Search Results (240)

The dichromate ion (Cr₂O₇²⁻), a highly toxic chromium VI species, is widely used in industrial processes, generating serious environmental problems when released into water bodies. This investigation proposes the use of a functionalized polymer as an adsorbent material for its removal in the aqueous phase. Poly(butyl methacrylate) (PBMA) was synthesized and modified by impregnation with resorcinarenes derived from long-chain aliphatic aldehydes. To improve the affinity for the dichromate, the resorcinarenes were functionalized with sulfomethyl groups by treatment with Na₂SO₃. The resulting matrices were characterized using IR-ATR, ¹H-NMR, and ¹³C-NMR, and their adsorbent performance was evaluated via UV-Vis spectroscopy in batch extraction assays. The results showed that the functionalized polymer exhibited a higher adsorption capacity than the base polymer, reaching up to 81.1% removal at pH 5.0 in one hour. These results highlight the potential of PBMA as an effective support and raise a promising research perspective for functionalized resorcinarenes in the development of new materials for the treatment of contaminated water. Full article

The incorporation of commercial graphene oxide (GO) into composites offers significant improvements in mechanical, thermal, and electrical properties, making it a promising material for industrial applications. This study presents a comprehensive characterization analysis of five commercial GOs, using advanced techniques to evaluate their structural, chemical, and especially their behavior when submitted to thermal treatment. The aim is to enable the use of GO in industrial processes of particular technological importance, where its thermal stability/integrity is required, such as in polymer composites, electronic and energy storage devices, among others. Raman spectroscopy and attenuated total reflectance–Fourier-transform infrared (ATR-FTIR) spectroscopy are employed to examine the structural defects and functional groups of GOs, while X-ray diffraction (XRD) provides insight into the crystallinity and interlayer spacing. Thermogravimetric analysis (TGA) assesses the thermal stability, and X-ray photoelectron spectroscopy (XPS) offers detailed information on the surface chemistry and relevant elemental composition of GOs. Additionally, the temperature-dependent behavior of GOs is explored through temperature-dependent XRD and IR measurements to investigate the thermal expansion and functional group stability. The study highlights the critical role of oxygen-containing groups—such as epoxides, hydroxyls, and carboxyls—while variations in the type and concentration of these functional groups across commercial GOs could influence the compatibility and performance of nanocomposites. This research attempts to fill to some extent the gap in understanding how the unique properties of different commercial GOs can be strategically applied to meet specific industrial performance requirements, such as barrier properties, transport efficiency, or mechanical strength, among others. Full article

Lanthanide-based metal–organic frameworks (Ln-MOFs) represent a key material in various optical applications. Thus, they offer the possibility of fine-tuning their functional properties by adjusting the composition, stoichiometry, and ligand nature. This work reports for the first time the environmentally friendly one-pot synthesis of Eu-Tb-doped yttrium-1,3,5-benzenetricarboxylate MOF, i.e., Y-BTC: Eu (10%), Tb (10%), under mild conditions of temperature and pressure. Structural and morphological investigations were conducted through ATR-IR, XRD, and FE-SEM characterization. The doping percentage was analyzed by EDX spectroscopy. The luminescence properties confirm the down-shifting behavior of the MOF, paving the way for using this Eu-Tb-doped Y-BTC system in photovoltaic technology. Full article

Nowadays, nitrate ions and azo dyes are a significant source of water pollution due to their high toxicity, persistence, and potential to be carcinogenic. Both contaminants are the result of anthropogenic sources, such as sewage or industrial wastewater discharge; the first one results also as a consequence of the intensive use of fertilizers. In this work we report the use of a new quaternized pentablock copolymer (PTBr) for the removal of nitrate ions and methyl orange (MO) dye from water by adsorption processes. Morphological, chemical, and thermal properties of the pentablock copolymer were investigated, respectively, by scanning electron microscopy (SEM), Attenuated Total Reflectance Infrared Spectroscopy (ATR-FTIR) (FT-IR), and X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), and differential scanning calorimetry (DSC) analyses. Anionic removal ability and adsorption rate in water solutions containing either a single contaminant species or a mix of the two contaminants were studied by UV–VIS absorbance spectroscopy as a function of time and initial concentration. The presence of imidazole groups confers on PTBr a positive charge and a hydrophilic character that are responsible for an effective removal of anions from water. PTBr film reports an adsorption efficiency of 10.15 mg/g for nitrate removal and this value is in line with others reported in the literature. In the case of the simultaneous presence of nitrate and MO, it is found that nitrate ions removal is slightly affected by the presence of the dye, since both contaminants compete for electrostatic interaction with imidazole groups. On the contrary, the dye removal does not show significant change with or without the presence of nitrate ions, probably due to other kinds of interaction that it can establish with the polymer surface (π-π interaction). The adsorption process and the related mechanisms are described using kinetic and isothermal models. Despite a certain reduction in the adsorption efficiency for one of the investigated contaminants, the results confirm the possibility of using the quaternized pentablock copolymer for the co-adsorption of both inorganic and organic anions. Full article

Fourier-transform infrared (FTIR) spectroscopy can detect biomolecular changes in bacterial cells in response to drugs or other stimuli. Fully developing this area requires an understanding of IR spectral changes associated with the growth of unperturbed cells. Such an understanding is still lacking, however. To address this issue, attenuated total reflectance (ATR) FTIR spectroscopy has been used to probe changes in the composition of Staphylococcus aureus ATCC 6538 cells during exponential growth, with a 30 min time resolution. We find prominent spectral changes in proteins, nucleic acids, and carbohydrates evolving from the early (30–120 min) to the late (240–360 min) log phase of growth. Principal component analysis (PCA) shows that spectra obtained for cells during the early and late log phases of growth can be discriminated against with 100% accuracy. Protein-related spectral features are most significant in spectra collected at 30- and 90-min post-inoculation and provide a robust basis for temporal differentiation. Spectral changes that occur during the first 30 min after inoculation are shown to reverse over the next 30–120 min, indicating dynamic adaptations during cellular growth. Overall, we demonstrate a band assignment strategy based on time resolution, underscoring the utility of FTIR spectroscopy in dynamic studies of bacterial cells. Full article

The existence of historical pigments databases is important to speed up cultural heritage research. Knowledge of their chemical composition and their manufacture contributes to the study of art history and helps develop accurate conservation-restoration strategies. In this study, a total of nineteen pigments, among which we find silicates (Egyptian blue, natural and synthetic blue ultramarine, green earth and chrysocolla), oxides (natural and synthetic hematite, red and yellow natural ochres, and chromium green), carbonates (natural and synthetic azurite, natural and synthetic malachite, and white lead), sulphides (natural and synthetic cinnabar, and orpiment) and acetates, (verdigris) have been characterized by Fourier Transform Infrared-Spectroscopy in Attenuated Total Reflection (ATR-FTIR) and Diffuse Reflectance (DRIFT) modalities. Considering the latter, there is still a great deal of uncertainty in the interpretation of the different IR vibrational bands. Therefore, a comparative study between these two techniques has been carried out to highlight the potential of DRIFT spectroscopy as a portable and non-destructive technique that allows the differentiation and characterization of historical pigments in the field of cultural heritage. Before performing FTIR analysis, pigments were analysed using X-ray diffraction (XRD) to detect impurities and/or additives in the pigments. Differentiation between natural and synthetic pigments was possible due to the identification of impurities in natural pigments, and manufacture-related compounds or additives in synthetic pigments. Results obtained in this study have proven DRIFT to be a very useful analytical technique for in situ characterization of heritage materials. This study serves as an initial step in clarifying the challenges and uncertainties associated with interpreting spectra obtained through the DRIFT modality. However, the use of other complementary analytical techniques is required. Full article

This study investigates the biodegradation behavior of poly(butylene succinate) (PBS) copolyesters containing dilinoleic acid (DLA) co-monomeric units and wood flour (WF) as a filler. PBS-DLA is a segmented thermoplastic elastomer (TPE), where the soft amorphous phase is formed by DLA ester segments, while the hard phase consists of crystallizable PBS domains. Wood–plastic composites (WPCs) were prepared with WF at weight fractions of 10%, 20%, 30%, and 40% wt. and analyzed in terms of surface morphology, chemical structure, mechanical performance, and thermal stability before and after biodegradation in soil conditions. The results of microscopic analysis confirmed that the PBS-DLA copolymer and its composites undergo surface biodegradation as manifested by increased surface roughness and microcrack formation, particularly in composites with a higher WF content. ATR FT-IR spectroscopy indicated oxidation and hydrolysis, supporting the hypothesis of progressive surface erosion. Mechanical tests showed a decline in tensile strength and elongation at break, with the most pronounced changes in composites containing 20% WF. Thermal analysis (DSC, DMTA, and TGA) confirmed that the PBS-DLA copolymer retains its thermoplastic elastomeric behavior after a 3-month biodegradation experiment. The storage modulus (E′) remained stable, while only minor variations in melting and crystallization temperatures were observed. These findings reinforce the hypothesis of surface erosion rather than a bulk degradation mechanism. Given their biodegradability and retained thermoplastic behavior, WPC composites based on PBS-DLA copolyester could be promising for eco-friendly applications where controlled degradation is desirable, such as in packaging, agriculture, or biodegradable consumer goods. Full article

Due to rising concerns regarding the adulteration and mislabeling of honey, new directives at the European level encourage researchers to develop reliable honey authentication models based on rapid and cost-effective analytical techniques, such as vibrational spectroscopies. The present study discusses the identification of the main vibrational bands of the FT-Raman and ATR-IR spectra of the most consumed honey varieties in Transylvania: acacia, honeydew, and rapeseed, exposing the ways the spectral fingerprint differs based on the honey’s varietal-dependent composition. Additionally, a pilot study on honey authentication describes a new methodology of processing the combined vibrational data with the most efficient machine learning algorithms. By employing the proposed methodology, the developed model was capable of distinguishing honey produced in a narrow geographical region (Transylvania) with an accuracy of 85.2% and 93.8% on training and testing datasets when the Trilayered Neural Network algorithm was applied to the combined IR and Raman data. Moreover, acacia honey was differentiated against fifteen other sources with a 87% accuracy on training and testing datasets. The proposed methodology proved efficiency and can be further employed for label control and food safety enhancement. Full article

Nanosized manganese dioxide (MnO₂) material has been successfully incorporated into a graphene oxide (GO) sensitive layer. Since this type of heterojunction has never been reported in the literature related to gas sensing, these sensors were prepared, tested, and reported. The morphological properties and composition of the MnO₂@GO material have been thoroughly studied via FESEM, XRD, Raman spectroscopy, HR-TEM, and ATR-IR. Gas sensitivity and selectivity towards mainly NO₂ and other gases (NH₃, CO, ethanol, benzene, and H₂) have also been studied. The obtained sensors were exposed to different concentrations of NO₂ ranging from 200 ppb to 1000 ppb at 150 °C and under close to real conditions (25% relative humidity and 70% relative humidity). The MnO₂@GO sensors have shown a high response of 16.3% towards 1 ppm of NO₂ under dry conditions and a higher response of 44% at 70% RH towards the same concentration. Finally, it has also shown a strong sensitivity for NO₂. Full article

(1) Background: Over 90% of hop crops are currently used in beer production, with a small part used in the cosmetics and pharmaceutical industries. Spent hops as a waste product contain one of the strongest antioxidants, xanthohumol. The aim of the study was to purify spent hop extracts by magnetic dispersive extraction using iron oxide nanoparticles (IONP) to obtain pure xanthohumol; (2) Methods: The extract from the waste product obtained after supercritical carbon dioxide extraction of hops was prepared by ultrasound-assisted extraction utilizing different solvents, i.e., ethyl acetate, propanol, acetone, 80% methanol, ethyl acetate-methanol (1:1, v/v), and propanol-methanol (1:1, v/v). The hydrodynamic diameters and zeta potential of IONPs before and after incubation were measured by dynamic light scattering (DLS). The extracts were analyzed by reversed-phase high-performance liquid chromatography (HPLC). Isolated xanthohumol was identified based on the DAD spectrum in the range of 200–600 nm and by Fourier transform infrared spectroscopy/attenuated total reflectance (FT-IR/ATR); The antioxidant activity of extracts before and after incubation with IONPs was assessed using SNPAC (Silver Nanoparticle Antioxidant Capacity), DPPH (2,2-diphenyl-1-picrylhydrazyl radical), and FRAP (Ferric Reducing Antioxidant Power) assays, as well as total phenolic content (TPC) and total flavonoid content (TFC). (3) Results: The amount of added IONPs, the kind of solvent, and the contact time of the extract with nanoparticles were optimized. We found that 80% MeOH extract after incubation with IONPs (865 µg IONPs/g of spent hops) at room temperature for 48 h contains 74.61% of initial xanthohumol content, providing a final xanthohumol concentration of 43 µg mL⁻¹. (4) Conclusions: The proposed method of magnetic dispersive extraction using IONPs allows for the purification of spent hops extract and obtaining a pure product, namely xanthohumol, with a wide potential for practical applications in medicine, pharmacy, cosmetics, and agriculture. This is clear evidence of the usefulness of IONP as an effective sorbent. The method allows the use of residues from the brewing industry, i.e., the biomass of used hop cones to obtain a valuable substance. Full article

The non-isothermal melt crystallization process of poly[(R)-3-hydroxybutyrate-co-(R)-3-hydroxyhexanoateate] (PHBHx) was monitored using attenuated total reflection infrared (ATR IR) measurement. The resulting time- and temperature-dependent spectra were subjected to the two-dimensional correlation spectroscopy (2D-COS) analysis. The C=O stretching region of the PHBHx sample consisted of several distinct IR contributions attributable to the population of amorphous component, well-ordered type I lamellar crystal, and less ordered inter-lamellar type II crystal. The spectral intensity change in type I crystal occurs in the earlier stage of the crystallization at a higher temperature range compared to the overall intensity decrease in the amorphous component occurring throughout the crystallization process. The growth of the type II crystal started in a later stage at a lower temperature than the creation of the type I crystal. An early decrease in a small but distinct portion of the amorphous component may be related to a crystallization precursor species with some level of molecular order. Hetero-mode correlation analyses revealed that the crystalline band intensity changes in the C-H stretching and fingerprint regions all occur later than the population changes in crystalline species reflected by the carbonyl stretching bands. This observation suggests that the spectral intensity changes in the C-H stretching and fingerprint regions do not directly represent the population dynamics of the crystalline and amorphous species but probe instead the molecular state of the crystalline entities still undergoing the evolutionary changes. Full article

The molecular interactions of water-soluble crown resorcinarenes with choline were analyzed. To this end, four sulfonated resorcinarenes were synthesized and characterized by ATR-IR, ¹H-NMR, and ¹³C-NMR spectroscopy. The molecular interaction studies with choline were carried out through FT-IR spectroscopy, ¹H-NMR titrations, and conductimetric titrations, with which it was possible to determine that the complexes formed 1:1 stoichiometries with the host, in addition to showing good interaction in the electronic cavity of the macrocycle, demonstrating great potential for host–guest systems for choline detection in aqueous media. Finally, the incidence of the structural aspects of sulfonated resorcinarenes were analyzed. Full article

Silica aerogels are extensively used as catalyst supports due to their mesoporous structure and chemical inertness. In this study, SiO₂–AuNP aerogels containing gold nanoparticles (AuNPs) were synthesized using the sol-gel method followed by supercritical CO₂ drying. The inclusion of polyvinyl pyrrolidone (PVP) as a stabilizing agent preserved the gold particle sizes during the gelation process. In contrast, aerogels synthesized without PVP contained enlarged AuNP aggregates, resulting in a shift in the plasmon resonance color from red to bluish or blue–grey. Thermal treatment of these bluish-colored aerogels at high temperatures restored their red coloration, visually indicating the breakdown of large gold clusters into individual nanoparticles. Both types of aerogels were characterized using SEM, TEM, 3D optical microscopy, UV–vis and ATR-IR spectroscopy, and N₂ porosimetry, with their properties analyzed as a function of annealing temperature. Their catalytic activity was evaluated through the reduction of 4-nitrophenol with sodium borohydride, and both aerogel types demonstrated catalytic activity. This thermal conversion of large clusters into individual nanoparticles within an aerogel matrix introduces a new and promising approach for creating catalytically active nanogold-containing aerogel catalysts. Full article

To obtain sustainable food packaging materials, alternatives to traditional ones must be researched. In this work, two different kinds of zeolites, i.e., a natural one, Clinoptilolite, and a synthetic one, Zeolite Na-X, were mixed with thermoplastic polyurethane for the fabrication of composites. Composite films were prepared via a hot mixing stage and then by means of a hot compression molding process. Several TPU/zeolite composites were produced with a filler concentration ranging from 5% to 10%wt. Finally, the obtained films were characterized by Fourier Transform Spectroscopy (FT-IR, ATR), thermal analysis (TGA and DSC), frequency sweep test, scanning electron microscopy (SEM), mechanical tensile test and oxygen permeability test. For both fillers and at all concentrations, the inclusion of zeolites significantly influenced the analyzed properties. In the TPU/zeolite composites, an overall enhancement was observed compared to the neat polymer, attributed to improved processability, superior barrier properties and the potential to create active materials by loading zeolite combined with various chemicals for specific applications. These findings suggest that the resulting composites hold considerable promise for applications in the food packaging sector. Full article

Supercapacitors are advanced energy storage devices renowned for their rapid energy delivery and long operational lifespan, making them indispensable across various industries. Their relevance has grown in recent years due to the adoption of environmentally friendly materials. One such material is bacterial nanocellulose (BNC), produced entirely from microbial sources, offering sustainability and a bioprocess-driven synthesis. In this study, BNC was synthesized using a symbiotic microbial community. After production and purification, pristine BNC membranes, with an average thickness of 80 microns, were impregnated with an alkali-alcohol meta-polybenzimidazole (PBI) solution. This process yielded hybrid BNC/PBI membranes with improved ion-transport properties. The BNC membranes were then doped with a 6 M KOH solution, to enhance OH⁻ conductivity, and characterized using optical microscopy, ATR FT-IR, XRD, CVT, BET analysis, and impedance spectroscopy. Both BNC and BNC/PBI membranes were tested as separators in laboratory-scale symmetric supercapacitor cells, with performance compared to a commercial Viledon^® separator. The supercapacitors employing BNC membranes exhibited high specific capacitance and excellent cycling stability, retaining performance over 10,000 charge/discharge cycles. These findings underscore the potential of BNC/KOH membranes for next-generation supercapacitor applications. Full article