Search results for: scanning electron microscopy (SEM)

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: 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

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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: Andile Mkhohlakali, Tien-Chien Jen, James Tshilongo, Happy Mabowa

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Among different parameters, oxygen is one of the most important analytes of interest, dissolved oxygen (DO) concentration is very crucial and significant for various areas of physical, chemical, and environmental monitoring. Herein we report oxygen-sensitive luminophores -based lanthanum(III) trifluoromethanesulfonate), [La]³⁺ was encapsulated into SiO₂-based xerogel matrix. The nanosensor is composed of organically modified silica nanoparticles, doped with the luminescent oxygen–sensitive lanthanum(III) trifluoromethanesulfonate complex. The precursor materials used for sensing film were triethyl ethoxy silane (TEOS) and (3-Mercaptopropyltriethoxysilane) (MPTMS- TEOS) used for SiO2-baed matrices. Brunauer–Emmett–Teller (BET), and BJH indicate that the SiO₂ transformed from microporous to mesoporous upon the addition of La³⁺ luminophore with increased surface area (SBET). The typical amorphous SiO₂ based xerogels were revealed with X-Ray diffraction (XRD) and Selected Area Electron Diffraction (SAED) analysis. Scanning electron microscope- (SEM) and transmission electron microscope (TEM) showed the porous morphology and reduced particle for SiO₂ and La-SiO₂ xerogels respectively. The existence of elements, siloxane networks, and thermal stability of xerogel was confirmed by energy dispersive spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), and Thermographic analysis (TGA). UV-Vis spectroscopy and photoluminescence (PL) have been used to characterize the optical properties of xerogels. La-SiO₂ demonstrates promising characteristic features of an active sensing film for dissolved oxygen in the water. Keywords: Sol-gel, ORMOSILs, encapsulation, Luminophores quenching, O₂-sensing

Keywords: sol-gel, ORMOSILs, luminophores quenching, O₂-sensing

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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: Iftikhar Ahmad, Mohammad Islam

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Thermally exfoliated graphene nanomaterial was reinforced into Al2O3 ceramic and the nanocomposites were consolidated using rapid high-frequency induction heat sintering route. The resulting nanocomposites demonstrated higher mechanical properties due to efficient GNS incorporation and chemical interaction with the Al2O3 matrix grains. The enhancement in mechanical properties is attributed to (i) uniformly-dispersed GNS in the consolidated structure (ii) ability of GNS to decorate Al2O3 nanoparticles and (iii) strong GNS/Al2O3 chemical interaction during colloidal mixing and pullout/crack bridging toughening mechanisms during mechanical testing. The GNS/Al2O3 interaction during different processing stages was thoroughly examined by thermal and structural investigation of the interfacial area. The formation of an intermediate aluminum oxycarbide phase (Al2OC) via a confined carbothermal reduction reaction at the GNS/Al2O3 interface was observed using advanced electron microscopes. The GNS surface roughness improves GNS/Al2O3 mechanical locking and chemical compatibility. The sturdy interface phase facilitates efficient load transfer and delayed failure through impediment of crack propagation. The resulting nanocomposites, therefore, offer superior toughness.

Keywords: ceramics, nanocomposites, interfaces, nanostructures, electron microscopy, Al2O3

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Authors: Abdelghani Boucheham, Ahcene Karaali, Amar Manseri

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Nanostructured Titania layers formed on the surface of titanium and titanium alloys by anodic oxidation play an important role in the enhancement of their biocompatibility and osseointegration in the human body. In the current work, highly ordered titania nanotube array films were elaborated on Ti₆Al₄V medical grade alloys in organic electrolyte containing ethylene glycol, 0.2 wt. % NH₄F and 4 vol. % H₂O at an applied potential of 60 V for different durations. The diameters, lengths and wall thicknesses of the obtained nanotubes were characterized by scanning electronic microscopy (SEM).

Keywords: anodization, dental implants, titania nanotubes, titanium alloys, SEM

Procedia PDF Downloads 241

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

Procedia PDF Downloads 182

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: G. Singh, H.Schuster, U. Füssel

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The stability of electric arc and durability of electrode tip used in Tungsten Inert Gas (TIG) welding demand a metallurgical study about the chemical transport mechanism of emitter oxide particles in tungsten electrode during its real welding conditions. The tungsten electrodes doped with emitter oxides of rare earth oxides such as La₂O₃, Th₂O₃, Y₂O₃, CeO₂ and ZrO₂ feature a comparatively lower work function than tungsten and thus have superior emission characteristics due to lesser surface temperature of the cathode. The local change in concentration of these emitter particles in tungsten electrode due to high temperature diffusion (chemical transport) can change its functional properties like electrode temperature, work function, electron emission, and stability of the electrode tip shape. The resulting increment in tip surface temperature results in the electrode material loss. It was also observed that the tungsten recrystallizes to large grains at high temperature. When the shape of grain boundaries are granular in shape, the intergranular diffusion of oxide emitter particles takes more time to reach the electrode surface. In the experimental work, the microstructure of the used electrode's tip surface will be studied by scanning electron microscope and reflective X-ray technique in order to gauge the extent of the diffusion and chemical reaction of emitter particles. Besides, a simulated model is proposed to explain the effect of oxide particles diffusion on the electrode’s microstructure, electron emission characteristics, and electrode tip erosion. This model suggests metallurgical modifications in tungsten electrode to enhance its erosion resistance.

Keywords: rare-earth emitter particles, temperature-dependent diffusion, TIG welding, Tungsten electrode

Procedia PDF Downloads 181

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: 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: F. Motamedi Sedeh, Sh. Chahardoli, H. Mahravani, N. Harzandi, M. Sotoodeh, S. K. Shafaei

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Foot-and-mouth disease virus (FMDV) is the most economically important disease of livestock. The aim of the study is inactivation of FMD virus type O/IRN/2010 by electron beam without antigenic changes as electron radio vaccine. The BALB/C mice were divided into three groups, each group containing five mice. Three groups of mice were inoculated with conventional vaccine and electron beam irradiated vaccine FMDV type O/IRN/2010 subcutaneously three weeks interval, the final group as negative control. The sera were separated from the blood samples of mice 14 days after last vaccination and tested for the presence of antibodies against FMDV type O/IRN/2010 by serum neutralization test. The Serum Neutralization Test (SNT) was carried out and antibody titration was calculated according to the Kraber protocol. The results of the SNT in three groups of mice showed the titration of neutralizing antibody in the vaccinated mice groups; electron radio vaccine and conventional vaccine were significantly higher than negative control group (P<0.05). Therefore, the radio vaccine is a good candidate to immunize animals against FMDV type O/IRN/2010.

Keywords: FMDV type O/IRN/2010, neutralizing antibody response, electron beam, radio vaccine

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Authors: R. Vasireddi, J. Kruse, M. Vakili, M. Trebbin

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Here we present a gas dynamic virtual nozzle (GDVN) based microfluidic jetting devices for spinning of nano/microfibers. The device is fabricated by soft lithography techniques and is based on the principle of a GDVN for precise three-dimensional gas focusing of the spinning solution. The nozzle device is used to produce micro/nanofibers of a perfluorinated terpolymer (THV), which were collected on an aluminum substrate for scanning electron microscopy (SEM) analysis. The influences of air pressure, polymer concentration, flow rate and nozzle geometry on the fiber properties were investigated. It was revealed that surface properties are controlled by air pressure and polymer concentration while the diameter and shape of the fibers are influenced mostly by the concentration of the polymer solution and pressure. Alterations of the nozzle geometry had a negligible effect on the fiber properties, however, the jetting stability was affected. Round and flat fibers with differing surface properties from craters, grooves to smooth surfaces could be fabricated by controlling the above-mentioned parameters. Furthermore, the formation of surface roughness was attributed to the fast evaporation rate and velocity (mis)match between the polymer solution jet and the surrounding air stream. The diameter of the fibers could be tuned from ~250 nm to ~15 µm. Because of the simplicity of the setup, the precise control of the fiber properties, access to biocompatible nanofiber fabrication and the easy scale-up of parallel channels for high throughput, this method offers significant benefits compared to existing solution-based fiber production methods.

Keywords: gas dynamic virtual nozzle (GDVN) principle, microfluidic device, spinning, uniform nanofibers

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Authors: Mihir Hota, Namita Jena, S. N. Sahu

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LEEH (L-cysteine ethyl ester hydrochloride) capped CdS semiconductor nanocrystals are grown at 800C using a simple chemical route. Photoluminescence (PL), Optical absorption (UV) and Transmission Electron Microscopy (TEM) have been carried out to evaluate the structural and optical properties of the nanocrystal. Optical absorption studies have been carried out to optimize the sample. XRD and TEM analysis shows that the nanocrystal belongs to FCC structure having average size of 3nm while a bandgap of 2.84eV is estimated from Photoluminescence analysis. The nanocrystal emits bluish light when excited with 355nm LASER.

Keywords: cadmium sulphide, nanostructures, luminescence, optical properties

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Authors: Urbi Pal, Piyas Palit, Jitendra Mathur, Abhay Chaturvedi, Sandip Bhattacharya

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The hot rolled slab lifting crane cable reel drum (CRD) failed due to failure of cable reel flat spring which are inside the cassette of CRD. CRD is used for the movement of tong cable. Stereoscopic observation revealed beach marks and Scanning Electron Microscopy showed striations confirming fatigue mode of failure. Chemical composition should be spring steel (Cr-Mo-V) as per IS 3431:1982 instead of C-Mn steel. To find out the reason of fatigue failure, the theoretical fatigue life of flat spiral spring has been calculated. The calculation of number of fatigue cycles included bending moment, maximum stress on the spring, ultimate tensile strength and alternative stress. The bending moment determination has been taken account with various parameters like Young’s Modulus, width, thickness, outer diameter, arbor diameter, pay out the length and angular deflection in rotations. With all the required data, the calculated fatigue life turned to be 10000 cycles, but the spring served 15000 cycles which clearly indicated beyond fatigue life usage. Different UTS values have been plotted with respect to the number of fatigue cycles and clearly showed that the increase in UTS by 40% increases fatigue life by 50%. The significance of higher UTS lied here, and higher UTS depends on modified chemistry with proper tempered martensite microstructure. This kind of failure can be easily avoided by changing the crane spring maintenance schedule from 2 years to 1.5 years considering 600 cycles per month. The plant has changed changing the schedule of cable reel spring and procured new flat reel spring made of 50CrV2 steel.

Keywords: cable reel spring, fatigue life, stress, spring steel

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Authors: Muhammad Shahzad Tufail, Iram Liaqat

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Silver nanoparticles (AgNPs) have wider biomedical applications due to their intensive antimicrobial activities. However, toxicity and side effects of nanomaterials like AgNPs is a subject of great controversy towards the further studies in this direction. In this study, biogenically synthesized AgNPs, previously characterized via ultraviolet (UV) visible spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy (FTIR), were subjected to toxicity evaluation using mice model. Albino male mice (BALB/c) were administered with 50 mgkg-1, 100 mgkg-1 and 150 mgkg-1 of AgNPs, respectively, except for control for 30 days. Log-probit regression analysis was used to measure the dosage response to determine the median lethal dose (LD50). Exposure to AgNPs caused significant changes in the levels of serum AST (P ˂ 0.05) at the 100mgkg-1 and 150mgkg-1 of AgNPs exposure, while ALT and serum creatinine (P ˃ 0.05) levels remained normal. Histopathology of male albino mice liver and kidney was studied after 30 days experimental period. Results revealed that mice exposed to heavy dose (150 mgkg-1) of AgNPs showed cell distortion, necrosis and detachment of hepatocytes in the liver. Regarding kidney, at lower concentration, normal renal structure with normal glomeruli was observed. However, at higher concentration (150 mgkg-1), kidneys showed smooth surface and dark red colour with proliferation of podocytes. It can be concluded from present study that biologically synthesized AgNPs are small to be eliminated easily by kidney and therefore the liver and kidney did not show toxicity at low concentrations.

Keywords: silver nanoparticles, pseudomonas aeruginosa, male albino mice, toxicity assessment

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Authors: Young-Min Kang

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M-type Sr-hexaferrites (SrFe12O19) is one of the most utilized materials in permanent magnets due to their low price, outstanding chemical stability, and appropriate hard magnetic properties. For a M-type Sr-hexaferrite with a saturation magnetization (MS) of ~74.0 emu/g the practical limits of remanent flux density (Br) and maximum energy product (BH) max are ~4.6 kG and ~5.3 MGOe. Meanwhile, W-type hexaferrite (SrFe18O27) with higher MS ~81emu/g can be a good candidate for the development of enhanced ferrite magnet. However the W-type hexaferrite is stable at the temperature over 1350 ºC in air, and thus it is hard to control grain size and the coercivity. We report here high-MS M-W composite hexaferrites synthesized at 1250 ºC in air by doping Ca, Co, Mn, and Zn into the hexaferrite structures. The hexaferrites samples of stoichiometric SrFe12O19 (SrM) and Ca-Co-Mn-Zn doped hexaferrite (Sr0.7Ca0.3Fen-0.6Co0.2Mn0.2Zn0.2Oa) were prepared by conventional solid state reaction process with varying Fe content (10 ≤ n ≤ 17). Analysis by x-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) were performed for phase identification and microstructural observation respectively. Magnetic hysteresis curves were measured using vibrating sample magnetometer (VSM) at room temperature (300 K). Single M-type phase could be obtained in the non-doped SrM sample after calcinations at the range of 1200 ºC ~ 1300 ºC, showing MS in the range of 72 ~ 72.6 emu/g. The Ca-Co-Mn-Zn doped SrM with Fe content, 10 ≤ n ≤ 13, showed both M and W-phases peaks in the XRD after respective calcinations at 1250 ºC. The sample with n=13 showed the MS of 70.7, 75.3, 78.0 emu/g, respectively, after calcination at 1200, 1250, 1300 ºC. The high MS over that of non-doped SrM (~72 emu/g) is attributed to the volume portion of W-phase. It is also revealed that the high MS W-phase could not formed if only one of the Ca, Co, Zn is missed in the substitution. These elements are critical to form the W-phase at the calcinations temperature of 1250 ºC, which is 100 ºC lower than the calcinations temperature for non-doped Sr-hexaferrites.

Keywords: M-type hexaferrite, W-type hexaferrite, saturation magnetization, low-temperature synthesis

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Authors: Pooja Mongia Raj, Rakesh Raj, Alpana Ram

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Background: The use of multiparticulate drug delivery systems in preference to single unit dosage forms for colon targeting purposes dates back to 1985 when Hardy and co-workers showed that multiparticulate systems enabled the drug to reach the colon quickly and were retained in the ascending colon for a relatively long period of time. Methods: Site-specific colonic drug delivery system (nanoparticles) of 5-ASA were prepared and coated with pH sensitive polymer. Chitosan nanoparticles (CTNP) bearing 5-Amino salicylic acid (5-ASA) were prepared, by ionotropic gelation method. Nanoparticulate dosage form consisting of a hydrophobic core enteric coated with pH-dependent polymer Eudragit S-100 by solvent evaporation method, for the effective delivery of drug to the colon for treatment of ulcerative colitis. Results: The mean diameter of CTNP and ECTNP formulations were 159 and 661 nm, respectively. Also optimum value of polydispersity index was found to be 0.249 [count rate (kcps) was 251.2] and 0.170 [count rate (kcps) was 173.9] was obtained for both the formulations respectively. Conclusion: CTNP and Eudragit chitosan nanoparticles (ECTNP) was characterized for shape and surface morphology by scanning electron microscopy (SEM) appeared to be spherical in shape. The in vitro drug release was investigated using USP dissolution test apparatus in different simulated GIT fluids showed promising release. In vivo experiments are in further proceeding for fruitful results.

Keywords: colon targeting, nanoparticles, polymer, 5-amino salicylic acid, edragit

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