Search results for: NMR spectroscopy

Authors: Ahmed Alkarimi, Kevin Welham

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Organic mixed mode monolithic columns were fabricated from; glycidyl methacrylate-co-ethylene dimethacrylate-co-stearyl methacrylate, using glycidyl methacrylate and stearyl methacrylate as co monomers representing 30% and 70% respectively of the liquid volume with ethylene dimethacrylate crosslinker and 2,2-dimethoxy-2-phenylacetophenone as the free radical initiator. The monomers were mixed with a binary porogenic solvent, comprising propan-1-ol, and methanol (0.825 mL each). The monolith was formed by photo polymerization (365 nm) inside a borosilicate glass tube (1.5 mm ID and 3 mm OD x 50 mm length). The monolith was observed to have formed correctly by optical examination and generated reasonable backpressure, approximately 650 psi at a flow rate of 0.2 mL min⁻¹ 50:50 acetonitrile: water. The morphological properties of the monolithic columns were investigated using scanning electron microscopy images, and Brunauer-Emmett-Teller analysis, the results showed that the monolith was formed properly with 19.98 ± 0.01 mm² surface area, 0.0205 ± 0.01 cm³ g⁻¹ pore volume and 6.93 ± 0.01 nm average pore size. The polymer monolith formed was further investigated using proton nuclear magnetic resonance, and Fourier transform infrared spectroscopy. The monolithic columns were investigated using high-performance liquid chromatography to test their ability to separate different samples with a range of properties. The columns displayed both hydrophobic/hydrophilic and hydrophobic/ion exchange interactions with the compounds tested indicating that true mixed mode separations. The mixed mode monolithic columns exhibited significant separation of proteins.

Keywords: LC separation, proteins separation, monolithic column, mixed mode

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Authors: Raana Babadi Fathipour

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Hydrogels are three-dimensional structures formed by the interweaving of polymeric materials, possessing the remarkable ability to imbibe copious amounts of water. Numerous methodologies have been devised for examining and understanding the properties of these synthesized gels. Amongst them, spectroscopic techniques such as ultraviolet/visible (UV/Vis) and Fourier-transform infrared (FTIR) spectroscopy offer a glimpse into molecular and atomic aspects. Additionally, diffraction methods like X-ray diffraction (XRD) enable one to measure crystallinity within the gel's structure, while microscopy tools encompassing scanning electron microscopy (SEM) and transmission electron microscopy (TEM) provide insights into surface texture and morphology. Furthermore, rheology serves as an invaluable tool for unraveling the viscoelastic behavior inherent in hydrogels—a parameter crucial not only to numerous industries, including pharmaceuticals, cosmetics, food processing, agriculture and water treatment, but also pivotal to related fields of research. Likewise, the ultimate configuration of the product is contingent upon its characterization at a microscopic scale in order to comprehend the intricacies of the hydrogel network's structure and interaction dynamics in response to external forces. Within this present scrutiny, our attention has been devoted to unraveling the intricate rheological tendencies exhibited by materials founded on synthetic, natural, and semi-synthetic hydrogels. We also explore their practical utilization within various facets of everyday life from an industrial perspective.

Keywords: rheology, hydrogels characterization, viscoelastic behavior, application

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Authors: M. Cabuk, M. Yavuz, T. A. Yesil, H. I. Unal

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Electrorheological (ER) fluids are a class of smart materials exhibiting reversible changes in their rheological and mechanical properties under an applied electric field (E). ER fluids generally are composed of polarisable solid particles dispersed in non-conducting oil. ER fluids are fluids which exhibit. The resistance to motion of the ER fluid can be controlled by adjusting the applied E, due to their fast and reversible changes in their rheological properties presence of E. In this study, a series of chitosan/expanded perlite (CS/EP) composites with different chitosan mass fractions (10%, 20%, and 50%) was used. Characterizations of the composites were carried out by Fourier Transform Infrared (FTIR), X-ray diffraction (XRD) and Scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) techniques. Antisedimentation stability and dielectric properties of the composites were also determined. The effects of volume fraction, electric field strength, shear rate, shear stress, and temperature onto ER properties of the CS/EP composite particles dispersed in silicone oil (SO) were investigated in detail. Vibration damping behavior of the CS/EP composites were determined as a function of frequence, storage (Gʹ) and loss (Gʹ ʹ) moduli. It was observed that ER response of the CS/EP/SO ER fluids increased with increasing electric field strength and exhibited the typical shear thinning non-Newtonian viscoelastic behaviors with increasing shear rate. The maximum yield stress was obtained with 1250 Pa under E = 3 kV/mm. Further, the CS/EP/SO ER fluids were observed to sensitive to vibration control by showing reversible viscosity enhancements (Gʹ > Gʹ ʹ). Acknowledgements: The authors thank the TÜBİTAK (214Z199) for the financial support of this work.

Keywords: chitosan, electrorheology, perlite, vibration control

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Authors: Issam Lakdhar, Akram Alhussein, Juan Creus

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With the huge increase in world energy consumption, researchers are working to find other alternative sources of energy instead of fossil fuel one causing many environmental problems as the production of greenhouse effect gases. Hydrogen is considered a green energy source, which its combustion does not cause environmental pollution. The transport and the storage of the gas molecules or the other products containing this smallest chemical element in metallic structures (pipelines, tanks) are crucial issues. The dissolve and the permeation of hydrogen into the metal lattice lead to the formation of hydride phases and the embrittlement of structures. To protect the metallic structures, a surface treatment could be a good solution. Among the different techniques, magnetron sputtering is used to elaborate micrometric coatings capable of slowing down or stop hydrogen permeation. In the plasma environment, the deposition parameters of new thin-film metallic glasses Al-Ti-W were optimized and controlled in order to obtain, hydrogen barrier. Many characterizations were carried out (SEM, XRD and Nano-indentation…) to control the composition and understand the influence of film microstructure and chemical composition on the hydrogen permeation through the coatings. The coating performance was evaluated under two hydrogen production methods: chemical and electrochemical (cathodic protection) techniques. The hydrogen quantity absorbed was experimentally determined using the Thermal-Desorption Spectroscopy method (TDS)). An ideal ATW thin film was developed and showed excellent behavior against the diffusion of hydrogen.

Keywords: thin films, hydrogen, PVD, plasma technology, electrochemical properties

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Authors: Victor Igwemezie, Ali Mehmanparast

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The correct knowledge of corrosion fatigue mechanism in marine steel is very important. This is because it enables the design, selection, and use of steels for offshore applications. It also supports realistic corrosion fatigue life prediction of marine structures. A study has been conducted to increase the understanding of corrosion fatigue mechanism in marine steels. The materials investigated are normalized and advanced S355 Thermomechanical control process (TMCP) steels commonly used in the design of offshore wind turbine support structures. The experimental study was carried out by conducting corrosion fatigue tests under conditions pertinent to offshore wind turbine operations, using the state of the art facilities. A careful microstructural study of the crack growth path was conducted using metallurgical optical microscope (OM), scanning electron microscope (SEM) and Energy Dispersive X-Ray Spectroscopy (EDX). The test was conducted on three subgrades of S355 steel: S355J2+N, S355G8+M and S355G10+M and the data compared with similar studies in the literature. The result shows that the ferrite-pearlite morphology primarily controls the corrosion-fatigue crack growth path in marine steels. A corrosion fatigue mechanism which relies on the hydrogen embrittlement of the grain boundaries and pearlite phase is used to explain the crack propagation behaviour. The crack growth trend in the Paris region of the da/dN vs. ΔK curve is used to explain the dependency of the corrosion-fatigue crack growth rate on the ferrite-pearlite morphology.

Keywords: corrosion-fatigue mechanism, fatigue crack growth rate, ferritic-pearlitic steel, microstructure, phase morphology

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Authors: Elhamalsadat Ghaffari, Moghan Amirhosseinian, Amir Khaleghipour

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Multifunctional bioactive glasses (BGs) are designed with a focus on the provision of bactericidal and biological properties desired for angiogenesis, osteogenesis, and ultimately potential applications in bone tissue engineering. To achieve these, six sol-gel copper/magnesium substituted derivatives of 58S-BG, i.e. a mol% series of 60SiO₂-4P₂O₅-5CuO-(31-x) CaO/xMgO (where x=0, 1, 3, 5, 8, and 10), were synthesized. Afterwards, the effect of MgO/CaO substitution on the in vitro formation of nano-hydroxyapatite (HA), osteoblast-like cell responses and BGs antibacterial performance were studied. During the BGs synthesis, the elimination of nitrates was achieved at 700 °C that prevented the BGs crystallization and stabilized the obtained dried gels. The structural and morphological evaluations were performed with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). These characterizations revealed that Cu-substituted 58S-BG consisting of 5 mol% MgO (BG-5/5) slightly had retarded the formation of HA. In addition, Cu-substituted 58S-BGs consisting 8 mol% and 10 mol% MgO (BG-5/8 and BG-5/10) displayed lower bioactivity probably due to the lower ion release rate of Ca–Si into the simulated body fluid (SBF). The determination of 3-(4, 5 dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide (MTT) and alkaline phosphate (ALP) activities proved that the highest values of both differentiation and proliferation of MC3T3-E1 cells can be obtained from a 5 mol% MgO substituted BG, while the over addition of MgO (8 mol% and 10 mol%) decreased the bioactivity. Furthermore, these novel Cu/Mg-substituted 58S-BGs displayed antibacterial effect against methicillin-resistant Staphylococcus aureus bacteria. Taken together, the results suggest the equally-substituted BG-5/5 (i.e. the one consists of 5 mol% of both CuO and MgO) as a promising candidate for bone tissue engineering, among all newly designed BGs in this work, owing to its desirable cell proliferation, ALP activity and antibacterial properties.

Keywords: apatite, bioactivity, biomedical applications, sol-gel processes

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Authors: Saja M. Nabat Al-Ajrash, Charles Browning, Rose Eckerle, Li Cao

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Three preceramic polymer formulations for potential use in 3D printing technologies were investigated. The polymeric precursors include an allyl hydrido polycarbosilane (SMP-10), SMP-10/1,6-dexanediol diacrylate (HDDA) mixture, and polydimethylsiloxane (PDMS). The rheological property of the polymeric precursors, including the viscosity within a wide shear rate range was compared to determine the applicability in additive manufacturing technology. The structural properties of the polymeric solutions and their photocureability were investigated using Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). Moreover, thermogravimetric analysis (TGA) and X-ray diffraction (XRD) were utilized to study polymeric to ceramic conversion for versatile precursors. The prepared precursor resin proved to have outstanding photo-curing properties and the ability to transform to the silicon carbide phase at temperatures as low as 850 °C. The obtained ceramic was fully dense with nearly linear shrinkage and a shiny, smooth surface after pyrolysis. Furthermore, after pyrolysis to 1350 °C and TGA analysis, PDMS polymer showed the highest onset decomposition temperature and the lowest retained weight (52 wt%), while SMP.10/HDDA showed the lowest onset temperature and ceramic yield (71.7 wt%). In terms of crystallography, the ceramic matrix composite appeared to have three coexisting phases, including silicon carbide, and silicon oxycarbide. The results are very promising to fabricate ceramic materials working at high temperatures with complex geometries.

Keywords: preceramic polymer, silicon carbide, photocuring, allyl hydrido polycarbosilane, SMP-10

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Authors: Rita Ghosh, Joykrishna Dey

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PEG-based amphiphiles are of tremendous importance for its widespread applications in pharmaceutics, household purposes, and drug delivery. Previously, a number of single PEG-tailed amphiphiles having significant applications have been reported from our group. Therefore, it was of immense interest to explore the properties and application potential of PEG-based double tailed amphiphiles. Herein, for the first time, two novel double PEG-tailed amphiphiles having different PEG chain lengths have been developed. The self-assembly behavior of the newly developed amphiphiles in aqueous buffer (pH 7.0) was thoroughly investigated at 25 oC by a number of techniques including, 1H-NMR, and steady-state and time-dependent fluorescence spectroscopy, dynamic light scattering, transmission electron microscopy, atomic force microscopy, and isothermal titration calorimetry. Despite having two polar PEG chains both molecules were found to have strong tendency to self-assemble in aqueous buffered solution above a very low concentration. Surprisingly, the amphiphiles were shown to form stable vesicles spontaneously at room temperature without any external stimuli. The results of calorimetric measurements showed that the vesicle formation is driven by the hydrophobic effect (positive entropy change) of the system, which is associated with the helix-to-random coil transition of the PEG chain. The spectroscopic data confirmed that the bilayer membrane of the vesicles is constituted by the PEG chains of the amphiphilic molecule. Interestingly, the vesicles were also found to exhibit structural transitions upon addition of salts in solution. These properties of the vesicles enable them as potential candidate for drug delivery.

Keywords: double-tailed amphiphiles, fluorescence, microscopy, PEG, vesicles

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Authors: Rajendra N. Ghosh, Paramjeet Singh, Niranjan Khandelwal, Sameer Vyas, Pratibha Singhi, Naveen Sankhyan

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Background: Tuberculoma and neurocysticercosis (NCC) are two most common intracranial infections in developing country. They often simulate on neuroimaging and in absence of typical imaging features cause significant diagnostic dilemmas. Differentiation is extremely important to avoid empirical exposure to antitubercular medications or nonspecific treatment causing disease progression. Purpose: Better characterization and differentiation of CNS tuberculoma and NCC by using morphological and multiple advanced functional MRI. Material and Methods: Total fifty untreated patients (20 tuberculoma and 30 NCC) were evaluated by using conventional and advanced sequences like CISS, SWI, DWI, DTI, Magnetization transfer (MT), T2Relaxometry (T2R), Perfusion and Spectroscopy. rCBV,ADC,FA,T2R,MTR values and metabolite ratios were calculated from lesion and normal parenchyma. Diagnosis was confirmed by typical biochemical, histopathological and imaging features. Results: CISS was most useful sequence for scolex detection (90% on CISS vs 73% on routine sequences). SWI showed higher scolex detection ability. Mean values of ADC, FA,T2R from core and rCBV from wall of lesion were significantly different in tuberculoma and NCC (P < 0.05). Mean values of rCBV, ADC, T2R and FA for tuberculoma and NCC were (3.36 vs1.3), (1.09x10⁻³vs 1.4x10⁻³), (0.13 x10⁻³ vs 0.09 x10⁻³) and (88.65 ms vs 272.3 ms) respectively. Tuberculomas showed high lipid peak, more choline and lower creatinine with Ch/Cr ratio > 1. T2R value was most significant parameter for differentiation. Cut off values for each significant parameters have proposed. Conclusion: Quantitative MRI in combination with conventional sequences can better characterize and differentiate similar appearing tuberculoma and NCC and may be incorporated in routine protocol which may avoid brain biopsy and empirical therapy.

Keywords: advanced functional MRI, differentiation, neurcysticercosis, tuberculoma

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Authors: Baljinder Singh, Navneet Sharma

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The skin can be used as the site for drug administration for continuous transdermal drug infusion into the systemic circulation. For the continuous diffusion/penetration of the drugs through the intact skin surface membrane-moderated systems, matrix dispersion type systems, adhesive diffusion controlled systems and micro reservoir systems have been developed. Various penetration enhancers are used for the drug diffusion through skin. In matrix dispersion type systems, the drug is dispersed in the solvent along with the polymers and solvent allowed to evaporate forming a homogeneous drug-polymer matrix. Matrix type systems were developed in the present study. In the present work, an attempt has been made to develop a matrix-type transdermal therapeutic system comprising of ondansetron-HCl with different ratios of hydrophilic and hydrophobic polymeric combinations using solvent evaporation technique. The physicochemical compatibility of the drug and the polymers was studied by infrared spectroscopy. The results obtained showed no physical-chemical incompatibility between the drug and the polymers. The patches were further subjected to various physical evaluations along with the in-vitro permeation studies using rat skin. On the basis of results obtained form the in vitro study and physical evaluation, the patches containing hydrophilic polymers i.e. polyvinyl alcohol and poly vinyl pyrrolidone with oleic acid as the penetration enhancer(5%) were considered as suitable for large scale manufacturing with a backing layer and a suitable adhesive membrane.

Keywords: transdermal drug delivery, penetration enhancers, hydrophilic and hydrophobic polymers, ondansetron HCl

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Authors: Preeti Pal, Anjali Pal

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Chitosan is an effective sorbent for removal of contaminants from wastewater. However, the ability of pure chitosan is specific because of its cationic charge. It causes repulsion in the removal process of various cationic charged molecules. The present study has been carried out for the successful removal of Pb²⁺ ions from aqueous solution by modified chitosan beads. Surface modification of chitosan (CS) beads was performed by using the anionic surfactant (AS), sodium dodecyl sulfate (SDS). Micelle aggregation property of SDS has been utilized for the formation of bilayer over the CS beads to produce surfactant modified chitosan (SMCS) beads. Prepared adsorbents were characterized by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) in order to find out their composition and surface morphology. SMCS beads, when compared to the pure CS beads, showed three times higher adsorption. This higher adsorption is believed to be due to the adsolubilization of Pb²⁺ ions on SDS bilayer. This bilayer provides more adsorption sites for quick and effective removal of Pb²⁺ ions from the aqueous phase. Moreover, the kinetic and adsorption isotherm models were employed to the obtained data for the description of the lead adsorption processes. It was found that the removal kinetics follows pseudo-second order model. Adsorption isotherm data fits well to the Langmuir model. The maximum adsorption capacity obtained is 100 mg/g at the dosage of 0.675 g/L for 50 mg/L of Pb²⁺. The adsorption capacity is subject to increase with increasing the Pb²⁺ ions concentration in the solution. The results indicated that the prepared hydrogel beads are efficient adsorbent for removal of Pb²⁺ ions from the aqueous medium.

Keywords: adsolubilisation, anionic surfactant, bilayer, chitosan, Pb²⁺

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Authors: Elbadawy A. Kamoun

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Magnetically responsive hydrogel nanocomposite (NCH) based on composites of superparamagnetic of Fe3O4 nano-particles and temperature responsive hydrogel matrices were developed. The nanocomposite hydrogel system based on the temperature sensitive N-isopropylacrylamide hydrogels crosslinked by poly(ethylene glycol)-400 dimethacrylate (PEG400DMA) incorporating with chitosan derivative, was synthesized and characterized. Likewise, the NCH system was synthesized by visible-light free radical photopolymerization, using carboxylated camphorquinone-amine system to avoid the common risks of the use of UV-light especially in hyperthermia treatment. Superparamagnetic of iron oxide nanoparticles were introduced into the hydrogel system by polymerizing mixture technique and monomer solution. FT-IR with Raman spectroscopy and Wide angle-XRD analysis were utilized to verify the chemical structure of NCH and exfoliation reaction for nanoparticles, respectively. Additionally, morphological structure of NCH was investigated using SEM and TEM photographs. The swelling responsive of the current nanocomposite hydrogel system with different crosslinking conditions, temperature, magnetic field efficiency, and the presence effect of magnetic nanoparticles were evaluated. Notably, hydrolytic degradation of this system was proved in vitro application. While, in-vivo release profile behavior is under investigation nowadays. Moreover, the compatibility and cytotoxicity tests were previously investigated in our studies for photoinitiating system. These systems show promised polymeric material candidate devices and are expected to have a wide applicability in various biomedical applications as mildly.

Keywords: hydrogel nanocomposites, tempretaure-responsive hydrogel, superparamagnetic nanoparticles, hyperthermia therapy

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Authors: Mohamed Saad Gad Elzoghby

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Nanomaterials are widely used nowadays for the consolidation of degraded archaeological limestone. It’s one of the most predominant stones in monumental buildings and statuary works. It is exposed to different weathering processes that cause degradation and the presence of deterioration pattern as cracks, fissures, and granular disintegration. Nanomaterials have been applied to limestone consolidation. Among these nanomaterials are nanolimes, i.e., dispersions of lime nanoparticles in alcohols, and nano-silica, i.e., dispersions of silica nanoparticles in water, promising consolidating products for limestone. It was investigated and applied to overcome the disadvantages of traditional consolidation materials such as lime water, water glass, and paraliod. So, researchers investigated and tested the effectiveness of nanomaterials as consolidation materials for limestone. The present study includes an evaluation of some nanomaterials in consolidation limestone stone in comparison with traditional consolidants. These consolidation materials are nano calcium hydroxide nanolime, and nanosilica. The latter is known commercially as Nano Estel and the former Known as Nanorestore compared to traditional consolidants Wacker OH (ethyl silicate) and Paraloid B72 (a copolymer of ethyl methacrylate and methyl acrylate). The study evaluated the consolidation effectiveness of nanomaterials and traditional consolidants by using followed methods, characterization of physical properties of stone, scanning electron microscopy (SEM), X-ray diffractometry, Fourier transforms infrared spectroscopy, and mechanical properties. The study confirmed that nanomaterials were better in the distribution and encapsulation of calcite grains in limestone, and traditional materials were better in improving the physical properties of limestone. It demonstrated that good results could be achieved through mixtures of nanomaterials and traditional consolidants.

Keywords: nanomaterials, limestone, consolidation, evaluation, weathering, nanolime, nanosilica, scanning electron microscope

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Authors: A. E. Yakshin, D. Ijpes, J. M. Sturm, I. A. Makhotkin, M. D. Ackermann

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Applications like synchrotron optics, soft X-ray microscopy, X-ray astronomy, and wavelength dispersive X-ray fluorescence (WD-XRF) rely heavily on short- and ultra-short-period multilayer (ML) structures. In WD-XRF, ML serves as an analyzer crystal to disperse emission lines of light elements. The key requirement for the ML is to be highly reflective while also providing sufficient angular dispersion to resolve specific XRF lines. For these reasons, MLs with periods ranging from 1.0 to 2.5 nm are of great interest in this field. Due to the short period, the reflectance of such MLs is extremely sensitive to interface imperfections such as roughness and interdiffusion. Moreover, the thickness of the individual layers is only a few angstroms, which is close to the limit of materials to grow a continuous film. MLs with a period between 2.5 nm and 1.0 nm, combining tungsten (W) reflector with B₄C, Si, and Al spacers, were created and examined. These combinations show high theoretical reflectance in the full range from C-Kα (4.48nm) down to S-Kα (0.54nm). However, the formation of optically unfavorable compounds, intermixing, and interface roughness result in limited reflectance. A variety of techniques, including diffusion barriers, seed layers, and ion polishing for sputter-deposited MLs, were used to address these issues. Diffuse scattering measurements, photo-electron spectroscopy analysis, and X-ray reflectivity measurements showed a noticeable reduction of compound formation, intermixing, and interface roughness. This also resulted in a substantial increase in soft X-ray reflectance for W/Si, W/B4C, and W/Al MLs. In particular, the reflectivity of 1 nm period W/Si multilayers at the wavelength of 0.84 nm increased more than 3-fold – propelling forward the applicability of such multilayers for shorter wavelengths.

Keywords: interface engineering, reflectance, short period multilayer structures, x-ray optics

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Authors: Laura Frydel, Piotr M. Slomkiewicz, Beata Szczepanik

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Triclosan has been used as a disinfectant in many medical products, such as: hand disinfectant soaps, creams, mouthwashes, pastes and household cleaners. Due to its strong antimicrobial activity, triclosan is becoming more and more popular and the consumption of disinfectants with triclosan in it is increasing. As a result, this compound increasingly finds its way into waters and soils in an unchanged form, pollutes the environment and may have a negative effect on organisms. The aim of this study was to investigate the synthesis of cellulose-based halloysite-carbon adsorbent and perform its characterization. The template in the halloysite-carbon adsorbent was halloysite nanotubes and the carbon precursor was microcrystalline cellulose. Scanning electron microscope (SEM) images were obtained and the elementary composition (qualitative and quantitative) of the sample was determined by energy dispersion spectroscopy (EDS). The identification of the crystallographic composition of the halloysite nanotubes and the sample of the halloysite-carbon composite was carried out using the X-ray powder diffraction (XRPD) method. The FTIR spectra were acquired before and after the adsorption process in order to determine the functional groups on the adsorbent surface and confirm the interactions between adsorbent and adsorbate molecules. The parameters of the porous structure of the adsorbent, such as the specific surface area (Brunauer-Emmett-Teller method), the total pore volume and the volume of mesopores and micropores were determined. Total carbon and total organic carbon were also determined in the samples. A cellulose-based halloysite-carbon adsorbent was used to remove triclosan from water. The degree of removal of triclosan from water was approximately 90%. The results indicate that the halloysite-carbon composite can be successfully used as an effective adsorbent for removing triclosan from water.

Keywords: Adsorption, cellulose, halloysite, triclosan

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Authors: Swati Bishnoi, D. Haranath, Vinay Gupta

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In this work, we demonstrate that the power conversion efficiency (PCE) of organic solar cells (OSCs) could be improved significantly by using ZnO doped with Aluminum (Al) and Europium (Eu) as cathode buffer layer (CBL). The ZnO:Al,Eu nanoparticle layer has broadband absorption in the ultraviolet (300-400 nm) region. The Al doping contributes to the enhancement in the conductivity whereas Eu doping significantly improves emission in the visible region. Moreover, this emission overlaps with the absorption range of polymer poly [N -9′-heptadecanyl-2,7-carbazole-alt-5,5-(4′,7′-di-2-thienyl-2′,1′,3′- benzothiadiazole)] (PCDTBT) significantly and results in an enhanced absorption by the active layer and hence high photocurrent. An increase in the power conversion efficiency (PCE) of 6.8% has been obtained for ZnO: Al,Eu CBL as compared to 5.9% for pristine ZnO, in the inverted device configuration ITO/CBL/active layer/MoOx/Al. The active layer comprises of a blend of PCDTBT donor and [6-6]-phenyl C71 butyric acid methyl ester (PC71BM) acceptor. In the reference device pristine ZnO has been used as CBL, whereas in the other one ZnO:Al,Eu has been used as CBL. The role of the luminescent CBL layer is to down-shift the UV light into visible range which overlaps with the absorption of PCDTBT polymer, resulting in an energy transfer from ZnO:Al,Eu to PCDTBT polymer and the absorption by active layer is enhanced as revealed by transient spectroscopy. This enhancement resulted in an increase in the short circuit current which contributes in an increased PCE in the device employing ZnO: Al,Eu CBL. Thus, the luminescent ZnO: Al, Eu nanoparticle CBL has great potential in organic solar cells.

Keywords: cathode buffer layer, energy transfer, organic solar cell, power conversion efficiency

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Authors: Orose Rugchati, Khumthong Mahawongwiriya

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Dendrobium hybrid cv. Ear-Sakul has become one of the important commercial commodities in Thailand agricultural industry worldwide, either as potted plants or as cut flowers due to the attractive color produced in flower petals. Anthocyanins are the main flower pigments and responsible for the natural attractive display of petal colors. These pigments play an important role in functionality, such as to attract animal pollinators, classification, and grading of these orchids. Dendrobium hybrid cv. Ear-Sakul has been collected from local area farm in different stage flowers (F1, F2-F5, and F6). Anthocyanins pigment were extracted from the fresh flower by solvent extraction (MeOH–TFA 99.5:0.5v/v at 4ºC) and purification with ethyl acetate. The main anthocyanins components are cyanidin, pelargonidin, and delphinidin. Pure anthocyanin contents were analysis by UV-Visible spectroscopy technique at λ max 535, 520 and 546 nm respectively. The anthocyanins contents were converted in term of monomeric anthocyanins pigment (mg/L). The anthocyanins contents of all sample were compared with standard pigments cyanidin, pelargonidin and delphinidin. From this experiment is a simple extraction and analysis anthocyanins content in different stage of flowers results shown that monomeric anthocyanins pigment contents of different stage flowers (F1, F2-F5 and F6 ): cyanidin – 3 – glucoside (mg/l) are 0.85+0.08, 24.22+0.12 and 62.12+0.6; Pelargonidin 3,5-di- glucoside(mg/l) 10.37+0.12, 31.06+0.8 and 81.58+ 0.5; Delphinidin (mg/l) 6.34+0.17, 18.98+0.56 and 49.87+0.7; and the appearance of extraction pure anthocyanins in L(a, b): 2.71(1.38, -0.48), 1.06(0.39,-0.66) and 2.64(2.71,-3.61) respectively. Dendrobium Hybrid cv. Ear-Sakul could be used as a source of anthocyanins by simple solvent extraction and stage of flowers as a guideline for the prediction amount of main anthocyanins components are cyanidin, pelargonidin, and delphinidin could be application and development in quantities, and qualities with the advantage for food pharmaceutical and cosmetic industries.

Keywords: analysis, anthocyanins contents, different stage flowers, Dendrobium Hybrid cv. Ear-Sakul

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Authors: Noraziah Nordin, Najihah Mohd Hashim, Nazia Abdul Majid, Mashitoh Abdul Rahman, Hamed Karimian, Hapipah Mohd Ali

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Enicosanthellum pulchrum belongs to family Annonaceae is also known as family of 'mempisang' in Malaysia. Liriodenine was isolated by prep-HPLC method. This method was first technique used for the isolation of this compound. The structure of the liriodenine was elucidated by 1D and 2D spectroscopy techniques. Liriodenine was tested on ovarian cancer cells line (CAOV-3) for MTT, AO/PI and cytotoxicity 3 assays. The MTT assay was performed to determine the cytotoxicity effect of lirodenine on CAOV-3 cells. The morphological changes on CAOV-3 cells were observed by AO/PI assay for the early and late stage of apoptosis, as well as necrosis. Meanwhile, the measurement of cell loss, nuclear morphology, DNA content, cell membrane permeability, mitochondrial membrane potential changes and cytochrome c release from mitochondria were detected through cytotoxicity 3 assay. The IC50 results showed liriodenine inhibits the growth of CAOV-3 cells after 24 h of treatment at 10.25 ± 1.06 µg/mL. After 48 and 72 h of treatments, the IC50 values were decreased to 7.65 ± 0:07 and 6.35 ± 1.62 µg/mL, respectively. The morphology changes can be seen on CAOV-3 with a production of cell membrane blebbing, cromatin condensation and apoptotic bodies with increasing time of treatment from 24 to 72 h. Evaluation of cytotoxicity 3 on CAOV-3 cells after treated with liriodenine, resulting loss of mitochondrial membrane potential and release of cytochrome c from mitochondria. The results demonstrated the capability of liriodenine as a promising anticancer agent, particularly on human ovarian cancer.

Keywords: Enicosanthellum pulchrum, ovarian cancer, apoptosis, cytotoxicity

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Authors: Danish Idrees, Vijay Kumar, Samudrala Gourinath

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Amyotrophic lateral sclerosis (ALS) is a neurodegenerative disease caused by misfolding and aggregation of Cu, Zn superoxide dismutase (SOD1). The use of small molecules has been shown to stabilize the SOD1 dimer and preventing its dissociation and aggregation. In this study, we employed molecular docking, molecular dynamics simulation and surface plasmon resonance (SPR) to study the interactions between SOD1 and natural polyphenolic compounds. In order to explore the noncovalent interaction between SOD1 and natural polyphenolic compounds, molecular docking and molecular dynamic (MD) simulations were employed to gain insights into the binding modes and free energies of SOD1-polyphenolic compounds. MM/PBSA methods were used to calculate free energies from obtained MD trajectories. The compounds, Hesperidin, Ergosterol, and Rutin showed the excellent binding affinity in micromolar range with SOD1. Ergosterol and Hesperidin have the strongest binding affinity to SOD1 and was subjected to further characterization. Biophysical experiments using Circular Dichroism and Thioflavin T fluorescence spectroscopy results show that the binding of these two compounds can stabilize SOD1 dimer and inhibit the aggregation of SOD1. Molecular simulation results also suggest that these compounds reduce the dissociation of SOD1 dimers through direct interaction with the dimer interface. This study will be helpful to develop other drug-like molecules which may have the effect to reduce the aggregation of SOD1.

Keywords: amyotrophic lateral sclerosis, molecular dynamics simulation, surface plasmon resonance, superoxide dismutase

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Authors: Mohamed Saad Gad Eloghby

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Nanomaterials are widely used nowadays for the consolidation of degraded archaeological limestone. It’s one of the most predominant stones in monumental buildings and statuary works. Exposure to different weathering processes caused degradation and the presence of deterioration pattern as cracks, fissures, and granular disintegration. Nanomaterials have been applied to limestone consolidation. Among these nanomaterials are nanolimes, i.e., dispersions of lime nanoparticles in alcohols and nanosilica, i.e., dispersions of silica nanoparticles in water promising consolidating products for limestone. It was investigated and applied to overcome the disadvantages of traditional consolidation materials such as lime water, water glass and paraliod. So, researchers investigated and tested the effectiveness of nanomaterials as consolidation materials for limestone. The present study includes the evaluation of some nano materials in consolidation limestone stone in comparison with traditional consolidantes. These consolidation materials are nano calcium hydroxide nanolime and nanosilica. The latter is known commercially as Nano Estel and the former is known as Nanorestore compared to traditional consolidantes Wacker OH (ethyl silicate) and Paraloid B72 (a copolymer of ethyl methacrylate and methyl acrylate). The study evaluated the consolidation effectiveness of nanomaterials and traditional consolidantes by using followed methods, Characterization of physical properties of stone, Scanning electron microscopy (SEM), X-ray diffractometry, Fourier transform infrared spectroscopy and Mechanical properties. The study confirmed that nanomaterials were better in the distribution and encapsulation of calcite grains in limestone, and traditional materials were better in improving the physical properties of limestone. It demonstrated that good results can be achieved through mixtures of nanomaterials and traditional consolidants.

Keywords: nanomaterials, limestone, consolidation, evaluation, weathering, nanolime, nanosilica, scanning electron microscope

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Authors: Suminar Pratapa, Agus Riyanto, Silmi Machmudah, Sri Yani Purwaningsih

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The objective of this study was to investigate the optical properties of polyvinyl alcohol (PVA) and its prospective applications by adding crystalline silica which is usually used as a reinforcing agent. To do this, we synthesized and evaluated PVA-based composites reinforced with silica crystals, namely cristobalite, derived from rice husk. The experimental procedure involved the production of SiO2 particles using rice husk precursors, which were subsequently subjected to calcination at a rate of 10 °C/min for a duration of 3 hours. This process primarily resulted in the formation of SiO2 crystals in the cristobalite phase, according to X-ray diffraction (XRD). Following this, the crystals were incorporated into polyvinyl alcohol (PVA) via a casting technique, resulting in the formation of composite sheets. The SiO2 contents in the composites were 0, 2.5, 5.0, and 10.%. XRD and Fourier-transform infrared spectroscopy (FTIR) techniques provided confirmation of the composites' successful synthesis, i.e., it did not yield any indications of chemical bonding between polyvinyl alcohol (PVA) and silicon dioxide (SiO2), indicating that the interaction was limited to interfacial reactions. The incorporation of SiO2 crystals resulted in a notable enhancement in UV-vis light absorption and a decrease in the optical band gap. Addition of 2.5, 5.0, and 10.% SiO2, for example, decreases the direct optical band gap of the composites form 5.37, 5.19, and 5.02 eV respectively, while the indirect band gaps of the samples were 4.44, 4.84, and 4.48 eV, correspondingly. These findings emphasize the efficacy of rice husk-derived SiO2 crystals as both reinforcement agents and modifiers of optical properties in the polymer composites, showcasing their significant potential to modify the composite's structural and optical characteristics.

Keywords: rice husk, cristaline SiO₂, PVA-based composites, structural characteristics, optical properties.

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Authors: Mohamed Ahmed Abd El Kader

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This paper describes the conservation processes of an Ancient Egyptian wooden coffin dating back to the Middle Kingdom, ancient Egypt, using several scientific and analytical methods in order to provide a deeper understanding of the deterioration status and a greater awareness of how well preserved the object is. Visual observation and 2D Programs, as well as Optical Microscopy (OM), Environmental scanning Electron Microscopy (ESEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) were used in our study. The identification of wood species and the composition of the pigments and previous restoration materials were made. The coffin was previously conserved and stored in improper conditions, which led to its further deterioration; the surface of the lid dust, which obscured the decorations as well as all necessary restoration work was promptly carried out as soon as the coffin was transferred from the display hall from the Egyptian Museum to the Wood Conservation Laboratory of the Grand Egyptian Museum-Conservation Center (GEM-CC). The analyses provided detailed information concerning the original materials and the materials added during the previous treatment interventions, which was considered when applying the conservation plan. Conservation procedures have been applied with high accuracy to conserve the coffin including cleaning, consolidation of fragile painted layers, and the wooden boards forming the sides of the coffin were reassembled in their original positions. The materials and methods that were applied were extremely effective in stability and reinforcement of the coffin without harmfulness to the original materials and the coffin was successfully conserved and ready to display in the Grand Egyptian Museum (GEM).

Keywords: coffin, middle kingdom, deterioration, 2d program

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Authors: Alireza Rahimi, Abdolreza Farhadian, Arash Tajik, Elaheh Sadeh, Avni Berisha, Esmaeil Akbari Nezhad

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Although natural polymers have been shown to have some inhibitory properties on sour corrosion, they are not considered very effective green corrosion inhibitors. Accordingly, effective corrosion inhibitors should be developed based on natural resources to mitigate sour corrosion in the oil and gas industry. Here, Arabic gum was employed as an eco-friendly precursor for the synthesis of innovative polyurethanes designed as highly efficient corrosion inhibitors for sour oilfield solutions. A comprehensive assessment, combining experimental and computational analyses, was conducted to evaluate the inhibitory performance of the inhibitor. Electrochemical measurements demonstrated that a concentration of 200 mM of the inhibitor offered substantial protection to mild steel against sour corrosion, yielding inhibition efficiencies of 98% and 95% at 25 ºC and 60 ºC, respectively. Additionally, the presence of the inhibitor led to a smoother steel surface, indicating the adsorption of polyurethane molecules onto the metal surface. X-ray photoelectron spectroscopy results further validated the chemical adsorption of the inhibitor on mild steel surfaces. Scanning Kelvin probe microscopy revealed a shift in the potential distribution of the steel surface towards negative values, indicating inhibitor adsorption and corrosion process inhibition. Molecular dynamic simulation indicated high adsorption energy values for the inhibitor, suggesting its spontaneous adsorption onto the Fe (110) surface. These findings underscore the potential of Arabic gum as a viable resource for the development of polyurethanes under mild conditions, serving as effective corrosion inhibitors for sour solutions.

Keywords: environmental effect, Arabic gum, corrosion inhibitor, sour corrosion, molecular dynamics simulation

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Authors: Nidhi Adhlakha, K. L. Yadav

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Three phase magnetoelectric (ME) composites (1-x)(0.7BiFeO3-0.3CoFe2O4)-xPbTiO3 (or equivalently written as (1-x)(0.7BFO-0.3CFO)-xPT) with x variations 0, 0.30, 0.35, 0.40, 0.45 and 1.0 were synthesized using hybrid processing route. The effects of PT addition on structural, multiferroic and optical properties have been subsequently investigated. A detailed Rietveld refinement analysis of X-ray diffraction patterns has been performed, which confirms the presence of structural phases of individual constituents in the composites. Field emission scanning electron microscopy (FESEM) images are taken for microstructural analysis and grain size determination. Transmission electron microscopy (TEM) analysis of 0.3CFO-0.7BFO reveals the average particle size to be lying in the window of 8-10 nm. The temperature dependent dielectric constant at various frequencies (1 kHz, 10 kHz, 50 kHz, 100 kHz and 500 kHz) has been studied and the dielectric study reveals that the increase of dielectric constant and decrease of average dielectric loss of composites with incorporation of PT content. The room temperature ferromagnetic behavior of composites is confirmed through the observation of Magnetization vs. Magnetic field (M-H) hysteresis loops. The variation of magnetization with temperature indicates the presence of spin glass behavior in composites. Magnetoelectric coupling is evidenced in the composites through the observation of the dependence of the dielectric constant on the magnetic field, and magnetodielectric response of 2.05 % is observed for 45 mol% addition of PT content. The fractional change of magnetic field induced dielectric constant can also be expressed as ∆ε_r~γM^2 and the value of γ is found to be ~1.08×10-2 (emu/g)-2 for composite with x=0.40. Fourier transformed infrared (FTIR) spectroscopy of samples is carried out to analyze various bonds formation in the composites.

Keywords: composite, X-ray diffraction, dielectric properties, optical properties

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Authors: H. Lee, J. Park

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In this present study, for the first time, we retrieved the Formaldehyde (HCHO) Vertical Column Density (HCHOVCD) using Pandora instruments in Seoul, a megacity in northeast Asia, for the period between 2012 and 2014 and investigated the temporal characteristics of HCHOVCD. HCHO Slant Column Density (HCHOSCD) was obtained using the Differential Optical Absorption Spectroscopy (DOAS) method. HCHOSCD was converted to HCHOVCD using geometric Air Mass Factor (AMFG) as Pandora is the direct-sun measurement. The HCHOVCDs is low at 12:00 Local Time (LT) and is high in the morning (10:00 LT) and late afternoon (16:00 LT) except for winter. The maximum (minimum) values of Pandora HCHOVCD are 2.68×1016 (1.63×10¹⁶), 3.19×10¹⁶ (2.23×10¹⁶), 2.00×10¹⁶ (1.26×10¹⁶), and 1.63×10¹⁶ (0.82×10¹⁶) molecules cm⁻² in spring, summer, autumn, and winter, respectively. In terms of seasonal variations, HCHOVCD was high in summer and low in winter which implies that photo-oxidation plays an important role in HCHO production in Seoul. In comparison with the Ozone Monitoring Instrument (OMI) measurements, the HCHOVCDs from the OMI are lower than those from Pandora. The correlation coefficient (R) between monthly HCHOVCDs values from Pandora and OMI is 0.61, with slop of 0.35. Furthermore, to understand HCHO mixing ratio within Planetary Boundary Layer (PBL) in Seoul, we converted Pandora HCHOVCDs to HCHO mixing ratio in the PBL using several meteorological input data from the Atmospheric InfraRed Sounder (AIRS). Seasonal HCHO mixing ratio in PBL converted from Pandora (OMI) HCHOVCDs are estimated to be 6.57 (5.17), 7.08 (6.68), 7.60 (4.70), and 5.00 (4.76) ppbv in spring, summer, autumn, and winter, respectively.

Keywords: formaldehyde, OMI, Pandora, remote sensing

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Authors: Kulvinder Bajwa, Narsi R. Bishnoi

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Finding a sustainable alternative for today’s petrochemical industry is a major challenge facing by researchers, scientists, chemical engineers, and society at the global level. Microorganisms are considered to be sustainable feedstock for 3rd generation biofuel production. In this study, we have investigated the potential of a native bacterial strain isolated from a petrol contaminated site for the production of biodiesel. The bacterium was identified to be Rhodococcus opacus by biochemical test and 16S rRNA. Compositional analysis of bacterial biomass has been carried out by Fourier transform infrared spectroscopy (FTIR) in order to confirm lipid profile. Lipid and biomass were optimized by combination with Box Behnken design (BBD) of response surface methodology. The factors selected for the optimization of growth condition were glucose, yeast extract, and ammonium nitrate concentration. The experimental model developed through RSM in terms of effective operational factors (BBD) was found to be suitable to describe the lipid and biomass production, which indicated higher lipid and biomass with a minimum concentration of ammonium nitrate, yeast extract, and quite higher dose of glucose supplementation. Optimum results of the experiments were found to be 2.88 gL⁻¹ biomass and lipid content 38.75% at glucose 20 gL⁻¹, ammonium nitrate 0.5 gL⁻¹ and yeast extract 1.25 gL⁻¹. Furthermore, GCMS study revealed that Rhodococcus opacus has favorable fatty acid profile for biodiesel production.

Keywords: biofuel, Oleaginious bacteria, Rhodococcus opacus, FTIR, BBD, free fatty acids

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Authors: Hyeonseok Yoo, Kiseok Oh, Jinsub Choi

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Titanium oxide nanotubes have attracted great attention because of its photocatalytic activity and large surface area. For enhancing electrochemical properties, catalysts should be doped into the structure because titanium oxide nanotubes themselves have low electroconductivity and catalytic activity. It has been reported that Ru and Ir doped titanium oxide electrodes exhibit high efficiency and low overpotential in the oxygen evolution reaction (OER) for water splitting. In general, titanium oxide nanotubes with high aspect ratio cannot be easily doped by conventional complex methods. Herein, two types of facile routes, namely single step anodization and potential shock, for Ru doping into high aspect ratio titanium oxide nanotubes are introduced in detail. When single step anodization was carried out, stability of electrodes were increased. However, onset potential was shifted to anodic direction. On the other hand, when high potential shock voltage was applied, a large amount of ruthenium/ruthenium oxides were doped into titanium oxide nanotubes and thick barrier oxide layers were formed simultaneously. Regardless of doping routes, ruthenium/ ruthenium oxides were homogeneously doped into titanium oxide nanotubes. In spite of doping routes, doping in aqueous solution generally led to incorporate high amount of Ru in titanium oxide nanotubes, compared to that in non-aqueous solution. The amounts of doped catalyst were analyzed by X-ray photoelectron spectroscopy (XPS). The optimum condition for water splitting was investigated in terms of the amount of doped Ru and thickness of barrier oxide layer.

Keywords: doping, potential shock, single step anodization, titanium oxide nanotubes

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Authors: Laroussi Chaabane, Emmanuel Beyou, Amel El Ghali, Mohammed Hassen V. Baouab

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The functionalization of graphene oxide sheets by ethylenediamine (EDA) was accomplished followed by the grafting of bis(2-pyridylmethyl)amino group (BPED) onto the activated graphene oxide sheets in the presence of chloroacetylchloride (CAC) produced the martial [(Go-EDA-CAC)-BPED]. The physic-chemical properties of [(Go-EDA-CAC)-BPED] composites were investigated by Fourier transform infrared (FT-IR), X-ray photoelectron spectroscopy (XPs), Scanning electron microscopy (SEM) and Thermogravimetric analysis (TGA). Moreover, [(Go-EDA-CAC)-BPED] was used for removing M(II) (where M=Cu, Ni and Co) ions from aqueous solutions using a batch process. The effect of pH, contact time and temperature were investigated. More importantly, the [(Go-EDA-CAC)-BPED] adsorbent exhibited remarkable performance in capturing heavy metal ions from water. The maximum adsorption capacity values of Cu(II), Ni(II) and Co(II) on the [(GO-EDA-CAC)-BPED] at the pH of 7 is 3.05 mmol.g⁻¹, 3.25 mmol.g⁻¹ and 3.05 mmol.g⁻¹ respectively. To examine the underlying mechanism of the adsorption process, pseudo-first, pseudo-second-order, and intraparticle diffusion models were fitted to experimental kinetic data. Results showed that the pseudo-second-order equation was appropriate to describe the three metal ions adsorption by [(Go-EDA-CAC)-BPED]. Adsorption data were further analyzed by the Langmuir, Freundlich, and Jossensadsorption approaches. Additionally, the adsorption properties of the [(Go-EDA-CAC)-BPED], their reusability (more than 10 cycles) and durability in the aqueous solutions open the path to removal of metal ions (Cu(II), Ni(II) and Co(II) from water solution. Based on the results obtained, we conclude that [(Go-EDA-CAC)-BPED] can be an effective and potential adsorbent for removing metal ions from an aqueous solution.

Keywords: graphene oxide, bis(2-pyridylmethyl)amino, adsorption kinetics, isotherms

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Authors: Mohamed Gouda

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Antibacterial wound dressings based on cellulose nanofibers containing different metal nanoparticles (CMC-MNPs) were synthesized using an electrospinning technique. First, the composite of carboxymethyl cellulose containing different metal nanoparticles (CMC/MNPs), such as copper nanoparticles (CuNPs), iron nanoparticles (FeNPs), zinc nanoparticles (ZnNPs), cadmium nanoparticles (CdNPs) and cobalt nanoparticles (CoNPs) were synthesized, and finally, these composites were transferred to the electrospinning process. Synthesized CMC-MNPs were characterized using scanning electron microscopy (SEM) coupled with high-energy dispersive X-ray (EDX) and UV-visible spectroscopy used to confirm nanoparticle formation. The SEM images clearly showed regular flat shapes with semi-porous surfaces. All MNPs were well distributed inside the backbone of the cellulose without aggregation. The average particle diameters were 29-39 nm for ZnNPs, 29-33 nm for CdNPs, 25-33 nm for CoNPs, 23-27 nm for CuNPs and 22-26 nm for FeNPs. Surface morphology, water uptake and release of MNPs from the nanofibers in water and antimicrobial efficacy were studied. SEM images revealed that electrospun CMC-MNPs nanofibers are smooth and uniformly distributed without bead formation with average fiber diameters in the range of 300 to 450 nm. Fiber diameters were not affected by the presence of MNPs. TEM images showed that MNPs are present in/on the electrospun CMC-MNPs nanofibers. The diameter of the electrospun nanofibers containing MNPs was in the range of 300–450 nm. The MNPs were observed to be spherical in shape. The CMC-MNPs nanofibers showed good hydrophilic properties and had excellent antibacterial activity against the Gram-negative bacteria Escherichia coli and the Gram-positive bacteria Staphylococcus aureus.

Keywords: electrospinning technique, metal nanoparticles, cellulosic nanofibers, wound dressing

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Authors: Muhammad Yasir, Debarun Dutta, Mark Willcox

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Biomaterial-associated infections are a multi-billion dollar burden globally. Antimicrobial peptide-based coatings may be able to prevent such infections. The aim of this study was to investigate the mechanism of action surface bound peptides (AMPs) against Pseudomonas aeruginosa 6294. Melimine and Mel4 were covalently attached to glass coverslips using azido-benzoic acid. Attachment was confirmed using X-ray photoelectron spectroscopy. P. aeruginosa was allowed to attach to AMP-coated glass for up to 6 hours. The effect of the surface-bound AMPs on bacterial cell membranes was evaluated using the dyes DiSC3-(5), Sytox green, SYTO 9 and propidium iodide with fluorescence microscopy. Release of cytoplasmic materials ATP and DNA/RNA were determined in the surrounding fluid. The amount of cell death was estimated by agar plate counts. The AMPs were successfully covalently bound to the glass as demonstrated by increases in %nitrogen of 3.6% (melimine) and 2.3% (Mel4) compared to controls. Immobilized peptides disrupted the cytoplasmic membrane potential of P. aeruginosa within 10 min. This was followed by the release of ATP after 2 h. Membrane permeabilization started at 3 h of contact with glass coated AMPs. There was a significant number of bacteria (59% for melimine; 36% for Mel-4) with damaged membranes after 4 h of contact. At the 6 h time point, release of DNA occurred with melimine releasing 2 times the amount of DNA/RNA than Mel4 surfaces (p < 0.05). Surface bound AMPs were able to disrupt cell membranes with subsequent release of cytoplasmic materials, and ultimately resulting in bacterial death.

Keywords: biomaterials, immobilized antimicrobial peptides, P. aeruginosa, mode of action

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