Search Results (869)

X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) are analytical techniques enabling precise analysis of the electronic structure and local atomic environment in chemical compounds and materials. Their application spans materials science, chemistry, biology, and environmental sciences, supporting studies on catalytic mechanisms, redox processes, and metal speciation. A key advantage of both techniques is element selectivity, allowing the analysis of specific elements without matrix interference. Their high sensitivity to chemical state and coordination enables determination of oxidation states, electronic configuration, and local geometry. These methods are applicable to solids, liquids, and gases without special sample preparation. Modern XAS and XES studies are typically performed using synchrotron radiation, which provides an intense, monochromatic X-ray source and allows advanced in situ and operando experiments. Sub-techniques such as XANES (X-ray absorption near-edge structure), EXAFS (Extended X-ray Absorption Fine Structure), and RIXS (resonant inelastic X-ray scattering) offer enhanced insights into oxidation states, local structure, and electronic excitations. Despite their broad scientific use, applications in pharmaceutical research remain limited. Nevertheless, recent studies highlight their potential in analyzing crystalline active pharmaceutical ingredients (APIs), drug–biomolecule interactions, and differences in drug activity. This review introduces the fundamental aspects of XAS and XES, with an emphasis on practical considerations for pharmaceutical applications, including experimental design and basic spectral interpretation. Full article

The urgent need for advanced analytical tools for environmental monitoring and food safety drives the development of novel biosensing approaches and solutions. A computationally driven workflow for the development of a rapid electrochemical aptasensor for okadaic acid (OA), a critical marine biotoxin, is reported. The core of this strategy is a rational design process, where in silico modeling was employed to optimize the biological recognition element. A 63-nucleotide aptamer was successfully truncated to a highly efficient 31-nucleotide variant. Molecular docking simulations confirmed the high binding affinity of the minimized aptamer and guided the design of the surface immobilization chemistry to ensure robust performance. The fabricated sensor, which utilizes a ferrocene-labeled aptamer, delivered a sensitive response with a detection limit of 2.5 nM (n = 5) over a linear range of 5–200 nM. A significant advantage for practical applications is the remarkably short assay time of 5 min. The sensor’s applicability was successfully validated in complex food matrices, achieving excellent recovery rates of 82–103% in spiked mussel samples. This study establishes an integrated computational–experimental methodology that streamlines the development of high-performance biosensors for critical food safety and environmental monitoring challenges. Full article

Thermo-catalytic decomposition (TCD) presents a promising pathway for producing hydrogen from natural gas without emitting CO₂. This process represents a form of fossil fuel decarbonization where the byproduct, rather than being a greenhouse gas, is a solid carbon material with potential for commercial value. This study examines the dynamic behavior of TCD, showing that carbon formed during the reaction first enhances and later dominates methane decomposition. Three types of carbon materials were employed as starting catalysts. Methane decomposition was continuously monitored using on-line Fourier transform infrared (FT-IR) spectroscopy. The concentration and nature of surface-active sites were determined using a two-step approach: oxygen chemisorption followed by elemental analysis through X-ray photoelectron spectroscopy (XPS). Changes in the morphology and nanostructure of the carbon catalysts, both before and after TCD, were examined using high-resolution transmission electron microscopy (HRTEM). Thermogravimetric analysis (TGA) was used to study the reactivity of the TCD deposits in relation to the initial catalysts. Partial oxidation altered the structural and surface chemistry of the initial carbon catalysts, resulting in activation energies of 69.7–136.7 kJ/mol for methane. The presence of C₂ and C₃ species doubled methane decomposition (12% → 24%). TCD carbon displayed higher reactivity than the nascent catalysts and sustained long-term activity. Full article

This study investigated the effects of silver doping, natural ageing, and thermal-induced oxidation on the surface chemistry, morphology, and thermal performance of copper thin films. Ag is used as a doping element in Cu because, in bulk materials it usually refines microstructures, leading to increased hardness and mechanical strength through mechanisms such as solid solution strengthening and twinning. In this work was also used due to its oxidation resistance. Thin films of pure and silver-doped copper (Cu_2Ag and Cu_4Ag) were deposited by RF magnetron sputtering and characterized as-deposited, naturally aged, at room temperature and humidity for one year, and thermally treated at 200 °C, in air. The characterization included X-ray photoelectron spectroscopy (XPS), Atomic Force microscopy (AFM), and thermal analysis, specifically thermal conductivity (λ), thermal diffusivity (α), and thermal capacity (ρ.Cp). Surface XPS analysis revealed changes in copper and silver oxidation states after natural aging and annealing. AFM revelead that the incorporation of silver and heat treatment altered the surface roughness and morphology. Thermal analysis found that for lower silver concentrations, the thermal conductivity increased, but aging and annealing had varying effects depending on the silver content. The Cu_4Ag film showed the best thermal stability after natural ageing. Overall, the results suggest that carefully controlled silver doping can enhance the thermal stability of copper thin films for applications where aging is a concern, such as microelectronics. Full article

Background/Objectives: This in vitro study evaluated the effects of fluoride-free toothpaste, fluoride-containing toothpaste, and a color-correcting gel on the morphology, composition, and mechanical properties of demineralized human enamel. The hypothesis was that fluoride-containing formulations would better preserve enamel integrity compared to non-fluoride and cosmetic products. Methods: Extracted human teeth (n = 3 per group) were demineralized with 36% phosphoric acid and assigned to four groups: E0 (control), E1 (fluoride-free toothpaste), E2 (fluoride-containing toothpaste), and E3 (color-correcting gel). Brushing was performed manually twice daily for 7 days using standardized force. Surface morphology and elemental composition were assessed via SEM–EDX; chemical changes were analyzed by FTIR; mechanical properties were evaluated using the Vickers microhardness test. Results: E1 exhibited the highest microhardness (343.6 HV) but also the highest Ca/P ratio (2.37) and most pronounced surface roughness (p < 0.05 vs. control). E2 showed a balanced Ca/P ratio (2.07), smoother morphology, and detectable fluoride incorporation, despite a lower hardness value (214.5 HV). E3 presented moderate changes in both morphology and composition, with a Ca/P ratio similar to the control (2.06) but surface irregularities visible by SEM. The apparent paradox in E1—high hardness with structural damage—may be due to superficial mineral precipitation without true remineralization. Conclusions: Fluoride-containing toothpaste preserved enamel morphology and chemistry more effectively than the other formulations. Increased hardness in E1 does not necessarily indicate clinical benefit. In vivo studies with longer protocols and pH cycling are needed to confirm these findings. Full article

Rapid and accurate bacteria identification, particularly Escherichia coli (E. coli), is essential in the monitoring of health, environment, and food safety. E. coli, a prevalent pathogenic bacterium, serves as a key indicator of food and water contamination. Carbon quantum dots (CQDs) have appeared as promising fluorescent probes because of their small size, ease of synthesis, low toxicity, and tunable fluorescence using different carbon-rich precursors. Advances in both bottom-up and top-down synthesis procedures have enabled precise control over CQD properties and surface functionalities, enhancing their capabilities in biosensing. Among the critical factors influencing CQD performance is the strategic selection of precursors, which determines the surface chemistry and recognition potential of the resulting nanodots. The integration with other nanomaterials and the surface modification of CQDs with specific functional groups or recognition elements further improves their sensitivity and selectivity toward E. coli. This review summarizes recent progress in the modification of CQDs for the fluorescent detection of E. coli, highlighting relevant sensing mechanisms and the influence of different precursors, such as antibiotics and sugars, as well as various functionalization and surface modification strategies. The aim is to provide insight into the rational design of efficient, selective, and cost-effective CQD-based biosensors for bacterial detection. Full article

The present work is aimed at shedding light on the evolution of surface chemistry of a commercial activated carbon (AC) support during the preparation of supported metal oxide (MO) catalysts by the conventional wet impregnation method. Particular attention is paid to the chemical changes of oxygen-containing surface functionalities across three preparation stages of impregnation, oven-drying, and thermal treatment. AC was impregnated with aqueous solutions of several MO precursors (Al(NO₃)₃, Fe(NO₃)₃, Zn(NO₃)₂, SnCl₂, and Na₂WO₄) at 80 °C for 5 h, oven-dried at 120 °C for 24 h, and heat-treated at 200 °C and 850 °C for 2 h under an inert atmosphere. The surface chemistry of the resulting catalyst samples, classified in three series by the thermal treatment, was mainly studied by FT-IR spectroscopy, complemented by elemental analysis and pH of the point of zero charge (pH_pzc) measurements. During impregnation, phenolic hydroxyl and carboxylic acid groups were predominantly formed by wet oxidation of chromene, 2-pyrone, and ether-type structures found in the pristine AC. The extent of these oxidations correlated with the oxidising power of the precursor solutions. As expected, thermal treatment at 850 °C brought about markedly stronger chemical changes, with most of the above oxygen functionalities decomposing and forming less acidic structures, such as 4-pyrone groups, metal carboxylates, and C-O-M atomic groupings. All these surface chemical modifications result in a lowering of the strong basicity of the raw carbon support (pH_pzc ≈ 10.5), thus leading to pH_pzc values for the catalysts widely ranging from 1.6 to 9.7. Full article

Multiple ironstone beds formed during the Callovian-Oxfordian times as a consequence of intense continental weathering, upwelling, and hydrothermal activity. This study examines the compositional differences between core and rim, and the origin of iron ooids along the northwestern margin of the Neo-Tethys Ocean to highlight sea-level fluctuations, redox conditions, and elemental influx. An integrated sedimentological study, including petrography, mineralogy, micro-texture, and mineral chemistry, was carried out to explain the origin and implications of ironstones. The ~14 m thick Callovian-Oxfordian, marginal marine deposits in the Kutch Basin, in western India, exhibit iron ooids, predominantly formed in oolitic shoals during transgression, associated with lagoonal siliciclastics. Callovian shoals interbedded with lagoonal facies record minor sea-level fluctuations, whereas the Oxfordian deposit records a major transgression and condensation, resulting in extensive ironstone deposits. The ooid cortices and nuclei exhibit distinctive mineralogy and micro-textures: glauconitic smectite exhibits poorly-developed rosettes, chamosite displays flower-like, and goethite shows rod-like features. Three types of ooids are formed: (i) monomineralic ooids are entirely of chamosite or goethite, (ii) quartz-nucleated ooids, and (iii) composite ooids with either chamosite core and goethite rim, or chamosite core and glauconitic smectite rim. The assemblages within iron ooids reflect variation in depositional redox conditions: glauconitic smectite develops under suboxic lagoonal flank, chamosite forms in anoxic central lagoon, and goethite precipitates on oxic shoals. Full article

In this study, zinc oxide nanoparticles (ZnO NPs) were synthesized via a green chemistry approach using aqueous extract of Camellia sinensis var. assamica (Assam green tea) as a bioreductant and stabilizing agent. Phytochemical analysis of the extract revealed high levels of phenolics (338.57 ± 3.90 mg GAE/mL) and flavonoids (123.92 ± 1.34 µg QE/mL), along with strong antioxidant and reducing activity, supporting its efficacy in nanoparticle formation. ZnO NPs were synthesized at various extract concentrations, with 25% yielding optimal characteristics based on UV–Vis spectrophotometry (λ_Max ≈ 390–410 nm). Structural characterization using XRD confirmed the hexagonal wurtzite phase, and SAXS indicated particle sizes of 58–60 nm. FE-SEM analysis showed semi-spherical agglomerated particles ranging from 74 to 76 nm, while EDX verified the elemental purity of Zn and O. FT-IR spectroscopy confirmed the presence of Zn–O stretching and phytochemical residues on the nanoparticle surface. Stability studies over four weeks revealed red shifts in absorbance and reduced peak intensity at ambient and elevated temperatures, suggesting nanoparticle agglomeration. Antimicrobial assays demonstrated strong antifungal activity of the ZnO NP solution against Candida albicans and, upon concentration, significant antibacterial activity against Streptococcus mutans. The synthesized ZnO NPs exhibit promising potential as eco-friendly antimicrobial agents, particularly for applications in oral healthcare. Full article

The CO₂ hydrogenation process is thought to be one of the feasible methods for producing methanol fuel, which might be used to fulfill future energy demands. Improving the catalytic efficiency and understanding of the process are essential elements for the viability of CO₂ conversion routes. Here, a co-precipitation method was used to synthesize Ni-Cu bimetallic catalysts supported by chromium oxide (Cr₂O₃). To examine nickel (Ni)’s promoting role, the synthesized catalysts were incorporated with different concentrations of Ni. The N₂ adsorption–desorption isotherm exposed the mesoporous nature of Cr₂O₃-based Ni-Cu catalysts. A Fourier Transform Infrared (FTIR) spectroscopy investigation revealed the effective doping of Ni-Cu metal oxides on the surface of Cr₂O₃ by instigating an FTIR absorption band in the region associated with the FTIR absorption of metal oxides. The uniform morphology and homogenous, as well as highly dispersed, form of both Ni and Cu metal were recorded using a Field Emission Scanning Electron Microscope (FESEM) and X-ray Diffraction (XRD) techniques. The surface chemistry, metal–metal, and metal–support interactions of the Ni-Cu/Cr₂O₃ catalysts were disclosed via temperature program reduction (TPR) as well as X-ray photoelectron spectroscopy (XPS). The synergism between the Ni and Cu metals was revealed using both XPS and TPR techniques, which resulted in improving the catalytic profile of Ni-Cu/Cr₂O₃ catalysts. The activity data obtained by applying a slurry reactor demonstrated the active profile of Ni for CO₂ reduction to methanol in terms of the methanol synthesis rate. The promoting role of Ni was established by observing the progressing and linear increase in methanol selectivity by Ni enrichment to the Ni-Cu/Cr₂O₃ catalysts. Structure and activity studies recognized the promoting role of Ni by experiencing metal–metal and metal–support interactions with highly dispersed metal oxides over the Cr₂O₃ support in the current case. Full article

Optimal sensing devices exhibit a combination of key performance attributes, including an extensive detection limit, exceptional selectivity, high sensitivity, consistent repeatability, precise measurement, and rapid response times with efficient analyte flow. In recent years, biosensing platforms incorporating nanoscale materials have garnered considerable attention due to their diverse applications across various scientific and technological domains. The integration of nanoparticles (NPs) in biosensor design primarily bridges the dimensional gap between the signal transduction element and the biological recognition component, both of which operate at nanometer scales. The synergistic combination of NPs with electrochemical techniques has facilitated the development of biosensors characterized by enhanced sensitivity and superior analyte discrimination capabilities. This comprehensive analysis examines the evolution and recent advancements in nanomaterial (NM)-based biosensors, encompassing an extensive array of nanostructures. These consists of one-dimensional nanostructures including carbon nanotubes (CNTs), nanowires (NWs), nanorods (NRs), and quantum dots (QDs), as well as noble metal and metal and metal oxide nanoparticles (NPs). The article examines how advancements in biosensing techniques across a range of applications have been fueled by the growth of nanotechnology. Researchers have significantly improved biosensor performance parameters by utilizing the distinct physiochemical properties of these NMs. The developments have increased the potential uses of nanobiosensors in a wide range of fields, from food safety and biodefense to medical diagnostics and environmental monitoring. The continuous developments in NM-based biosensors are the result of the integration of several scientific areas, such as analytical chemistry, materials science, and biotechnology. This interdisciplinary approach continues to drive innovations in sensor design, signal amplification strategies, and data analysis techniques, ultimately leading to more sophisticated and capable biosensing platforms. As the field progresses, challenges related to the scalability, reproducibility, and long-term stability of nanobiosensors are being addressed through innovative fabrication methods and surface modification techniques. These efforts aim to translate the promising results observed in laboratory settings into practical, commercially viable biosensing devices that can address real-world analytical challenges across various sectors. Full article

In the present study, ultrasound-assisted extraction using deep eutectic solvents was proposed for the preparation of uniced and iced gingerbread cookies prior to the determination of four macronutrients (potassium, sodium, magnesium, calcium), four micronutrients (manganese, zinc, iron, copper), the presence of toxic metal (cadmium), and antioxidant capacity. With the addition of 30% water in each green solvent, three acidic deep eutectic solvents, comprising xylitol with malic acid, choline chloride with malic acid, and choline chloride with lactic acid, were tested for their efficiencies in the simultaneous extraction of elements and antioxidants. The synthesized deep eutectic solvents were characterized by infrared spectroscopy, which provided evidence of generating new hydrogen bonds between two components of these solvents. Element profiles were analyzed by inductively coupled plasma–mass spectrometry after the extraction using green solvents and the microwave-assisted acid digestion of gingerbread samples. It was found that two deep eutectic solvents containing malic acid exhibited high abilities for solubilization of macronutrients and manganese from the samples studied, while the best extraction efficiencies for Zn, Fe and Cu micronutrients were achieved when the lactic acid-based deep eutectic solvent was used. However, the antioxidant capacity, evaluated by 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), 2,2-diphenyl-1-picrylhydrazyl (DPPH), and cupric reducing antioxidant capacity (CUPRAC) methods, led to the selection of choline chloride–lactic acid as the most promising green solvent for extracting antioxidants from two types of gingerbread cookies. The deep eutectic solvent-based extraction conforms to the principles of green chemistry and is suitable for releasing elements and antioxidants from gingerbread cookies. Full article

With the increase in contamination by microbial agents (bacteria, viruses, etc.) in the fields of agri-food, healthcare, and environment, it is necessary to detect and quantify these biological elements present in complex fluids in a short time with high selectivity, high sensitivity, and, if possible, moderate cost. Acoustic wave biosensors, based on immuno-detection, appear to meet a certain number of these criteria. In this context, we are developing a generic antibody-based biointerface that can detect a wide range of pathogenic bacterial agents using a specific bioreceptor. Based on the silane–oxide chemistry, the process is transferable to any kind of surface that can be either oxidized in surface or activated with O₂-plasma, for instance. For this proof of concept, we have chosen to develop our biointerface on titanium and lithium niobate surfaces. The development of the biointerface consists of grafting antibodies via a self-assembled monolayer (SAM) composed of an aminopropyltriethoxysilane (APTES) and a linker (phenylene diisothiocyanate, PDITC). Two functionalization routes were tested for grafting APTES: in anhydrous toluene followed by a heating step at 110 °C or in chloroform at room temperature. The results obtained on titanium show comparable grafting efficiency between these two routes, allowing us to consider the transposition of the route at room temperature on lithium niobate. The latest route was chosen for fragile materials that do not require the heating steps necessary when using toluene for grafting aminopropyltriethoxysilane. Different surface characterization techniques were used, such as IR spectroscopy (FTIR-ATR), X-ray photoelectron spectroscopy (XPS), and contact angle (WCA), to verify the successful grafting of each layer. Biodetection experiments in static conditions were also carried out to demonstrate the specificity of pathogenic detection, testing an ideal medium with solely bacteria, with no other food sampling nutrients. This paper demonstrates the successful elaboration of a biointerface using APTES as the first anchoring layer, with chloroform as a mild solvent. The process is easily transferable to any kind of fragile surface. Moreover, following anti-L. monocytogenes antibodies, our biointerface shows a specificity of capture in static mode (at a concentration of 10⁷ CFU/mL for an incubation time of 4 h at 37 °C) of up to 98% compared to a species negative control (E. coli) and up to 85% in terms of strain specificity (L. innocua). Full article

Lanthanum-cerium rare earth (RE) elements play a vital role in metallurgy as essential microalloying elements. Their addition significantly modifies inclusion characteristics, enhances mechanical properties, and improves corrosion resistance. This review emphasizes the distinct and synergistic roles of lanthanum (La) and cerium (Ce) in steel at the atomic scale, elucidated through first-principles calculations based on density-functional theory (DFT). The primary focus includes the nucleation mechanisms and characteristics of rare earth inclusions, the solid solution and segregation behavior of rare earth atoms, and their microalloying effects on electronic structure and interfacial bonding. Although both elements form stable inclusions Re₂O₃ and ReAlO₃ and exhibit grain refinement effects, Ce exhibits a unique dual valence state (Ce³⁺/Ce⁴⁺). This results in nucleation behavior and oxide stability for Ce ions that differ slightly from those of La. Both elements alter the electronic structure of the Fe matrix through hybridization with d-orbitals, reducing magnetic moment and enhancing toughness. Compared to other alloying elements, La and Ce exhibit unique behaviors due to their large atomic radii and high chemical reactivity, which influence their solid solubility, segregation tendencies, and interactions with other atoms such as Cr, C, and N. Finally, this paper discusses the challenges that exist when first-principles computational methods are used to study the mechanism of action of RE elements in steel, and proposes measures and methods to address these challenges, aiming to provide an in-depth understanding of the mechanism of action of REs in steel at the microscopic level and to promote the application of computational chemistry in the field of metallurgy. Full article

The anomalous enrichment of arsenic (As) and fluoride (F) in groundwater in the oasis area at the southern margin of the Tarim Basin has become a critical environmental and sustainability challenge. It poses not only potential health risks but also profound socio-economic impacts on local communities, threatening the long-term security of water resources in arid regions. Therefore, an in-depth investigation of the hydrochemical characteristics of groundwater and the co-enrichment mechanism of As and F is essential for advancing sustainable groundwater management. In this study, 110 phreatic water samples and 50 confined water samples were collected, and mathematical and statistical methods were applied to analyze the hydrochemical characteristics, sources, and co-enrichment mechanisms of As and F. The results show that (1) the groundwater chemistry types are mainly Cl·SO₄-Na, SO₄·Cl-Na·Mg, Cl·SO₄-Na·Mg, and Cl-Na, and the chemistry is primarily controlled by evaporation and concentration processes, with additional influence from human activities and cation exchange; (2) As and F mainly originate from soils and minerals, and are released through dissolution; (3) As and F enrichment is positively correlated with pH, Na⁺, and HCO₃⁻, but negatively correlated with Ca²⁺, Mg²⁺, and SO₄²⁻, indicating that a weakly alkaline hydrochemical environment with high HCO₃⁻ and Na⁺, and low Ca²⁺ promotes their enrichment; (4) strong evaporative concentration in retention zones, combined with artificial groundwater extraction, further intensifies As and F accumulation. This study not only provides an innovative theoretical and methodological framework for exploring trace element enrichment mechanisms in groundwater under arid conditions but also delivers critical scientific evidence for developing sustainable water resource management strategies, mitigating water-related health risks, and supporting regional socio-economic resilience under global climate change. Full article