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Ayman El-Faham,1,2 Hessa H Al-Rasheed,1 Essam N Sholkamy,3 Sameh M Osman,1,4 Zeid A ALOthman1,4 1Department of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi Arabia; 2Department of Chemistry, Faculty of Science, Alexandria University, Ibrahimia, Alexandria 21321, Egypt; 3Department of Botany and Microbiology, College of Science, King Saud University, Riyadh 11451, Saudi Arabia; 4Advanced Materials Research Chair, Department of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaCorrespondence: Ayman El-Faham Tel +966114673195Fax +966114675992Email aelfaham@ksu.edu.saPurpose: Simple methodology for preparation of metal nanoparticles such as AgNPs uses an methanolic aqueous medium at room temperature or a solvent-free procedure under microwave irradiation. The prepared AgNPs showed a significant antimicrobial effect against Gram-positive bacteria, Gram-negative bacteria, and fungi.Methods: The modified methoxypolyethylene glycol bishydrazino-s-triazine (mPEGTH2) showed remarkable activity for reducing Ag+ to Ag0 in an aqueous methanolic solution and using a solvent-free method (solid phase) under microwave irradiation. In the solid phase synthesis, the size and shape of the AgNPs can be controlled by varying the weight ratio of mPEGTH2 to AgNO3 used. In addition, the antimicrobial activity depends on the ratio of mPEGTH2 to AgNO3. The mPEGTH2-AgNPs (2:1) demonstrated higher antimicrobial activity compared to mPEGTH2-AgNPs (1:1) against Gram-positive bacteria, Gram-negative bacteria, and C.albicans.Results: This work presents simple methods for the synthesis of AgNPs using modified methoxypolyethylene glycol with bishydrazino-s-triazine (mPEGTH2); a solution method, using methanol-water medium at room temperature, and a solvent-free (solid phase) method, employing microwave irradiation or direct heating which could be used for the preparation of AgNPs on large scale. In the solid phase, ratios of mPEGTH2 to AgNO3 (1:1 or 2:1, respectively) are very important to control the size and shape of AgNPs. While in solution phase is not necessary where the molar ratio used is 10:1. Most of the experimental methods resulted in AgNPs ranging in size from 7 to 10 nm as observed from XRD and TEM characterization. The antimicrobial activity of the AgNPs was also dependent on the weight ratio of mPEGTH2 to AgNO3, with a large effect as observed when using the solvent-free method. The mPEGTH2-AgNPs (2:1) demonstrated higher antimicrobial activities compared to mPEGTH2-AgNPs (1:1) against S. aureus, S. epidermidis, E. faecalis, E. coli, P. aeruginosa, S. typhimurium, and C. albicans. In all cases, the MICs and MBCs of mPEGTH2-AgNPs (1:1) were lower than those of mPEGTH2-AgNPs (2:1).Conclusion: In summary, mPEGTH2-AgNPs (2:1) is a promising candidate to kill pathogenic microbes. In particular, the method used for the preparation of AgNPs by using polyethylene glycol polymer modified with bishydrazino-s-triazine has the most potential and would be the most cost-effective method. This method of the synthesis of nanoparticles may be suitable for the preparation of other metal nanoparticles, which would allow for numerous applications in medicinal and industrial.Keywords: methoxypolyethylene glycol bishydrazino-s-triazine, silver nanoparticles, solution phase, solid phase, antimicrobial activity

Goeun Choi,1 Huiyan Piao,1 Zeid A Alothman,2 Ajayan Vinu,3 Chae-Ok Yun,4 Jin-Ho Choy1 1Center for Intelligent Nano-Bio Materials, Department of Chemistry and Nano Science, Ewha Womans University, Seoul, Korea; 2Advanced Materials Research Chair, Chemistry Department, College of Science, King Saud University, Riyadh, Saudi Arabia; 3Future Industries Institute, University of South Australia, Mawson Lakes, SA, Australia; 4Department of Bioengineering, College of Engineering, Hanyang University, Seoul, Korea Abstract: Methotrexate (MTX), an anticancer agent, was successfully intercalated into the anionic clay, layered double hydroxides to form a new nanohybrid drug. The coprecipitation and subsequent hydrothermal method were used to prepare chemically, structurally, and morphologically well-defined two-dimensional drug-clay nanohybrid. The resulting two-dimensional drug-clay nanohybrid showed excellent colloidal stability not only in deionized water but also in an electrolyte solution of Dulbecco’s Modified Eagle’s Medium with 10% fetal bovine serum, in which the average particle size in colloid and the polydispersity index were determined to be around 100 and 0.250 nm, respectively. The targeting property of the nanohybrid drug was confirmed by evaluating the tumor-to-blood and tumor-to-liver ratios of the MTX with anionic clay carrier, and these ratios were compared to those of free MTX in the C33A orthotopic cervical cancer model. The biodistribution studies indicated that the mice treated with the former showed 3.5-fold higher tumor-to-liver ratio and fivefold higher tumor-to-blood ratio of MTX than those treated with the latter at 30 minutes postinjection. Keywords: anionic clay, biodistribution, cervical cancer, colloidal stability, layered double hydroxide, methotrexate

A bio-composite material was developed that contains chitosan, food-grade algae, and zeolite for the removal of brilliant green (BG) dye. The synthesized bio-composite was dried via two different methods (air-drying; AD, and freeze-drying; FD). The physicochemical characterization of air-dried chitosan-algae-zeolite (Cs-Alg-Zl-AD) and freeze-dried chitosan-algae-zeolite (Cs-Alg-Zl-FD) were investigated by spectroscopy (FTIR, SEM-EDX, and XPS), diffraction (XRD), surface charge via pH pzc , specific surface area (SSA) and elemental analyses. The utilization of Box-Behnken Design (BBD) was intended to optimize the three input variables, which are adsorbent dosage, pH of medium, and contact time. The adsorption optimization process yielded optimal conditions, which were verified through a desirability test and implemented in batch-mode equilibrium experiments. The Cs-Alg-Zl-FD has a higher specific surface area (SSA = 3.29 m 2 /g) compared to Cs-Alg-Zl-AD (SSA = 1.79 m 2 /g). The Cs-Alg-Zl-FD shows greater adsorptive removal of BG (98.6 %) over Cs-Alg-Zl-AD (88.6 %), in parallel agreement with differences in the SSA. Moreover, the maximum BG dye adsorption capacities of Cs-Alg-Zl-FD (119.5 mg/g) and Cs-Alg-Zl-AD (108 mg/g) at pH = 8.1 and 25 °C. The Freundlich model fits best with Cs-Alg-Zl-AD while Langmuir and Temkin models account for the Cs-Alg-Zl-FD dye adsorption. The Cs-Alg-Zl-FD shows greater dye adsorption over four adsorption cycles, as compared with the Cs-Alg-Zl-AD., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

In this study, antiulcer activity of ethanolic extract and solvent fractions of the aerial part of Calendula tripterocarpa was investigated using ethanol-induced model of gastric ulceration in rats. The results showed that ethyl acetate, non-polar components and diethyl ether fractions have a remarkable antiulcerogenic activity; because they exhibited control-ulcer protection by 85.2%, 77.7% and 62.9%, respectively. The acute toxicity study showed that the extract is highly safe; the median lethal dose (LD 50 ) was more than 5000 mg/kg. Moreover, the obtained results were confirmed by the sub-chronic toxicity and showed no alteration in the liver and kidney functions. Our data suggests that C. tripterocarpa possesses significant antiulcer activity and it can be used as a source for an antiulcer drug. Around 100 compounds are elucidated from this plant using direct analysis in real-time of flight-mass spectrometry for the first time, of which four well-known compounds were not isolated or reported previously.

Herein, a mesoporous magnetic chitosan-salicylaldehyde/calcium oxide nanoparticle (CS-SL/CaO/Fe 3 O 4 ) biocomposite adsorbent that was prepared via freeze-drying. The CS-SL/CaO/Fe 3 O 4 was utilized for the adsorption of ramazol brilliant blue (RBB) dye from aqueous solution. The physicochemical properties of the CS-SL/CaO/Fe 3 O 4 were evaluated using diverse characterization techniques, including BET, XRD, FTIR, FESEM-EDX, CHNS, and pH pzc . The three main factors for adsorption included the following A: CS-SL/CaO/Fe 3 O 4 dosage (0.02-0.1 g/100 mL), B: pH (4-10), and C: Time (60-540 min). These factors were improved using statistical methods, specifically the Box-Behnken design (BBD). The optimal conditions for achieving maximum RBB removal (62.5 %) are listed: CS-SL/CaO/Fe 3 O 4 dosage of 0.1 g/100 mL, a solution pH of 7, and a contact time of 540 min. The adsorption kinetics and equilibrium isotherms were well described by the pseudo first order (PFO) kinetic and Langmuir isotherm models, respectively. Thus, the CS-SL/CaO/Fe 3 O 4 material has a maximum adsorption capacity (q max ) of 63.3 mg/g for RBB at 25 °C. The adsorption mechanism of RBB onto the CS-SL/CaO/Fe 3 O 4 surface was attributed to electrostatic forces, n-π stacking, H-bonding, and Pi-Pi interactions. Thus, CS-SL/CaO/Fe 3 O 4 represents a recoverable magnetic adsorbent with potential for capture of organic dyes from wastewater., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Chitosan salicylaldehyde/calcium oxide nanoparticle (CS-SL/CaO) was synthesized by hydrothermal process and isolated via different drying processes, namely, air-drying (AD) and freeze-drying (FD). The physicochemical properties of freeze-dried CS-SL/CaO nanoparticle (CS-SL/CaO-FD) and air-dried CS-SL/CaO nanoparticle (CS-SL/CaO-AD) were compared. In particular, the adsorption properties reveal that the specific surface area of CS-SL/CaO-FD increased by ca. 6 times (BET SA = 7.28 m 2 /g) greater than CS-SL/CaO-FD (BET SA = 1.26 m 2 /g). Also, the adsorptive removal of acid red 88 dye (AR88) from aqueous media was optimized by employing the Box-Behnken design (BBD). The optimal adsorption conditions obtained from desirability functions test for the removal of AR88 dye employed a dosage of 0.09 g/100 mL of adsorbent dosage at a solution pH of 5.6 and 25 °C. The best AR88 dye removal was found for the adsorbents CS-SL/CaO-AD (38.2 %) and CS-SL/CaO-FD (86.1 %), which concur with differences in the adsorbent surface areas. Moreover, the adsorption kinetics and isotherm profiles for CS-SL/CaO-FD were described by the pseudo second order (PSO) and Temkin models, where the maximum adsorption capacity of AR88 by CS-SL/CaO-FD 175.4 was mg/g. These findings reveal the potential application of the CS-SL/CaO-FD towards removal of toxic cationic dye (AR88) from an aqueous environment., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

A very simple and cost-effective silica-based hybrid stationary phase was synthesized for the separation of five synthetic peptides, five proteins, and benzene derivatives. Silica monolith was synthesized via sol-gel process. Particles obtained through the grinding of silica monolith were suspended in methanol and sedimented under gravity to obtain sub-2 μm particles. A hybrid LC stationary phase was obtained by coating an ethylene glycol dimethacrylate co-polymer onto the particles via RAFT polymerization. The resultant stationary phase was characterized using SEM, FTIR, BET, and EDX analysis. A stainless steel column (200 mm long × 0.2 mm ID) was packed with the resultant stationary phase via pressure tapering protocol using a slurry packing machine. The column resulted in the average number of theoretical plates/meter (287 500 for synthetic peptides, 276 800 for proteins, and 226 100 for benzene derivatives) under the elution conditions of acetonitrile/50 mM ammonium format (68/32 v/v%) with a flow rate of 0.785 μL min -1 . Since the column resulted in the separation of synthetic peptides, proteins, and benzene derivatives with very good chromatographic performance, it could possibly separate any complex mixture of peptides and proteins with better chromatographic performance., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)

In this study, chitosan grafted salicylaldehyde/coal fly ash/algae (Chi-SL/CFA/Alg) was synthesized by assistance of hydrothermal process to be an effective adsorbent to remove cationic dye (malachite green: MG) from water. The physicochemical properties of the Chi-SL/CFA/Alg biomaterial were examined using SEM-EDX, pH pzc , specific surface area (BET), and FTIR analyses. The optimization process of the adsorption operation parameters for MG removal by Chi-SL/CFA/Alg were optimized using a Box-Behnken design (BBD). The selected adsorption operation parameters Chi-SL/CFA/Alg dosage (A: 0.02-0.1 g/100 mL), solution pH (B: 4-8), and contact time (C: 20-360 min). Analysis of variance (ANOVA) test was applied to determine the significant interaction between the adsorption operation parameters and to validate BBD output. The adsorption kinetics and isotherms of MG dye by Chi-SL/CFA/Alg were well described by pseudo-second order (PSO) kinetic and Freundlich isotherm model respectively. Thus, the maximum adsorption capacity (q max ) of MG dye by Chi-SL/CFA/Alg was found to be 493.7 mg/g at basic pH environment (pH = 8) and working temperature 25 °C. The adsorption mechanism can be ascribed to various interactions, including hydrogen bonding, π-π interactions, electrostatic attraction, and n-π interactions. Thus, Chi-SL/CFA/Alg can be considered as preferable and potential adsorbent for removing cationic dye from aqueous environment., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

There are scarce data regarding the effects of soil amendments on biophysicochemical responses of plants at the early stages of growth/germination. This study critically compares the effects of ethylene-diamine-tetra-acetic-acid (EDTA) and calcium (Ca) on biophysicochemical responses of germinating pea seedlings under varied arsenic levels (As, 25, 125, 250 µM). Arsenic alone enhanced hydrogen peroxide (H 2 O 2 ) level in pea roots (176%) and shoot (89%), which significantly reduced seed germination percentage, pigment contents, and growth parameters. Presence of EDTA and Ca in growth culture minimized the toxic effects of As on pea seedlings, EDTA being more pertinent than Ca. Both the amendments decreased H 2 O 2 levels in pea tissues (16% in shoot and 13% in roots by EDTA, and 7% by Ca in shoot), and maintained seed germination, pigment contents, and growth parameters of peas close to those of the control treatment. The effects of all As-treatments were more pronounced in the pea roots than in the shoot. The presence of organic and inorganic amendments can play a useful role in alleviating As toxicity at the early stages of pea growth. The scarcity of data demands comparing plant biophysicochemical responses at different stages of plant growth (germinating vs mature) in future studies.

The present work develops an effective bioadsorbent of cross-linked chitosan-genipin/SiO 2 adsorbent (CHI-GNP/SiO 2 ). The developed CHI-GNP/SiO 2 was employed for the removal of organic dye (reactive orange 16, RO16) from simulated wastewater. The optimization of the fundamental adsorption variables (CHI-GNP/SiO 2 dose, time, and pH) via the Box-Behnken design (BBD) was attained for achieving maximal adsorption capacity and high removal efficiency. The good agreement between the Freundlich isotherms and empirical data of RO16 adsorption by CHI-GNP/SiO 2 indicates that the adsorption process follows a multilayer adsorption mechanism. The reasonable agreement between the pseudo-second-order model and the kinetic data of RO16 adsorption by CHI-GNP/SiO 2 was obtained. The maximum RO16 adsorption capacity (q max ) of CHI-GNP/SiO 2 was identified to be 57.1 mg/g. The adsorption capacity of CHI-GNP/SiO 2 is attributed to its unique surface properties, including its highly porous structure and the presence of functional groups such as amino and hydroxyl groups. According to the results of this investigation, CHI-GNP/SiO 2 has the potential to be an adsorbent for the removal of acidic dyes from wastewater., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

In this study, a hydrothermal approach was employed to graft chitosan (Chit)/algae (ALG) with salicylaldehyde (SA), resulting in the synthesis of a biocomposite named salicylaldehyde-based chitosan Schiff base/algae (Chit-SA/ALG). The main objective of this biocomposite was to effectively remove methyl violet (MV), an organic dye, from aqueous solutions. The adsorption performance of Chit-SA/ALG toward MV was investigated in detail, considering the effects of three factors: (A) Chit-SA/ALG dose (ranging from 0.02 to 0.1 g/100 mL), (B) pH (ranging from 4 to 10), and (C) time (ranging from 10 to 120 min). The Box-Behnken design (BBD) was utilized for experimental design and analysis. The experimental results exhibited a good fit with both the pseudo-second-order kinetic model and the Freundlich isotherm, suggesting their suitability for describing the MV adsorption process on Chit-SA/ALG. The maximum adsorption capacity of Chit-SA/ALG, as calculated by the Langmuir model, was found to be 115.6 mg/g. The remarkable adsorption of MV onto Chit-SA/ALG can be primarily attributed to the electrostatic forces between Chit-SA/ALG and MV as well as the involvement of various interactions such as n-π, π-π, and H-bond interactions. This research demonstrates that Chit-SA/ALG exhibits promising potential as a highly efficient adsorbent for the removal of organic dyes from water systems.

The thermally stable zirconium-based MOF, UiO-66, was employed for the preparation of bonded porous-layer open-tubular (PLOT) GC columns. The synthesis included the in situ growth of the UiO-66 film on the inner wall of the capillary through a one-step solvothermal procedure. SEM-EDX analysis revealed the formation of a thin, continuous, uniform, and compact layer of UiO-66 polycrystals on the functionalized inner wall of the column. The average polarity (Δ I av = 700) and the McReynolds constants reflected the polar nature of the UiO-66 stationary phase. Several mixtures of small organic compounds and real samples were used to evaluate the separation performance of the fabricated columns. Linear alkanes from n -pentane to n -decane were baseline separated within 1.35 min. Also, a series of six n -alkylbenzenes (C 3 -C 8 ) were separated within 3 min with a minimum resolution of 3.09, whereas monohalobenzene mixtures were separated at 220 °C within 14s. UiO-66 PLOT columns are ideally suited for the isothermal separation of chlorobenzene structural isomers at 210 °C within 45 s with R s ≥ 1.37. The prepared column featured outstanding thermal stability (up to 450 °C) without any observed bleeding or significant impact on its performance. This feature enabled the analysis of various petroleum-based samples.

Polymer monolithic stationary phases were prepared based on a cyclic anhydride as a reactive and tunable platform via ring-opening post-polymerization using primary amines, octadecylamine and benzylamine. The characterization techniques indicated the insertion of the functional groups into the original monoliths and confirmed the amidation reactions. The post-polymerization modification also improved the monolith's thermal and mechanical stability and induced significant improvement in their surface area. The stationary phases were synthesized inside small dimension stainless-steel columns (2.1 mm i.d. × 50 mm length). The prepared columns before and after modifications have been tested for the separation of the alkylbenzene series and some polycyclic aromatic hydrocarbons (PAHs) as model compounds. In all cases, the chromatographic performance in terms of the height equivalent to a theoretical plate on the functionalized monoliths was remarkably improved when compared with that on the unmodified monolith, which was between 9.59-39.49 μm and 4.08-31.50 μm using monoliths modified with octadecylamine and benzylamine, respectively. Under the same chromatographic conditions, the functionalization of monoliths with octadecylamine provided more hydrophobic interactions and enhanced the retention of alkylbenzenes, while the modification of monoliths with benzyl groups improved the separation and the retention of the PAHs through the strong π-π interactions. However, post-modification polymerization with octadecylamine and benzylamine enhanced the separation efficiency of the prepared columns toward all studied compounds. The repeatability of the injections on the same column and the reproducibility of the prepared columns have been studied for some selected parameters and estimated in terms of percent relative standard deviation (%RSD) for some of the studied compounds. The repeatability of the prepared columns was ≤9.42% ( n = 5) based on run-to-run injections and ≤9.48% based on day-to-day injections for five successive days. The reproducibility levels, on the other hand, were ≤20.95% for all studied parameters in all cases. To assess their performance for the analysis of real samples, the applicability of the prepared columns was examined for the separation of the active ingredients extracted from some commercial pharmaceutical formulations and for the separation of tea water extract constituents. The validation data show the suitability of the columns for practical use in the routine analysis of these samples.

Exploring new strategies to design non-precious and efficient electrocatalysts can provide a solution for sluggish electrocatalytic kinetics and sustainable hydrogen energy. Transition metal selenides are potential contenders for bifunctional electrocatalysis owing to their unique layered structure, low band gap, and high intrinsic activities. However, insufficient access to active sites, lethargic water dissociation, and structural degradation of active materials during electrochemical reactions limit their activities, especially in alkaline media. In this article, we report a useful strategy to assemble vanadium diselenide (VSe 2 ) into a 3D MXene/rGO-based sponge-like architecture (VSe 2 @G/MXe) using hydrothermal and freeze-drying approaches. The 3D hierarchical meso/macro-pore rich sponge-like morphology not only prevents aggregation of VSe 2 nanosheets but also offers a kinetics-favorable framework and high robustness to the electrocatalyst. Synergistic coupling of VSe 2 and a MXene/rGO matrix yields a heterostructure with a large specific surface area, high conductivity, and multi-dimensional anisotropic pore channels for uninterrupted mass transport and gas diffusion. Consequently, VSe 2 @G/MXe presented superior electrochemical activity for both the HER and OER compared to its counterparts (VSe 2 and VSe 2 @G), in alkaline media. The overpotentials required to reach a cathodic and anodic current density of 10 mA cm -2 were 153 mV (Tafel slope = 84 mV dec -1 ) and 241 mV (Tafel slope = 87 mV dec -1 ), respectively. The R ct values at the open circuit voltage were as low as 9.1 Ω and 1.41 Ω for the HER and OER activity, respectively. Importantly, VSe 2 @G/MXe withstands a steady current output for a long 24 h operating time. Hence, this work presents a rational design for 3D microstructures with optimum characteristics for efficient bifunctional alkaline water-splitting.

In this study, pineapple crown (PC) feedstock residues were utilized as a potential precursor toward producing activated carbon (PCAC) via pyrolysis induced with ZnCl 2 activation. The PCAC has a surface area (457.8 m 2 /g) and a mesoporous structure with an average pore diameter of 3.35 nm, according to the Brunauer-Emmett-Teller estimate. The removal of cationic dye (Fuchsin basic; FB) was used for investigating the adsorption parameters of PCAC. The optimization of significant adsorption variables (A: PCAC dose (0.02-0.1 g/100 mL); B: pH (4-10); C: time (10-90); and D: initial FB concentration (10-50 mg/L) was conducted using the Box-Behnken design (BBD). The pseudo-second-order (PSO) model characterized the dye adsorption kinetic profile, whereas the Freundlich model reflected the equilibrium adsorption profile. The maximum adsorption capacity ( q max ) of PCAC for FB dye was determined to be 171.5 mg/g. Numerous factors contribute to the FB dye adsorption mechanism onto the surface of PCAC, which include electrostatic attraction, H-bonding, pore diffusion, and π-π stacking. This study illustrates the utilization of PC biomass feedstock for the fabrication of PCAC and its successful application in wastewater remediation.

Due to a great demand for amylose and cellulose polymeric chromatographic chiral columns, the enantiomeric separation of thiourea derivatives of naringenin was achieved on the different amylose (Chiralpak-IB) and cellulose chiral (Chiralcel-OJ and Chiralcel-OD-3R) columns with varied chromatographic conditions. The isocratic mobile phases used were ethanol and methanol, where ethanol/hexane and methanol/hexane were used as gradient mode and were prepared in volume/volume relation. The separation and resolution factors for all the enantiomers were in the range of 1.25 to 3.47 and 0.48 to 1.75, respectively. The enantiomeric resolution was obtained within 12 min making fast separation. The docking studies confirmed the chiral recognition mechanisms with binding affinities in the range of -4.7 to -5.7 kcal/mol. The reported compounds have good anticoagulant activities and may be used as anticoagulants in the future. Besides, chiral separation is fast and is useful for enantiomeric separation in any laboratory in the world., (© 2024 Wiley Periodicals LLC.)

In this investigation, microwave irradiation assisted by ZnCl 2 was used to transform pineapple crown (PN) waste into mesoporous activated carbon (PNAC). Complementary techniques were employed to examine the physicochemical characteristics of PNAC, including BET, FTIR, SEM-EDX, XRD, and pH at the point-of-zero-charge (pH pzc ). PNAC is mesoporous adsorbent with a surface area of 1070 m 2 /g. The statistical optimization for the adsorption process of two model cationic dyes (methylene blue: MB and, crystal violet: CV) was conducted using the response surface methodology-Box-Behnken design (RSM-BBD). The parameters include solution pH (4-10), contact time (2-12) min, and PNAC dosage (0.02-0.1 g/100 mL). The Freundlich and Langmuir models adequately described the dye adsorption isotherm results for the MB and CV systems, whereas the pseudo-second order kinetic model accounted for the time dependent adsorption results. The maximum adsorption capacity ( q max ) for PNAC with the two tested dyes are listed: 263.9 mg/g for CV and 274.8 mg/g for MB. The unique adsorption mechanism of MB and CV dyes by PNAC implicates multiple contributions to the adsorption process such as pore filling, electrostatic forces, H-bonding, and π-π interactions. This study illustrates the possibility of transforming PN into activated carbon (PNAC) with the potential to remove two cationic dyes from aqueous media.

Herein, a natural material including chitosan (CTS) and algae (food-grade algae, FGA) was exploited to attain a bio-adsorbent (CTS/FGA) for enhanced methyl violet 2B dye removal. A study of the FGA loading into CTS matrix showed that the best mixing ratio between CTS and FGA to be used for the MV 2B removal was 50 %:50 % (CTS/FGA; 50:50 w/w). The present study employed the Box-Behnken design (RSM-BBD) to investigate the impact of three processing factors, namely CTS/FGA-(50:50) dose (0.02-0.1 g/100 mL), pH of solution (4-10), and contact time (5-15 min) on the decolorization rate of MV 2B dye. The results obtained from the equilibrium and kinetic experiments indicate that the adsorption of MV 2B dye on CTS/FGA-(50:50) follows the Langmuir and pseudo-second-order models, respectively. The CTS/FGA exhibits an adsorption capacity of 179.8 mg/g. The characterization of CTS/FGA-(50:50) involves the proposed mechanism of MV 2B adsorption, which primarily encompasses various interactions such as electrostatic forces, n-π stacking, and H-bonding. The present study demonstrates that CTS/FGA-(50:50) synthesized material exhibits a distinctive structure and excellent adsorption properties, thereby providing a viable option for the elimination of toxic cationic dyes from polluted water., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Mercury [Hg(II)] contamination is an indefatigable global hazard that causes severe permanent damage to human health. Extensive research has been carried out to produce mercury adsorbents; however, they still face certain challenges, limiting their upscaling. Herein, we report the synthesis of a novel amine-impregnated inverse vulcanized copolymer for effective mercury removal. Poly(S-MA) was prepared using sulfur and methacrylic acid employing the inverse vulcanization method, followed by functionalization. The polyethylenimine (PEI) was impregnated on poly(S-MA) to increase the adsorption active sites. The adsorbent was then characterized byusing Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). FTIR spectroscopy confirmed the formation of the copolymer, and successful impregnation of PEI and SEM revealed the composite porous morphology of the copolymer. Amine-impregnated copolymer [amine@poly(S-MA)] outperformed poly(S-MA) in mercury as it showed 20% superior performance with 44.7 mg/g of mercury adsorption capacity. The adsorption data best fit the pseudo-second-order, indicating that chemisorption is the most effective mechanism, in this case, indicating the involvement of NH 2 in mercury removal. The adsorption is mainly a monolayer on a homogeneous surface as indicated by the 0.76 value of Redlich-Peterson exponent ( g ), which describes the adsorption nature advent from the R 2 value of 0.99., Competing Interests: The authors declare no competing financial interest., (© 2024 The Authors. Published by American Chemical Society.)

Females of some mosquito species are anthropophilic, as they feed on human blood to support egg production and, hence, are forensically valuable if found at a crime scene. The present study investigated the blood meal digestion process in Culex pipiens L. both with and without heroin and proposed a method for estimating the post-feeding interval (PFI). Mosquitoes were fed on a control mouse, a heroin-injected mouse, or in vitro heroin-treated mouse blood. The blood meal digestion was then investigated at different hours post-feeding. Data showed that the blood meal size ingested by control mosquitoes was 0.681 ± 0.04 mg/mosquito and was completely digested within 45 h post-feeding. An estimation of the PFI was proposed in terms of the rate of hemoglobin (Hb) digestion. The blood meal size of the mosquitoes fed on the in vitro heroin-treated blood and the heroin-injected mouse was 0.96 ± 0.06 and 0.79 ± 0.01 mg/mosquito and was completely digested within 50 and 55 h post-feeding, respectively. The digestion of Hb started similarly in all experimental mosquitoes until 10 h post-feeding, after which it significantly decreased in heroin-treated blood meals compared with the control ones. This may suggest that heroin impacted the digestion process, as it took an extra 5-10 h to complete. These findings could be valuable in the forensic context since an estimation of PFI is proposed as a potential estimation of the postmortem interval (PMI). However, care should be taken as heroin in the host blood has significantly impacted the overall digestion process and, hence, may bias the PFI/PMI estimation., (© The Author(s) 2023. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.)

In this study, bamboo waste (BW) was subjected to pyrolysis-assisted ZnCl 2 activation to produce mesoporous activated carbon (BW-AC), which was then evaluated for its ability to remove cationic dyes, specifically methylene blue (MB) and crystal violet (CV), from aqueous environments. The properties of BW-AC were characterized using various techniques, including potentiometric-based point of zero charge (pH pzc ), scanning electron microscopy with energy dispersive X-rays (SEM-EDX), X-ray diffraction (XRD), gas adsorption with Brunauer-Emmett-Teller (BET) analysis, infrared (IR) spectroscopy. To optimize the adsorption characteristics (BW-AC dosage, pH, and contact time) of PBW, a Box-Behnken design (BBD) was employed. The BW-AC dose of 0.05 g, solution pH of 10, and time of 8 min are identified as optimal operational conditions for achieving maximum CV (89.8%) and MB (96.3%) adsorption according to the BBD model. The dye removal kinetics for CV and MB are described by the pseudo-second-order model. The dye adsorption isotherms revealed that adsorption of CV and MB onto BW-AC follow the Freundlich model. The maximum dye adsorption capacities ( q max ) of BW-AC for CV (530 mg/g) and MB (520 mg/g) are favorable, along with the thermodynamics of the adsorption process, which is characterized as endothermic and spontaneous. The adsorption mechanism of CV and MB dyes by BW-AC was attributed to multiple contributions: hydrogen bonding, electrostatic forces, π-π attraction, and pore filling. The findings of this study highlight the potential of BW-AC as an effective adsorbent in wastewater treatment applications, contributing to the overall goal of mitigating the environmental impact of cationic dyes and ensuring the quality of water resources.

In this study, chitosan/nano SiO 2 (CTS/NS) was chemically modified with bisphenol A diglycidyl ether (BADGE) cross-linker-assisted hydrothermal process to create an effective adsorbent, CTS-BADGE/NS, for the removal of reactive orange 16 (RO16) dye from aquatic systems. Box-Behnken design (BBD) was used to optimize the adsorption process by varying the adsorbent dose (0.02-0.1 g/100 mL), pH (4-10), and time (20-360 min). The adsorption isotherm results indicated that the Langmuir model fits the experimental data well, suggesting that the adsorption process involves a monolayer formation of RO16 on the surface of CTS-BADGE/NS. The kinetic modeling of RO16 adsorption by CTS-BADGE/NS demonstrated that the pseudo-first-order model fits the adsorption data. CTS-BADGE/NS achieved an adsorption capacity of 97.8 mg/g for RO16 dye at optimum desirability functions of dosage 0.099 g/100 mL, solution pH of 4.44, and temperature of 25 °C. Overall, the π-π electron donor-acceptor system significantly improved the adsorption performance of the CTS-BADGE/NS. The results of the regeneration investigation demonstrate that the CTS-BADGE/NS exhibits effective adsorption of RO16, even after undergoing five consecutive cycles. The results of this study suggest that the developed CTS-BADGE/NS composite can be a promising adsorbent for water purification applications., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Herein, this work targets to employ the blended fruit wastes including rambutan ( Nephelium lappaceum ) peel and durian ( Durio zibethinus) seed as a promising precursor to produce activated carbon (RPDSAC). The generation of RPDSAC was accomplished through a rapid and practical procedure (microwave-ZnCl 2 activation). To evaluate the adsorptive capabilities of RPDSAC, its efficacy in eliminating methylene blue (MB), a simulated cationic dye, was measured. The Box-Behnken design (BBD) was utilized to optimize the crucial adsorption parameters, namely A : RPDSAC dose (0.02-01 g/100 mL), B : pH (4-10), and C : time (2-6 min). The BBD design determined that the highest level of MB removal (79.4%) was achieved with the condition dosage of RPDSAC at 0.1 g/100 mL, contact time (6 min), and pH (10). The adsorption isotherm data is consistent with the Freundlich concept, and the pseudo-second-order versions adequately describe the kinetic data. The monolayer adsorption capacity ( q max ) of RPDSAC reached 120.4 mg/g at 25 °C. Various adsorption mechanisms are involved in the adsorption of MB dye onto the surface of RPDSAC, including π-π stacking, H-bonding, pore filling, and electrostatic forces. This study exhibits the potential of the RPDSAC as an adsorbent for removal of toxic cationic dye (MB) from contaminated wastewater.

In this study, the focus was on utilizing tropical plant biomass waste, specifically bamboo (BB), as a sustainable precursor for the production of activated carbon (BBAC) via pyrolysis-induced K 2 CO 3 activation. The potential application of BBAC as an effective adsorbent for the removal of methylene blue (MB) dye from aqueous solutions was investigated. Response surface methodology (RSM) was employed to evaluate key adsorption characteristics, which included BBAC dosage (A: 0.02-0.08 g/L), pH (B: 4-10), and time (C: 2-8 min). The adsorption isotherm analysis revealed that the adsorption of MB followed the Freundlich model. Moreover, the kinetic data were well-described by the pseudo-second-order model, suggesting the role of a chemisorption process. The BBAC demonstrated a notable MB adsorption capacity of 195.8 mg/g, highlighting its effectiveness as an adsorbent. Multiple mechanisms were identified as controlling factors in MB adsorption by BBAC, including electrostatic forces, π-π stacking, and H-bonding interactions. The findings of this study indicate that BBAC derived from bamboo has the potential to be a promising adsorbent for the treatment of wastewater containing organic dyes. The employment of sustainable precursors like bamboo for activated carbon production contributes to environmentally friendly waste management practices and offers a solution for the remediation of dye-contaminated wastewater.

A major worldwide challenge that presents significant economic, environmental, and social concerns is the rising generation of food waste. The current work used chicken bones (CB) and rice (R) food waste as alternate precursors for the production of activated carbon (CBRAC) by microwave radiation-assisted ZnCl 2 activation. The adsorption characteristics of CBRAC were investigated in depth by removing an organic dye (crystal violet, CV) from an aquatic environment. To establish ideal conditions from the significant adsorption factors (A: CBRAC dosage (0.02-0.12 g/100 mL); B: pH (4-10); and C: duration (30-420), a numerical desirability function of Box-Behnken design (BBD) was utilized. The highest CV decolorization by CBRAC was reported to be 90.06% when the following conditions were met: dose = 0.118 g/100 mL, pH = 9.0, and time = 408 min. Adsorption kinetics revealed that the pseudo-first order (PFO) model best matches the data, whereas the Langmuir model was characterized by equilibrium adsorption, where the adsorption capacity of CBRAC for CV dye was calculated to be 57.9 mg/g. CV adsorption is accomplished by several processes, including electrostatic forces, pore diffusion, π-π stacking, and H-bonding. This study demonstrates the use of CB and R as biomass precursors for the efficient creation of CBRAC and their use in wastewater treatment, resulting in a greener environment.

In this study, a new biocomposite magnetic adsorbent (magnetic glyoxal-chitosan Schiff base/organically modified montmorillonite (MCTS-GOX/OMMT)) was synthesized and employed for the adsorption of reactive blue 19 dye (RB19) from aqueous environment. The physicochemical properties of the MCTS-GOX/OMMT were confirmed by using various characterization techniques such as BET, XRD, FTIR, SEM-EDX, VSM, and pH pzc . The adsorption key variables were statistically optimized via Box-Behnken design (BBD) And accordingly the best operational conditions to achieve maximum RB19 removal were recorded at MCTS-GOX/OMMT dosage = 0.1 g/0.1 L, solution pH = 4, and working temperature = 25 °C. The adsorption process for RB19 appeared to follow the pseudo-second-order kinetic and the Langmuir isotherm models, according to the findings of the adsorption kinetics and equilibrium investigations. The maximum adsorption capacity of the MCTS-GOX/OMMT towards RB19 was 122.3 mg/g, demonstrating its preferable adsorption capability. The successful development of this novel magnetic bioadsorbent with excellent adsorption ability towards organic dyes and efficient separation ability opens possibilities for its practical application in wastewater treatment and dye removal processes., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Herein, a quadruple biomagnetic nanocomposite of cross-linked chitosan-ethylene glycol diglycidyl ether/organo-nanoclay (MCH-EGDE/ORNC) was designed for the uptake of remazol brilliant blue R (RBBR) dye from aqueous environment. The adsorption process was systematically improved via the Box-Behnken design (BBD) to determine the influence of key uptake parameters, including MCH-EGDE/ORNC dosage, pH, and time, on the RBBR removal. The highest RBBR removal of 87.5 % was achieved at the following conditions: MCH-EGDE/ORNC dosage: 0.1 g/100 mL; pH: 4.0; contact time: 25 min. The findings of the kinetics and equilibrium studies revealed an excellent fit to the pseudo-second order and the Freundlich models, respectively. The adsorption capacity of the MCH-EGDE/ORNC for RBBR was found to be 168.4 mg/g, showcasing its remarkable adsorption capability. The present work highlights the potential of MCH-EGDE/ORNC biomaterial as an advanced adsorbent and lays the foundation for future applications in water purification and environmental remediation., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

This work aims to apply the use of food-grade algae (FGA) composited with chitosan-benzaldehyde Schiff base biopolymer (CHA-BD) as a new adsorbent (CHA-BA/FGA) for methyl violet 2B (MV 2B) dye removal from aqueous solutions. The effect of three processing variables, including CHA-BA/FGA dosage (0.02-0.1 g/100 mL), pH solution (4-10), and contact duration (10-120 min) on the removal of MV 2B was investigated using the Box-Behnken design (BBD) model. Kinetic and equilibrium dye adsorption profiles reveal that the uptake of MV 2B dye by CHA-BA/FGA is described by the pseudo-second kinetics and the Langmuir models. The thermodynamics of the adsorption process (ΔG°, ΔH°, and ΔS°) reveal spontaneous and favorable adsorption parameters of MV 2B dye onto the CHA-BA/FGA biocomposite at ambient conditions. The CHA-BA/FGA exhibited the maximum ability to absorb MV 2B of 126.51 mg/g (operating conditions: CHA-BA/FGA dose = 0.09 g/100 mL, solution pH = 8.68, and temperature = 25 °C). Various interactions, including H-bonding, electrostatic forces, π-π stacking, and n-π stacking provide an account of the hypothesized mechanism of MV 2B adsorption onto the surface of CHA-BA/FGA. This research reveals that CHA-BA/FGA with its unique biocomposite structure and favorable adsorption properties can be used to remove harmful cationic dyes from wastewater.

Herein, a highly efficient and sustainable adsorbent of cross-linked chitosan-glyoxal/algae biocomposite (CHT-GLX/ALG) adsorbent was developed through an innovative hydrothermal cross-linking method. The CHT-GLX/ALG biocomposite was characterized using several complementary analytical methods that include CHN-O, XRD, FTIR, SEM-EDX, and pH pzc . This new adsorbent, named CHT-GLX/ALG, was utilized for the adsorption of a cationic dye (methyl violet 2B; MV 2B), from synthetic wastewater. The optimization of the dye adsorption process involved key parameters is listed: CHT-GLX/ALG dosage (from 0.02 to 0.1 g/100 mL), pH (from 4 to 10), and contact time (from 20 to 180 min) that was conducted using the Box-Behnken design (BBD). The optimal adsorption conditions for the highest decolorization efficiency of MV 2B (97.02 %) were estimated using the statistical model of the Box-Behnken design. These conditions include a fixed adsorbent dosage of 0.099 g/100 mL, pH 9.9, and a 179.9 min contact time. The empirical data of MV 2B adsorption by CHT-GLX/ALG exhibited favorable agreement with the Freundlich isotherm model. The kinetic adsorption profile of MV 2B by CHT-GLX/ALG revealed a good fit with the pseudo-second-order model. The maximum adsorption capacity (q max ) for MV 2B by CHT-GLX/ALG was estimated at 110.8 mg/g. The adsorption of MV 2B onto the adsorbent can be attributed to several factors, including electrostatic interactions between the negatively charged surface of CHT-GLX/ALG and the MV 2B cation, as well as n-π and H-bonding. These interactions play a crucial role in facilitating the effective adsorption of MV 2B onto the biocomposite adsorbent. Generally, this study highlights the potential of CHT-GLX/ALG as an efficient and sustainable adsorbent for the effective removal of organic dyes., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

A very simple mesotrione-sensing medium with enhanced sensitivity detection limits has been proposed. A renovated hydrothermal method was adopted for synthesizing fluorescent carbon dots from ethylenediamine and glucose using a Teflon-lined simple autoclave in a GC oven. The resultant carbon dots were characterized via TEM, FTIR, UV-vis, particle size distribution, and EDX and evaluated in a fluorimeter as the sensing medium for mesotrione detection. The binding approach of the Co (II)-integrated glucose-bound carbon dots toward mesotrione is selective, making them an effective sensor for the real sample applications, where majority of the coexisting substances showed insignificant interference effect. Formation of the metastable state due to the molecular interaction between carbon dots and Co (II) resulted in fluorescence quenching at 456 nm. Enhancement in the fluorescence intensity occurred when mesotrione was added in the concentration range of 0.2-5.0 μg mL -1 , with a limit of detection, limit of quantification, standard deviation, and relative standard deviation of 0.054, 0.164, 0.00082 μg mL -1 , and 0.682%, respectively. Mesotrione determination was demonstrated in soil, water, and tomato samples with recoveries in the range of 95.38-104.7%. The selectivity of the sensor was found to be good enough when checked for the complex tomato sample spiked with different pesticides of the triketone family having structural similarities to mesotrione., Competing Interests: The authors declare no competing financial interest., (© 2023 The Authors. Published by American Chemical Society.)

Chromium (Cr), due to its greater contamination in aquifers and distinct eco-toxic impacts, is of greater environmental concern. This study aimed to synthesize nanocomposites of almond shells biochar (BC) with zerovalent bismuth and/or copper (Bi 0 /BC, Cu 0 /BC, and Bi 0 -Cu 0 /BC) for the removal of Cr from aqueous solution. The synthesized nanocomposites were investigated using various characterization techniques such as XRD, FTIR spectroscopy, SEM, and EDX. The Cr removal potential by the nanocomposites was explored under different Cr concentrations (25-100 mg/L), adsorbent doses (0.5-2.0 g/L), solution pH (2-8), and contact time (10-160 min). The above-mentioned advanced techniques verified successful formation of Bi 0 /Cu 0 and their composite with BC. The synthesized nanocomposites were highly effective in the removal of Cr. The Bi 0 -Cu 0 /BC nano-biocomposites showed higher Cr removal efficiency (92%) compared to Cu 0 /BC (85%), Bi 0 /BC (76%), and BC (67%). The prepared nanocomposites led to effective Cr removal at lower Cr concentrations (25 mg/L) and acidic pH (4.0). The Cr solubility changes with pH, resulting in different degrees of Cr removal by Bi 0 -Cu 0 /BC, with Cr(VI) being more soluble and easier to adsorb at low pH levels and Cr(III) being less soluble and more difficult to adsorb at high pH levels. The experimental Cr adsorption well fitted with the Freundlich adsorption isotherm model (R 2  > 0.99) and pseudo-second-order kinetic model. Among the prepared nanocomposites, the Bi 0 -Cu 0 /BC showed greater stability and reusability. It was established that the as-synthesized Bi 0 -Cu 0 /BC nano-biocomposite showed excellent adsorption potential for practical Cr removal from contaminated water., (© 2023. The Author(s), under exclusive licence to Springer Nature B.V.)

Batch scale removal of arsenic (As) from aqueous media was explored using nano-zero valent iron (Fe 0 ) and copper (Cu 0 ) particles. The synthesized particles were characterized using a Brunauer-Emmett-Teller (BET) surface area analyzer, a scanning electron microscope (SEM), and Fourier transform infrared spectroscopy (FTIR). The BET result showed that the surface area (31.5 m 2 /g) and pore volume (0.0415 cm 3 /g) of synthesized Fe 0 were higher than the surface area (17.56 m 2 /g) and pore volume (0.0287 cm 3 /g) of Cu 0 . The SEM results showed that the morphology of the Fe 0 and Cu 0 was flowery microspheres and highly agglomerated with thin flakes. The FTIR spectra for Fe 0 showed broad and intense peaks as compared to Cu 0 . The effects of the adsorbent dose (1-4 g/L), initial concentration of As (2 mg/L to 10 mg/L) and solution pH (2-12) were evaluated on the removal of As. Results revealed that effective removal of As was obtained at pH 4 with Fe 0 (94.95%) and Cu 0 (74.86%). When the dosage increased from 1 to 4 g L -1 , the As removal increased from 70.59 to 93.02% with Fe 0 and from 67 to 70.59% with Cu 0 . However, increasing the initial As concentration decreased the As removal significantly. Health risk indices, including estimated daily intake (EDI), hazard quotient (HQ), and cancer risk (CR) were employed and a significant decline (up to 99%) in risk indices was observed in As-treated water using Fe 0 /Cu 0 . Among the adsorption isotherm models, the values of R 2 showed that isothermal As adsorption by Fe 0 and Cu 0 was well explained by the Freundlich adsorption isotherm model (R 2  > 0.98) while the kinetic experimental data was well-fitted with the Pseudo second order model. The Fe 0 showed excellent stability and reusability over five sorption cycles, and it was concluded that, compared to the Cu 0 , the Fe 0 could be a promising technology for remediating As-contaminated groundwater., (© 2023. The Author(s), under exclusive licence to Springer Nature B.V.)

Herein, the polymer nanomatrix of chitosan/SiO 2 (CHI/n-SiO 2 ) was enriched with a π-π electron donor-acceptor system using diaromatic rings of benzil (BEZ) assisted via a hydrothermal process to obtain an effective adsorbent of chitosan-benzil/SiO 2 (CHI-BEZ/n-SiO 2 ). The polymer nanomatrix (CHI/n-SiO 2 ) and the resulting adsorbent (CHI-BEZ/n-SiO 2 ) were applied to remove the anionic acid red 88 (AR88) dye from aqueous media in a comparative mode. Box-Behnken design (BBD) was adopted to optimize AR88 adsorption onto CHI/n-SiO 2 and CHI-BEZ/n-SiO 2 with respect to variables that influence AR88 adsorption (adsorbent dose: 0.02-0.1 g/100 mL; pH: 4-10; and time: 10-90). The adsorption studies at equilibrium were conducted with a variety of initial AR88 dye concentrations (20-200 mg/L). The adsorption isotherm results reveal that the AR88 adsorption by CHI/n-SiO 2 and CHI-BEZ/n-SiO 2 are described by the Langmuir model. The kinetic adsorption profiles of AR88 with CHI/n-SiO 2 and CHI-BEZ/n-SiO 2 reveal that the pseudo-first-order model provides the best fit results. Interestingly, CHI-BEZ/n-SiO 2 has a high adsorption capacity (261.2 mg/g), which exceeds the adsorption capacity of CHI/n-SiO 2 (215.1 mg/g) that relates to the surface effects of SiO 2 and the functionalization of chitosan with BEZ. These findings show that CHI-BEZ/n-SiO 2 represents a highly efficient adsorbent for the removal of harmful pollutants from water, which outperforming the CHI/n-SiO 2 system., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Groundwater is the most valuable natural source in our earth's planet, being contaminated in various regions worldwide. Despite considerable research, there are scarce data regarding arsenic (As) levels in groundwater and its build-up in biological samples in Pakistan. The current investigation analyzed As contamination in four tehsils of District Khanewal (Kabirwala tehsil, Jahaniyan tehsil, Mian Channu tehsil, and Khanewal tehsil). For that, 123 groundwater samples, 19 animal milk samples, 20 human nails, and 20 human hair samples were collected from the study area. Arsenic concentration in groundwater was up to 51.8 µg/L with an average value of 7.2 µg/L. About 28 water samples (23%) had As contents > WHO limit and 38 samples (31%) > DEP-NJ limit. Low levels of As were detected in biological samples. Average As levels were 23 µg/L in the milk samples and 298 µg/kg in human hair. Arsenic contents were not detected in nail samples, except in one sample from Kabirwala tehsil. The maximum values of hazard quotient and cancer risk in District Khanewal were 4.9 and 0.0022, respectively. It is anticipated that long-term use of As-containing water may led to poisoning of humans in the study area, especially in Kabirwala. Therefore, it is necessary to monitor As contamination in the groundwater of Kabirwala tehsil to reduce the potential health hazards., (© 2023. The Author(s), under exclusive licence to Springer Nature B.V.)

Ti 3 C 2 -MXene material, known for its strong electronic conductivity and optical properties, has emerged as a promising alternative to noble metals as a cocatalyst for the development of efficient photocatalysts used in environmental cleanup. In this study, we investigated the photodegradation of crystal-violet (CV) dye when exposed to UV light using a newly developed photocatalyst known as Ti 3 C 2 -MXene/NiO nanocomposite-decorated CsPbI 3 perovskite, which was synthesized through a hydrothermal method. Our research investigation into the structural, morphological, and optical characteristics of the Ti 3 C 2 -MXene/NiO/CsPbI 3 composite using techniques such as FTIR, XRD, TEM, SEM-EDS mapping, XPS, UV-Vis, and PL spectroscopy. The photocatalytic efficacy of the Ti 3 C 2 -MXene/NiO/CsPbI 3 composite was assessed by evaluating its ability to degrade CV dye in an aqueous solution under UV-light irradiation. Remarkably, the Ti 3 C 2 -MXene/NiO/CsPbI 3 composite displayed a significant improvement in both the degradation rate and stability of CV dye when compared to the Ti 3 C 2 -MXene/NiO nanocomposite and CsPbI 3 perovskite materials. Furthermore, the UV-visible absorption spectrum of the Ti 3 C 2 -MXene/NiO/CsPbI 3 composite demonstrated a reduced band gap of 2.41 eV, which is lower than that of Ti 3 C 2 -MXene/NiO (3.10 eV) and Ti 3 C 2 -MXene (1.60 eV). In practical terms, the Ti 3 C 2 -MXene/NiO/CsPbI 3 composite achieved an impressive 92.8% degradation of CV dye within 90 min of UV light exposure. We also confirmed the significant role of photogenerated holes and radicals in the CV dye removal process through radical scavenger trapping experiments. Based on our findings, we proposed a plausible photocatalytic mechanism for the Ti 3 C 2 -MXene/NiO/CsPbI 3 composite. This research may open up new avenues for the development of cost-effective and high-performance MXene-based perovskite photocatalysts, utilizing abundant and sustainable materials for environmental remediation.

The extraction of berberine was carried out from Berberis vulgaris, Berberis aquifolium, and Hydrastis canadensis plants using ethanol and water (70:30, v/v). The extracted berberine was characterized by ultraviolet-visible and Fourier-transform infrared spectroscopy. The purity of berberine was ascertained by thin-layer chromatography using n-propanol-formic acid-water (95:1:4) and (90:1:9) solvents. hR f values were in the range of 44-49 with compact spots (diameter 0.2-0.4 cm). HPLC was carried out using ammonium acetate buffer and acetonitrile in gradient mode with Zodiac (4.6 × 150 mm, 3 μm) column. The flow rate was 1.0 mL/min and detection was at 220 nm. The values of separation and resolution factors of the standard and the extracted berberine were in the range of 1.13-1.16 and 1.40-1.71, respectively. A comparison has shown that both thin-layer chromatography and high-performance liquid chromatography (HPLC) methods found applications in different situations and requirements. The extracted berberine samples were used to treat Leishmaniosis and the results showed better activity of berberine in comparison to the standard drug Amphotericin B. Briefly, the reported research is a novel and may be used to extract berberine from plants, separation and identification of berberine by thin layer chromatography and HPLC and to treat Leishmaniosis., (© 2023 Wiley-VCH GmbH.)

Municipal wastewater contains emergent chemical and biological pollutants that are resistant to conventional wastewater treatments. Therefore, the focus of the current study was to address the challenge of removing emergent chemical and biological pollutants present in municipal wastewater. To achieve this, a photo electro-catalytic (PEC) treatment approach was employed, focusing on the removal of both micro and biological pollutants that are of emergent concern, as well as the reduction of Chemical Oxidation Demand (COD) and Total Organic Carbon (TOC). The treatment involved the use of a modified multi-layer catalytic anode photo-electroactive anode as an effective anode for PEC treatment of municipal wastewater. In the continuous mode of operation, %COD removal was optimized for the treatment of municipal wastewater under Ultra-Violet C (UVc), 280 nm, and Visible (Vis) radiation, 400 nm. Therefore, a comparative study was performed to investigate the effect of Vis radiation on %COD removal, micropollutants removal, and disinfection of municipal wastewater. Micropollutants present in municipal wastewater were effectively oxidized/degraded with the highest reduction rate between 100% and 80% under the influence of UVc and Vis radiation respectively by the PEC treatment process. Disinfection of various microorganisms present in the wastewater with the effect of UVc and Vis assisted PEC treatment was also monitored. Overall, 75-80% of the disinfection of municipal wastewater was contributed by the modified multi-layer catalytic anode. The UVc in the PEC system, contributes approximately 20-25% to the overall disinfection of municipal wastewater., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Crown Copyright © 2023. Published by Elsevier Ltd. All rights reserved.)

Preconcentration for on-site detection or subsequent determination is a promising technique for selective sensing explosive markers at low concentrations. Here, we report divinylbenzene monolithic polymer in its blank form (neat-DVB) and as a composite incorporated with sodalite topology zeolite-like metal-organic frameworks (3-ZMOF@DVB), as a sensitive, selective, and cost-effective porous preconcentrator for aliphatic nitroalkanes in the vapor phase as explosive markers at infinite dilution. The developed materials were fabricated as 18 cm gas chromatography (GC) monolithic capillary columns to study their separation performance of nitroalkane mixture and the subsequent physicochemical study of adsorption using the inverse gas chromatography (IGC) technique. A strong preconcentration effect was indicated by a specific retention volume adsorption/desorption ratio equal to 3 for nitromethane on the neat-DVB monolith host-guest interaction, and a 14% higher ratio was observed using the 3-ZMOF@DVB monolithic composite despite the low percentage of 0.7 wt.% of sod-ZMOF added. Furthermore, Incorporating ZMOF resulted in a higher percentage of micropores, increasing the degree of freedom more than bringing stronger adsorption and entropic-driven interaction more than enthalpic. The specific free energy of adsorption (ΔG S ) values increased for polar probes and nitroalkanes, denoting that adding ZMOFs earned the DVB monolithic matrix a more specific character. Afterward, Lewis acid-base properties were calculated, estimating the electron acceptor (K A ) and electron donor (K B ) constants. The neat-DVB was found to have a Lewis basic character with K B /K A  = 7.71, and the 3-ZMOF@DVB had a less Lewis basic character with K B /K A  = 3.82. An increased electron-accepting nature can be directly related to incorporating sod-ZMOF into the DVB monolithic matrix. This work considers the initial step in presenting a portable explosives detector or preconcentrating explosive markers trace prior to more sophisticated analysis. Additionally, the IGC technique allows for understanding the factors that led to the superior adsorption of nitroalkanes for the developed materials., Competing Interests: Declaration of Competing Interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Kareem Yusuf reports financial support was provided by Deputyship for Research & Innovation, Ministry of Education in Saudi Arabia. (IFKSURC-1-3301), (Copyright © 2023 Elsevier B.V. All rights reserved.)

A polymer-based nanosensor and electrochemical methods were developed for the quantitative analysis of vanillin. The sample preparation was done using nano solid phase micro membrane tip extraction (NSPMMTE). A novel poly(phenylalanine)/TiO 2 /CPE sensor was built as the working electrode for the first time for the analysis of the vanillin substance. The electrochemical behavior and analytical performance of vanillin were examined in detail by cyclic voltammetry (CV) and differential pulse stripping voltammetry (DPSV) techniques via the oxidation process. The optimized modules of the DPSV technique that affected the vanillin peak current and peak potential were pH, pulse amplitude, step potential, and deposition time. The electroactive surface areas of bare CPE, TiO 2 /CPE, and poly(phenylalanine)/TiO 2 /CPE electrodes were found to be 0.135 cm 2 , 0.155 cm 2 , and 0.221 cm 2 , respectively. The limit of detection (LOD) was 32.6 μg/L in the 0.25-15.0 mg/L working range at pH 7.0. The selectivity of the proposed DPSV method for the determination of vanillin on the modified electrode was investigated in the presence of various organic and inorganic substances, and the determination of vanillin with high recovery was achieved with less than 5% relative error. The analytical application was applied in chocolate samples and the DPSV method was found highly efficient, reproducible, and selective., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Inc. All rights reserved.)

Herein, Fe 3 O 4 core-TiO 2 /mesoSiO 2 and Fe 3 O 4 core-mesoSiO 2 /TiO 2 double shell nanoparticles were prepared by first (R1) and second (R2) routes and applied for the removal of methylene blue. The reported adsorption capacities for R1-0.2, R1-0.4 and R2 samples were 128, 118 and 133 mg.g -1 , respectively, which were obtained after 80 min as equilibrium contact time, and pH of 6 using a methylene blue concentration of 200 ppm. The adsorption of methylene blue using the prepared Fe 3 O 4 core-meso SiO 2 /TiO 2 double shell was analyzed by kinetic and isotherms models. In addition, thermodynamic investigations were applied to assess the spontaneous nature of the process. The obtained results confirmed that the pseudo-second order model is well fitted with the adsorption data and the Freundlich-isotherm assumption suggested a multilayer adsorption mechanism. In addition, results of the thermodynamic investigation indicated that ΔG° was in the range of -2.3 to -6.8 kJ/mol for R1-0.2, -2.8 to -6.3 kJ/mol for R1-0.4 and -2.0 to -5.2 kJ/mol for R2. In addition, the ΔH° and ΔS° values were found in the range of 26.4 to 36.19 kJ.mol -1 and 94.9 to 126.3 Jmol -1 K -1 , respectively. These results confirm that the surfaces of Fe 3 O 4 core-mesoSiO 2 /TiO 2 and Fe 3 O 4 core-TiO 2 /mesoSiO 2 double shell exhibit a spontaneous tendency to adsorb methylene blue from the aqueous solutions. The achieved performance of Fe 3 O 4 core-meso SiO 2 /TiO 2 and Fe 3 O 4 core-TiO 2 /meso SiO 2 double shell as adsorbent for methylene blue removal will encourage future research investigations on the removal of a broad range of contaminants from wastewater.

Herein, a novel nanohybrid composite of magnetic chitosan-salicylaldehyde/nanoclay (MCH-SAL/NCLA) was hydrothermally synthesized for removal of azo dye (acid red 88, AR88) from simulated wastewater. Response surface methodology combined with the Box-Behnken design (RSM-BBD) was applied with 29 experiments to assess the impact of adsorption variables, that include A: % NCLA loading (0-50), B: MCH-SAL/NCLA dose (0.02-0.1 g/100 mL), C: pH (4-10), and time D: (10-90 min) on AR88 dye adsorption. The highest AR88 removal (75.16 %) as per desirability function was attained at the optimum conditions (NCLA loading = 41.8 %, dosage = 0.06 g/100 mL, solution pH = 4, and time = 86. 17 min). The kinetic and equilibrium adsorption results of AR88 by MCH-SAL/NCLA reveal that the process follows the pseudo-first-order and Temkin models. The MCH-SAL/NCLA composite has a maximum adsorption capacity (173.5 mg/g) with the AR88 dye. The adsorption of AR88 onto the MCH-SAL/NCLA surface is determined by a variety of processes, including electrostatic, hydrogen bonding, n-π, and n-π interactions. This research revealed that MCH-SAL/NCLA can be used as a versatile and efficient bio-adsorbent for azo dye removal from contaminated wastewater., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

An effective hydrothermally prepared chitosan-benzaldehyde/SiO 2 adsorbent (CTA-BZA/SiO 2 ) employed functionalization of a CTA biopolymer with SiO 2 nanoparticles and BZA. CTA-BZA/SiO 2 is an adsorbent that was utilized for the adsorption of an acidic dye (acid red 88, AR88) from synthetic wastewater. The fundamental adsorption variables (A: CTA-BZA/SiO 2 dosage (0.02-0.1 g); B: pH (4-10); and C: duration (10-60)) were optimized via the Box-Behnken design (BBD). The Langmuir and Freundlich isotherms (coefficients of determination R 2  = 0.99) agreed well with empirical data of AR88 adsorption by CTA-BZA/SiO 2 . The pseudo-first-order model showed reasonable agreement with the kinetic data of AR88 adsorption by CTA-BZA/SiO 2 . The maximal AR88 adsorption capacity (q max ) for CTA-BZA/SiO 2 was identified to be 252.4 mg/g. The electrostatic attractions between both the positively charged CTA-BZA/SiO 2 adsorbent and the AR88 anions, plus the n-π, π-π, and H-bond interactions contribute to the favourable adsorption process. This study reveals that CTA-BZA/SiO 2 has the capacity to be a suitable adsorbent for the removal of a wider range of organic dyes from industrial effluents., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Recycling waste from the production and consumption of heat-resistant alloys to return them to production is an urgent task due to the high cost of the components contained in these alloys. The kinetics and conditions of the acid leaching process of the grinding waste of a heat-resistant nickel alloy are studied depending on the composition of the acid solution (H 2 SO 4 , HCl, HNO 3 , and their mixtures) at room temperature to boiling point temperature and various acid concentrations (1.5 to 3.0 mol/L), ratios of waste to solution (1:10 to 3:10), fraction sizes (0.04-1 mm), and contact duration (1 to 120 h). The linearization of experimental data by the Gray-Weddington, Gistling-Brownstein, and Kazeev-Erofeev equations showed that the rate of the leaching process was influenced by both the chemical reactions between sulfuric acid and metals included in the grinding waste and the diffusion of reagents through the film of reaction products and undissolved impurities. Optimal conditions for acid dissolution of the grinding waste have been established to obtain the maximum degree of extraction of the main component of the alloy, nickel. The processing of powder particles with a size of less than 0.1 mm should be carried out in a solution of sulfuric acid with a concentration of 3.0 mol/L at a temperature of 100 °C for 6 h with a ratio of solid to liquid phases of 1:10. The reported results are very important for industry personnel to recover metals and for environmentalists to treat the alloy waste.

In this study, a magnetic chitosan grafted-benzaldehyde (CS-BD/Fe 3 O 4 ) was hydrothermally prepared using benzaldehyde as a grafting agent to produce a promising adsorbent for the removal of acid red 88 (AR88) dye. The CS-BD/Fe 3 O 4 was characterized by infrared spectroscopy, surface area analysis, scanning electron microscopy-energy dispersive X-ray, vibrating sample magnetometry, powder X-ray diffraction, CHN elemental analysis, and point of zero charge (pH PZC ). The Box-Behnken design (BBD) was adopted to study the role of variables that influence AR88 dye adsorption (A: CS-BD/Fe 3 O 4 dose (0.02-0.1 g), B: pH (4-10), and time C: (10-90 min)). The ANOVA results of the BBD model indicated that the F-value for the AR88 removal was 22.19 %, with the corresponding p-value of 0.0002. The adsorption profiles at equilibrium and dynamic conditions reveal that the Temkin model and the pseudo-first-order kinetics model provide an adequate description of the isotherm results, where the maximum adsorption capacity (q max ) with the AR88 dye was 154.1 mg/g. Several mechanisms, including electrostatic attraction, n-π interaction, π-π interaction, and hydrogen bonding, regulate the adsorption of AR88 dyes onto the CS-BD/Fe 3 O 4 surface. As a result, this research indicates that CS-BD/Fe 3 O 4 can be utilized as an effective and promising bio-adsorbent for azo dye removal from contaminated wastewater., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Contemporary food marketing is ruined by flavor enhancers rather than emphasizing the nutritional value of food. Vanillin is an overexploited flavor enhancer added to food items, thereby necessitating its detection. In this study, an electrochemical sensor was designed using a modified electrode made up of La 2 NiO 4 functionalized carbon nanofiber (f-CNF) to effectively detect vanillin in food samples. To confirm the successful formation of La 2 NiO 4 /f-CNF, structural and morphological studies were performed using X-ray diffraction, Raman spectroscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy. Further electrochemical analysis was performed using cyclic voltammetry and differential pulse voltammetry techniques, which resulted in high sensitivity (0.2899 µA·μM -1 ·cm -2 ) and low limit of detection (LOD) (6 nM). This modified electrode material was tested in food samples, which showed an excellent response with recovery percentage and is a promising electrocatalyst for vanillin detection., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

The sophisticatedly altered Hummer's and sol-gel procedures were applied for the synthesis of graphene oxides and porous silica monolith particles respectively. The Fischer esterification protocol was used for coupling silica monoliths with graphene oxides. A N -phenyl acrylamide-incorporated porous polymer was synthesized at the surface of composites via reversible addition fragmentation chain transfer polymerization. The composition was confirmed by Fourier transform infra-red spectroscopy, FE-SEM, X-ray diffraction, zeta potential (zeta pH), Brunauer-Emmett-Teller (BET/BJH) analysis, and EDAX analysis. The resulting polymer-bound composite efficiently removed Cr(vi) and Cr(iii) from waste water. Adsorption parameters such as contact time, pH effect, temperature, and adsorbent and adsorbate concentration were optimized for the optimal output of the composite. The kinetic and equilibrium models were applied to the adsorption of Cr(vi) and Cr(iii) at the adsorbent surface. The maximum adsorption capacity ( q e ) of Cr(vi) and Cr(iii) was found to be 298.507 mg g -1 and 401.874 mg g -1 , respectively, using the same initial concentration of Cr(vi) and Cr(iii) [10-60 ppm]. The adsorption data of both states of the Cr-metal followed the pseudo 2nd-order kinetic model with regression values of 0.996 ∼ Cr(vi) and 0.999 ∼ Cr(iii) at ambient temperature. Similarly, the adsorption data of Cr(vi) best fit into the Langmuir adsorption isotherm ( R 2 = 0.972) while that of Cr(iii) followed the Freundlich model ( R 2 = 0.983)., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)

Organic monolithic columns are mainly used to separate macromolecules; however, many attempts to extend their performance toward small molecules were examined by incorporating micro- and nanoparticles. The incorporation technique enabled utilizing organic monoliths in gas chromatography (GC) for small molecules, which are still scarce. Here, we prepared a composite matrix of capillary monolithic columns of a zeolite-like metal-organic framework with a sodalite topology (sod-ZMOF) and Divinylbenzene polymer (DVB) for GC separations under 0.5 MPa. Relatively short DVB monolithic columns (18 cm long × 0.25 mm i.d.) incorporated with a tiny amount of sod-ZMOF nanoparticles (0.7 and 1.17 wt%) with an average particle size of 225 nm were successfully fabricated and used to separate linear alkanes and polar probes mixtures with increasing resolution up to 3.7 and 5.1 times, respectively, compared to a blank DVB monolithic column. A high-performance separation of linear alkanes series mixture (methane to decane) was exhibited in less than 2 min. McReynolds constants revealed that sod-ZMOF provided the composite monolith with a nonpolar character yielding a negative average polarity value smaller than the standard squalene column. An Excellent retention time of pentane and octane day-to-day reproducibility was achieved during 16 days and over more than 500 runs with RSD% of 2.25% and 3.3% using a composite monolithic column with 5 mg mL -1 sod-ZMOF (5-ZMOF@DVB). In addition, a qualitative determination of the gas mixture content of three commercially available Lighter gas cartridges was performed via the 5-ZMOF@DVB column. Finally, successfully separating an azeotropic freon mixture of difluoromethane (R-32) and pentafluoroethane (R-125) was achieved with a selectivity of up to 4.84. A further thermodynamic study related the preferential adsorption of R-125 to entropic factors rather than enthalpic while trapping inside ZMOF pores. This work sheds light on utilizing the infinite diversity of MOFs and combining their properties with high permeability and easily fabricated organic monoliths for GC separations of light molecules and gasses. Furthermore, the study highlights the role of GC as an easy and fast approach for the preliminary evaluation of the separation efficiency of porous polymers., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Thermal treatment is applied for the direct conversion of palm stalk waste to Fe 3 O 4 (np)@carbon sheets (Fe 3 O 4 (np)@CSs). The effect of conversion temperature was investigated. The TEM examination of the prepared magnetic Fe 3 O 4 (np)@CSs showed the formation of Fe 3 O 4 (np) in a matrix of carbon sheets as a coated layer with surface functional groups including carbonyl and hydroxyl groups. Removal of dyes such as methyl orange, methylene blue, and neutral red was achieved using fabricated Fe 3 O 4 (np)@CSs which were prepared at 250 °C, 400 °C, and 700 °C in a weak acidic medium. By studying the contact time effect for the adsorption of methylene blue, neutral red, and methyl orange, using the fabricated Fe 3 O 4 (np)@CSs which were prepared at 250 °C and 400 °C, equilibrium occurred between 120 min and 180 min. In addition, the first-order and second-order kinetic models were applied to the adsorption data. The results revealed that the adsorption data fit better with the second-order kinetic model. Furthermore, the Freundlich model was found to be more suitable for describing the process of the separation of the dyes onto Fe 3 O 4 (np)@CSs which were prepared at 250 °C and 400 °C, suggesting heterogenous surfaces and multi-layer adsorption.