Search Results (701)

Dry Turkish oak (Quercus cerris) sawdust, untreated and treated with three activators, (H₃PO₄, NaOH and H₂O₂) was pyrolyzed under limited-oxygen conditions to obtain biochar samples. The electrochemical properties of these samples were tested and compared to the properties of several commercial carbon blacks. The electrochemical characterization was performed via cyclic voltammetry, analyzing the response toward two commonly used redox probes, [Fe(CN)₆]^3−/−4− and [Ru(NH₃)₆]^2+/3+. The influence of the scan rate on this response was investigated, and the resulting data were used to obtain the values of the heterogenous charge transfer constant, k₀. Higher k₀ values were observed for carbon blacks than for investigated biochar samples. The detection of 4-nitrophenol and heavy metal ions was used to assess the applicability of biochars for electroanalytical purposes. The response of untreated biochar was comparable with the response of Vulcan carbon black, which showed the best response of all analyzed carbon blacks. Full article

Volcanic rock is a natural mineral material which has garnered interest for its potential application in water treatment due to its unique physicochemical properties. In this study, we prepared a polysilicate aluminum chloride (PSAC) coagulant using volcanic rock which exhibited good coagulation–flocculation performance. Further investigation into the influence of synthetic parameters, such as calcination temperature, reaction time, and alkali types, on the structure and performance of a volcanic rock-derived coagulant was conducted. Techniques including Scanning Electron Microscopy, Energy-Dispersive Spectroscopy, Fourier-Transform Infrared Spectroscopy, and X-Ray Diffraction were utilized to characterize it. Also, a ferron-complexation timed spectrophotometric method was used to study the distribution of aluminum species in the coagulant. Results indicated that the volcanic rock that was treated with acidic and alkaline solutions had the potential to form PSAC with Al-OH, Al-O-Si, Fe-OH, and Fe-O-Si bonds, which influenced the coagulation–flocculation efficiency. An acid leaching temperature of 90 °C, 8 mL of 2 mol/L NaOH, a reaction time of 0.5 h, and a reaction temperature of 60 °C were conducive to the preparation. A higher temperature could result in a higher proportion of Alb species, and, at 100 °C, the Ala, Alc, and Alb were 29%, 24%, and 47%, respectively, achieving a residual turbidity lower than 1 NTU at an appropriate dosage, as well as a reduction of over 0.1 to 0.018 in the level of UV₂₅₄. The findings of this study provide a feasible method to prepare a flocculant using volcanic rock. Further application is expected to yield good results in wastewater/water treatment. Full article

Poly(acrylic acid) (PAA) and hydroxypropylcellulose (HPC) hydrogels were synthesized in the absence of a crosslinker. Chemical crosslinking between PAA and HPC was demonstrated through free radical polymerization by a precipitation reaction in acetone as the solvent. These hydrogels exhibited smaller swelling ratios (1 to 5 g H₂O/g) than homo PAA hydrogels synthesized in water as the solvent. They were swollen in a 0.1 M NaOH solution and subsequently used to remove Ni²⁺ ions from aqueous solutions with concentrations ranging from 1000 to 4000 ppm. The absorption capacity of these hydrogels ranged from 91 to 340 mg of Ni²⁺/g in a rapid 1 h process, and from 122 to 435 mg of Ni²⁺/g in a 24 h process, demonstrating an improvement in Ni²⁺ absorption compared to previously reported hydrogels. The colored 1000 and 2000 ppm Ni²⁺ solutions became clear after treatment, while the PAA-HPC hydrogels turned green due to the uptake of Ni²⁺ ions, which were partially chelated by carboxylate groups as nickel polyacrylate and partially precipitated as Ni(OH)₂, resulting in an average absorption efficiency of 80%. The hydrogel was able to release the absorbed Ni²⁺ upon immersion in an HCl solution, with an average release percentage of 76.4%, indicating its potential for reuse. These findings support the use of PAA-HPC hydrogels for cleaning Ni²⁺-polluted water. The cost of producing 1 g of these hydrogels in laboratory conditions is approximately 0.2 USD. Full article

This study addresses the challenge of chitosan (CS) being difficult to dissolve in water due to its highly ordered crystalline structure. Chitosan is modified with chloroacetic acid to reduce its crystallinity and enhance its water solubility. Through single-factor experiments, the optimal conditions for preparing carboxymethyl chitosan film (CMCS) were determined: under conditions of 50 °C, a cellulose substrate (CS) concentration of 18.75 g/L, a NaOH concentration of 112.5 g/L, and a chloroacetic acid concentration of 18.75 g/L, the reaction proceeded for 5 h. Under these conditions, the resulting carboxymethyl chitosan film exhibited the best flocculation effect, forming chitosan films in water that had flocculation activity toward mung bean starch protein wastewater. The successful introduction of carboxyl groups at the N and O positions of the chitosan molecular chain, which reduced the crystallinity of chitosan and enhanced its water solubility, was confirmed through analysis using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The prepared carboxymethyl chitosan film (CMCS) was applied in the flocculation recovery of protein. Through single-factor and response surface experiments, the optimal process conditions for flocculating and recovering protein with CMCS were determined: a CMCS dosage of 1.1 g/L, a reaction time of 39.6 min, a reaction temperature of 42.7 °C, and a pH of 5.2. Under these conditions, the protein recovery rate reached 56.97%. The composition and amino acid profile of the flocculated product were analyzed, revealing that the mung bean protein flocculated product contained 62.33% crude protein. The total essential amino acids (EAAs) accounted for 52.91%, non-essential amino acids (NEAAs) for 47.09%, hydrophobic amino acids for 39.56%, and hydrophilic amino acids for 12.67%. The ratio of aromatic to branched-chain amino acids was 0.31, and the ratio of basic to acidic amino acids was 1.68. These findings indicate that the recovered product has high surface activity and good protein stability, foaming ability, and emulsifying properties. Full article

This paper presents the synthesis of La₂Ti₂O₇ nanoparticles by the sol–gel method starting from lanthanum nitrate and titanium alkoxide (noted as LTA). Subsequently, the lanthanum titanium oxide nanoparticles are modified with noble metals (platinum) using the chemical impregnation method, followed by a reduction process with NaBH₄. The comparative analysis of the structure and surface characteristics of the nanopowders subjected to thermal treatment at 900 °C is conducted using Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray fluorescence (XRF), ultraviolet-visible (UV–Vis) spectroscopy, as well as specific surface area and porosity measurements. The photocatalytic activity is evaluated in the oxidative photodegradation of ethanol (CH₃CH₂OH) under simulated solar irradiation. The modified sample shows higher specific surfaces areas and improved photocatalytic properties, proving the better conversion of CH₃CH₂OH than the pure sample. The highest conversion of ethanol (29.75%) is obtained in the case of LTA-Pt after 3 h of simulated solar light irradiation. Full article

The use of construction and demolition waste (CDW) as an alternative binder to ordinary Portland cement presents a promising solution through alkaline activation. This study evaluates the physical, mechanical, and microstructural behaviour of pastes and mortars produced with CDW—specifically concrete (RH) and ceramic (RC) waste—activated with NaOH and Na₂SiO₃ (SS) solutions. Mortars were prepared with NaOH/SS ratios of 0.2 and 0.3 and an activator-to-precursor (AA/P) ratio of 0.2. Results showed that higher NaOH content accelerated alkaline activation, reducing setting times from 6.2 h to 3.7 h for RC and from 4.6 h to 3.2 h for RH. Conversely, increasing Na₂SiO₃ content led to greater drying shrinkage, from −0.42% to −0.49% in RC and from −0.46% to −0.52% in RH. Compressive strength values at 28 days ranged from 7.6 to 8.2 MPa. X-ray diffraction (XRD) revealed the presence of non-reactive crystalline phases in both precursors, while Fourier transform infrared (FTIR) spectroscopy indicated the formation of CASH, CSH, and/or (N)CASH gels. This study highlights the potential of CDW as a sustainable alternative binder and the usefulness of the proposed method for optimising alkali-activated systems, contributing to circular economy strategies in the construction sector. Full article

This study presents the influence of pH control agents and pH value on the physical properties of ZnO thin films obtained by chemical bath deposition. ZnO thin films were synthesized on glass substrates using precursor solutions of different pHs prepared from two bases: sodium hydroxide (NaOH) and ammonia (NH₃). The effect of pH values on the morphological, structural, and optical properties of ZnO thin films was investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and UV–Visible spectroscopy. XRD results showed that all the synthesized ZnO thin films are polycrystalline and crystallize in a hexagonal wurtzite structure. The crystallite size, calculated using the Debye–Scherrer formula, varied from 10.50 nm to 11.69 nm for ZnO thin films obtained with NH₃ and from 20.79 nm to 27.76 nm for those obtained with NaOH. FTIR analysis confirmed the presence of functional groups. SEM images indicated that not only the base but also the pH affects the morphology of the films, giving rise to different granular shapes. Overall, the ZnO thin films obtained with NaOH looked more mesoporous compared to those obtained with NH₃. Optical characterization results showed that whatever the base used, the pH of the precursor solution affected the ZnO thin film transmittance. Films synthesized with NH₃ exhibited the best transmittance (80%) at pH 8.5, while the best transmittance (81%) of films synthesized with NaOH was obtained at pH 8 in the visible region. Based on optical and morphological properties, ZnO films obtained from NH₃ at pH 8.5 are found to be more suitable as photoanodes in dye-sensitized solar cells. Full article

Nanotechnology, specifically magnetic nanoparticles (MNPs), is revolutionizing cancer treatment. Magnetic hyperthermia is a treatment that, using MNPs, can selectively kill cancer cells without causing damage to the surrounding tissues. Background/Objectives: This work aimed to analyze how the synthesis conditions, namely, how the pH of the reaction can influence the magnetic properties of Fe₃O₄ nanoparticles for magnetic hyperthermia, using the hydrothermal synthesis. Methods: For the hydrothermal synthesis, FeCl₃·6H₂O and FeCl₂·4H₂O were mixed with different quantities of NaOH to adjust the pH. After obtaining a black precipitate, the samples were placed in an autoclave at 200 °C for 60 h, followed by a washing and drying phase. The obtained MNPs were analyzed using X-Ray Diffraction (XRD), Transmission Electron Microscopy, a Superconducting Quantum Interference Device, Specific Absorption Rate analysis, and cytotoxicity assays. Results: Different MNPs were analyzed (9.06 < pH < 12.75). The XRD results showed the presence of various iron oxide phases (magnetite, maghemite, and hematite), resulting from the oxidization of the iron phases present in the autoclave. In terms of the average particle size, it was verified that, by increasing the pH value, the size decreases (from 53.53 nm to 9.49 nm). Additionally, MNPs possess a superparamagnetic behaviour with high SAR values (above 69.3 W/g). Conclusions: It was found that the pH of the reaction can influence the size, morphology, magnetization, and thermal efficiency of the MNP. The MNP with the highest composition of Fe₃O₄ was synthesized with a pH of 12.75, with a cubic morphology and a SAR value of 92.7 ± 3.2 W/g. Full article

A novel bioactive glass–ceramic was developed using biogenic hydroxyapatite (BHA) synthesized from Rapana venosa (Black Sea) shells and monocalcium phosphate monohydrate [Ca(H₂PO₄)₂·H₂O] via solid-state synthesis. The prepared batches were obtained by combining BHA with SiO₂, B₂O₃, and Na₂O, melted at 1200 °C and melt-quenched in water to form glass–ceramic materials. Dense biogenic hydroxyapatite-based ceramics were successfully sintered at 1200 °C (2 h hold) using a 25 mass % sintering additive composed of 35 mass % B₂O₃, 45 mass % SiO₂, 10 mass % Al₂O₃, and 10 mass % Na₂O. Structural characterization was carried out using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The resulting materials consisted of a well-defined crystalline hydroxyapatite phase [Ca₁₀(PO₄)₆(OH)₂] alongside an amorphous phase. In samples with increased SiO₂ and reduced B₂O₃ content (composition 3), a finely dispersed Na₃Ca₆(PO₄)₅ crystalline phase appeared, with a reduced presence of hydroxyapatite. Bioactivity was assessed in simulated body fluid (SBF) after 10 and 20 days of immersion, confirming the material’s ability to support apatite layer formation. The main structural units SiO₄, PO₄, and BO₃ are interconnected through Si–O–Si, B–O–B, P–O–P, and mixed Si–O–Al linkages, contributing to both structural stability and bioactivity. Full article

This study presents a novel, eco-friendly synthesis route for zinc oxide (ZnO) nanoparticles using cladode extracts of Hylocereus undatus acting simultaneously as reducing and improving agents, in alignment with green chemistry principles. The synthesis involved the reaction of zinc sulfate heptahydrate with the plant extract, with the medium pH adjusted using sodium hydroxide (NaOH), followed by calcination at 300 °C, 400 °C, and 500 °C, and then by a washing step to enhance purity. Comprehensive characterization was performed using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and electrical impedance spectroscopy to investigate the structural, morphological, and dielectric properties of the nanoparticles. The sample calcined at 400 °C, followed by washing (HT400W), exhibits highly crystalline ZnO nanoparticles with a predominant wurtzite structure (93.15 wt% ZnO) and minimal impurities (6.85 wt% Na₂SO₄). SEM analysis indicated a flake-like morphology with nanoscale features (50–100 nm), while Raman spectroscopy confirmed enhanced crystallinity and purity post-washing. Additionally, the HT400W sample exhibited a dielectric constant (ε′) of 16.96 and a low loss tangent (tan δ) of 0.14 at 1 MHz, suggesting superior energy efficiency for high-frequency applications. This green synthesis approach not only eliminates hazardous reagents but also delivers ZnO nanoparticles with good dielectric performance. Furthermore, this work demonstrates the efficacy of a sustainable biotemplate, offering an environmentally friendly approach for synthesizing ZnO nanoparticles with tailored physicochemical properties. Full article

To enhance the signal intensity of kynurenines, which are present at trace concentrations in biological fluids, a novel analytical approach was developed, combining pressure-assisted electrokinetic injection (PAEKI) with a mixed micelle system based on sodium dodecyl sulfate (SDS) and Brij-35. The method was applied to key compounds of the kynurenine pathway, including L-tryptophan, kynurenine, 3-hydroxykynurenine, and kynurenic acid, as well as to the aromatic amino acids (AAs) L-tyrosine and L-phenylalanine. PAEKI was performed by electrokinetic injection for 2 min at −6.5 kV (reversed polarity) and 0.5 psi (3.45 kPa) using a fused silica capillary (50 cm in length, 50 µm inner diameter). The background electrolyte (BGE) consisted of 20 mM Na₂B₄O₇ (pH 9.2), 2 mM Brij-35, 20 mM SDS, and 20% (v/v) methanol (MeOH). The limit of detection (LOD) using a diode array detector (DAD) was 1.2 ng/mL for kynurenine and ranged from 1.5 to 3.0 ng/mL for the other analytes. The application of PAEKI in conjunction with micellar electrokinetic capillary chromatography (MEKC) and solid-phase extraction (SPE) of artificial urine samples resulted in a 146-fold increase in signal intensity for kynurenines compared to that observed using the hydrodynamic injection (HDI) mode. The developed method demonstrates strong potential for determining kynurenine pathway metabolites in complex biological matrices. Full article

Recently, the development of nanoparticle pigments has attracted interest in chemical preparation due to their potential functional properties, such as phosphate-based pigments. The present research focuses on the feasibility of synthesising the BaCr₂(P₂O₇)₂ pigment under hydrothermal conditions. The effect of the microstructural features of ceramic pigments (the crystalline structure, morphology, and particle size) on their optical properties (colour and reflectance) was also studied. The BaCr₂(P₂O₇)₂ compound was prepared in different fluid media, including water and NaOH solutions (0.5–1.0 M), at several reaction temperatures (170–240 °C) and intervals (6–48 h). The single-phase BaCr₂(P₂O₇)₂ did not crystallise without by-products (BaCr₂O₁₀, BaCr₂(PO₇)₂) in water and the alkaline solutions, even at 240 °C for 48 h; in these fluids, the ionic Cr³⁺ species oxidised to Cr⁶⁺. In contrast, the BaCr₂(P₂O₇)₂ single-phase crystallisation was favoured by adding urea as a reductant agent (25.0–300.0 mmol). Monodispersed BaCr₂(P₂O₇)₂ fine particles with a mean size of 44.0 nm were synthesised at a low temperature of 170 °C for 6 h with 0.5 M NaOH solution in the presence of 50.0 mmol urea. The phosphate pigment particle grew to approximately 62.0 nm by increasing the treatment temperature to 240 °C. A secondary dissolution–recrystallisation achieved after 24 h triggered a change in the particle morphology coupled with the incrementation of the concentration of NaOH in the solution. The pyrophosphate BaCr₂(P₂O₇)₂ pigments prepared in this study belong to the green colour spectral space according to the CIELab coordinates measurement, and exhibit 67.5% high near-infrared (NIR) solar reflectance. Full article

The equivalent conductivities of two aqueous silicate species, ${\left[\mathrm{SiO}{\left(\mathrm{OH}\right)}_3\right]}^{-}$ and ${\left[\mathrm{Si}{\mathrm{O}}_2{\left(\mathrm{OH}\right)}_2\right]}^{2-}$, are fundamental to understanding many physico-chemical phenomena of silicate materials in electrolyte solutions. These phenomena include diffusion, adsorption, and phase transformations. But significant inconsistencies have been presented in published equivalent conductivities of the two silicate aqueous ions. Also, little work has so far been undertaken to discuss how aspects, such as temperature and solution composition, may influence electrolytic conductivity of silicate aqueous solutions. This work presents the equivalent conductivities of the two silicate species, measured with electrochemical impedance spectroscopy (EIS) from 277.85 K to 308.45 K. A conductivity model for mixed electrolytes of high alkaline was first established. This model was then verified with the electrolyte conductivities of $\mathrm{NaOH}\text{-}{\mathrm{H}}_2\mathrm{O}$ solutions and $\mathrm{NaOH}\text{-}\mathrm{N}{\mathrm{a}}_2\mathrm{C}{\mathrm{O}}_3\text{-}{\mathrm{H}}_2\mathrm{O}$ solutions. Next, the equivalent conductivities of ${\left[\mathrm{SiO}{\left(\mathrm{OH}\right)}_3\right]}^{-}$ and ${\left[\mathrm{Si}{\mathrm{O}}_2{\left(\mathrm{OH}\right)}_2\right]}^{2-}$, were calculated by solving the overdetermined equation groups for different temperatures, based on electrolyte conductivities of $\mathrm{NaOH}\text{-}\mathrm{N}{\mathrm{a}}_2\mathrm{Si}{\mathrm{O}}_3\text{-}{\mathrm{H}}_2\mathrm{O}$ solutions. The accuracy of both calculations and measurements are examined in depth from various viewpoints. This work presents essential inputs for quantitatively understanding multiple physico-chemical properties of silicate materials in electrolyte solutions. Full article

An integrated process scheme is developed for valorizing filtered liquid digestates (FLD) from an industrial anaerobic digestion (AD) plant treating dairy-processing effluents with relatively low nutrient concentrations. The process scheme involves FLD treatment by nanofiltration (NF) membranes, followed by struvite recovery from the NF-retentate. An NF pilot unit (designed for this purpose) is combined with a state-of-the-art NF/RO process simulator. Validation of simulator results with pilot data enables reliable predictions required for scaling up NF systems. The NF permeate meets the standards for restricted irrigation and/or reuse. Considering the significant nutrient concentrations in the NF retentate (i.e., ~500 mg/L NH4-N, ~230 mg/L PO4-P), struvite recovery/precipitation is investigated, including determination of near-optimal processing conditions. Maximum removal of nutrients, through production of struvite-rich precipitate, is obtained at a molar ratio of NH₄:Mg:PO₄ = 1:1.5:1.5 and pH = 10 in the treated stream, attained through the addition of Κ₂HPO₄, ΜgCl₂·6H₂O, and NaOH. Furthermore, almost complete struvite precipitation is achieved within ~30 min, whereas precipitate/solid drying at modest/ambient temperature is appropriate to avoid struvite degradation. Under the aforementioned conditions, a significant amount of dry precipitate is obtained, i.e., ~12 g dry mass per L of treated retentate, including crystalline struvite. The approach taken and the obtained positive results provide a firm basis for further development of this integrated process scheme towards sustainable large-scale applications. Full article

The construction industry generates large amounts of waste and high CO₂ emissions, especially from cement production. Sustainable alternatives, such as geopolymers, help reduce these impacts by promoting eco-friendly materials. This study aimed to develop geopolymer mortar using ignimbrite (IG) residues from the Arequipa region, Peru, combined with metakaolin (MK). The raw materials were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS) to assess the chemical composition, structure, and morphology. Geopolymeric mortars were synthesized with varying MK/IG ratios while maintaining a fixed fine sand proportion. An activating solution of 9 mol/L NaOH was used with different liquid-to-solid ratios. Geopolymers cured at room temperature for 28 days exhibited lower compressive strength than those dried at 50 °C for 48 h or sequentially at 50 °C for 48 h followed by 90 °C for 12 h. The highest IG-content mixture achieved a compressive strength of 18 MPa, while the MK-based geopolymer reached 12 MPa, both under high-temperature curing. An increase in the SiO₂/Al₂O₃ molar ratio was also associated with improved mechanical performance, reinforcing the influence of precursor composition on geopolymerization. These results highlight the potential of regional ignimbrite for the production of geopolymer mortar, promoting sustainable and innovative building materials. Full article