, a conventional aggregate known for its thermal properties. Starch is employed as a natural binder in three different formulations to further reduce the carbon footprint of the building material. Considering aggregates, the first formulation contains only BSGs, the second consists of half BSGs and half hemp shives, and the third uses only hemp shives. In addition, morphological analysis using Scanning Electron Microscopy (SEM) is conducted to examine the microstructure and porosity of the raw BSG and hemp shives. Hygrothermal properties are measured using Heat Flow Meter (HFM) and Dynamic Vapor Sorption (DVS) techniques, while mechanical properties are also assessed. Results indicate that the thermal conductivity of the BSG formulation (0.131 W/(m·K)) is double that of the hemp shives formulation (0.067 W/(m·K)), whereas the mixed BSG/hemp shives formulation exhibits a thermal conductivity of 0.106 W/(m·K). However, DVS measurements reveal better hygrothermal properties for the BSG formulation compared to the hemp shives formulation. Lastly, mechanical properties are found to be nearly equivalent across the three formulations. These findings suggest that BSG waste has potential as a viable material for use in construction. Further work on formulation optimization and durability is necessary to fully realize the potential of this waste in promoting a circular economy within the building materials industry. Full article

Metal–organic frameworks (MOFs) are hybrid inorganic–organic 3D coordination polymers with metal sites and organic linkers, which are a “hot” topic in the research of sorption, separations, catalysis, sensing, and environmental remediation. In this study, we explore the molecular mechanism and kinetics of interaction of the new copper porphyrin aluminum metal–organic framework (actAl-MOF-TCPPCu) compound 4 with a vapor of the volatile organic sulfur compound (VOSC) diethyl sulfide (DES). First, compound 4 was synthesized by post-synthetic modification (PSM) of Al-MOF-TCPPH₂ compound 2 by inserting Cu²⁺ ions into the porphyrin ring and characterized by complementary qualitative and quantitative chemical, structural, and spectroscopic analysis. Second, the interaction of compound 4 with DES vapor was analyzed dynamically by the novel method of in situ time-dependent attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy at controlled humidity levels. The sorbent–adsorbate interactions, as analyzed by the shifts in IR peaks, indicate that the bonding includes the hydroxy O-H, carboxylate COO⁻, and phenyl groups. The kinetics of sorption obeys the Langmuir pseudo-first-order rate law. The pre-adsorption of water vapor by compound 4 at the controlled relative humidity under static (equilibrium) conditions yields the binary stoichiometric adsorption complex (Al-MOF-TCPPCu)_1.0(H₂O)_8.0. The pre-adsorption of water vapor makes the subsequent sorption of DES slower, while the kinetics obey the same rate law. Then, static pre-adsorption of water vapor was followed by static sorption of DES vapor, and the ternary adsorption complex (Al-MOF-TCPPCu)_1.0(H₂O)_8.0(DES)₃.₈ was obtained. Despite the pre-adsorption of significant amounts of water, the binary complex adsorbs a large amount of DES: ca. 36.6 wt. % (per compound 4). Finally, the ternary complex is facilely regenerated by gentle heating under vacuum. Compound 4 and related MOFs are promising for adsorptive removal of vapor of DES and related VOSCs from dry and humid air. Full article

Dehydration is the principal conservation process for waterlogged archaeological wood (WAW), with the aim of preventing shrinkage and cracking. For well-preserved WAW, shrinkage mainly takes place when the moisture content is below the fiber saturation point. Here, we conduct a new trial using ionic liquid as a dimensional stabilizer to maintain a stable swollen state of WAW. Molecular dynamics simulation (MD), shrinkage measurement, Fourier transform infrared spectroscopy (FTIR), and dynamic vapor sorption (DVS) were adopted to investigate the interactions and effects of 1-Butyl-3-methylimidazolium chloride ([Bmim][Cl]) on WAW (Dipterocarpaceae Dipterocarpus sp. with a maximum moisture content of 80.3%) in comparison with the conventional material polyethylene glycol (PEG). The results show that [Bmim][Cl] and its water mixtures have a comparable or slightly greater ability to swell amorphous cellulose than does water at room temperature, while crystalline cellulose is left intact. The samples treated with [Bmim][Cl] show less shrinkage than the PEG 300- and PEG 2000-treated samples at all tested concentrations after air-drying. The best dimension control was achieved by 40 wt% [Bmim][Cl], with volumetric shrinkage reduced from 5.03% to 0.47%. DVS analysis reveals that [Bmim][Cl] reduces moisture contents at moderate and low relative humidity (<80%) when the concentration is at or below 20 wt%, which suggests that good dimensional stability was not achieved by simply preserving the moisture content but possibly through the interaction of the ionic liquid with the wood polymers. Full article

Palm leaf manuscripts are a valuable part of world cultural heritage. Studying the mechanical properties of palm leaf manuscripts and their changes due to environmental influences is of great significance for understanding the material characteristics, aging mechanisms, and preventive conservation of these manuscripts. This study used dynamic vapor sorption (DVS) and a thermomechanical analyzer (TMA) to investigate the changes to the mechanical properties of palm leaf manuscripts in response to different relative humidity conditions and different time periods. The short-term study results show that exposure to varying relative humidities leads to changes in the equilibrium moisture content (EMC) of palm leaf manuscripts, causing the bending strength of the samples to decrease significantly with increasing humidity. The bending modulus initially increases and then decreases as the humidity increases. Moreover, the greater the desorption hysteresis of the samples, the more pronounced the changes to the mechanical properties. Therefore, a stable environment in terms of humidity can prevent changes in the mechanical properties of palm leaf manuscripts, thereby preventing the onset of degradation. The results of the long-term aging studies indicate that prolonged exposure to either very dry or very humid conditions greatly affects the mechanical properties of palm leaf manuscripts, which is detrimental to their preservation. The samples kept at 50% RH did not exhibit significant signs of deterioration, with no notable changes in their mechanical properties or chemical structure. This suggests that 50% RH is a relatively optimal humidity condition for the preservation of palm leaf manuscripts. Full article