Search results for: confocal scanning microscopy

Authors: Eva Filová, Jana Daňková, Věra Sovková, Matej Daniel

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Titanium alloys are biocompatible metals that are widely used in clinical practice as load bearing implants. The chemical modification may influence cell adhesion, proliferation, and differentiation as well as stiffness of the material. The aim of the study was to evaluate the adhesion, growth and differentiation of pig mesenchymal stem cells on the novel beta titanium alloy Ti36Nb6Ta compared to standard medical titanium alloy Ti6Al4V. Discs of Ti36Nb6Ta and Ti6Al4V alloy were sterilized by ethanol, put in 48-well plates, and seeded by pig mesenchymal stem cells at the density of 60×103/cm2 and cultured in Minimum essential medium (Sigma) supplemented with 10% fetal bovine serum and penicillin/streptomycin. Cell viability was evaluated using MTS assay (CellTiter 96® AQueous One Solution Cell Proliferation Assay;Promega), cell proliferation using Quant-iT™ ds DNA Assay Kit (Life Technologies). Cells were stained immunohistochemically using monoclonal antibody beta-actin, and secondary antibody conjugated with AlexaFluor®488 and subsequently the spread area of cells was measured. Cell differentiation was evaluated by alkaline phosphatase assay using p-nitrophenyl phosphate (pNPP) as a substrate; the reaction was stopped by NaOH, and the absorbance was measured at 405 nm. Osteocalcin, specific bone marker was stained immunohistochemically and subsequently visualized using confocal microscopy; the fluorescence intensity was analyzed and quantified. Moreover, gene expression of osteogenic markers osteocalcin and type I collagen was evaluated by real-time reverse transcription-PCR (qRT-PCR). For statistical evaluation, One-way ANOVA followed by Student-Newman-Keuls Method was used. For qRT-PCR, the nonparametric Kruskal-Wallis Test and Dunn's Multiple Comparison Test were used. The absorbance in MTS assay was significantly higher on titanium alloy Ti6Al4V compared to beta titanium alloy Ti36Nb6Ta on days 7 and 14. Mesenchymal stem cells were well spread on both alloys, but no difference in spread area was found. No differences in alkaline phosphatase assay, fluorescence intensity of osteocalcin as well as the expression of type I collagen, and osteocalcin genes were observed. Higher expression of type I collagen compared to osteocalcin was observed for cells on both alloys. Both beta titanium alloy Ti36Nb6Ta and titanium alloy Ti6Al4V Ti36Nb6Ta supported mesenchymal stem cellsˈ adhesion, proliferation and osteogenic differentiation. Novel beta titanium alloys Ti36Nb6Ta is a promising material for bone implantation. The project was supported by the Czech Science Foundation: grant No. 16-14758S, the Grant Agency of the Charles University, grant No. 1246314 and by the Ministry of Education, Youth and Sports NPU I: LO1309.

Keywords: beta titanium, cell growth, mesenchymal stem cells, titanium alloy, implant

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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: Mahdieh Farzin Asanjan, Erkan Unal Mumcuoglu

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Mitochondria are cytoplasmic organelles of the cell, which have a significant role in the variety of cellular metabolic functions. Mitochondria act as the power plants of the cell and are surrounded by two membranes. Significant morphological alterations are often due to changes in mitochondrial functions. A powerful technique in order to study the three-dimensional (3D) structure of mitochondria and its alterations in disease states is Electron microscope tomography. Detection of mitochondria in electron microscopy images due to the presence of various subcellular structures and imaging artifacts is a challenging problem. Another challenge is that each image typically contains more than one mitochondrion. Hand segmentation of mitochondria is tedious and time-consuming and also special knowledge about the mitochondria is needed. Fully automatic segmentation methods lead to over-segmentation and mitochondria are not segmented properly. Therefore, semi-automatic segmentation methods with minimum manual effort are required to edit the results of fully automatic segmentation methods. Here two editing tools were implemented by applying spline surface dragging and interactive live-wire segmentation tools. These editing tools were applied separately to the results of fully automatic segmentation. 3D extension of these tools was also studied and tested. Dice coefficients of 2D and 3D for surface dragging using splines were 0.93 and 0.92. This metric for 2D and 3D for live-wire method were 0.94 and 0.91 respectively. The root mean square symmetric surface distance values of 2D and 3D for surface dragging was measured as 0.69, 0.93. The same metrics for live-wire tool were 0.60 and 2.11. Comparing the results of these editing tools with the results of automatic segmentation method, it shows that these editing tools, led to better results and these results were more similar to ground truth image but the required time was higher than hand-segmentation time

Keywords: medical image segmentation, semi-automatic methods, transmission electron microscopy, surface dragging using splines, live-wire

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Authors: Gianmarco Taveri, Ivo Dlouhy

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Geopolymers are well-suited materials to abate CO2 emission coming from the Portland cement production, and then replace them, in the near future, in building and other applications. The cost of production of geopolymers may be seen the only weakness, but the use of wastes as raw materials could provide a valid solution to this problem, as demonstrated by the successful incorporation of fly-ash, a by-product of thermal power plants, and waste glasses. Recycled glass in waste-derived geopolymers was lately employed as a further silica source. In this work we present, for the first time, the introduction of recycled borosilicate glass (BSG). BSG is actually a waste glass, since it derives from dismantled pharmaceutical vials and cannot be reused in the manufacturing of the original articles. Owing to the specific chemical composition (BSG is an ‘alumino-boro-silicate’), it was conceived to provide the key components of zeolitic networks, such as amorphous silica and alumina, as well as boria (B2O3), which may replace Al2O3 and contribute to the polycondensation process. The solid–state MAS NMR spectroscopy was used to assess the extent of boron oxide incorporation in the structure of geopolymers, and to define the degree of networking. FTIR spectroscopy was utilized to define the degree of polymerization and to detect boron bond vibration into the structure. Mechanical performance was tested by means of 3 point bending (flexural strength), chevron notch test (fracture toughness), compression test (compressive strength), micro-indentation test (Vicker’s hardness). Spectroscopy (SEM and Confocal spectroscopy) was performed on the specimens conducted to failure. FTIR showed a characteristic absorption band attributed to the stretching modes of tetrahedral boron ions, whose tetrahedral configuration is compatible to the reaction product of geopolymerization. 27Al NMR and 29Si NMR spectra were instrumental in understanding the extent of the reaction. 11B NMR spectroscopies evidenced a change of the trigonal boron (BO3) inside the BSG in favor of a quasi-total tetrahedral boron configuration (BO4). Thanks to these results, it was inferred that boron is part of the geopolymeric structure, replacing the Si in the network, similarly to the aluminum, and therefore improving the quality of the microstructure, in favor of a more cross-linked network. As expected, the material gained as much as 25% in compressive strength (45 MPa) compared to the literature, whereas no improvements were detected in flexural strength (~ 5 MPa) and superficial hardness (~ 78 HV). The material also exhibited a low fracture toughness (0.35 MPa*m1/2), with a tangible brittleness. SEM micrographies corroborated this behavior, showing a ragged surface, along with several cracks, due to the high presence of porosity and impurities, acting as preferential points for crack initiation. The 3D pattern of the surface fracture, following the confocal spectroscopy, evidenced an irregular crack propagation, whose proclivity was mainly, but not always, to follow the porosity. Hence, the crack initiation and propagation are largely unpredictable.

Keywords: borosilicate glass, characterization, fly-ash, geopolymerization

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Authors: Eyob Belew Abebe

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Nickel-rich layered oxide cathode materials having a Ni content of ≥ 90% have great potential for use in next-generation lithium-ion batteries (LIBs), due to their high energy densities and relatively low cost. They suffer, however, from poor cycling performance and rate capability, significantly hampering their widespread applicability. In this study we synthesized a Ni-rich precursor through a co-precipitation method and added different amounts of Li-excess on the precursors using a solid-state method to obtain sintered Li1+x(Ni0.9Co0.05Mn0.05)1–xO2 (denoted as L1+x-NCM; x = 0.00, 0.02, 0.04, 0.06, and 0.08) transition metal (TM) oxide cathode materials. The L1+x-NCM cathode having a Li-excess of 4% exhibited a discharge capacity of ca. 216.17 mAh g–1 at 2.7–4.3 V, 0.1C and retained 95.7% of its initial discharge capacity (ca. 181.39 mAh g–1) after 100 cycles of 1C charge/discharge which is the best performance as compared with stoichiometric Li1+x(Ni0.9Co0.05Mn0.05)1-xO2 (i.e. x=0, Li:TM = 1:1). Furthermore, a high-rate capability of ca. 162.92 mAh g–1 at a rate of 10C, led to the 4% Li-excess optimizing the electrochemical performance, relative to the other Li-excess samples. Ex/in-situ X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy revealed that the 4% Li-excess in the Ni-rich NCM90 cathode material: (i). decreased the Li+/Ni2+ disorder by increasing the content of Ni3+ in the TM slab, (ii). increased the crystallinity, and (iii). accelerated Li+ ion transport by widening the Li-slab. Furthermore, electrochemical impedance spectroscopy and cyclic voltammetry confirmed that the appropriate Li-excess lowered the electrochemical impedance and improved the reversibility of the electrochemical reaction. Therefore, our results revealed that NCM90 cathode materials featuring an optimal Li-excess are potential candidates for use in next-generation Li-ion batteries.

Keywords: LiNi₀.₉Co₀.₀₉Mn₀.₀₉O₂, li-excess, cation mixing, structure change, cycle stability, electrochemical properties

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Authors: D. G. Rejon-Parra, B. Escobar-Morales, Romeli Barbosa, J. C. Cruz

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In the southeast of Yucatan Peninsula, sedimentary limestone has different degrees of compaction. Due to its recent geological formation (Quaternary) and weathering effects causing an affordable aggregate for local manufacturers of concrete. It is characterized as lightweight aggregates (average density of 2,50), susceptible to abrasion and varying porosities (water content exceeding 7,50 % of its mass, in saturated condition). In this study, local aggregates with two moisture conditions (saturated and dry), have been examined in order to compare them for optimizing the performance of concrete. It is possible that these aggregates favour a phenomenon of mass transport (self-curing by porous aggregate); influencing the water reactions to form crystalline and gel hydration products. Based on the ACI methodology, a concrete mixture of 250 kg/cm2 was designed, with portland blended cement 30R. The bond between the mortar and the coarse aggregate was characterized as physicochemical based on trials which were carefully observed during time span of 28 days. The BET technique was used to analyse the micro porosity and surface areas of contact of the different crystalline phases of the limestone. Its chemical composition and crystal structures were verified with scanning electron microscopy SEM-EDS. On the third day, the samples with saturated aggregate reached 237 kg/cm2 of resistence, nearly the design strength; while samples with dry aggregate, exceeded the design strength, with a capacity of 308 kg/cm2. Aggregates in dry conditions demand a high quantity of water in the initial mixture, causing high resistance at the early stages. In saturated conditions, the development of resistance is progressive but constant.

Keywords: concrete, internal curing, limestone aggregate, porosity

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Authors: F. Z. Abir, M. Mesnaoui, Y. Abouliatim, L. Nibou, Y. El Hafiane, A. Smith

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The cement industry has been taking significant steps for years to reduce its carbon footprint by opting for an eco-friendly alternative such as Calcium Sulfoaluminate Cements (CSA). These binders, compared to Ordinary Portland Cements (OPC), have two advantages: reduction of the CO2 emissions and energy-saving because the sintering temperature of CSA cements is between 1250 and 1350 °C, which means 100 to 200 °C less than OPC. The aim of this work is to study the impurities effect, such as iron oxide, on the formation of the ye'elimite phase, which represents the main phase of Calcium Sulfoaluminate Cements and the consequence on its hydration. Several elaborations and characterization techniques were used to study the structure and microstructure of ye'elimite, such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), thermal analysis, specific surface area measurement, and electrical conductivity of diluted solutions. This study details the protocol for the solid-state synthesis of ye'elimite containing increasing amounts of iron (general formula: Ca4Al(6-2x)Fe2xSO16 with x = 0.00 to 1.13). Ye'elimite is formed by solid-state reactions between Al2O3, CaO and CaSO4 and the maximum ye'elimite content is reached at a sintering temperature of 1300 °C. The presence of iron promotes the formation of cubic ye'elimite at the expense of the orthorhombic phase. The total incorporation of iron in ye'elimite structure is possible when x < 0.12. Beyond this content, the ferritic phase (CaO)2(Al2O3,Fe2O3) appears as a minor phase and develops two different morphologies during cooling: dendritic crystals and melt morphology. The formation of the ferrous liquid phase affects the evolution of grain size of the ye’elimite and calcium aluminates.

Keywords: calcium sulfoaluminate cement, ferritic phase, sintering, solid-state synthesis, ye’elimite

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Authors: Fatih Kılıç, Burak Birol, Necmettin Maraşlı

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The directional solidification process is generally used for homogeneous compound production, single crystal growth, and refining (zone refining), etc. processes. The most important two parameters that control eutectic structures are temperature gradient and grain growth rate which are called as solidification parameters The solidification behavior and microstructure characteristics is an interesting topic due to their effects on the properties and performance of the alloys containing eutectic compositions. The solidification behavior of multicomponent and multiphase systems is an important parameter for determining various properties of these materials. The researches have been conducted mostly on the solidification of pure materials or alloys containing two phases. However, there are very few studies on the literature about multiphase reactions and microstructure formation of multicomponent alloys during solidification. Because of this situation, it is important to study the microstructure formation and the thermodynamical, thermophysical and microstructural properties of these alloys. The production process is difficult due to easy oxidation of magnesium and therefore, there is not a comprehensive study concerning alloys containing high Mg (> 30 wt.% Mg). With the increasing amount of Mg inside Al alloys, the specific weight decreases, and the strength shows a slight increase, while due to formation of β-Al8Mg5 phase, ductility lowers. For this reason, production, examination and development of high Mg containing alloys will initiate the production of new advanced engineering materials. The original value of this research can be described as obtaining high Mg containing (> 30% Mg) Al based multicomponent alloys by melting under vacuum; controlled directional solidification with various growth rates at a constant temperature gradient; and establishing relationship between solidification rate and microstructural, mechanical, electrical and thermal properties. Therefore, within the scope of this research, some > 30% Mg containing ternary or quaternary Al alloy compositions were determined, and it was planned to investigate the effects of directional solidification rate on the mechanical, electrical and thermal properties of these alloys. Within the scope of the research, the influence of the growth rate on microstructure parameters, microhardness, tensile strength, electrical conductivity and thermal conductivity of directionally solidified high Mg containing Al-32,2Mg-0,37Si; Al-30Mg-12Zn; Al-32Mg-1,7Ni; Al-32,2Mg-0,37Fe; Al-32Mg-1,7Ni-0,4Si; Al-33,3Mg-0,35Si-0,11Fe (wt.%) alloys with wide range of growth rate (50-2500 µm/s) and fixed temperature gradient, will be investigated. The work can be planned as; (a) directional solidification of Al-Mg based Al-Mg-Si, Al-Mg-Zn, Al-Mg-Ni, Al-Mg-Fe, Al-Mg-Ni-Si, Al-Mg-Si-Fe within wide range of growth rates (50-2500 µm/s) at a constant temperature gradient by Bridgman type solidification system, (b) analysis of microstructure parameters of directionally solidified alloys by using an optical light microscopy and Scanning Electron Microscopy (SEM), (c) measurement of microhardness and tensile strength of directionally solidified alloys, (d) measurement of electrical conductivity by four point probe technique at room temperature (e) measurement of thermal conductivity by linear heat flow method at room temperature.

Keywords: directional solidification, electrical conductivity, high Mg containing multicomponent Al alloys, microhardness, microstructure, tensile strength, thermal conductivity

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Authors: Ceren Karaman, Onur Karaman

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The adsorption of Remazol Black B (RBB), an anionic dye, onto dried orange pulp (DOP) adsorbent prepared by only drying and by treating with cetyltrimetylammonium bromide (CTAB), a cationic surfactant, surface-modified orange pulp (SMOP) was studied in a stirred batch experiments system at 25°C. The adsorption of RBB on each adsorbent as a function of surfactant dosage, initial pH of the solution and initial dye concentration was investigated. The optimum amount of CTAB was found to be 25g/l. For RBB adsorption studies, while working pH value for the DOP adsorbent system was determined as 2.0, it was observed that this value shifted to 8.0 when the 25 g/l CTAB treated-orange pulp (SMOP) adsorbent was used. It was obtained that the adsorption rate and capacity increased to a certain value, and the adsorption efficiency decreased with increasing initial RBB concentration for both DOP and SMOP adsorbents at pH 2.0 and pH 8.0. While the highest adsorption capacity for DOP was determined as 62.4 mg/g at pH 2.0, and as 325.0 mg/g for SMOP at pH 8.0. As a result, it can be said that permanent cationic coating of the adsorbent surface by CTAB surfactant shifted the working pH from 2.0 to 8.0 and it increased the dye adsorption rate and capacity of orange pulp much more significantly at pH 8.0. The equilibrium RBB adsorption data on each adsorbent were best described by the Langmuir isotherm model. The adsorption kinetics of RBB on each adsorbent followed a pseudo-second-order model. Moreover, the intraparticle diffusion model was used to describe the kinetic data. It was found that diffusion is not the only rate controlling step. The adsorbent was characterized by the Brunauer–Emmett–Teller (BET) analysis, Fourier-transform-infrared (FTIR) spectroscopy, and scanning-electron-microscopy (SEM). The mechanism for the adsorption of RBB on the SMOP may include hydrophobic interaction, van der Waals interaction, stacking and electrostatic interaction.

Keywords: adsorption, Cetyltrimethylammonium Bromide (CTAB), orange pulp, Remazol Black B (RBB), surface modification

Procedia PDF Downloads 248

Authors: Asma Ansari, Afsheen Aman, Shah Ali Ul Qader

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In the past few years, numerous concerns have been raised against increased bacterial resistance towards effective drugs and become a debated issue all over the world. With the emergence of drug resistant pathogens, the interaction of natural antimicrobial compounds and antibacterial nanoparticles has emerged as a potential candidate for combating infectious diseases. Microbial diversity in the biome provides an opportunity to screen new species which are capable of producing large number of antimicrobial compounds. Among these antimicrobial compounds, bacteriocins are highly specific and efficient antagonists. A combination of bacteriocin along with nanoparticles could prove to be more potent due to broadened antibacterial spectrum with possibly lower doses. In the current study, silver nanoparticles were synthesized through biological reduction using various isolated bacterial, fungal and yeast strains. Spectroscopy and scanning electron microscopy (SEM) was performed for the confirmation of nanoparticles. Bacteriocin was characterized and purified to homogeneity through gel permeation chromatography. The estimated molecular weight of bacteriocin was 10 kDa. Amino acid analysis and N-terminal sequencing revealed the novelty of the protein. Then antibacterial potential of silver nanoparticles and broad inhibitory spectrum bacteriocin was determined through agar well diffusion assay. These synthesized bacteriocin-Nanoparticles exhibit a good potential for clinical applications as compared to bacteriocin alone. This combination of bacteriocin with nanoparticles will be used as a new sort of biocide in the field of nano-proteomics. The advancement of nanoparticles-mediated drug delivery system will open a new age for rapid eradication of pathogens from biological systems.

Keywords: BAC-IB17, multidrug resistance, purification, silver nanoparticles

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Authors: Rajnarayan Damor, Gayatri Swarnakar

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Fasciola gigantica are present in the biliary ducts of liver and gall bladder of domestic buffaloes. They are very harmful and causes significant lose to live stock owners, on account of poor growth and lower productivity of domestic buffaloes. Synthetic veterinary drugs have been used to eliminate parasites from cattle but these drugs are unaffordable and inaccessible for poor cattle farmers. The in vitro anthelmintic effect of Citrullus colocynthis fruit extract against Fasciola gigantica parasites were observed by light and scanning electron microscopy. Fruit extracts of C. colocynthis exhibit highest mortality 100% at 50 mg/ml in 15th hour of exposure. The oral and ventral sucker appeared to be slightly more swollen than control and synthetic drug albendazole. The tegument showed submerged spines by the swollen tegument around them. The tegument of the middle region showed deep furrows, folding and submerged spines which either lied very flat against the surface or had become submerged in the tegument by the swollen tegument around them leaving deep furrows. Posterior region showed with deep folding in the tegument, completely disappearance of spines and swelling of the tegument led to completely submerged spines leaving spine socket. The present study revealed that fruit extracts of Citrullus colocynthis found to be potential sources for novel anthelmintic and justify their ethno-veterinary use.

Keywords: anthelmintic, buffalo, Citrullus colocynthis, Fasciola gigantica, mortality, tegument

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Authors: Phillip Ahn, Bryan Kim

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Copper is perhaps the most prevalent heavy metal used in the manufacturing industries, from food additives to metal-mechanic factories. Common methodologies to remove copper are expensive and produce undesired by-products. A good decontaminating candidate should be environment-friendly, inexpensive, and capable of eliminating low concentrations of the metal. This work suggests chemically modified spent tea leaves of chamomile, peppermint and green tea in their thiolated, sulfonated and carboxylated forms as candidates for the removal of copper from solutions. Batch experiments were conducted to maximize the adsorption of copper (II) ions. Effects such as acidity, salinity, adsorbent dose, metal concentration, and presence of surfactant were explored. Experimental data show that maximum adsorption is reached at neutral pH. The results indicate that Cu(II) can be removed up to 53%, 22% and 19% with the thiolated, carboxylated and sulfonated adsorbents, respectively. Maximum adsorption of copper on TPM (53%) is achieved with 150 mg and decreases with the presence of salts and surfactants. Conversely, sulfonated and carboxylated adsorbents show better adsorption in the presence of surfactants. Time-dependent experiments show that adsorption is reached in less than 25 min for TCM and 5 min for SCM. Instrumental analyses determined the presence of active functional groups, thermal resistance, and scanning electron microscopy, indicating that both adsorbents are promising materials for the selective recovery and treatment of metal ions from wastewaters. Finally, columns were prepared with these adsorbents to explore their application in scaled-up processes, with very positive results. A long-term goal involves the recycling of the exhausted adsorbent and/or their use in the preparation of biofuels due to changes in materials’ structures.

Keywords: heavy metal removal, adsorption, wastewaters, water remediation

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Authors: Pauline Ribert, Gaelle Roudaut, Sebastien Dupont, Laurent Beney

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Yeasts, anhydrobiotic organisms, can survive extreme water disturbances, thanks to the prolonged and reversible suspension of their cellular activity as well as the establishment of a defense arsenal. This property is exploited by many industrialists. One of the protection systems implemented by yeast is the vitrification of its cytoplasm by trehalose. The thermal resistance of dry yeasts is a crucial parameter for their use. However, studies on the thermal resistance of dry yeasts are often based on yeasts produced in laboratory conditions with non-optimal drying processes. We, therefore, propose a study on the thermal resistance of industrial dry yeasts in relation to their thermophysical properties. Heat stress was applied at three temperatures (50, 75, and 100°C) for 10, 30, or 60-minute treatments. The survival of yeasts to these treatments was estimated, and their thermophysical properties were studied by differential scanning calorimetry. The industrial dry yeasts resisted 60 minutes at 50°C and 75°C and 10 minutes at a temperature close to 100°C. At 100°C, yeast was above their glass transition temperature. Industrial dry yeasts are therefore capable of withstanding high thermal stress if maintained in a specific thermophysical state.

Keywords: dry yeast, glass transition, thermal resistance, vitrification

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Authors: N. Boudinar, A. Djekoun, A. Otmani, B. Bouzabata, J. M. Greneche

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High-energy ball milling is a solid-state powder processing technique that allows synthesizing a variety of equilibrium and non-equilibrium alloy phases starting from elemental powders. The advantage of this process technology is that the powder can be produced in large quantities and the processing parameters can be easily controlled, thus it is a suitable method for commercial applications. It can also be used to produce amorphous and nanocrystalline materials in commercially relevant amounts and is also amenable to the production of a variety of alloy compositions. Mechanical alloying (high-energy ball milling) provides an inter-dispersion of elements through a repeated cold welding and fracture of free powder particles; the grain size decreases to nano metric scale and the element mix together. Progressively, the concentration gradients disappear and eventually the elements are mixed at the atomic scale. The end products depend on many parameters such as the milling conditions and the thermodynamic properties of the milled system. Here, the mechanical alloying technique has been used to prepare nano crystalline Fe_50 and Fe_64 wt.% Ni alloys from powder mixtures. Scanning electron microscopy (SEM) with energy-dispersive, X-ray analyses and Mössbauer spectroscopy were used to study the mixing at nanometric scale. The Mössbauer Spectroscopy confirmed the ferromagnetic ordering and was use to calculate the distribution of hyperfin field. The Mössbauer spectrum for both alloys shows the existence of a ferromagnetic phase attributed to γ-Fe-Ni solid solution.

Keywords: nanocrystalline, mechanical alloying, X-ray diffraction, Mössbauer spectroscopy, phase transformations

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Authors: Mostafa Mabrouk, Basma E. Abdel-Ghany, Mona Moaness, Bothaina M. Abdel-Hady, Hanan H. Beherei

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Tissue engineering became a promising field for bone repair and regenerative medicine in which cultured cells, scaffolds and osteogenic inductive signals are used to regenerate tissues. The annual cost of treating bone defects in Egypt has been estimated to be many billions, while enormous costs are spent on imported bone grafts for bone injuries, tumors, and other pathologies associated with defective fracture healing. The current study is aimed at developing a more strategic approach in order to speed-up recovery after bone damage. This will reduce the risk of fatal surgical complications and improve the quality of life of people affected with such fractures. 3D scaffolds loaded with cheap nano-particles that possess an osteogenic effect were prepared by nano-electrospinning. The Microstructure and morphology characterizations of the 3D scaffolds were monitored using scanning electron microscopy (SEM). The physicochemical characterization was investigated using X-ray diffractometry (XRD) and infrared spectroscopy (IR). The Physicomechanical properties of the 3D scaffold were determined by a universal testing machine. The in vitro bioactivity of the 3D scaffold was assessed in simulated body fluid (SBF). The bone-bonding ability of novel 3D scaffolds was also evaluated. The obtained nanofibrous scaffolds demonstrated promising microstructure, physicochemical and physicomechanical features appropriate for enhanced bone regeneration. Therefore, the utilized nanomaterials loaded with the drug are greatly recommended as cheap alternatives to growth factors.

Keywords: bone regeneration, cheap scaffolds, nanomaterials, active molecules

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Authors: A. Jourani, C. Trevisiol, S. Bouvier

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The aim of this work is to study the coupled effect of microstructure and surface roughness on friction coefficient, wear resistance and wear mechanisms. Friction tests on 35NCD16 steel are performed under different normal loads (50-110 N) on a pin-on-plane configuration at cyclic sliding with abrasive silicon carbide grains ranging from 35 µm to 200 µm. To vary hardness and microstructure, the specimens are subjected to water quenching and tempering at various temperatures from 200°C to 600°C. The evolution of microstructures and wear mechanisms of worn surfaces are analyzed using scanning electron microscopy (SEM). For a given microstructure and hardness, the friction coefficient decreases with increasing of normal load and decreasing of the abrasive particle size. The wear rate increase with increasing of normal load and abrasive particle size. The results also reveal that there is a critical hardness Hcᵣᵢₜᵢcₐₗ around 430 Hv which maximizes the friction coefficient and wear rate. This corresponds to a microstructure transition from martensite laths to carbides and equiaxed grains, for a tempering around 400°C. Above Hcᵣᵢₜᵢcₐₗ the friction coefficient and the amount of material loss decrease with an increase of hardness and martensite volume fraction. This study also shows that the debris size and the space between the abrasive particles decrease with a reduction in the particle size. The coarsest abrasive grains lost their cutting edges, accompanied by particle damage and empty space due to the particle detachment from the resin matrix. The compact packing nature of finer abrasive papers implicates lower particle detachment and facilitates the clogging and the transition from abrasive to adhesive wear.

Keywords: martensite, microstructure, friction, wear, surface roughness

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

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A process that utilizes a combination of additive manufacturing (AM), a preceramic polymer, and a chopped carbon fiber precursorto fabricate Silicon Carbon/ Carbon fibers (SiC/C) composites have been developed. The study has shown a promising, cost-effective, and efficient route to fabricate complex SiC/C composites using additive manufacturing. A key part of this effort was the mapping of the material’s microstructure through the thickness of the composite. Microstructural features in the pyrolyzed composites through the successive AM layers, such as defects, crystal size and their distribution, interatomic spacing, chemical bonds, were investigated using high-resolution scanning and transmission electron microscopy. As a result, the microstructure developed in SiC/C composites after printing, cure, and pyrolysis has been successfully mapped through the thickness of the derived composites. Dense and nearly defect-free parts after polymer to ceramic conversion were observed. The ceramic matrix composite displayed three coexisting phases, including silicon carbide, silicon oxycarbide, and turbostratic carbon. Lattice fringes imaging and X-Ray Diffraction analysis showed well-defined SiC and turbostratic carbon features. The cross-sectional mapping of the printed-then-pyrolyzed structures has confirmed consistent structural and chemical features within the internal layers of the AM parts. Noteworthy, however, is that a crust-like area with high crystallinity has been observed in the first and last external layers. Not only do these crust-like regions have structural characteristics distinct from the internal layers, but they also have elemental distributions different than the internal layers.

Keywords: SiC, preceramic polymer, additive manufacturing, ceramic

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Authors: Gabriel K. Nzulu, Lina Rostorm, Hans Högberg, Jun Liu, per Eklund, Lars Hultman, Martin Magnuson

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Altered and gangue quartz in hydrothermal veins from the Kubi Gold deposit in Dunkwa on Offin in the central region of Ghana are investigated for possible Au associated pathfinder minerals and to provide understanding and increase the knowledge of the mineral hosting and alteration processes in quartz. X-ray diffraction, air annealing furnace, differential scanning calorimetry, energy dispersive X-ray spectroscopy, and transmission electron microscopy have been applied on different quartz types outcropping from surface and bed rocks at the Kubi Gold Mining to reveal the material properties at different temperatures. From the diffraction results of the fresh and annealed quartz samples, we find that the samples contain pathfinder and the impurity minerals FeS₂, biotite, TiO₂, and magnetite. These minerals, under oxidation process between 574-1400 °C temperatures experienced hematite alterations and a transformation from α-quartz to β-quartz and further to cristobalite as observed from the calorimetry scans for hydrothermally exposed materials. The energy dispersive spectroscopy revealed elemental species of Fe, S, Mg, K, Al, Ti, Na, Si, O, and Ca contained in the samples and these are attributed to the impurity phase minerals observed in the diffraction. The findings also suggest that during the hydrothermal flow regime, impurity minerals and metals can be trapped by voids and faults. Under favorable temperature conditions the trapped minerals can be altered to change color at different depositional stages by oxidation and reduction processes leading to hematite alteration which is a useful pathfinder in mineral exploration.

Keywords: quartz, hydrothermal, minerals, hematite, x-ray diffraction, crystal-structure, defects

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Authors: Abbas Jafarizad, Duygu Ekinci

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In this work targeted drug delivery is proposed to decrease adverse effect of drugs with concomitant reduces in consumption and treatment outgoings. Nanoparticles (NPs) can be prepared from a variety of materials such as lipid, biodegradable polymer that prevent the drugs cytotoxicity in healthy cells, etc. One of the most important drugs used in chemotherapy is mitoxantrone (MTX) which prevents cell proliferation by inhibition of topoisomerase II and DNA repair; however, it is not selective and has some serious side effects. In this study, mentioned aim is achieved by using several nanocarriers like magnetite (Fe3O4) and their composites with magnetic graphene oxide (Fe3O4@GO). Also, cytotoxic potential of Fe3O4, Fe3O4-MTX, and Fe3O4@GO-MTX nanocomposite were evaluated on mesenchymal stem cells (MSCs). In this study, we reported the synthesis of monodisperse Fe3O4 NPs and Fe3O4@GO nanocomposite and their structures were investigated by using field emission scanning electron microscope (FESEM), Fourier transform infrared (FTIR) spectra, atomic force microscopy (AFM), Brauneur Emmet Teller (BET) isotherm and contact angle studies. Moreover, we used 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay to evaluate cytotoxic effects of MTX, Fe3O4 NPs, Fe3O4-MTX and Fe3O4@GO-MTX nanocomposite on MSCs. The in-vitro MTT results indicated that all concentrations of MTX and Fe3O4@GO-MTX nanocomposites showed cytotoxic effects while all concentrations of Fe3O4 NPs and Fe3O4-MTX NPs did not show any cytotoxic effect on stem cells. The results from this study indicated that using Fe3O4 NPs as anticancer drug delivery systems could be a trustworthy method for cancer treatment. But for reaching excellent and accurate results, further investigation is necessary.

Keywords: mitoxantrone, magnetite, magnetic graphene oxide, MTT assay, mesenchymal stem cells

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Authors: Filipa Vasconcelos

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The administration of endoplasmic reticulum amino peptidases (ERAP1 or ERAP2) inhibitors can be used for therapeutic approaches against cancer and auto-immune diseases. However, one of the main shortcomings of drug delivery systems (DDS) is associated with the drug off-target distribution, which can lead to an increase in its side effects on the patient’s body. To overcome such limitations, the encapsulation of four representative compounds of ERAP inhibitors into Polycaprolactone (PCL), Polyvinyl-alcohol (PVA), crosslinked PVA, and PVA with nanoparticles (liposomes) electrospun fibrous meshes is proposed as a safe and controlled drug release system. The use of electrospun fibrous meshes as a DDS allows efficient solvent evaporation giving limited time to the encapsulated drug to recrystallize, continuous delivery of the drug while the fibers degrade, prevention of initial burst release (sustained release), tunable dosages, and the encapsulation of other agents. This is possible due to the fibers' small diameters and resemblance to the extracellular matrix (confirmed by scanning electron microscopy results), high specific surface area, and good mechanical strength/stability. Furthermore, release studies conducted on PCL, PVA, crosslinked PVA, and PVA with nanoparticles (liposomes) electrospun fibrous meshes with each of the ERAP compounds encapsulated demonstrated that they were capable of releasing >60%, 50%, 40%, and 45% of the total ERAP concentration, respectively. Fibrous meshes with ERAP_E compound encapsulated achieved higher released concentrations (75.65%, 62.41%, 56.05%, and 65.39%, respectively). Toxicity studies of fibrous meshes with encapsulated compounds are currently being accessed in vitro, as well as pharmacokinetics and dynamics studies. The last step includes the implantation of the drug-loaded fibrous meshes in vivo.

Keywords: drug delivery, electrospinning, ERAP inhibitors, liposomes

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Authors: Natalie A. Sterk, Bernard van Vuuren, Petrie Marais, Bongani Mthombeni

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Injuries to the internal structures of the thorax and abdomen remain a leading cause of death among soldiers. Body armour is a standard issue piece of military equipment designed to protect the vital organs against ballistic and stab threats. When configured for maximum protection, the excessive weight and size of the armour may limit soldier mobility and increase physical fatigue and discomfort. Providing soldiers with more armour than necessary may, therefore, hinder their ability to react rapidly in life-threatening situations. The capability to determine the optimal trade-off between the amount of essential anatomical coverage and hindrance on soldier performance may significantly enhance the design of armour systems. The current study aimed to develop and pilot a methodology for relating internal anatomical structures with actual armour plate coverage in real-time using low-dose diagnostic X-ray scanning. Several pilot scanning sessions were held at Lodox Systems (Pty) Ltd head-office in South Africa. Testing involved using the Lodox eXero-dr to scan dummy trunk rigs at various degrees and heights of measurement; as well as human participants, wearing correctly fitted body armour while positioned in supine, prone shooting, seated and kneeling shooting postures. The verification of sizing and metrics obtained from the Lodox eXero-dr were then confirmed through a verification board with known dimensions. Results indicated that the low-dose diagnostic X-ray has the capability to clearly identify the vital internal structures of the aortic arch, heart, and lungs in relation to the position of the external armour plates. Further testing is still required in order to fully and accurately identify the inferior liver boundary, inferior vena cava, and spleen. The scans produced in the supine, prone, and seated postures provided superior image quality over the kneeling posture. The X-ray-source and-detector distance from the object must be standardised to control for possible magnification changes and for comparison purposes. To account for this, specific scanning heights and angles were identified to allow for parallel scanning of relevant areas. The low-dose diagnostic X-ray provides a non-invasive, safe, and rapid technique for relating vital internal structures with external structures. This capability can be used for the re-evaluation of anatomical coverage required for essential protection while optimising armour design and fit for soldier performance.

Keywords: body armour, low-dose diagnostic X-ray, scanning, vital organ coverage

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Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are used as core components of nuclear reactors due to their high wear resistance, good corrosion properties, and good mechanical stability at high temperatures. The present work simulates the contact between the calandria tube and the liquid injection shutdown system (LISS) nozzle. The Calandria tube is the outer covering of the pressure tube. Water flows inside the pressure tube through fuel claddings which produces vibration in the pressure tube along with vibration in the calandria tube. Fretting wear takes place at the point of contact between the calandria tube and the LISS nozzle. Fretting tests were performed under different conditions, such as; varying fretting duration (i.e., 1 to 4 hours), varying frequency (i.e., 5 to 6.5 Hz), and varying amplitude (100 to 400 µm). The formation of the oxide layer was observed during the fretting wear test; as a result, the worn product. The worn surfaces were analyzed with scanning electron microscopy (SEM) to analyze the wear mechanism involved in the fretting test, and Energy dispersive x-ray spectroscopy (EDS) and Raman spectroscopy were used to confirm the presence of an oxide layer on the worn surface. The oxide layer becomes more uniform with fretting duration in case of water submerged condition as compared to dry contact condition. The oxide layer is deeply removed at high amplitude due to the change of wear mechanism from adhesion to abrasion, as confirmed by the presence of micro ploughing and micro cutting. Low amplitude fretting favors the formation of the tribo-oxide layer.

Keywords: tribo-oxide layer, wear, mechanically mixed layer, zircaloy

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Authors: Saci Abdelhakim Ferkous, Khedoudja Soudani, Smail Haddadi

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This paper presents the results of a laboratory experimental study that explores the skid resistance of asphalt concrete mixtures made of local low-performance aggregates by partially replacing sand with olive mill waste (OMW). OMW was mixed with aggregates using a dry process by replacing sand with contents of 5%, 7%, 10% and 15%. The mechanical performances of the mixtures were evaluated using the Marshall and Duriez tests. A modified accelerated polishing machine was used as polishing equipment, and a British pendulum tester (BPT) was used to test the skid resistance of the samples. Finally, texture parameter analysis was performed using scanning electron microscopy (SEM) and Mountains Map software to assess the effect of OMW on the friction coefficient evolution. Using a distinct road wheel for a modified version of an accelerated polishing machine, which is normally used to determine the polished stone value of aggregates, the results showed that the addition of OMW up to 10% conferred a better skid resistance in comparison to normal asphalt concrete. The presence of olive mill waste in the mixture until 15% guarantees a gain of 22%-29% in skid resistance after polishing compared with the reference mix. Indeed, from texture parameter analysis, it was observed that there was differential wear of the lightweight aggregates (OMW) compared to the other aggregates during the polishing process, which created a new surface microtexture that had new peaks and led to a good level of friction compared to the mixtures without OMW. In general, it was found that OMW is a promising modifier for asphalt mixtures with both engineering and economic merits.

Keywords: skid resistance, olive mill waste, polishing resistance, accelerated polishing machine, local materials, sustainable development.

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Authors: Kateryna Zhdanova, Evelyn Szeinbaum, Michelle Lo, Yeonjae Jo, Abel E. Navarro

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Alginate hydrogel beads (AB), spent peppermint leaf (PM), and a hybrid adsorbent of these two materials (ABPM) were studied as potential biosorbents of Cobalt (II) ions from aqueous solutions. Cobalt ion is a commonly underestimated pollutant that is responsible for several health problems. Discontinuous batch experiments were conducted at room temperature to evaluate the effect of solution acidity, mass of adsorbent on the adsorption of Co(II) ions. The interfering effect of salinity, the presence of surfactants, an organic dye, and Pb(II) ions were also studied to resemble the application of these adsorbents in real wastewater. Equilibrium results indicate that Co(II) uptake is maximized at pH values higher than 5, with adsorbent doses of 200 mg, 200 mg, and 120 mg for AB, PM, and ABPM, respectively. Co(II) adsorption followed the trend AB > ABPM > PM with Adsorption percentages of 77%, 71% and 64%, respectively. Salts had a strong negative effect on the adsorption due to the increase of the ionic strength and the competition for adsorption sites. The presence of Pb(II) ions, surfactant, and dye BY57 had a slightly negative effect on the adsorption, apparently due to their interaction with different adsorption sites that do not interfere with the removal of Co(II). A polar-electrostatic adsorption mechanism is proposed based on the experimental results. Scanning electron microscopy indicates that adsorbent has appropriate morphological and textural properties, and also that ABPM encapsulated most of the PM inside of the hydrogel beads. These experimental results revealed that AB, PM, and ABPM are promising adsorbents for the elimination of Co(II) ions from aqueous solutions under different experimental conditions. These biopolymers are proposed as eco-friendly alternatives for the removal of heavy metal ions at lower costs than the conventional techniques.

Keywords: adsorption, Co(II) ions, alginate hydrogel beads, spent peppermint leaf, pH

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Authors: Anna-Caroline Lavergne-Bril, Jean-François Colin, David Peralta, Pascale Maldivi

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Cobalt is a critical material, widely used in Li-ion batteries. Due to the planned electrification of European vehicles, cobalt needs are expending – and resources are limited. To meet the needs in cobalt to come, it is necessary to develop new efficient ways to recycle cobalt. One of the biggest sources comes from old electrical vehicles batteries (batteries sold in 2019: 500 000 tons of waste to be). A closed loop process of cobalt recycling has been developed and this presentation aims to present the selectivity mechanism of cobalt over manganese and nickel in solution. Cobalt precipitation as a ZIF material (Zeolitic Imidazolate framework) from a starting solution composed of equimolar nickel, manganese and cobalt is studied. A 2-MeIm (2-methylimidazole) linker is introduced in a multimetallic Ni, Mn, Co solution and the resulting ZIF-67 is 100% pure Co among its metallic centers. Selectivity of Co over Ni is experimentally studied and DFT modelisation calculation are conducted to understand the geometry of ligand-metal-solvent complexes in solution. Selectivity of Co over Mn is experimentally studied, and DFT modelisation calcucation are conducted to understand the link between pKa of the ligand and precipitration of Mn impurities within the final material. Those calculation open the way to other ligand being used in the same process, with more efficiency. Experimental material are synthetized from bimetallic (Ni²⁺/Co²⁺, Mn²⁺/Co²⁺, Mn²⁺/Ni²⁺) solutions. Their crystallographic structure is analysed by XRD diffraction (Brüker AXS D8 diffractometer, Cu anticathode). Morphology is studied by scanning electron microscopy, using a LEO 1530 FE-SEM microscope. The chemical analysis is performed by using ICP-OES (Agilent Technologies 700 series ICP-OES). Modelisation calculation are DFT calculation (density functional theory), using B3LYP, conducted with Orca 4.2.

Keywords: MOFs, ZIFs, recycling, closed-loop, cobalt, li-ion batteries

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Authors: Bouhafara Djaber, Menail Younes, Mesrafet Farouk, Aissaoui Mohammed Islem

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This article presents results of experimental investigations of the durability of (GFRP) composite exposed to typical environments of marine industries applications,The use of fiber-glass reinforced polyester composites in marine applications such as Hulls of voyage boats and hulls of small vessels for the military navy , this type of composite is becoming attractive because of their reduced weight and improved corrosion resistance. However,a deep understating of oil ageing effect on composite structures is essential to ensure long-term performance and durability. in this work evaluate the effect of oil ageing on absorptıon behavıor and ımpact properties of glass/polyester composites manufactured with two types of fiber fabrics (fibreglass mat and fiberglass woven roving) and isophthalic polyester resin. The specimens obtained from commercial (GFRP) profiles made of unsaturated polyester resin were subjected to immersion in (i) marine oil for boats and (ii) salt water at ambient temperature for up to 1 month. The effects of such exposure conditions on this types of profile we analysed in what concerns their (i) mass change,(ii) mechanical response in impact, namely on the mechanical response – oil immersion caused a higher level of degradation, compared with salt water immersion;fracture surface examination by scanning electron microscopy revealed delamination, fiber debonding and resin crumbling due to oil effect.

Keywords: Marine Engine Oil, Absorption, Polyester, Glass Fibre

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Authors: P. Mirahmadpour, M. H. Banitaba, D. Nematollahi

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The chemistry of coordination polymers in recent years has grown exponentially not only because of their interesting architectures but also due to their various technical applications in many fields including ion exchange, chemical catalysis, small molecule separations, and drug release. The use of bridging ligands for the controlled self-assembly of one, two or three dimensional metallo-supramolecular species is the subject of serious study in last decade. Numerous different synthetic methods have been offered for the preparation of coordination polymers such as (a) diffusion from the gas phase, (b) slow diffusion of the reactants into a polymeric matrix, (c) evaporation of the solvent at ambient or reduced temperatures, (d) temperature controlled cooling, (e) precipitation or recrystallisation from a mixture of solvents and (f) hydrothermal synthesis. The electrosynthetic process suggested several advantages over conventional approaches. A general advantage of electrochemical synthesis is that it allows synthesis under milder conditions than typical solvothermal or microwave synthesis. In this work we have introduced a simple electrochemical method for growing metal coordination polymers based on copper with a flexible 2,2’-thiodiacetic acid (TDA) and rigid 1,2,4,5-benzenetetracarboxylate (BTC) ligands. The structure of coordination polymers were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), elemental analysis, thermal gravimetric (TG) and differential thermal analyses (DTA). The single-crystal X-ray diffraction analysis revealed that different conformations of the ligands and different coordination modes of the carboxylate group as well as different coordination geometries of the copper atoms. Electrochemical synthesis of coordination polymers has different advantages such as faster synthesis at lower temperature in compare with conventional chemical methods and crystallization of desired materials in a single synthetic step.

Keywords: 1, 2, 4, 5-benzenetetracarboxylate, coordination polymer, copper, 2, 2’-thiodiacetic acid

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Authors: Ravi Sheshala, Annie Lee, Ai Lin Ong, Ling Ling Cheu, Thiagarajan Madheswaran, Thankur R. R. Singh

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The objectives of the present research work were to develop and characterize biodegradable controlled release photo cross-linked implants of Triamcinolone Acetonide (TA) for the treatment of chronic ocular diseases. The photo cross-linked implants were prepared using film casting technique by mixing TA (2.5%) polyethylene glycol diacrylate (PEGDA 700), pore formers (mannitol, maltose, and gelatin) and the photoinitiator (Irgacure 2959). The resulting mixture was injected into moulds using 21 G and subjected to photocrosslinking at 365 nm. Scanning electron microscopy results demonstrated that more pores were formed in the films with the increase in the concentration of pore formers from 2%-10%. The maximum force required to break the films containing 2-10% of pore formers were determined in both dry and wet conditions using texture analyzer and found that films in a dry condition required a higher force to break compared to wet condition and blank films. In vitro drug release from photo cross-linked films were determined by incubating samples in 50 ml PBS pH 7.4 at 37 C and the samples were analyzed for drug release by HPLC. The films demonstrated a biphasic release profile i.e. an initial burst release (<20%) on the first day followed by a constant and continuous drug release in a controlled manner for 42 days. The drug release from all formulations followed the first-order release pattern and the combination of diffusion and erosion release mechanism. In conclusion, the developed formulations were able to provide controlled drug delivery to treat the chronic ocular diseases.

Keywords: controlled release, ophthalmic, PEGDA, photocrosslinking, pore formers

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Authors: A. Katsman, L. Bloch, Y. Etinger, Y. Kauffmann, B. Pokroy

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Various nanosized amorphous alumina thin films in the range of (2.4 - 63.1) nm were deposited onto amorphous carbon and amorphous Si3N4 membrane grids. Transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), X-ray photoelectron spectroscopy (XPS) and differential scanning calorimetry (DSC) techniques were used to probe the size effect on the short range order and the amorphous to crystalline phase transition temperature. It was found that the short-range order changes as a function of size: the fraction of tetrahedral Al sites is greater in thinner amorphous films. This result correlates with the change of amorphous alumina density with the film thickness demonstrated by the reflectivity experiments: the thinner amorphous films have the less density. These effects are discussed in terms of surface reconstruction of the amorphous alumina films. The average atomic binding energy in the thin film layer decreases with decease of the thickness, while the average O-Al interatomic distance increases. The reconstruction of amorphous alumina is induced by the surface reconstruction, and the short range order changes being dependent on the density. Decrease of the surface energy during reconstruction is the driving force of the alumina reconstruction (density change) followed by relaxation process (short range order change). The amorphous to crystalline phase transition temperature measured by DSC rises with the decrease in thickness from 997.6°C for 13.9 nm to 1020.4 °C for 2.7 nm thick. This effect was attributed to the different film densities: formation of nanovoids preceding and accompanying crystallization process influences the crystallization rate, and by these means, the temperature of crystallization peak.

Keywords: amorphous alumina, density, short range order, size effect

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