Search Results (1,150)

A metal-ion-free method was developed to prepare κ-carrageenan/cellulose hydrogel beads for efficient cationic dye removal. The beads were fabricated using a mixture of 1-ethyl-3-methylimidazolium acetate and N,N-dimethylformamide as the solvent system, followed by aqueous ethanol-induced phase separation. This process eliminated the need for metal-ion crosslinkers, which typically neutralize anionic sulfate groups in κ-carrageenan, thereby preserving a high density of accessible binding sites. The resulting beads formed robust interpenetrating polymer networks. The initial swelling ratio reached up to 28.3 g/g, and even after drying, the adsorption capacity remained over 50% of the original. The maximum adsorption capacity for crystal violet was 241 mg/g, increasing proportionally with κ-carrageenan content due to the higher surface concentration of anionic sulfate groups. Kinetic and isotherm analyses revealed pseudo-second-order and Langmuir-type monolayer adsorption, respectively, while thermodynamic parameters indicated that the process was spontaneous and exothermic. The beads retained structural integrity and adsorption performance across pH 3–9 and maintained over 90% of their capacity after five reuse cycles. These findings demonstrate that κ-carrageenan/cellulose hydrogel beads prepared via a metal-ion-free strategy offer a sustainable and effective platform for cationic dye removal from wastewater, with potential for heavy metal ion adsorption. Full article

A thermochromic cholesteric liquid crystal (CLC) mixture was prepared using epoxies. The structural color of the CLCN film was tuned by changing the concentration of a chiral dopant and the polymerization temperature. It was found the yellow CLCN film can be used as a sensor for the discrimination of methanol and ethanol which was proposed to be driven by the difference between the solubility parameters. Moreover, a colorful pattern was prepared based on the thermochromic property of the CLC mixture, which could be applied for decoration and as a sensor for chloroform. Full article

Four novel crystalline architectures based on benzo[c]cinnolininium trifluoromethanesulonate salts, [C₁₂H₉N₂]⁺[CF₃SO₃]⁻, have been isolated as single-crystals, and their structures have been determined by X-ray diffraction analysis. The formation of the new salts results from reactions involving the dimeric hydroxo di-n-butylstannane trifluoromethanesulfonato complex [n-Bu₂Sn(OH)(H₂O)(CF₃SO₃)]₂ (1) and benzo[c]cinnoline (C₁₂H₈N₂, BCC). Organic salts I, II, III, and IV were crystallized through slow evaporation at room temperature from a mixture of toluene/dichloromethane. The cystallographic structures of I, II, and IV exhibit the presence of monoprotonated benzo[c]cinnolinium cations in interactions with a free benzo[c]cinnoline molecule through N–H···N hydrogen bonding, while for salt III, the monoprotonated cation directly interacts with the CF₃SO₃⁻ anion via an N–H···O interaction. For all four salts, aromatic π-π interactions involving rings of various components (free benzo[c]cinnoline molecule, benzo[c]cinnolinium cation, toluene molecule), combined with weak C–H···O and C–H···F interactions implying the trifluoromethanesulfonate anion, promote the solid-state self-assembly of supramolecular stacks. In parallel to the formation of benzo[c]cinnolinium based-salts, organotin(IV) 1 was converted into a distannoxane compound, ²_∞{[n-Bu₂(μ-OH)SnOSn(μ-η²-O₃SCF₃)n-Bu₂]₂[n-Bu₂(η¹-O₃SCF₃)SnOSn(μ-OH)n-Bu₂]₂} (3), which was also isolated as a single crystal and whose crystallographic structure was previously established by us. Full article

The effect of severe plastic deformation during milling and conventional and Spark Plasma Sintering (SPS) on the wt. % microstructural, structural, thermal, magnetic, and mechanical properties of the Al–16 wt. % Mn–7 wt. % Cu alloy was studied. A milling process for up to 24 h (A24) leads to microstructure refinement and the presence of Al, Mn, and Cu solid solutions. The energy dispersive spectroscopy (EDS) analysis reveals the existence of Cu–Al, Mn–Al, and Al–Mn enriched particles. The powders exhibit weak ferromagnetism and an exchange bias (EB) behaviour that decreases with increasing milling time. The Ms values fitted using the law of approach to saturation (LAS) are comparable to the experimental values. The exothermic and endothermic peaks that appear in the differential scanning calorimetry (DSC) scans in the 500–900 °C range on heating/cooling are related to different phase transformations. The crystal structure of the A24 powders heated up to 900 °C (A24_900 °C) consists of a dual-phase microstructure of Al₂₀Cu₂Mn₃ nanoprecipitates (~28%) and Al matrix (~72%). The sintering of the A24 powders at 500 °C for one hour (A24S) leads to the precipitation of Al₆Mn, Al₂Cu, and the Al₂₀Cu₂Mn₃ T-phase into the Al-enriched matrix. In contrast, the consolidation by SPS (A24SPS) leads to a mixture of an Al solid solution, Al₆Mn, T-phase, and α-Mn with an increased weight fraction of the T-phase and Al₆Mn. The sintered samples exhibit the coexistence of a significant PM/AFM contribution to the M-H curves, with increasing Hc and decreasing EB. A higher microhardness value of about 581 HV is achieved for the A24SPS sample compared to those of the A24 (68 HV) and A24S (80 HV) samples. Full article

Rare earth elements (REEs) have garnered significant global attention due to their essential role in advanced technologies. Sri Lanka is endowed with various REE-bearing minerals, including the apatite-rich deposit in the Eppawala area, commonly known as Eppawala rock phosphate (ERP). However, direct extraction of REEs from ERP is technically challenging and economically unfeasible. This study introduces a novel, integrated approach for recovering REEs from ERP as a by-product of nitrophosphate fertilizer production. The process involves nitric acid-based acidolysis of apatite, optimized at 10 M nitric acid for 2 h at 70 °C with a pulp density of 2.4 mL/g. During cooling crystallization, 42 wt% of calcium was removed as Ca(NO₃)₂.4H₂O while REEs remained in the solution. REEs were then selectively precipitated as REE phosphates via pH-controlled addition of ammonium hydroxide, minimizing the co-precipitation with calcium. Further separation was achieved through selective dissolution in a sulfuric–phosphoric acid mixture, followed by precipitation as sodium rare earth double sulfates. The process achieved over 90% total REE recovery with extraction efficiencies in the order of Pr > Nd > Ce > Gd > Sm > Y > Dy. Samples were characterized for their phase composition, elemental content, and morphology. The fertilizer results confirmed the successful production of a nutrient-rich nitrophosphate (NP) with 18.2% nitrogen and 13.9% phosphorus (as P₂O₅) with a low moisture content (0.6%) and minimal free acid (0.1%), indicating strong agronomic value and storage stability. This study represents one of the pioneering efforts to valorize Sri Lanka’s apatite through a novel, dual-purpose, and circular approach, recovering REEs while simultaneously producing high-quality fertilizer. Full article

The aim of this study was to evaluate the effect of the iota, kappa and lambda carrageenan fractions on the physical properties and crystal structure of a fruit sorbet prepared from frozen mango fruits. During this study, physical properties such as density, cryoscopic temperature, osmotic pressure, overrun and melting time were analyzed. In order to assess the crystal structure and its changes, microscope images were taken of each sample after 1, 30 and 90 days of storage. The stabilizers showed no significant effect on the physical properties of the ice cream mixture; however, the sample with iota carrageenan stood out for having the highest overrun (58.7%) and the sample with kappa carrageenan took the longest to melt of all tested samples (almost 21 min). This study shows a significant effect of carrageenans in reducing the initial size of ice crystals as well as reducing recrystallization during storage. The stabilizing blend using ι-carrageenan provided the most effective cryoprotective properties, with an ice crystal diameter of 9 µm. Full article

Ultrafine fibers from poly(3-hydroxybutyrate) (PHB) and polyvinylpyrrolidone (PVP) and their blends with different component ratios in the range of 0/100 to 100/0 wt.% were obtained, and their structure and dynamic properties were studied. The polymers were obtained via electrospinning in solution mode. The structure, morphology, and segmental dynamic behavior of the fibers were determined using optical microscopy, SEM, EPR, DSC, and IR spectroscopy. The low-temperature maximum on the DSC endotherms provided information on the state of the PVP hydrogen bond network, which made it possible to determine the enthalpies of thermal destruction of these bonds. The PHB/PVP fiber blend ratio significantly affected the structural and dynamic parameters of the system. Thus, at low concentrations of PVP (up to 9%) in the structure of ultra-fine fibers, the distribution of this polymer occurs in the form of tiny particles, which are crystallization centers, which causes a significant increase in the degree of crystallinity (χ) activation energy (E_act) and slowing down of molecular dynamics (τ). At higher concentrations of PVP, loose interphase layers were formed in the system, which caused a decrease in these parameters. The strongest changes in the concentration of hydrogen bonds occurred when PVP was added to the composition from 17 to 50%, which was due to the formation of intermolecular hydrogen bonds both in PVP and during the interaction of PVP and PHB. The diffusion coefficient of water vapor in the studied systems (D) decreased as the concentration of glassy PVP in the composition increased. The concentration of the radical decreased with an increase in the proportion of PVP, which can be explained by the glassy state of this polymer at room temperature. A characteristic point of the 50/50% mixture component ratio was found in the region where an inversion transition of PHB from a dispersion material to a dispersed medium was assumed. The conducted studies made it possible for the first time to conduct a comprehensive analysis of the effect of the component ratio on the structural and dynamic characteristics of the PHB/PVP fibrous material at the molecular scale. Full article

This study reports the discovery and structural characterization of a novel polymorph, designated as Form III, of Alclometasone dipropionate, a corticosteroid commonly used in the treatment of inflammatory dermatoses. Form III was obtained by modifying the crystallization conditions reported in prior art and was thoroughly characterized using Powder X-ray Diffraction (PXRD), Fourier Transform Infrared (FT-IR) spectroscopy, melting-point determination, Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), including its first derivative (DTG), optical microscopy, and Scanning Electron Microscopy (SEM). In parallel, pure Form II, previously observed only in mixtures with Form I, was successfully isolated and characterized using the same analytical techniques. Both forms were compared in terms of structural, thermal, and morphological properties. PXRD analysis revealed that Form III crystallizes in a triclinic system; FT-IR spectroscopy revealed unique vibrational signatures, and microscopy showed rod-like crystal morphology. The discovery of Form III expands the current understanding of the solid-state landscape of Alclometasone dipropionate and opens opportunities for the identification of new industrial purification methods for the compound. Full article

Mining activities generate large volumes of tailings with significant environmental impact but also the potential for sustainable reuse in construction materials. This study evaluates the production of ceramic aggregates from mixtures of clay, sand, and iron ore waste subjected to thermal treatment at temperatures ranging from 600 to 1100 °C. The influence of calcination temperature on mineralogical transformations and mechanical integrity was investigated using X-ray diffraction (XRD) and the $\alpha$-Treton parameter, derived from standardized impact resistance testing. The results indicate that the formation of metakaolinite between 700 and 900 °C enhances mechanical resistance, while higher temperatures (>900 °C) lead to structural degradation, followed by partial recovery due to mullite crystallization. The $\alpha$-Treton curve exhibited clear correlation with the phase changes identified by XRD, demonstrating its applicability as a low-cost, sensitive proxy for optimizing thermal activation. A simplified methodology is proposed to optimize the thermal activation of such materials by correlating firing temperature with mineralogical evolution and mechanical integrity, contributing to the development of sustainable ceramic aggregates for pavement applications. Full article

Ethyl cellulose (EC) and its derivatives are known to exhibit the cholesteric liquid crystal (CLC) phase with visible light reflection in a lyotropic manner after adding appropriate solvents. Generally, the reflection peak of conventional CLCs is easily wavelength shifted by temperature. However, our previous study showed that the reflection wavelength can be maintained even after heating for the lyotropic CLCs of completely pentyl-etherified EC derivatives with methacrylic acid (MAA). However, the emergence of thermally stable reflection colors still remains obscure in the mechanism at the mesoscopic scale. In this study, we evaluated the temperature dependence of the reflection wavelength for the lyotropic CLCs of a series of completely etherified EC derivatives possessing different alkoxy chains by addition of MAA. It was found that butyl- or pentyl-etherified EC derivatives are suitable for preparation of the lyotropic CLCs with visible Bragg reflection, whereas visible light reflection cannot be observed for the other mixtures of propyl- and hexyl-etherified EC derivatives with MAA. Furthermore, it turned out that lyotropic CLCs of pentyl-etherified EC derivatives with MAA show the smallest temperature dependence of their reflection wavelength. Based on the results of ultra-small-angle X-ray scattering (USAXS) and small-angle X-ray scattering (SAXS) measurements of CLC films, we presumed that the emergence of thermally stable reflection colors from the lyotropic CLCs of pentyl-etherified EC derivatives with MAA arises from their phase separation at the mesoscopic scale by changing the temperature. Full article

Microorganisms take an active part in the processes of microbiologically influenced corrosion, which is protected against by using bactericides—often toxic compounds—with inhibitory properties. There are many studies of eco-friendly “green” biocides/inhibitors, in particular those based on microbial metabolites. Indicators for the processes of microbial corrosion of steel 3 induced by the sulfate-reducing bacteria Desulfovibrio oryzae NUChC SRB2 under the influence of the strains Bacillus velezensis NUChC C2b and Streptomyces gardneri ChNPU F3 have not been investigated, which was the aim of this study. The agar well diffusion method (to determine the antibacterial properties of the supernatants) was used, along with the crystal violet (to determine the biomass of the biofilm on the steel) and gravimetric methods (to determine the corrosion rate). A moderate adhesiveness to steel 3 was established for D. oryzae due to its biofilm-forming ability. The presence of a supernatant on cultures of S. gardneri, B. velezensis and their mixture (2:1) did not reduce the biofilm-forming properties of D. oryzae. Compared to the control, a decrease in the corrosion rate was recorded for the variant of the mixture of the studied bacterial culture supernatants. This indicates the potential of this mixture for use in corrosion protection in environments with sulfate-reducing bacteria, which requires further research. Full article

The intermediate compound 4′-phenyl-1′,4′-dihydro-2,2′:6′,2″-terpyridine (pdhtpy) was isolated for the first time during the synthesis of 4′-phenyl-2,2′:6′,2″-terpyridine (ptpy) and characterised by single-crystal X-ray diffraction. Pdhtpy crystallises in the triclinic crystal system with space group P$\bar{1}$ with the following unit cell parameters at 100 K: a = 6.1325(4) Å; b = 8.2667(5) Å; c = 16.052(2) Å; α = 86.829(2)°; β = 82.507(2)°; γ = 84.603(2)°; V = 802.49(9) ų. The absence of stabilising electron-withdrawing groups renders pdhtpy prone to oxidative conditions. Pdhtpy was obtained as a mixture with ptpy, confirmed by Rietveld refinement of the powder X-ray diffraction pattern. Notably, pdhtpy is the first solid-state 1,4-dihydropyridine lacking electron-withdrawing groups at both positions 3 and 5, distinguishing it from Hantzsch esters and related compounds. Full article

Y₅F₃[AsO₃]₄ crystallizes needle-shaped in the tetragonal space group P4/ncc with the lattice parameters a = 1143.80(8) pm, c = 1078.41(7) pm and c/a = 0.9428 for Z = 4. The yttrium-fluoride substructure linked via secondary contacts forms a three-dimensional network $\begin{array}{c}3\\ \infty \end{array}${[Y₅F₃]¹²⁺} and the remaining part consists of ψ¹-tetrahedral [AsO₃]³⁻ units, which leave lone-pair channels along [001]. In contrast, platelet-shaped Y₅Cl₃[AsO₃]₄ crystals adopt the monoclinic space group C2/c with the lattice parameters a = 1860.56(9) pm, b = 536.27(3) pm, c = 1639.04(8) pm and β = 105.739(3)° for Z = 4. Condensation of [(Y1,2)O₈]¹³⁻ polyhedra via four common edges each leads to fluorite-like $\begin{array}{c}2\\ \infty \end{array}$ {[(Y1,2)O $\begin{array}{c}e\\ 8/2\end{array}$ ]⁵⁻} layers spreading out parallel to the (100) plane. Their three-dimensional linkage occurs via the (Y3)³⁺ cations with their Cl⁻ ligands on the one hand and the As³⁺ cations with their lone-pairs of electrons on the other, which also form within [AsO₃]³⁻ anions lone-pair channels along [010]. Both colorless compounds can be obtained by solid-state reactions from corresponding mixtures of the binaries (Y₂O₃, As₂O₃ and YX₃ with X = F and Cl) at elevated temperatures of 825 °C, most advantageously under halide-flux assistance (CsBr for Y₅F₃[AsO₃]₄ and ZnCl₂ for Y₅Cl₃[AsO₃]₄). By replacing a few percent of YX₃ with EuX₃ or TbX₃, Eu³⁺- or Tb³⁺-doped samples are accessible, which show red or green luminescence upon excitation with ultraviolet radiation. Full article

One of the effective types of heat-resistant insulating products with an operating temperature of 1050 °C is made from calcium silicates or their hydrates. These materials are made from synthetic xonotlite and 1.13 nm tobermorite. Various wastes and by-products from other industries can be used for the synthesis of the latter compound. However, such raw materials often contain various impurities, especially Al-containing compounds, which strongly influence the kinetics of 1.13 nm tobermorite formation and its properties. Using XRD, DSC, TG, and SEM/EDX methods, it was found that at the beginning of the hydrothermal synthesis, the Al₂O₃ additive promotes the formation of 1.13 nm tobermorite; however, it later begins to inhibit the recrystallization of semi-crystalline C-S-H(I)-type calcium silicate hydrate and pure, high-crystallinity 1.13 nm tobermorite is more easily formed in mixtures without the aluminum additive. Aluminum oxide also influence the morphology of 1.13 nm tobermorite. When hydrothermally curing the CaO–SiO₂ mixture, long, thin fibers (needles) are formed within 24 h. Later, they thicken and form rectangular parallelepiped crystals. After adding alumina, the product produced by 24 h synthesis is dominated by agglomerates, the surface of which is partially covered with crystal plates. By extending the synthesis duration, amorphous aggregates are absent and the crystal shape becomes increasingly square. Full article

Three liquid crystalline mixtures were investigated, consisting of compounds abbreviated as MHPOBC and 3F5FPhF6 with molar ratios 0.9:0.1 (MIX5FF6-1), 0.75:0.25 (MIX5FF6-2), and 0.5:0.5 (MIX5FF6-3). The presence of the smectic A*, smectic C*, and smectic C_A* phases was observed in all mixtures. The hexatic smectic X_A* phase, present in pure MHPOBC, disappeared quickly with an increasing admixture of 3F5FPhF6. Vitrification of smectic C_A* was observed for the equimolar mixture, with the glass transition temperature and fragility index comparable to the pure glassforming 3F5FPhF6 component. Partial crystallization to conformationally or orientationally disordered crystal phases was observed on cooling in two mixtures with a smaller fraction of 3F5FPhF6. Broadband dielectric spectroscopy was applied to study the relaxation times in smectic and crystal phases. Vogel–Fulcher–Tammann, Mauro–Yue–Ellison–Gupta–Allan, and critical-like models were applied for analysis of the α-relaxation time in supercooled smectic X_A* and smectic C_A* phases. Full article