X-ray Diffraction Research Articles

Azobenzene-Based Main-Chain Liquid Crystalline Polymers Bearing Periodically Installed Alkyl, PEG, or Fluoroalkyl Segments and Photoisomerization Studies

ABSTRACT In the present study, liquid crystalline polymers (LCPs) were prepared by melt-transesterification of azobenzene-bearing diols and diethyl malonate (DEM) derivatized monomers. The effect of the nature and length of the installed pendant segments on the mesomorphic properties of the prepared LCPs was investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD), and polarized optical microscopy (POM) studies. The formation of layered morphology was inferred from X-ray scattering analysis arising from the colocation of rigid azobenzene moieties in one layer and the flexible pendant segments in alternate layers due to the zigzag folding of the polymer backbone. The linear variation of the interlamellar spacing with the number of carbon atoms in the pendant alkyl segments corroborates the proposed zigzag backbone folding in the polymers. The rate constant values obtained from the photoisomerization studies of the isomeric polymers and model compound, which are in the same ballpark, reveal that the photoisomerization process of such polymers is not affected by the position or size of the azobenzene unit.

Novel peptides with calcium‐binding capacity from antler bone hydrolysate, its bioactivity on MC3T3‐E1 cells, and the possible chelating mode

AbstractIn this study, peptide‐calcium chelate was screened from antler bone hydrolysate, and its bioactivity on MC3T3‐E1 cells and its chelating mechanism were investigated. In vitro experiments showed that peptide‐calcium chelate promoted the differentiation and mineralization of MC3T3‐E1 cells. Subsequently, three novel calcium‐chelating peptides were obtained from antler bone hydrolysate using hydroxyapatite chromatography (HAC), Sephadex G‐25 gel filtration chromatography, and reversed‐phase high‐performance liquid chromatography (RP‐HPLC). Meanwhile, this work determined peptides' amino acid sequences as TKLGTQLQL, LETVILGLLKT, and KMVFLMDLLK based on LC–MS/MS. Then the present work prepared the three peptides, with the corresponding calcium‐chelating rates being verified as 87.68 ± 2.86%, 80.72 ± 0.93%, and 67.96 ± 0.98%, respectively. Fourier transform infrared (FTIR) spectroscopy, ultraviolet–visible absorption (UV–vis) spectroscopy, X‐ray diffraction (XRD), circular dichroism (CD), zeta potential, and molecular dynamics (MD) simulations were adopted to investigate the chelating mode of peptides with calcium ions. As a result, oxygen in the carboxyl group and the nitrogen in the amino group were related to calcium binding. In addition, the chelation site preferred the negatively charged carboxylate groups of Leu or Thr. The present work revealed that antler bone might be the new calcium‐chelating peptide source and elucidated their positive role in osteogenesis.

Effect of nanoparticles reinforcement of Silicon dioxide derived from prosopis juliflora on Silver-Grey Magnesium nanocomposite: Utilization of Silicon dioxide mechanical and tribological properties

Abstract The automotive and aviation industries require lightweight materials to enhance working efficiency. Composites combine materials such as aluminium, magnesium, titanium, steel, and copper with various forms of reinforcements to offer lightweight alternatives for a range of applications. The present investigation aims to fabricate a Silver-Grey Magnesium (Mg-25%Si) alloy-based nanocomposite with silicon dioxide (SiO2) nano reinforcement at weight % of 0, 3.25, 6.5 and 9.75 utilizing the two step stir casting method. Prosopis juliflora is utilized in the production of different weight percentages of SiO2 nano reinforcements. The microhardness, tensile, wear, and impact tests are performed on the Silver-Grey Magnesium nanocomposites (Mg-25%Si/SiO2) utilizing a computerized tensometer testing machine, a Vicker’s hardness tester, a pin-on-disc tribometer, and an Izod impact, respectively. The X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), and Energy-dispersive X-ray spectroscopy (EDAX) with elemental mapping microstructure were employed to scrutinize the tensile specimen fracture, EDAX, elemental mapping microstructure, wear, CoF, and worn surface characterization and impact strength analysis. When compared to the Silver-Grey Magnesium (Mg-25%Si) base alloy, the results of the Mg-25%Si/SiO2 nanocomposites demonstrated an increase in SiO2 nano reinforcements that significantly increased microhardness, tensile strength, wear resistance, and impact strength. The corresponding values are 113.36 VHN, yield and ultimate tensile strength of 603.25 MPa and 665.84 MPa, 0.00478 mm3/m, CoF of 0.38421 and 400 J/m.

Atomic Layer Deposition of Nickel Using Ni(dmamb)2 and ZnO Adhesion Layer Without Plasma

In this study, a novel deposition technique that utilizes diethylzinc (C4H10ZnO) with H2O to form a ZnO adhesion layer was proposed. This technique was followed by the deposition of vaporized nickel(II) 1-dimethylamino-2-methyl-2-butoxide (Ni(dmamb)2) and H2 gas to facilitate the deposit of uniform layers of nickel on the ZnO adhesion layer using atomic layer deposition. Deposition temperatures ranged from 220 to 300 °C. Thickness, composition, and crystallographic structure results were analyzed using spectroscopic ellipsometry, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD), respectively. An average growth rate of approximately 0.0105 angstroms per cycle at 260 °C was observed via ellipsometry. Uniform deposition of ZnO with less than 1% of Ni was displayed by utilizing the elemental analysis function via SEM, thereby providing high-quality images. XPS revealed ionizations consistent with nickel and ZnO through the kinetic and binding energies of each detected electron. XRD provided supplemental information regarding the validity of ZnO by exhibiting crystalline attributes, revealing the presence of its hexagonal wurtzite structure.

The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

The AUREX cell: a versatile <i>operando</i> electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

Impact of TBAI Doping on the Optical and Dielectric Features of PVC/MoO3/NiMoO4/PANI Polymer Composite for Optoelectronic and Energy Storage Applications

Abstract Poly (vinyl chloride, PVC)/MoO3/NiMoO4/polyaniline (PANI)/x wt % tetrabutylammonium iodide (TBAI) polymers were formed using casting and hydrothermal methods. The present study examined the nanocomposites' structural, electrical, and optical features comprising PVC/MoO3/NiMoO4/PANI/x wt %TBAI polymers. X-ray diffraction and scanning electron microscopy were used to investigate the structure and morphology of different samples. The influence of different amounts of TBAI on the linear and nonlinear optical features of PVC/MoO3/NiMoO4/PANI/x wt %TBAI polymers was explored. Adding MoO3/NiMoO4/PANI.TBAI reduced the direct and indirect optical band gaps to their minimum values (3.88, 3.04) eV and (3.58, 2.13) eV, respectively. Doped polymer with MoO3/NiMoO4 has the highest refractive index value. Only PVC filled with MoO3/NiMoO4 exhibits the highest non-linear optical parameters within the visible range. The fluorescence intensity and emitted colors influenced by the kind of dopant. The dielectric constant and ac conductivity values of the host polymer were affected by the amount of TBAI. The maximum energy density value was observed in PVC/MoO3/NiMoO4/PANI/10 wt %TBAI polymer. The Cole-Cole plot demonstrated an irregular shift for doped samples relative to the undoped. The obtained results nominated the nanocomposite films of PVC/MoO3/NiMoO4/PANI/x wt %TBAI to be used in diverse electric and optoelectrical applications.&amp;#xD;

Synergistic effect of curcumin and tamoxifen loaded in pH-responsive gemini surfactant nanoparticles on breast cancer cells

BackgroundDrug combination therapy is preferred over monotherapy in clinical research to improve therapeutic effects. Developing a new nanodelivery system for cancer drugs can reduce side effects and provide several advantages, including matched pharmacokinetics and potential synergistic activity. This study aimed to examine and determine the efficiency of the gemini surfactants (GSs) as a pH-sensitive polymeric carrier and cell-penetrating agent in cancer cells to achieve dual drug delivery and synergistic effects of curcumin (Cur) combined with tamoxifen citrate (TMX) in the treatment of MCF-7 and MDA-MB-231 human BC cell lines.MethodsThe synthesized NPs were self-assembled using a modified nanoprecipitation method. The functional groups and crystalline form of the nanoformulation were examined by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and dynamic light scattering (DLS) used to assess zeta potential and particle size, and the morphological analysis determined by transmission electron microscopy (TEM). The anticancer effect was evaluated through an in vitro cytotoxicity MTT assay, flow cytometry analysis, and apoptosis analysis performed for mechanism investigation.ResultsThe tailored NPs were developed with a size of 252.3 ± 24.6 nm and zeta potential of 18.2 ± 4.4 mV capable of crossing the membrane of cancer cells. The drug loading and release efficacy assessment showed that the loading of TMX and Cur were 93.84% ± 1.95% and 90.18% ± 0.56%, respectively. In addition, the drug release was more controlled and slower than the free state. Polymeric nanocarriers improved controlled drug release 72.19 ± 2.72% of Tmx and 55.50 ± 2.86% of Cur were released from the Tmx-Cur-Gs NPs after 72 h at pH = 5.5. This confirms the positive effect of polymeric nanocarriers on the controlled drug release mechanism. moreover, the toxicity test showed that combination-drug delivery was much more greater than single-drug delivery in MCF-7 and MDA-MB-231 cell lines. Cellular imaging showed excellent internalization of TMX-Cur-GS NPs in both MCF-7 and MDA-MB-231 cells and synergistic anticancer effects, with combination indices of 0.561 and 0.353, respectively.ConclusionThe combined drug delivery system had a greater toxic effect on cell lines than single-drug delivery. The synergistic effect of TMX and Cur with decreasing inhibitory concentrations could be a more promising system for BC-targeted therapy using GS NPs.

Characterisation and analysis of soil properties and trace elements in agricultural soils of Rabat-Sale-Kenitra, Morocco: focus on stable strontium and caesium

ABSTRACT This study explores strontium (Sr) and caesium (Cs) dynamics in Moroccan agricultural soils, focusing on contaminant impacts and soil properties. Soil samples from El Koudia, Merchouch, and El Guich exhibit different textures: clayey (Merchouch), sandy clay loam (El Koudia), and sandy (El Guich). Chemical analysis shows consistent pH, with %CaCO3 at 1%, 4%, and 6%, and organic matter content at 4.5%, 1.1%, and 3.3% in Merchouch, El Guich, and El Koudia, respectively. Cation exchange capacity (CEC) and levels of Ca, K, Na, Mn, and Fe were measured. X-ray diffraction (XRD) identified quartz as the main mineral, with site-specific variations. X-ray fluorescence spectrometry (XRF) indicated consistent Cr, Ni, Cu, Zn, As, and Pb levels, and Rb varied significantly. Sr concentrations were 0.17 ppm in El Koudia and Merchouch, and 0.32 ppm in El Guich. Cs was undetected. This research highlights complex soil properties, elemental composition, and contaminant distribution in agricultural soils.

Green Synthesis of Metal Nanoparticles with Borojó (Borojoa patinoi) Extracts and Their Application in As Removal in Water Matrix

The predominant aim of the current research was to generate a proposal for the removal of arsenic, a highly toxic pollutant, encountered within the Papallacta Lagoon in Ecuador. The average concentrations of As yielded ranges between 18 to 652 μg/L, through the use of metallic nanoparticles. Sampling was performed in the lagoon with their respective geographic locations and “in situ” parameters. Nanoparticles of Mn3O4 NPs, Fe3O4 NPs, and CuO NPs were synthesized at a 0.5 M concentration, using the precipitation method, and borojó (Borojoa patinoi) extract was added as an anti-caking agent as well as antioxidant. The nanoparticles were characterized by visible spectrophotometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and Raman spectroscopy. After arsenic removal treatment using nanoparticles, a randomized experimental design of different concentrations (5 mg/L, 10 mg/L, 25 mg/L, 50 mg/L, 100 mg/L, and 150 mg/L) was applied at laboratory level. The average diameter of Fe3O4NPs ranged from 9 nm to 36 nm, Mn3O4 NPs were 15–20 nm, and CuO NPs ranged from 25 nm to 30 nm. Arsenic removal percentages using Fe3O4 NPs with a concentration of 150 mg/L was 87%; with Mn3O4 NPs, the removal was 70% and CuO NPs of about 63.5%. Finally, these nanoparticles could be used in a water treatment plant for the Papallacta Lagoon.

Fabrication, characterization, and in vitro studies of Selenium-substituted hydroxyapatite coatings

Abstract The increasing demand for hydroxyapatite (HA) coatings with enhanced functionality have led to novel materials with compositions that are more closely resembling those of natural bone apatites. In the present study, selenium-substituted (Se–HA) powders with various Se quantities were prepared by chemical precipitation. By applying suspension plasma spray (SPS), the surface of Ti substrates was coated with corresponding Se-HA coatings. The microstructural and physicochemical properties of the powders and the coatings were studied. Analysis by X-ray diffraction indicates that SeO32− replaced the PO43− groups, affecting the crystal structure and crystallinity of HA. As the extent of Se substitution increases, the lattice volume expands and the crystallinity decreases. The synthesized Se–HA powders were confirmed to be calcium-deficient apatite through energy-dispersive X-ray spectroscopy. However, the high temperature of SPS accelerated volatilization of P, increasing the Ca/(P + Se) ratio of the coatings, whereas the chemical valence state of Se remained unchanged. The Se–HA coating exhibited a high bonding strength of &gt;33 MPa, fully meeting the requirement of 15 MPa as coating implant materials. Dissolution behavior tests indicate that the Se–HA coatings had high solubility in comparison to the HA coating. As the substitution degree of Se increased, the dissolution rate also increased, which greatly enhanced the capacity to generate a bone-like apatite layer. In vitro cell experiments indicate that the Se–HA coatings exhibited excellent biocompatibility, and facilitated adhesion and proliferation of osteoblast MC3T3-E1, even in the presence of fluorine. Furthermore, antibacterial properties of Se–HA coatings were also indicated by inhibition of Staphylococcus aureus, which is the main cause of most infections after orthopedic surgeries. Thus, the Se–HA coatings have potential as implant coating materials for orthopedic applications.&amp;#xD;

Swift and Cost-Effective Detection of Nitrite in Environmental Samples Using Ru@Pt Modified PGE

Abstract Abstract: The development of a straightforward method is crucial for detecting and quantifying nitrite ions within the surrounding environment. This study involves the electrochemical fabrication of a bi-metallic alloy composed of Ruthenium and Platinum on a graphene-modified pge, the first-ever electrodeposition on pencil graphite (RuNPs@PtNPs/Gr-CHI). This study aims to establish a highly responsive and specific approach for identifying nitrite ions while demonstrating the efficacy of a commercially available pencil graphite electrode in detecting this environmental contaminant. The prevalence and structural characteristics of bimetallic nanoalloy particles are confirmed through X-ray diffraction, scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS). The composite exhibited a core-shell shape at a size of 26.998 nm. The electrooxidation of nitrite at RuNPs@PtNPs/Gr-CHI/PGE was investigated using differential pulse voltammetry. The results demonstrated a satisfactory linear relationship from 0.025 mM to 1.625 mM. The method revealed a low detection limit of 0.33 µM. The composite electrode exhibited favorable outcomes regarding selectivity, sensitivity (25.5 µAµM-1cm-2), and repeatability, which are desirable characteristics of the electrochemical sensor material. The constructed electrode underwent testing for five weeks to determine the stability. The suggested sensor's capability is demonstrated by detecting nitrite ions in real samples such as water, soil, and fruit juice.

Antioxidant and Anti-Inflammatory Activity of Gold Nanoparticles Synthesized Employing Fruit Peel extract of Citrus sinensisL.Osbeck

Abstract Nanoparticle biosynthesis has attained a lot of attention because of its cost-efficiency and eco-friendly process. Only limited studies are available which explain the interrelationship between physical parameters (pH, gold concentration, extract concentration, and temperature) and biological synthesis mechanism. The goal of this study was to predict the antioxidant as well as anti-inflammatory activity of biosynthesized gold nanoparticles utilizing Citrus sinensis peel extract. The initial colour shift from yellow to ruby red served as proof that nanoparticles had been successfully synthesized. The nanoparticles that were synthesized underwent various characterization techniques such as AFM (Atomic Force Microscope), FTIR (Fourier Transform Infrared Spectroscopy), FESEM (Field Emission Scanning Electron Microscope), XRD (X-Ray Diffraction), and UV-Vis spectroscopy to examine their properties. Further, the synthesis method was optimized for different pH, various gold concentrations, extract concentrations, and temperatures. The nanoparticles displayed good activity as a powerful antioxidant and anti-inflammatory agent. Advanced studies are necessary to explore their therapeutic property.&amp;#xD;

Complex Formation of Gold Nanoparticles with Collagen in Aqueous Media Studied by X-ray Scattering and Absorption Spectroscopy

Complex Formation of Gold Nanoparticles with Collagen in Aqueous Media Studied by X-ray Scattering and Absorption Spectroscopy

Allanite-(Sm), CaSm(Al2Fe2+)(Si2O7)(SiO4)O(OH), the third samarium mineral from Jordanów Śląski, Lower Silesia, Poland

Abstract Allanite-(Sm), the third samarium mineral to be discovered, was studied using electron microprobe analysis and single-crystal X-ray diffraction. It is isostructural with monoclinic epidote-supergroup minerals and belongs to the allanite group. The mineral was found in a granitic pegmatite in a serpentine quarry near Jordanów Śląski in Lower Silesia, SW Poland. It occurs as subhedral to anhedral crystals with sizes of up to ~150 μm accompanied by allanite-(Nd), allanite-(Y), clinozoisite, hingganite-(Y), and xenotime-(Y). Allanite-(Sm) is yellowish-brown and shows a white streak, a vitreous luster, and a Mohs hardness of ~6. It is brittle, with conchoidal fracture and imperfect cleavage. The calculated density is 3.842 g·cm-3, and the calculated mean refractive index is close to 1.737. The holotype crystal contains (in wt%) 33.08(11) SiO2, 0.08(3) TiO2, 21.15(9) Al2O3, 0.45(6) Sc2O3, 0.48 Fe2O3(calc.), 0.02(1) V2O3, 2.49(31) Y2O3, 0.18(4) La2O3, 0.95(9) Ce2O3, 0.34(6) Pr2O3, 3.52(31) Nd2O3, 6.12(23) Sm2O3, 0.06(2) EuO, 3.25(21) Gd2O3, 0.34(2) Tb2O3, 0.94(7) Dy2O3, 0.15(4) Ho2O3, 0.16(3) Er2O3, 0.07(6) Tm2O3, 0.06(4) Yb2O3, 0.28(4) MnO, 8.38 FeO(calc.), 0.13(2) MgO, 13.71(15) CaO, and 1.95 H2O(+)calc.; the total is 98.04. The empirical EPMA + SREF formula is A1(Ca0.966Mn0.022Fe2+0.010)Σ0.998A2(Ca0.372Sm0.192Y0.121Nd0.114Gd0.098Ce0.032Dy0.028Pr0.011Tb0.010La0.006Er0.005Ho0.004Eu0.002Tm0.002Yb0.002)Σ0.998M1Al0.998M2Al0.998M3(Fe2+0.628Al0.275Sc0.036Fe3+0.033Mg0.018T i0.005V3+0.002)Σ0.998(T1–T3Si3.012O11)O(OH), the simplified formula is Ca(Sm,REE,Ca)Al2(Fe2+,Al,Fe3+)(Si2O7)(SiO4)O(OH), and the ideal formula is CaSm(Al2Fe2+)(Si2O7)(SiO4)O(OH), which requires (in wt.%) SiO2—30.37, Al2O3—17.18, Sm2O3—29.38, FeO—12.11, CaO—9.45, and H2O—1.52; the total is 100. Allanite-(Sm) is monoclinic, space-group P21/m, with the following unit-cell parameters: a = 8.8923(6), b = 5.7005(3), c = 10.1280(8) Å, β = 115.445(9)º, V = 463.59(6) Å3, Z = 2, and a : b : c = 1.5599 : 1 : 1.7767. The T site is exclusively occupied by Si, the A1 site is occupied by Ca and Mn, and the A2 site is mainly occupied by rare earth elements (REE), of which Sm is dominant. The M1 and M2 sites are occupied by Al and the M3 site by divalent cations, of which Fe2+, characteristic of allanite-type species, is dominant. Allanite-(Sm) and the associated allanite-(Y), allanite-(Nd), and hingganite-(Y) are secondary minerals precipitated from Ca-rich hydrothermal fluid during the metasomatic alteration of the Jordanów Śląski pegmatite. They accumulated REE released by the alteration of nearby xenotime-(Y). The disequilibrium rapid crystallization of REE-selective allanite and hingganite structures in an environment strongly enriched in heavy REE (HREE) relative to light REE (LREE), as well as small-scale heterogeneities in REE abundances in the fluid, resulted in the crystallization of exotic allanite species, including allanite-(Sm).

Enhancing photocatalytic activity via formation of heterojunctions introduced through postmetalation of metal organic frameworks with silver ions

The postmetalation of silver in zinc and manganese-based metal–organic frameworks (MOFs) represents a versatile and efficient approach for enhancing the degradation of methylene blue (MB) pollutant in aqueous environment. In the present study, zinc, manganese, and their bimetallic MOFs are synthesized using the solvothermal method. Subsequently, silver ions are incorporated into the synthesized MOFs. A suite of characterization techniques is employed to analyze the resulting material. Among the three silver loaded MOFs, Ag-mixed bimetallic MOF (Ag-BM) exhibits the least band gap of 2.28 eV, possessing a greater propensity for light absorption. The particle size of Ag-BM lies in the nanometer range, and it possesses the largest surface area. X-ray diffraction depicts the successful integration of Ag into MOF structure. The synthesized samples are used for degrading MB. Ag-BM outperforms the other MOFs in decomposing MB, with a degradation percentage of 91.8% in 120 min. The degradation process follows the first-order kinetics depicting that the rate of degradation positively correlates with the dye concentration remaining in the solution. Employing a reactive species quenching experiment with scavengers, hydroxyl radicals were identified as the principal active species responsible for MB degradation by Ag-BM.

Study of multiferroic properties of Mn substituted Bi0.8Sm0.1Dy0.1Fe1-xMnxO3 ceramics

Abstract Transition metal Mn substituted various multiferroic Bi0.8Sm0.1Dy0.1Fe1-xMnxO3 (x = 0.00, 0.01, 0.03 and 0.05) ceramics samples were fabricated by the solid-state reaction technique. The distorted rhombohedral perovskite structure with some phase impurity of all samples is confirmed by X-ray diffraction analysis. Field Emission Scanning Electron Microscope and Energy Dispersive X-ray spectroscopy are used for microstructural and quantitative analysis, respectively. Densities are decreased and the average grain size is increased with Mn contents. The initial permeability and relative quality factor (RQF) have found to be increased with Mn contents in the samples. The peaks in RQF shifts toward the lower frequency region with increasing Mn contents can be attributed by Snoek’s relation. All the samples show paramagnetic behavior at room temperature and magnetization slightly increases with Mn contents. The frequency dependent dielectric constant is investigated and found to consequence of space charge polarization. The dispersion behavior in dielectric constants can be explained by the Maxwell-Wagner model. The dielectric constants and dielectric loss decrease with increasing of Mn contents for all the samples. The value of electric modulus is observed to increases with the increasing of frequency and this dispersion phenomena is due to short range mobility of charge carriers in conduction. The effect of grain and grain boundaries on electric properties of samples are investigated by complex impedance analysis. The ac conductivity increases with frequency due to small polaron hopping and it can be attributed according to Jonscher’s power law.

Reexamination of the structure of nanomineral opal-CT using synchrotron X-ray diffraction, transmission electron microscopy, X-ray scattering structure factor and pair distribution function analyses

Reexamination of the structure of nanomineral opal-CT using synchrotron X-ray diffraction, transmission electron microscopy, X-ray scattering structure factor and pair distribution function analyses

Enhanced nanocellulose extraction from date palm waste: green solvent hydrolysis with transition metal complex

This study presents a novel method for nanocellulose production using [Bmim]Cl as a green solvent, with enhanced hydrolysis efficiency achieved through the addition of a transition metal complex as a catalyst. The redox capability of the transition metal complex to break the glycosidic bonds in cellulose is amplified by the addition of an oxidizing agent. This protocol represents the latest innovation in the field of nanocellulose production, resulting in improved yield and reduced particle size. Nanocellulose (NC) was extracted from date seeds using 1-butyl-3-methylimidazolium chloride [Bmim]Cl coupled with a transition metal complex comprising copper metal and pyridine as a ligand along with H2O2\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${\ ext{H}}_{2}{\ ext{O}}_{2}$$\\end{document} as an oxidizing agent. Unlike conventional [Bmim]Cl hydrolysis, which typically yields only microcrystalline cellulose (MCC), this approach resulted in a 25% higher yield of NC than that of MCC. Dynamic light scattering analysis showed a substantial reduction in hydrodiameter from 1200 nm for MCC to 128.7 nm for NC, highlighting the remarkable efficiency of this process. Thermal analysis demonstrated the high stability of NC, which showed a Tonset\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${T}_{onset}$$\\end{document} of 286 °C and an activation energy (Ea\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${E}_{a}$$\\end{document}) of 220.41 kJ/mol. X-ray diffraction analysis indicated that NC possessed a high degree of crystallinity (Crl=\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${C}_{rl}=$$\\end{document} 70.28%). Furthermore, NC underwent modification with 3-aminopropyltriethoxysilane to replace free hydroxyl groups (–OH), making it redispersal and suitable for various applications. This modification was confirmed through Fourier transform infrared spectroscopy, which showed the presence of characteristic functional groups, and energy-dispersive X-ray spectroscopy, which verified the elemental composition. Zeta potential measurements revealed surface charge differences, with MCC at − 27.87 mV, NC at − 27.28 mV, and modified NC at − 44.72 mV, indicating improved colloidal stability after modification. These findings highlight the protocol's effectiveness and its potential impact on the NC production industry, offering improved yields and the production of nanosized fibers using green solvents.

Use of a confocal optical device for centring a diamond anvil cell in single-crystal X-ray diffraction experiments

Use of a confocal optical device for centring a diamond anvil cell in single-crystal X-ray diffraction experiments

Adsorption behavior of graphite‐like walnut shell biochar modified with ammonia for ciprofloxacin in aqueous solution

AbstractBACKGROUNDGraphite‐like biochar of NWSC600K was prepared at 900 °C using walnut shell as the raw material and aqueous ammonia (NH3·H2O) as an activator, and characterized using transmission and scanning eletron microscopy (TEM, SEM), X‐ray diffraction (XRD), Brunauer–Emmett–Teller (BET), Raman spectroscopy and Fourier transform infrared (FTIR). The study investigated the adsorption performance and mechanism of NWSC600K for ciprofloxacin (CIP).RESULTSThe results showed that extremely tiny pores were found on the surface of NWSC600K, which increased its specific surface area to 823.91 m2 g−1, whereas the average pore size of NWSC600K decreased to 3.23 nm. The results of TEM, XRD and Raman spectroscopy detected well‐arranged lattice stripes as well as characteristic peaks corresponding to the graphite lattice appearing on the surface of NWSC600K. Moreover, the ID/IG value for NWSC600K was 1.429. The FTIR results showed that functional groups including the amino group were formed on NWSC600K.CONCLUSIONThe adsorption capacity of NWSC600K for CIP was 158.14 mg g−1 and the corresponding removal rate was 97.5% at pH 7. The pH value impact on the removal efficiency of CIP greatly, and the removal rate of CIP decreased linearly with increasing pH. The coexisting ions also would inhibit the adsorption of CIP on NWSC600K. Results obtained from kinetic and isotherm models, thermodynamics and characterization analyses suggested that pore‐filling, π–π stacking, hydrogen bonding, hydrophobicity and electrostatic interaction existed during the adsorption process. The adsorption was a nonspontaneous exothermic reaction. © 2024 Society of Chemical Industry (SCI).