Search Results (490)

Electric discharge cavitation is an effective method for water treatment that combines physical and chemical effects within a single process. It enables water disinfection, extraction acceleration, dispersion of solid particles, and enhancement of porous material permeability. Compared to conventional chemical treatment, it reduces the demand for reagents and minimizes secondary pollution. This new and developing technology significantly contributes to the preservation of natural aquatic ecosystems by providing a sustainable alternative to traditional decontamination methods, thereby reducing the overall anthropogenic pressure on the environment. This study focuses on developing a reliable method for assessing electric discharge cavitation intensity and controlling water purification processes. The proposed approach is based on the oxidation of iodide ions to molecular iodine by reactive species generated during electric discharge cavitation. The adapted iodometric method is sensitive, reproducible, and does not require complex optical or acoustic equipment. Experimental results confirmed that iodometry provides an accurate evaluation of cavitation intensity, allowing control of specific energy consumption and optimization of treatment parameters. Optimal operating conditions were established to control the water processing by electric discharge cavitation: stainless-steel electrodes, specific input energy not exceeding 280 kJ·L⁻¹, the presence of a free liquid surface in the working chamber, and a discharge pulse frequency below 10 Hz. The proposed method supports the development of energy-efficient, low-waste technologies for wastewater and natural water treatment and facilitates the integration of electric discharge systems into existing water treatment infrastructure, particularly under resource-limited conditions. Full article

Total nitrogen (TN) is a critical indicator of water eutrophication. Conventional detection methods (e.g., alkaline potassium persulfate digestion and the Kjeldahl method) suffer from complex sample preparation, time-consuming operations, and reagent-induced pollution. Laser-induced breakdown spectroscopy (LIBS) offers unique advantages for rapid water quality analysis, yet it predominantly relies on costly actively Q-switched lasers, with passive Q-switching rarely explored due to multi-pulse output instability. This study employed a passively Q-switched laser as the excitation source for water TN measurement. By optimizing the multi-pulse trigger position, the signal-to-background ratio (SBR) was effectively enhanced. Combined with the substrate liquid–solid conversion method, key parameters (trigger delay, laser energy, argon flow rate) were optimized. Laboratory measurements of KNO₃ standard solutions (0–25 mg/L) using cyanogen (CN) molecular spectral lines yielded a coefficient of determination (R²) of 0.98, and a limit of detection (LoD) of 2.19 mg/L. Tests on actual water samples showed relative deviations ranging from 3.93% to 6.39%. These results demonstrate that passively Q-switched LIBS is a viable, cost-effective solution for rapid water nitrogen detection. Full article

A robust Folin–Ciocalteu method, coupled with an optimized ultrasonic-assisted extraction, was established for accurate quantification of total polyphenols in high-oil grape seed matrices, where lipid interference and low extraction efficiency have been persistent challenges. Samples were first defatted with n-hexane to eliminate lipid interference. Key colorimetric parameters—Folin–Ciocalteu reagent volume, Na₂CO₃ concentration, reaction temperature, and time—were systematically optimized and validated for linearity, precision, and recovery. Subsequently, using defatted grape seed powder as the raw material, a four-factor, three-level Box–Behnken design combined with response surface methodology was employed to optimize the four extraction parameters: solid-to-liquid ratio, ethanol concentration, extraction temperature, and extraction time. The optimal conditions were 0.5 mL of Folin–Ciocalteu reagent, 20% Na₂CO₃, and reaction at 30 °C for 2.0 h, yielding a linear calibration curve (R² = 0.9991) with satisfactory methodological validation. Optimal extraction (52% ethanol, 1:50 w/v, 68 °C, 21 min) achieved a total polyphenol content of 2.93 × 10⁴ mg·kg⁻¹, closely matching the predicted value (relative error = 0.34%). Analysis of seven grape seed varieties from the Hebei Province revealed significant content variation (p < 0.05), ranging from 3.24 to 7.47 × 10⁴ mg·kg⁻¹, with Rose grape seeds exhibiting the highest level. The developed method effectively overcame matrix interference from high oil content, offering a reliable, efficient tool for screening high-polyphenol grape seed varieties and supporting the development of value-added functional products. Full article

The endosperm of Gleditsia japonica var. delavayi seeds is a valued medicinal and edible material, rich in polysaccharides exhibiting excellent functional properties for food applications. However, conventional methods for extracting Gleditsia japonica var. delavayi polysaccharides (GJP) are often inefficient and environmentally unfriendly. Thus, we developed a green, ultrasound-assisted process for extracting GJP. We systematically optimized key parameters (liquid-solid ratio and ultrasonic time, temperature, and power) using single-factor, Plackett–Burman and Box–Behnken experimental designs to maximize yield and characterize the product. The optimized process (200 mL/g, 62 min, 51 °C and 180 W) exhibited an extraction yield of 76.11%, producing GJP with a purity of 79.89%, which satisfies standards for food additives. The extracted GJP exhibited a semi-crystalline structure, high solubility (80.06%), low esterification degree (2.60%) and high viscosity and thermal stability between 30 °C and 70 °C. Crucially, this process required no chemical reagents and consumed only 0.18 kW·h of energy. Analysis indicates that the optimized ultrasound-assisted extraction of GJP is a green and efficient method with high extraction rates and reduced processing time and energy consumption; furthermore, it does not require any chemical reagents, making it a promising alternative to conventional techniques. Full article

Different methods are used today for polysaccharide quantitation, including HPLC and various colorimetric assays. Among these, the anthrone-sulfuric acid assay (anthrone assay) is popular when the sample matrix is suitable, such as in purified polysaccharides and monovalent bulk conjugate components of glycoconjugate vaccines. While relatively safe, quick, and affordable, the anthrone assay requires significant operator time to complete and is not suited to high-throughput processing. Furthermore, the anthrone-sulfuric acid reagent presents a unique challenge to automation efforts due to its corrosive properties. Reported here is an automated anthrone assay via a liquid handling system (LHS). Twenty-three serotypes of pneumococcal (PNU) polysaccharide were quantified with the traditional anthrone assay and subsequently analyzed using the anthrone LHS method. The anthrone LHS method was evaluated for accuracy compared to the manual method and later validated according to ICH Q2 (R2) guidelines. To our knowledge, this is the first fully unattended and corrosion-mitigated anthrone assay validated under ICH Q2 (R2), capable of overnight batch operation. The developed assay can quantify polysaccharides with an accuracy of 81–115%, is precise to a coefficient of variation of <7.0%, and is linear between 30 and 650 µg/mL range (R² ≥ 0.993). The assay can process eight samples per hour, can be utilized in overnight operation, and completes all pipetting, incubation, and data export steps automatically. Full article

High-ash coal slime water, characterized by its stable colloidal suspension of fine kaolinite particles, poses a significant challenge in the coal preparation industry because it is hard to achieve efficient solid–liquid separation. While traditional coagulants and flocculants often suffer from limited bridging capabilities and distinct pH sensitivity, novel molecular architectures offer potential solutions. In this study, a star-shaped inorganic–organic hybrid flocculant (Al-PAM) was synthesized via in situ polymerization. Its flocculation performance and interfacial adsorption mechanism on the specifically targeted aluminol basal plane of kaolinite were systematically investigated and compared with Polyaluminum Chloride (PAC), Non-ionic Polyacrylamide (NPAM), and their combination (PAC + NPAM). Settling tests revealed that Al-PAM exhibited superior performance at a significantly lower dosage (10 mg∙L⁻¹) compared to the PAC + NPAM binary reagent system. It achieved a rapid initial settling velocity and reduced the supernatant turbidity to 48.45 NTU, while maintaining a near-neutral pH favorable for water recycling. Furthermore, Quartz Crystal Microbalance with Dissipation (QCM-D) monitoring confirmed that Al-PAM forms a thick, viscoelastic, and irreversible adsorption layer on the Al₂O₃ substrate. The dissipation shifts (ΔD) revealed that the star-shaped architecture promotes distinct bridging and electrostatic adsorption, overcoming the limitation of linear polymers. This work elucidates the specific contribution of the alumina-surface interaction with flocculants and proposes an efficient strategy for treating refractory coal slime water. Full article

Non-thermal plasma-driven advanced oxidation is a promising method for treating organic wastewater, which exhibits rapid reaction kinetics and high pollutant removal and does not need chemical reagents. However, its practical application is often limited by high specific energy consumption and the inefficient mass transfer of short-lived reactive species across the gas–liquid interface. This review summarizes the fundamentals of non-thermal plasma chemistry and the process intensification of plasma multiphase reactors by mass transfer enhancement and waste energy-driven conversion. This review focus on four coupling approaches: microbubble-assisted plasma to expand the reactive interfacial area; plasma coupled with hydraulic cavitation to enhance convection and radical formation; plasma–piezoelectric catalysis coupling to harvest hydraulic energy and promote charge-driven reactions; and plasma-assisted Fenton oxidation to improve the utilization of weakly oxidizing species (H₂O₂). The energy efficiency of various plasma-based oxidation systems is compared and discussed clearly. Key remaining challenges are also discussed, including standardized energy efficiency assessment, scale-up and hydrodynamic control, catalyst stability and fouling, by-product formation and toxicity, and long-term operational reliability. Overall, this review aims to provide guidance for developing efficient plasma-based wastewater treatment systems for large-scale applications. Full article

This paper presents the results of a laboratory-based treatability study conducted for a confidential former wood treating site heavily impacted by a creosote non-aqueous-phase liquid (NAPL) containing pentachlorophenol (PCP). PCP impacts in the silty sands extended to approximately 33 ft (10 m) below the ground surface (bgs), with discrete soil samples containing PCP concentrations up to 14,500 mg/kg, and groundwater PCP concentrations forming a main plume exceeding 1 mg/L over 2.16 acres (0.87 ha). Treatability testing was performed on unspiked and NAPL-spiked site soils with total PCP concentrations ranging from 10 to 100 mg/kg, respectively, and leachable PCP concentrations of approximately 3 to 8 mg/L. Stabilization/solidification (S/S) mix designs using 5 to 10 weight percent (wt%, dry-reagent-to-wet-soil mass basis) of a Portland cement (PC) blend and 1 wt% powdered bentonite met the minimum unconfined compressive strength (UCS) and maximum hydraulic conductivity (K) performance criteria of 50 lb/in2 (345 kPa) and 1 × 10⁻⁶ cm/s, respectively, within the specified 28-day cure time. Long-term semi-dynamic leach testing was performed on S/S-treated soils using a modified United States Environmental Protection Agency (EPA) Method 1315 test incorporating a polydimethylsiloxane (PDMS) liner to improve the data reliability for hydrocarbons. Results showed that adding 1 wt% organoclay (OC) to the S/S mix designs did not substantially reduce leaching of common semi-volatile organic compounds (SVOCs) such as naphthalene, acenaphthene, phenanthrene and benzo(a)anthracene compared to mixes using only the PC blend with bentonite, consistent with previous studies. However, the inclusion of OC had a decisive effect on PCP immobilization, providing an order-of-magnitude (10×) reduction in the cumulative mass release of PCP over the test duration. This benefit diminished with decreasing degree of chlorination for other phenolic compounds. Full article

This study reports the synthesis and catalytic evaluation of a series of imidazolium-based polymeric ionic liquids (PILs) for the cycloaddition of CO₂ to epichlorohydrin (ECH). The synthesized catalysts include homopolymers, poly(3-hydroxyethyl-1-vinylimidazole chloride) (p[HVIm][Cl]) and poly(3-carboxymethyl-1-vinylimidazole chloride) (p[CMVIm][Cl]), and their block copolymers with polystyrene, synthesized for the first time, pS-b-p[HVIm][Cl] and pS-b-p[CMVIm][Cl]. Structural characterization by NMR, IR spectroscopy, and gel permeation chromatography confirmed the successful synthesis. The block copolymers exhibited a low polydispersity index (PDI 1.1–1.2), which is indicative of homogeneous chain lengths and the propensity to form ordered nanostructures, whereas the homopolymers showed higher PDI (2.4–2.9). Catalytic testing at 90 °C and 1 MPa CO₂ for 4 h revealed a clear activity trend: p[CMVIm][Cl] < p[HVIm][Cl] < pS-b-p[CMVIm][Cl] < pS-b-p[HVIm][Cl], with conversions exceeding 75% for all catalysts and a maximum of 82.69% for pS-b-p[HVIm][Cl]. These results demonstrate that the catalytic performance of PILs is governed by a synergistic interplay between the local chemical functionality of the ionic moiety and the overall polymer architecture. Based on these results, the synthesized polymeric ionic liquids, particularly pS-b-p[HVIm][Cl], demonstrate strong potential for creating multifunctional materials. Their ability to self-assemble into ordered nanostructures with distinct hydrophobic and hydrophilic domains provides a foundational architecture for combined gas separation and catalysis. The observed “micellar catalytic effect”, which enhances local reagent concentration near active sites, could be leveraged in a membrane reactor to simultaneously capture and convert CO₂ directly within the membrane. This integrated “separation–reaction” approach represents a promising strategy for advancing circular carbon economy technologies. Full article

Ibuprofen (IBU), paracetamol (PARA), and diclofenac (DIC) are three of the most used non-opioid analgesics and are most frequently detected in the environment. Some methods to analyze these compounds in water have been previously reported, but they have limitations such as long analysis time, high reagent consumption, and lack of sensitivity. An electrospray ionization high-performance liquid chromatography–mass spectrometry (ESI-HPLC-MS/MS)-based method was developed for the determination of these analgesics, applying 3D printing to improve the extraction process. The method was validated and applied to quantify the target pharmaceuticals using commercial tablets. For PARA and DIC, a gradient elution with 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) was employed. For the analysis of IBU, an isocratic elution with 10 mM acetate in water (A) and acetonitrile (B) was used. ESI-MS/MS spectra were obtained in positive polarity to identify DIC and PARA, while negative polarity was used for IBU. LOD were 40.91, 3.64, and 1.96, and the LOQ were 136.36, 12.15, and 6.52 ng/L for IBU, PARA, and DIC, respectively. R² was >0.99 and RSD < 10% in all cases. The 3D-printed extraction device can be used for up to 10 cycles. This method demonstrated a remarkable performance compared to previous studies, mainly in terms of precision (RSD = 0.6–4.16%), mobile phase consumption (4 mL), and analysis time (<7 min), and was applied in the analysis of surface water samples. Full article

The current state and prospects of microreactor synthesis of functional materials in single- and two-phase flows with a liquid continuous phase are analyzed. Microreactors allow fine control over the size, composition, structure, and properties of synthesized particles in co-precipitation processes. The results obtained by various teams provide grounds to expect fairly extensive capabilities for controlling the processes of nucleation and particle growth in microreactors—by controlling the pH, reagent concentrations, micromixing quality, and residence time in each of the reactor zones—in the nucleation growth zones. The advantages of microreactor synthesis have been demonstrated with a high quality of micromixing in a volume of 0.2–0.5 mL, which ensures the production of nanoparticles without impurities, a stoichiometric ratio of atoms in the product, and limitation of agglomerate growth due to a short residence time (in the order of several milliseconds). The transition to an industrial scale is very easy due to the fairly high productivity of a single microreactor (up to 10 m³/day for suspension, up to 200–300 kg/day for solid phase). Intensive mixing in microreactors with a diameter of 2–4 mm or less, due to Taylor vortices, contributed to the use of two-phase microreactors for the synthesis of both organic and inorganic substances. Full article

[^99mTc]sestamibi ([^99mTc][Tc(MIBI)₆]⁺; MIBI = 2-methoxybutylisonitrile) is a clinically established myocardial perfusion SPECT tracer. Its one-pot kit-based synthesis from [^99mTc]pertechnetate ([^99mTc][TcO₄]⁻) is complex, involving a 6-oxidation state transition (Tc(VII) to Tc(I)) and complete ligand replacement. We aimed to unravel this complex reaction, to inform rational quality control and identify new technetium synthons for molecular imaging. Generator-produced [^99mTc]pertechnetate was added to commercial or bespoke clinically used kits, varying the reaction time, temperature, and concentrations of reagents (individually and collectively) and carrier technetium-99. Radioactive products were analysed by thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) with optical, radiometric, and mass spectrometric (MS-ESI+) detection. At least 11 radioactive intermediates were detected by radio-HPLC. Technetium(V) and technetium(I) intermediates were identified or imputed by radio-HPLC-MS, including [Tc^VO(cysteinate)₂]⁺, [Tc^I(MIBI)₄L₂]⁺, and [Tc^I(MIBI)₅L₁]⁺ (L = labile monodentate ligand, e.g., H₂O). Tc(III) intermediates [Tc^III(cysteinate)₂(MIBI)]⁺ and [Tc^III(cysteinate)₂(MIBI)₂]⁺ were indicated by weak MS-ESI+ ions. We conclude that the reaction proceeds via reduction from [Tc^VIIO₄]⁻ via unknown intermediates to [Tc^VO(cysteinate)₂]⁺, then via Tc(III) intermediates containing both cysteinate and MIBI ligands (e.g., [Tc^III(cysteinate)₂(MIBI)₂]⁺), to form Tc(I) without cysteine and with <6 MIBI ligands, followed by further ligand displacement by MIBI to form [Tc(MIBI)₆]⁺. Once formed, [Tc(MIBI)₆]⁺ undergoes no further reaction. Full article

The aim of this study was to evaluate, on a preliminary basis, the ability of multivariate techniques to predict the antioxidant activity of selected Stachys and Betonica species, based on chromatographic data. The methanol extracts of six Stachys species and ten Betonica species were analyzed using reversed-phase high-performance liquid chromatography (RP-HPLC) to obtain their chromatographic profiles. The phytochemical similarity of the samples was assessed using a selected chemometric method (principal component analysis (PCA) and hierarchical cluster analysis (HCA)). The antioxidant activity of the studied extracts (DPPH with 2,2-diphenyl-1-picrylhydrazyl reagent and FRAP—ferric reducing antioxidant power) was determined using a spectrophotometric technique. A multivariate PLS model was then used to predict the antioxidant activity of the methanolic extracts of Stachys and Betonica species based on their RP-HPLC fingerprints. The two obtained PLS models proved useful for predicting the biological activity of the tested extracts. High correlation coefficients (DPPH: R² = 0.9963; FRAP: R² = 0.9895) confirmed the reliability of the PLS prediction model. The results confirmed the effectiveness of combining qualitative and quantitative chromatographic fingerprinting methods with antioxidant activity testing and chemometric analysis, demonstrating that extracts from Stachys and Betonica are a rich source of bioactive substances with antioxidant properties. Full article

Waste electrical and electronic equipment (WEEE) is a rapidly growing waste stream rich in precious metals, with gold in particular being concentrated in printed circuit boards and other high-value components. Historically, industrial recycling has relied on pyrometallurgy and non-selective hydrometallurgical leaching. These recovery routes have major drawbacks, including high energy demand, corrosion, the use of toxic reagents, and the complexity of pregnant leach solutions, which complicate downstream gold recovery. This review aims to synthesize recent advances in selective gold recovery from WEEE using a speciation-driven approach. Mechanical pretreatment and physical beneficiation methods are critically assessed as processes for concentrating gold and reducing the amount of material sent to downstream hydrometallurgical leaching. Different lixiviants, from conventional cyanide to halide-based, as well as greener chemistries such as thiosulfate and thiourea, are assessed for gold dissolution from the WEEE stream. Assessment of different extraction methods, including sorbents, ion exchange resins, solvent/ionic liquid, direct reduction/precipitation, and electrochemical recovery, is conducted. The review concludes with guidelines for potential process integration and highlights the need for scalable, reusable lixiviants and sorbent materials validated under realistic multi-metal conditions in real WEEE leachate. Full article

Biosurfactants produced by halophilic bacteria are gaining attention as eco-friendly and biocompatible alternatives to synthetic surfactants due to their high surface activity, stability under extreme conditions, and intrinsic antimicrobial properties. These amphiphilic biomolecules hold great promise for bioremediation, biomedical, and pharmaceutical applications. In this study, moderately halophilic bacteria capable of biosurfactant production were isolated from saline mud collected at the Burgas solar salterns (Bulgaria). The halophilic microbiota was enriched in Bushnell–Haas (BH) medium containing 10% NaCl amended with different carbon sources. Primary screening in BH liquid medium evaluated the isolates’ ability to degrade n-hexadecane while at the same time producing biosurfactants. Thirty halophilic bacterial strains were isolated on BH agar plates supplemented with 2% n-hexadecane, 2% olive oil, or 2% glycerol. Four isolates—BS7OL, BS8OL, BS9GL, and BS10HD—with strong emulsifying activity (E₂₄ = 56%) and reduced surface tension in the range of 27.3–45 mN/m were derived after 7 days of batch fermentation. Strain BS10HD was chosen as the most potent biosurfactant producer. Its phylogenetic affiliation was determined by 16S rRNA gene sequence analysis; according to the nucleotide sequence, it was assigned to Halomonas ventosae. The extract material was analysed by thin-layer chromatography (TLC) and Fourier transform infrared spectroscopy (FTIR). Upon spraying the TLC plate with ninhydrin reagent, the appearance of a pink spot indicated the presence of amine functional groups. FTIR analysis showed characteristic peaks for both lipid and peptide functional groups. Based on the observed physicochemical properties and analytical data, it can be suggested that the biosurfactant produced by Halomonas ventosae BS10HD is a lipopeptide compound. Full article