Barrett Joyner Halenda Research Articles

Copper‐Catalyzed Simultaneous Dehydrogenation and Enantioselective Allylic Oxidation of Alkanes Using Chiral Heterogeneous Ligands to Produce Allylic Esters and Theoretical Investigation of the Mechanism

ABSTRACTA new asymmetric method for preparing chiral allylic esters from various unactivated alkanes through simultaneous dehydrogenation and enantioselective allylic oxidation in the presence of chiral heterogeneous oxazoline–based ligands is reported for the first time. For this purpose, chiral amino oxazoline ligands, synthesized from chiral amino alcohols and cyanogen bromide, were immobilized on modified MCM‐41 mesoporous silica. These chiral heterogeneous ligands were then characterized using Fourier‐transform infrared spectroscopy, thermogravimetric analysis, X‐ray diffraction, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, and Brunauer–Emmett–Teller and Barrett–Joyner–Halenda techniques. Finally, copper complexes of these ligands were employed in the synthesis of chiral allylic esters, achieving the best result with a 90% yield and 77% enantiomeric excess. Evaluation of the recyclability of the chiral heterogeneous catalysts revealed that they can be reused three times without a noticeable reduction in the results. In addition, the mechanism of formation of the chiral allylic esters was investigated using a density functional theory method.

Nanostructured Magnetite Coated with BiOI Semiconductor: Readiness Level in Advanced Solar Photocatalytic Applications for the Remediation of Phenolic Compounds in Wastewater from the Wine and Pisco Industry

Heterogeneous photocatalysis is an advanced, efficient oxidation process that uses solar energy to be sustainable and low-cost compared to conventional wastewater treatments. This study synthesized BiOI/Fe3O4 using the solvothermal technique, evaluating stoichiometric ratios of Bi/Fe (2:1, 3:1, 5:1, and 7:1) under simulated solar irradiation to optimize the degradation of caffeic acid, a pollutant found in wastewater from the wine and pisco industry. The nanomaterial with a 5:1 ratio (BF-5) was the most effective, achieving a degradation of 77.2% in 180 min. Characterization by X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Brunauer–Emmett–Teller (BET), Barrett–Joyner–Halenda (BJH), Fourier Transform Infrared Spectroscopy (FTIR), Diffuse Reflectance Spectroscopy (DRS), and Vibrating Sample Magnetometry (VSM) showed that BF-5 has a porous three-dimensional structure with BiOI nanosheets coating the Fe3O4 surface, while retaining the pristine BiOI properties. The magnetite provided magnetic properties that facilitated the recovery of the photocatalyst, reaching 89.4% recovery. These findings highlight the potential of BF-5 as an efficient and recoverable photocatalyst for industrial applications. The technical, economic, and environmental feasibility were also evaluated at the technological readiness level (TRL) to project solar photocatalysis in real applications.

Initial evaluation of waste phosphogypsum for its use as a precursor for bioceramic materials

In this study, the phosphogypsum waste taken from various places in the factory dump located in Kėdainiai (Lithuania) was reinspected and characterised by different physico-chemical characterisation methods. The results of X-ray diffraction analysis, thermogravimetric analysis and differential scanning calorimetry, Fourier transform infrared spectroscopy, energy-dispersive X-ray analysis, elemental analysis using inductively coupled plasma optical emission and X-ray fluorescence spectroscopy confirmed that the main crystalline phase of the phosphogypsum waste is gypsum (CaSO4·2H2O). The surface morphology of the investigated materials was analysed using scanning electron microscopy. The specific surface area was determined by the Brunauer–Emmet–Teller method. The pore size distribution of the material produced was obtained using the Barrett–Joyner–Halenda method. This study also demonstrated that the phosphogypsum waste could be successfully used as a precursor for the dissolution-precipitation synthesis of high quality bioceramic calcium hydroxyapatite.

Green synthesis of silver/silver oxide nanostructures using the Malva sylvestris extract prior to simultaneous distillation extraction: synthesis, phytochemical and biological analysis.

Nanotechnology and nanoscience are due to their numerous uses in medicine, engineering, and water pollution sensors and their expanding research fields. In this study, the essential oil, methanolic extract, and biosynthesized silver/silver oxide nanostructures (Ag/AgO NSs) using the aqueous extract of the plant were prepared. The phytochemical compounds of the extract and essential oil were analyzed using gas chromatography/mass spectrometry (GC/MS), respectively. The GC/MS technique identified 34 compounds in the essential oil of the plant with the major constituents including oleic acid (18.5%), palmitic acid (11.08%), phytone (6.64%), p-vinylguaiacol (6.4%), and phytol (4.23%). After the phytochemical identification, the total flavonoid and polyphenol contents of the extract was determined, too. Prodelphinidin B3 compound in the Malva sylvestris extract was analyzed and detected by high-performance liquid chromatography/ultraviolet detector (HPLC-UV), at a retention time of around 10 min. In addition, M. sylvestris extract was used for green synthesis of Ag/AgO NSs. The as-prepared NPs were characterized using X-ray diffraction (XRD), UV-visible absorption spectroscopy, scanning electron microscope equipped with energy-dispersive X-ray spectroscopy (SEM/EDS), Brunauer-Emmett-Teller (BET), Barrett-Joyner-Halenda (BJH), and Fourier transform infrared (FT-IR) analyses. Surface plasmon resonance (SPR) absorption at λmax 320 nm in the UV-vis spectra confirms the formation of Ag/AgO NSs. The crystalline structure of Ag/AgO NSs was confirmed by XRD analysis.The nanoparticles were found to have a small size, measuring 64.16 nm, 44.33 nm, and 50 nm using the Williamson-Hall, Scherrer, and SEM/EDS methods, respectively. Besides, that spherical shape of Ag NPs with good size distribution was observed in the SEM/EDS analysis. The small size, around 50 nm, and spherical shape of Ag/AgO NSs with good size distribution were observed in the SEM/EDS analysis. Besides, the antibacterial activity of the extract was evaluated against three pathogenic bacteria, by disk diffusion method. Significant antibacterial activity was observed for the prepared extracts of M. sylvestris against the bacteria (Bacillus subtilis, Escherichia coli, and Pseudomonas aeruginosa), and the results were compared with the known antibiotics such as amoxicillin, cephalexin, erythromycin, and fluconazole.

Zeolitic imidazolate framework-67/barium zirconate titanate nanocomposite, Part I: Synthesis, characterization, and boosted photocatalytic activity

Using BaTi0.85Zr0.15O3/ZIF-67 (BTZ/ZIF-67) nanocomposite, tetracycline (TC) was photodegraded. Characterization of the samples was carried out using a variety of techniques, including XRD, FESEM-EDS (Field Emission Scanning Electron Microscopy – Energy Dispersive X-ray Spectroscopy), FT-IR (Fourier Transform Infra-Red), TEM (Transmission Electron Microscopy), BET (Brunauer-Emmett-Teller), BJH (Barrett-Joyner-Halenda), PL (Photoluminescence), TG-DTG (Thermogravimetry and Derivative Thermogravimetry), and UV–Vis DRS (Diffuse Reflectance Spectroscopy). BTZ/ZIF-67 nano-composites were synthesized using a one-step co-precipitation method. BTZ (30 %wt)/ZIF-67 showed the most impressive photocatalytic ability among the binary photocatalysts. Averaging the crystallite sizes of the nanocomposite samples identified by Scherrer and Williamson-Hall methods was 43.3 nm and 65.0 nm, respectively. The pHpzc values of samples of BTZ and BTZ (30 %wt)/ZIF-67 were approximately 6.7 and 10.0, respectively. Using the proposed method, we measured 357, 414, and 377 nm absorption edges for ZIF-67, BTZ, and BTZ (30 %wt)/ZIF-67 samples, which correspond to 3.47, 2.99, and 3.28 eV bandgap energies, respectively. The specific surface areas of BTZ, ZIF-67, and BTZ (30 %wt)/ZIF-67 nanocomposite are 122.15, 1218, and 1509 m2g−1, respectively. Under optimum conditions (0.8 g/L of the catalyst, CTC: 30 mg/L, and a pH 5), 89.5 % of total organic carbon (TOC) was removed within 180 min. Compared to BTZ photocatalyst, the BTZ (30 %wt)/ZIF-67 nanocomposite has a significantly larger surface area, thus enhancing photocatalytic activity. A synergistic effect was observed in the photodegradation of TC under Hg-lamp irradiation with the proposed BTZ/ZIF-67 composite. It is possible to alter the photocatalytic activity of the catalyst by changing the BTZ (30 %wt)/ZIF-67 ratio.

Sphere-like Nb2O5 nanoparticles by waste Brassica oleracea leaf extract for lead removal and photocatalytic degradation of methylene blue dye

Currently, water-soluble pollutants such as hazardous chemicals and pigments create severe environmental hazards. Heavy metals such as lead, chromium, mercury, and arsenic were dangerous to living beings even at very low levels. To overcome this limitation, Nb2O5 nanoparticles were created utilizing a novel green approach. Based on plant components, green technique is a low-cost, safe, and environmentally good solution. In the present inquiry, we employ phytonutrients from waste Brassica oleracea leaf juice as a capping and reducing component. The product was evaluated using XRD, FT-IR, UV, SEM, and TEM techniques. The findings showed that the produced Nb2O5 NPs had a sphere-like geometry having a median particle dimension of 9 nm confirmed by XRD analysis. SEM study reveals ultrafine, homogeneous morphological agglomerations and uniform granules in TEM analysis, 10–15 nm particles predicted by crystallography, orthorhombic Nb2O5 (001) planes matching 0.39 nm lattice edge measurement error, and a clearly defined SAED diffract signal implying polycrystalline calcined powder. Excitation absorbance bands at 350 nm may be caused by charged balancing in the Nb–O–Nb architecture increasing oxygen concentration confirmed by UV–Vis analysis. The Nb2O5 nanosphere has a surface area of 120 m2/g, 0.592 cm2/g of pores, and a mean pore dimension of 15.2 nm, determined using Barrett-Joyner-Halenda (BJH). A sequential Adsorption capacities assay shown that it is an effective absorber used to eliminate Pb (II) ions from aqueous solutions. Adsorbents was able to be readily removed from the resultant fluid and recycled repeatedly. The produced Nb2O5 Nanoparticles are capable of removing toxic heavy metals and synthetic colors from polluted waterways.

Resource recovery of water treatment plant sludge and river sediment as phosphorus removal material: feasibility and mechanisms

ABSTRACT Excessive phosphorus is a critical contributor to eutrophication, necessitating the use of substantial amounts of phosphorus removal materials. To address the challenge of managing water treatment plant sludge and river sediment while also supplying mass-produced phosphorus-removing materials for projects targeting phosphorus removal in water bodies, this paper attempted to study the feasibility of preparing phosphorus removal materials by mixing and calcining water treatment plant sludge and river sediment (C-WTPS/RS). The study examined the transformation of phosphorus forms in C-WTPS/RS before and after adsorption. Furthermore, X-ray fluorescence spectrometer, zeta potential, scanning electron microscope, Brunauer–Emmett–Teller equation, Barrett–Joyner–Halenda model, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy were employed to elucidate the phosphorus removal mechanisms. The results showed that C-WTPS/RS was effective in removing phosphorus from water and preventing the release of phosphorus from the sediment. Additionally, C-WTPS/RS had a low risk of releasing phosphorus and metals within the pH range of natural water bodies. These proved that it is feasible to remove phosphorus by C-WTPS/RS. After adsorption, the increased phosphorus in C-WTPS/RS was mainly dominated by the non-apatite inorganic phosphorus within inorganic phosphorus. The main phosphorus removal mechanisms of C-WTPS/RS were physical adsorption, electrostatic adsorption, chemical precipitation, and ligand exchange.

Dried Blood Matrix as a New Material for the Detection of DNA Viruses.

The gold standard for diagnosing viruses such as the Hepatitis B Virus has remained largely unchanged, relying on conventional methods involving extraction, purification, and polymerase chain reaction (PCR). This approach is hindered by limited availability, as it is time-consuming and requires highly trained personnel. Moreover, it suffers from low recovery rates of the nucleic acid molecules for samples with low copy numbers. To address the challenges of complex instrumentation and low recovery rate of DNA, a drying process coupled with thermal treatment of whole blood is employed, resulting in the creation of a dried blood matrix characterized by a porous structure with a high surface-to-volume ratio where it also inactivates the amplification inhibitors present in whole blood. Drawing on insights from Brunauer-Emmett-Teller (BET)- Barrett-Joyner-Halenda (BJH) analysis, scanning electron microscopy (SEM), and fluorescence recovery after photobleaching (FRAP), detection assay is devised for HBV, as a demonstration, from whole blood with high recovery of DNA and simplified instrumentation achieving a limit of detection (LOD) of 10 IU mL-1. This assay can be completed in <1.5 h using a simple heater, can be applied to other DNA viruses, and is expected to be suitable for point-of-care, especially in low-resource settings.

Electrochemical aptasensor based on RGO/PPy/Au*NPs for diagnostic biosensing of SARS-CoV-2 in clinical samples: Experimental and molecular dynamics simulations approaches

A highly sensitive and selective E-DNA biosensor was fabricated on a gold substrate using a reduced graphene oxide/polypyrrole/gold nanoparticle/oligonucleotide (RGO/PPy/Au*NPs/Apt) nanocomposite electrode to detect the nucleocapsid protein of SARS-CoV-2 in the patient blood plasma. The modified electrode was characterized by physicochemical techniques such as Fourier transform-infra red (FT-IR), Raman spectroscopy, X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS) analyses, Brunauer-Emmett-Teller (BET), and Barrett-Joyner-Halenda (BJH) analyses. Moreover, electrochemical analyses were employed to study the electrochemical performance of the electrodes including cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and square wave voltammetry (SWV). Computational investigations of N protein bindings such as hydrogen bonding, Van der Waals binding, and Gibbs binding energies of the N-protein, and aptamer were studied by Molecular Dynamics Simulations (MDS). The unique synergistic effect of RGO, PPy, and the well-known effect of Au nanoparticles makes the DNA probe immobilized on the gold electrode surface. After optimizing the systems, the E-DNA biosensor exhibited a fast SWV response, higher sensitivity (33.77 μA.nM−1.cm−2) and selectivity, high efficiency, good storage stability, and acceptable repeatability for monitoring DNA. The results of real samples based on SWV indicated the correct functioning of the aptasensor in the presence of the SARS-CoV-2 virus. The limit of detection was 3.16×10−17 M and the limit of quantitation was 1.42×10−16 M. The MDS results indicated the stable dynamic folding of the aptamer for beneficial binding. The results indicated that the RGO/PPy/Au*NPs/Apt biosensor is promising for detecting of SARS-CoV-2 virus.

PEDOT-Doped Mesoporous Nanocarbon Electrodes for High Capacitive Aqueous Symmetric Supercapacitors.

Poly(3,4-ethylenedioxythiophene) (PEDOT) and PEDOT-functionalized carbon nanoparticles (f-CNPs) were synthesized by in situ chemical oxidative polymerization and pyrolysis methods. f-CNP-PEDOT nanocomposites were prepared by varying the concentration of PEDOT from 1 to 20% by weight (i.e., 1, 2.5, 5, 10, and 20 wt%). Several characterization techniques, such as field-emission scanning electron microscopy (FESEM), attenuated total reflectance-Fourier transform infrared (ATR-FTIR), X-ray diffraction (XRD), N2 Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) analyses, as well as cyclic voltammetry (CV), galvanostatic charge discharge (GCD), and electrochemical impedance spectroscopy (EIS), were applied to investigate the morphology, the crystalline structure, the N2 adsorption/desorption capability, as well as the electrochemical properties of these new synthesized nanocomposite materials. FESEM analysis showed that these nanocomposites have defined porous structures, and BET surface area analysis showed that the standalone f-CNP exhibited the largest surface area of 801.6 m2/g, whereas the f-CNP-PEDOT with 20 wt% exhibited the smallest surface area of 116 m2/g. The BJH method showed that the nanocomposites were predominantly mesoporous. CV, GCD, and EIS measurements showed that f-CNP functionalized with 5 wt% PEDOT had a higher capacitive performance compared to the individual f-CNPs and PEDOT constituents, exhibiting an extraordinary specific capacitance of 258.7 F/g, at a current density of 0.25 A/g, due to the combined advantage of enhanced electrochemical activity induced by PEDOT doping, and highly developed porosity of f-CNPs. Symmetric aqueous supercapacitor devices were fabricated using the optimized f-CNP-PEDOT doped with 5 wt% of PEDOT as active material, exhibiting a high capacitance of 96.7 F/g at 1.4 V, holding practically their full charge, after 10,000 charge-discharge cycles at 2 A/g, thus providing the highest electrical electrodes performance. Hereafter, this work paves the way for the potential use of f-CNP-PEDOT nanocomposites in the development of high-energy-density supercapacitors.

Nano-CaO as a heterogeneous catalyst for biodiesel synthesis by transesterification of Jatropha oil

BackgroundThis research employs response surface methodology, specifically Central Composite Design (CCD), to optimize the process parameters for the effective production of biodiesel. Jatropha oil was utilized as the raw material to minimize expenses. A nanocatalyst was utilized as a solid catalyst, developed from CaCO3 via waste snail shells, offering advantages such as recyclability and improved catalytic activity during a transesterification process. The developed nanocatalyst was analyzed using various techniques, including dynamic light scattering (DLS), scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET) analysis, and Fourier-transform infrared (FTIR). The BET analysis revealed a surface area of 5.1m2/g and the Barrett-Joyner-Halenda (BJH) analysis provided insights into the pore volume and diameter of the synthesized nano-CaO, showing values of 0.002556 cc/g and 1.1 nm, respectively, indicating the presence of both microspores and active sites on the external surface of the nano-CaO catalyst. Biodiesel conversion was controlled by adjusting factors like the methanol to oil ratio, catalyst weight, reaction time, reaction temperature, and agitation speed. A quadratic model was established to explore the correlation between the independent variables and the biodiesel conversion rate. The results showed a maximum biodiesel conversion rate of 96.73% under the optimal conditions: methanol to oil ratio (6:1), catalyst weight (1.4 wt%), reaction time (60 min), reaction temperature (55 °C), and agitation speed (250 rpm). These parameters were determined through 32 experimental trials. The RSM technique yielded impressive results with a determined coefficient of determination (R2) of 0.9834, adjusted R2 of 0.8503, predicted R2 of 0.8309, and a coefficient of variance (CV) 0.75%. Based on the analysis of variance (ANOVA) findings, the model exhibits a high level of significance (p<0.0001), which is less than 0.05 and F- Value 29.71.The study aims to enhance the yield and efficiency of the transesterification process, thereby increasing the overall production of fatty acid methyl ester from Jatropha oil. This innovative approach efficiently generates biodiesel from renewable resources, in a manner that is both environmentally friendly and maximizes the effectiveness of the process parameters. The evaluation conform that the quality of the biodiesel met the standards set by ASTM D 6751 and EN 14214.

Metal-free adsorption and photodegradation methods for methylene blue dye removal using different reduction grades of graphene oxide

The release of organic pollutants and dyes into the environment by industries has had profound and harmful effects on both humans and ecosystems. Graphene oxide (GO) and its reduced form have been investigated for their effectiveness in removing pollutant dyes. GO nano-powder was synthesized using an improved version of Hummer's method and subsequently thermally reduced at various temperatures, including 125, 150, 175, and 200 °C, under vacuum conditions. In the X-ray diffraction spectra, an intense (001) diffraction peak was initially observed at 9.136° (2θ) for pristine GO. This peak gradually shifted towards higher angles as the reduction process took place and eventually disappeared when the GO was reduced at 200 °C. The intensity ratio of the D and G bands (ID/IG ratio) for GO nano-powder in the Raman spectra decreased from 0.94 to 0.76 due to the reduction process. The FTIR spectra of GO and reduced graphene oxide (rGO) also illustrated the reduction process. The bandgap of pristine GO significantly decreased from 2.31 to 0.73 eV, as determined by ultraviolet–visible (UV–Vis) diffuse reflectance spectrophotometry during the reduction process. The surface area and pore volume of both pristine GO and rGO-150 were determined using the BET (Brunauer-Emmett-Teller) and BJH (Barrett-Joyner-Halenda) methods. The results indicated an increase in the BET surface area from 6.61 to 7.86 m2/g and a corresponding enhancement in pore volume from 0.118 to 0.128 cc/g after reduction. The adsorption and photocatalytic degradation behavior of pristine GO and reduced graphene oxides (rGOs) were examined using methylene blue dye. The pristine GO demonstrated impressive adsorption capability, effectively removing the dye by 85.78 % within just 15 min and achieving nearly 97 % removal after 4 h. In contrast, the highest photocatalytic degradation of methylene blue, about 47.58 %, was attained for the rGO sample reduced at 150 °C under the illumination of visible light.

Fabrication of new in‐situ ternary nano/microcomposite LDH/Ag2O/Bayerite in trimetallic NiAg/Al layered double hydroxides for CO2 capture material

AbstractWe reported new in‐situ ternary nano/microcomposite layered double hydroxides/Ag2O/bayerite in trimetallic NiAg/Al layered double hydroxides (LDH) via hydrothermal technique; and characterization by powder X‐ray diffraction (XRD), Fourier transforms infrared spectroscopy (FT‐IR), field emission scanning electron microscopy (FE‐SEM), energy dispersive spectroscopy (EDS), and N2 adsorption‐desorption. The formation of bayerite and silver oxide species on the LDH nanosheet depended on the excess of Al3+ and Ag+ in the solution under alkaline and hydrothermal conditions. The nitrogen isotherm adsorption profile for all ternary composites exhibited uniformity with mesoporous and lamellar characteristics. The surface area of all the composites ranged from 81.17 to 150.23 m2. g−1, the Barret‐Joyner‐Halenda (BJH) pore volume from 0.22 to 0.27 cm3. g−1, and the average pore diameter ranged from 3.47 to 5.78 nm. All composites show a laminar plate‐like structure covered with elongated pieces. The particle size of the composites ranged from 54.86 to 115.96 nm, indicating the size changed from nano to microcomposite because of the different molar ratios of Ag and Ni in the solid. The ternary composite reveals CO2 capture activity with adsorption capacity ranging from 13.93 to 19.61 mmol g−1. © 2024 Society of Chemical Industry and John Wiley &amp; Sons, Ltd.

Synthesis and Characterization of Calcium Oxide Nanoparticles (CaO NPS) from Snail Shells Using Hydrothermal Method

Calcium oxide (CaO) holds significant importance as a catalyst and effective chemisorbent for hazardous gases. This study presents the synthesis of CaO nanoparticles (NPs) using the hydrothermal technique with snail shells' calcium carbonate (CaCO3) as the starting material. The hydrothermal method offers several advantages over alternative approaches for producing metal oxide NPs, including its simplicity, cost-effectiveness, and ability to operate at low temperatures and pressures. By utilizing waste materials like snail shells as a precursor, the entire process becomes more economical, environmentally friendly, and sustainable. The synthesized NPs were analyzed using various techniques, including Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), the Barrett-Joyner-Halenda (BJH) model for pore structure quantification, Brunauer-Emmett-Teller (BET) for surface area calculation, and thermo gravimetric analysis (TGA/DTA-DSC). XRD analysis confirmed that the size of the synthesized CaO NPs was 43.14 nm, determined using the Debye-Scherrer equation. The transmission electron microscopy (TEM) image provided valuable insight into the morphology of the nano-catalyst. The analysis revealed that the nano-catalyst displayed a spherical shape, with an average particle size measuring 50 nanometers. The FTIR and XRD results unequivocally demonstrated the successful conversion of calcium carbonate (CaCO3) derived from snail shells into calcium oxide (CaO). TGA exhibited a significant weight loss peak at 700 °C, indicating the transformation of CaCO3 into CaO. The DTA-DSC curve exhibited sharp endothermic peaks at 700 °C, suggesting a decomposition reaction and the formation of a new compound. SEM images displayed porous, rough, and fragile surfaces that became agglomerated at higher temperatures. In other words, the FE-SEM images of NPs illustrated that the particles were predominantly spherical in morphology. Hence, waste snail shells hold promise as a valuable source of calcium for various applications in different fields.

Production of biodiesel from waste cooking oil using a novel surface-functionalized CaMoO4/ TiO2 solid catalyst

This study involves the synthesis of a mesoporous CaMoO4/TiO2 solid catalyst through the impregnation method. The catalyst, known for its novelty, efficiency, and recyclability, was thoroughly characterized using various techniques, including Fourier Transform Infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Analysis (EDAX), Thermogravimetric Analysis (TGA), Brunauer-Emmett-Teller (BET), and Barrett-Joyner-Halenda (BJH) studies. Waste cooking oil is analysed using FTIR spectroscopy for its free fatty acid content. In addition, the specific catalytic activities are investigated under a variety of reaction conditions. A yield of 95.6 % is achieved under the standard trans esterification reaction operating parameters such as catalyst loading of 4 wt %, methanol to waste cooking oil molar ratio of 15:1 (v/v), reaction duration of 70 min, reaction temperature of 55 °C, stirring speed of 270 rpm, and temperature of calcination as 650 °C. The reaction kinetics (pseudo first order) is also studied. Solid catalysts can also be reused up to five successive times. Biodiesel is characterized by FTIR and 1H NMR studies to examine the presence of functional and methyl ester groups respectively, and the extracted biofuel met the specifications of ASTM D 6751 norms for standard diesel fuel.

Synthesis of Cu-MOF-derived complex copper–chromium oxides and their catalytic study on the thermal decomposition of ammonium perchlorate

In this work, a series of complex copper-chromium oxides were prepared by adjusting the molar ratio of Cr3+/Cu2+ using MOF-199 as a template. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) were used to characterize the structure, microscopic morphology and valence information of the samples. The specific surface area of the sample was estimated by the Brunauer-Emmett-Teller method (BET), and the pore size parameters of the sample were obtained by using the Barrett-Joyner-Halenda (BJH) model. The effect of the samples on the thermal decomposition process of ammonium perchlorate (AP) was investigated by differential scanning calorimetry-thermogravimetric analysis. The results show that the copper and chromium oxides in the complex exhibit good catalytic effects. Among them, CuCr(0.8) had the best catalytic effect, reducing the peak pyrolysis temperature of AP by 95.7 °C, increasing the heat release by 817 J/g, and reducing the reaction activation energy by 62.4 kJ/mol. Real-time FTIR was used to characterize the gas products during the thermal decomposition of AP, and the gas products of AP with CuCr(0.8) catalyst were different from those of pure AP, which may also be the reason for the increase of AP heat release after adding CuCr(0.8) catalyst.

ASSESSMENT OF SPECIFIC SURFACE AREA AND POROSITY OF SUBSOILS

Soils and subsoils have a complex structure consisting of several elements with different morphology and chemical composition, combining micro-, meso-, and macroporous substructures. Classical approaches, such as Brunauer-Emmett-Teller (BET) or Barrett-Joyner-Halenda (BJH) methods, cannot provide an accurate assessment of morphological characteristics of such solids, nor can do modern sophisticated numerical methods which depend on idealized models of pores that hardly reflect a real morphology of heterogeneous solids in question. The present study describes a way to overcome this difficulty by applying a combination of the αS-plot technique and a modified Remy-Poncelet method. The proposed approach allowed estimating the volumes of the untramicropores, supermicropores and the sum of meso- and macropores as well as the specific surface areas of the solid without ultramicropores and of the solid without all micropores. The former specific surface area is a more reasonable estimate of the area available for layer coverage than the BET specific surface area, and all together these characteristics provide a detail description of solid’s morphology. Subsoil samples excavated from different depths were used as exemplary solids. They mostly consisted of quartz, feldspar, and clay minerals and had different sorts of pores associated with the clay fraction and soil aggregates as well as a relatively large fraction of non-porous sand particles. Relations of the morphological properties with subsoil profile and mineralogical composition are discussed. For citation: Asnin L.D., Samoylov M.S., Pershina M.V., Tselishchev Yu.G., Sliusar N.N. Assessment of specific surface area and porosity of subsoils. ChemChemTech [Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol.]. 2024. V. 67. N 6. P. 55-64. DOI: 10.6060/ivkkt.20246706.6996.

Magnetic Three-Dimensional Graphene: A Superior Adsorbent for Selective and Sensitive Determination of Nitrite in Water Samples by Ion-Pair Based-Surfactant-Assisted Solid-Phase Extraction Combined with Spectrophotometry

A straightforward, fast and efficient analytical method was developed which utilizes a magnetic composite called three-dimensional graphene (3D-G@Fe3O4) as an adsorbent to recover nitrite ions (NO2−) from environmental water samples. The investigation into the synthesized adsorbent contained an examination of its morphology, chemical composition, structural attributes, and magnetic properties. This comprehensive analysis was conducted using various instrumental techniques, including Fourier transform-infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Raman spectroscopy, X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), Barrett-Joyner-Halenda (BJH), and vibrating sample magnetometry (VSM). The adsorbent surface was activated by adding cetyltrimethylammonium bromide (CTAB) to the sample solution. To improve the selectivity and sensitivity of the method, nitrite ions were reacted with sulfanilic acid and chromotropic acid sequentially. An orange-red azo-dye complex was formed in the presence of nitrite ions with a clear absorbance peak at 514 nm. The effect of the main experimental parameters such as the pH of the sample solution, adsorbent dosage, and CTAB dosage was explored, and the optimization process was performed using a central composite design (CCD). The linear dynamic range (20–100 ng mL−1) was determined under optimal experimental circumstances, yielding a reasonable determination coefficient (R2, 0.9993), a detection limit of 5.12 ng mL−1, an enrichment factor of 167, and precision values of 1.0% intraday and 2.9% inter-day. The methodology successfully identified minute nitrite ions in environmental water samples with relative recoveries that varied between 96.05 and 101.6 ng mL−1.

Implications of Temperature for the Modification of High-Overmature Shale Reservoirs: Experimental and Numerical Analysis

Summary High-temperature pore reconstruction technology is a reservoir reconstruction measure that has emerged in recent years. It is of great significance to study the variation in pore structure characteristics of shale under high temperature for reservoir reconstruction. To study the effect of high temperature on shale pores, scanning electron microscopy (SEM) experiments and fluid injection experiments were used to analyze the variation of pore structure characteristics under high temperature. Studies have shown that temperature has a great influence on the morphology and distribution characteristics of shale pores. In particular, there is a temperature between 300°C and 400°C that is suitable for modifying pores. The distribution characteristics, surface area, and volume of pores vary dramatically under this temperature threshold. The pore morphology and distribution characteristics changed from small and sparse to large and dense. The Brunauer-Emmett-Teller (BET) surface area increased by 95%. The cumulative surface area of Barrett-Joyner-Halenda (BJH) adsorption and desorption increased by 71.7% and 72%, respectively. The pore volume of the 2-nm to 20-nm pore size increased by 63.2%. The pore volume of pore sizes greater than 20 nm increased by 191.6%. The pore variation characteristics were in line with the typing law, and the fitting result R2 ranged from 0.92201 to 0.99882.

Ultrasound-assisted extractive-catalytic removal of micro-organic pollutants in liquid hydrocarbon fuels using highly active ZnO nanoparticles supported zinc-substituted phosphotungstate

To produce ultra-low sulfur diesel (ULSD), it is necessary to remove compounds such as 2-methylthiophene and 3-methylthiophene that cannot be isolated by conventional industrial methods. This paper presents, a phosphotungstate catalyst improved with zinc atoms placed on the surface of super active zinc oxide nanoparticles and is able to switch between two phases using a hydrophobic ionic liquid (transfer agent). Here, is a description of the synthesis of the α-keggin type hybrid nanocatalyst and its application for the removal of 2- methylthiophene and 3-methylthiophene. The nanocatalyst was subjected to various characterization techniques, including Fourier Transform Infrared Spectrometer (FTIR), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) Surface Area Analysis, Barrett-Joyner-Halenda (BJH) pore size and volume analysis and Energy-dispersive X-ray analysis(EDAX). The optimized conditions for the ultrasound-assisted extractive-catalytic oxidative desulfurization (UA-ECODS) process were determined using a statistical design, specifically the Box-Behnken design (BBD), which was proposed as a plan for designing experiments and studying the behavior of the parameters. The optimal conditions, which encompass four parameters, namely ultrasonic time, reactor temperature, amount of nanocatalyst, and oxidant concentration, are archived as 14.43 min, 40.52 °C, 86.27 mg catalyst, and 24 % H2O2 Respectively. The results indicated that the removal efficiency was higher for 2- methylthiophene than 3-methylthiophene. The paper concludes that the UA-ECODS method utilizing the synthesized nanocatalyst is a promising and effective approach for desulfurizing of liquid hydrocarbon fuels.