Search results for: nonlinear ultrasonic resonant spectroscopy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 3741

Search results for: nonlinear ultrasonic resonant spectroscopy

441 Modelling Dengue Disease With Climate Variables Using Geospatial Data For Mekong River Delta Region of Vietnam

Authors: Thi Thanh Nga Pham, Damien Philippon, Alexis Drogoul, Thi Thu Thuy Nguyen, Tien Cong Nguyen

Abstract:

Mekong River Delta region of Vietnam is recognized as one of the most vulnerable to climate change due to flooding and seawater rise and therefore an increased burden of climate change-related diseases. Changes in temperature and precipitation are likely to alter the incidence and distribution of vector-borne diseases such as dengue fever. In this region, the peak of the dengue epidemic period is around July to September during the rainy season. It is believed that climate is an important factor for dengue transmission. This study aims to enhance the capacity of dengue prediction by the relationship of dengue incidences with climate and environmental variables for Mekong River Delta of Vietnam during 2005-2015. Mathematical models for vector-host infectious disease, including larva, mosquito, and human being were used to calculate the impacts of climate to the dengue transmission with incorporating geospatial data for model input. Monthly dengue incidence data were collected at provincial level. Precipitation data were extracted from satellite observations of GSMaP (Global Satellite Mapping of Precipitation), land surface temperature and land cover data were from MODIS. The value of seasonal reproduction number was estimated to evaluate the potential, severity and persistence of dengue infection, while the final infected number was derived to check the outbreak of dengue. The result shows that the dengue infection depends on the seasonal variation of climate variables with the peak during the rainy season and predicted dengue incidence follows well with this dynamic for the whole studied region. However, the highest outbreak of 2007 dengue was not captured by the model reflecting nonlinear dependences of transmission on climate. Other possible effects will be discussed to address the limitation of the model. This suggested the need of considering of both climate variables and another variability across temporal and spatial scales.

Keywords: infectious disease, dengue, geospatial data, climate

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440 Design and Synthesis of Fully Benzoxazine-Based Porous Organic Polymer Through Sonogashira Coupling Reaction for CO₂ Capture and Energy Storage Application

Authors: Mohsin Ejaz, Shiao-Wei Kuo

Abstract:

The growing production and exploitation of fossil fuels have placed human society in serious environmental issues. As a result, it's critical to design efficient and eco-friendly energy production and storage techniques. Porous organic polymers (POPs) are multi-dimensional porous network materials developed through the formation of covalent bonds between different organic building blocks that possess distinct geometries and topologies. POPs have tunable porosities and high surface area making them a good candidate for an effective electrode material in energy storage applications. Herein, we prepared a fully benzoxazine-based porous organic polymers (TPA–DHTP–BZ POP) through sonogashira coupling of dihydroxyterephthalaldehyde (DHPT) and triphenylamine (TPA) containing benzoxazine (BZ) monomers. Firstly, both BZ monomers (TPA-BZ-Br and DHTP-BZ-Ea) were synthesized by three steps, including Schiff base, reduction, and mannich condensation reaction. Finally, the TPA–DHTP–BZ POP was prepared through the sonogashira coupling reaction of brominated monomer (TPA-BZ-Br) and ethynyl monomer (DHTP-BZ-Ea). Fourier transform infrared (FTIR) and solid-state nuclear magnetic resonance (NMR) spectroscopy confirmed the successful synthesis of monomers as well as POP. The porosity of TPA–DHTP–BZ POP was investigated by the N₂ absorption technique and showed a Brunauer–Emmett–Teller (BET) surface area of 196 m² g−¹, pore size 2.13 nm and pore volume of 0.54 cm³ g−¹, respectively. The TPA–DHTP–BZ POP experienced thermal ring-opening polymerization, resulting in poly (TPA–DHTP–BZ) POP having strong inter and intramolecular hydrogen bonds formed by phenolic groups and Mannich bridges, thereby enhancing CO₂ capture and supercapacitive performance. The poly(TPA–DHTP–BZ) POP demonstrated a remarkable CO₂ capture of 3.28 mmol g−¹ and a specific capacitance of 67 F g−¹ at 0.5 A g−¹. Thus, poly(TPA–DHTP–BZ) POP could potentially be used for energy storage and CO₂ capture applications.

Keywords: porous organic polymer, benzoxazine, sonogashira coupling, CO₂, supercapacitor

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439 Simulation Based Analysis of Gear Dynamic Behavior in Presence of Multiple Cracks

Authors: Ahmed Saeed, Sadok Sassi, Mohammad Roshun

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Gears are important components with a vital role in many rotating machines. One of the common gear failure causes is tooth fatigue crack; however, its early detection is still a challenging task. The objective of this study is to develop a numerical model that simulates the effect of teeth cracks on the resulting gears vibrations and permits consequently to perform an early fault detection. In contrast to other published papers, this work incorporates the possibility of multiple simultaneous cracks with different depths. As cracks alter significantly the stiffness of the tooth, finite element software is used to determine the stiffness variation with respect to the angular position, for different combinations of crack orientation and depth. A simplified six degrees of freedom nonlinear lumped parameter model of a one-stage spur gear system is proposed to study the vibration with and without cracks. The model developed for calculating the stiffness with the crack permitted to update the physical parameters of the second-degree-of-freedom equations of motions describing the vibration of the gearbox. The vibration simulation results of the gearbox were by obtained using Simulink/Matlab. The effect of one crack with different levels was studied thoroughly. The change in the mesh stiffness and the vibration response were found to be consistent with previously published works. In addition, various statistical time domain parameters were considered. They showed different degrees of sensitivity toward the crack depth. Multiple cracks were also introduced at different locations and the vibration response along with the statistical parameters were obtained again for a general case of degradation (increase in crack depth, crack number and crack locations). It was found that although some parameters increase in value as the deterioration level increases, they show almost no change or even decrease when the number of cracks increases. Therefore, the use of any statistical parameters could be misleading if not considered in an appropriate way.

Keywords: Spur gear, cracked tooth, numerical simulation, time-domain parameters

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438 Formulation of Hybrid Nanopowder-Molecular Ink for Fabricating Critical Material-Free Cu₂ZnSnS₄ Thin Film Solar Absorber

Authors: Anies Mutiari, Neha Bansal, Martin Artner, Veronika Mayer, Juergen Roth, Mathias Weil, Rachmat Adhi Wibowo

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Cu₂ZnSnS₄ (CZTS) compound (mineral name kesterite) has attracted considerable interests for photovoltaic application owing to its optoelectrical properties. Moreover, its elemental abundance in Earth’s crust offers a comparative advantage for envisaged large-scale photovoltaic deployment without any material shortage issues. In this contribution, we present an innovative route to prepare CZTS solar absorber layer for photovoltaic application from low-cost and up-scalable process. CZTS layers were spin coated on the Molybdenum-coated glass from two inks composed of different solvents; dimethylsulfoxide (DMSO) and ultrapure water. Into each solvent; 0.57M CuCl₂, 0.39M ZnCl₂, 0.53M SnCl₂, and 1.85M Thiourea or Na₂S₂O₃, as well as pre-synthesized CZTS nanopowder, were added as sources of Cu, Zn, Sn and S in the ink. The crystallisation of ink into CZTS dense layers was carried out by firstly annealing the as-deposited CZTS layer in open air at 300°C for 1 minute, followed by sulfurisation at 560–620°C under atmospheric pressure for 120 minutes. Complementary electron microscopy, grazing incidence X-ray diffraction and Raman spectroscopy investigations suggest that both solvents can be used for preparing high quality and device relevant CZTS solar absorber layers. The sulphurisation crystallizes the as-deposited CZTS into highly polycrystalline CZTS layer with tetragonal structure demonstrated by the presence of tetrahedrally-shaped grains with the size of 1 µm. An advancement of the CZTS layer preparation was made by gradual substitution of volatile organic compound solvent of DMSO with ultrapure water. It is revealed that by using similar air annealing and sulphurisation process, dense and compact CZTS layers can also be fabricated from an ink with reduced volatile organic compound content.

Keywords: kesterite, solar ink, spin coating, photovoltaics

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437 Effect of Polymer Molecular Structures on Properties of Dental Cement Restoratives

Authors: Dong Xie, Jun Zhao, Yiming Weng

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One of the challenges in dental cement biomaterials is how to make a restorative with mechanical strengths and wear resistance that are comparable to contemporary dental resin composites. Currently none of the dental cement restoratives has been used in high stress-bearing sites due to their low mechanical strengths and poor wear-resistance. The objective of this study was to synthesize and characterize the poly(alkenoic acid)s with different molecular structures, use these polymers to formulate a dental cement restorative, and study the effect of molecular structures on reaction kinetics, viscosity, and mechanical strengths of the formed polymers and cement restoratives. In this study, poly(alkenoic acid)s with different molecular structures were synthesized. The purified polymers were formulated with commercial Fuji II LC glass fillers to form the experimental cement restoratives. The reaction kinetics was studied via 1HNMR spectroscopy. The formed restoratives were evaluated using compressive strength, diametral tensile strength, flexural strength, hardness and wear-resistance tests. Specimens were conditioned in distilled water at 37 oC for 24 h prior to testing. Fuji II LC restorative was used as control. The results show that the higher the arm number and initiator concentration, the faster the reaction was. It was also found that the higher the arm number and branching that the polymer had, the lower the viscosity of the polymer in water and the lower the mechanical strengths of the formed restorative. The experimental restoratives were 31-53% in compressive strength, 37-55% in compressive modulus, 80-126% in diametral tensile strength, 76-94% in flexural strength, 4-21% in fracture toughness and 53-96% in hardness higher than Fuji II LC. For wear test, the experimental restoratives were only 5.4-13% of abrasive and 6.4-12% of attritional wear depths of Fuji II LC in each wear cycle. The aging study also showed that all the experimental restoratives increased their strength continuously during 30 days, unlike Fuji II LC. It is concluded that polymer molecular structures have significant and positive impact on mechanical properties of dental cement restoratives.

Keywords: dental materials, polymers, strength, biomaterials

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436 Designing Nickel Coated Activated Carbon (Ni/AC) Based Electrode Material for Supercapacitor Applications

Authors: Zahid Ali Ghazi

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Supercapacitors (SCs) have emerged as auspicious energy storage devices because of their fast charge-discharge characteristics and high power densities. In the current study, a simple approach is used to coat activated carbon (AC) with a thin layer of nickel (Ni) by an electroless deposition process to enhance the electrochemical performance of the SC. The synergistic combination of large surface area and high electrical conductivity of the AC, as well as the pseudocapacitive behavior of the metallic Ni, has shown great potential to overcome the limitations of traditional SC materials. First, the materials were characterized using X-ray diffraction (XRD) for crystallography, scanning electron microscopy (SEM) for surface morphology and energy dispersion X-ray (EDX) for elemental analysis. The electrochemical performance of the nickel-coated activated carbon (Ni-AC) is systematically evaluated through various techniques, including galvanostatic charge-discharge (GCD), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The GCD results revealed that Ni/AC has a higher specific capacitance (1559 F/g) than bare AC (222 F/g) at 1 A/g current density in a 2 M KOH electrolyte. Even at a higher current density of 20 A/g, the Ni/AC showed a high capacitance of 944 F/g as compared to 77 F/g by AC. The specific capacitance (1318 F/g) calculated from CV measurements for Ni-AC at 10mV/sec was in close agreement with GCD data. Furthermore, the bare AC exhibited a low energy of 15 Wh/kg at a power density of 356 W/kg whereas, an energy density of 111 Wh/kg at a power density of 360 W/kg was achieved by Ni/AC-850 electrode and demonstrated a long life cycle with 94% capacitance retention over 50000 charge/discharge cycles at 10 A/g. In addition, the EIS study disclosed that the Rs and Rct values of Ni/AC electrodes were much lower than those of bare AC. The superior performance of Ni/AC is mainly attributed to the presence of excessive redox active sites, large electroactive surface area and corrosive resistance properties of Ni. We believe that this study will provide new insights into the controlled coating of ACs and other porous materials with metals for developing high-performance SCs and other energy storage devices.

Keywords: supercapacitor, cyclic voltammetry, coating, energy density, activated carbon

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435 Microstructure of Virgin and Aged Asphalts by Small-Angle X-Ray Scattering

Authors: Dong Tang, Yongli Zhao

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The study of the microstructure of asphalt is of great importance for the analysis of its macroscopic properties. However, the peculiarities of the chemical composition of the asphalt itself and the limitations of existing direct imaging techniques have caused researchers to face many obstacles in studying the microstructure of asphalt. The advantage of small-angle X-ray scattering (SAXS) is that it allows quantitative determination of the internal structure of opaque materials and is suitable for analyzing the microstructure of materials. Therefore, the SAXS technique was used to study the evolution of microstructures on the nanoscale during asphalt aging. And the reasons for the change in scattering contrast during asphalt aging were also explained with the help of Fourier transform infrared spectroscopy (FTIR). SAXS experimental results show that the SAXS curves of asphalt are similar to the scattering curves of scattering objects with two-level structures. The Porod curve for asphalt shows that there is no obvious interface between the micelles and the surrounding mediums, and there is only a fluctuation of the hot electron density between the two. The Beaucage model fit SAXS patterns shows that the scattering coefficient P of the asphaltene clusters as well as the size of the micelles, gradually increase with the aging of the asphalt. Furthermore, aggregation exists between the micelles of asphalt and becomes more pronounced with increasing aging. During asphalt aging, the electron density difference between the micelles and the surrounding mediums gradually increases, leading to an increase in the scattering contrast of the asphalt. Under long-term aging conditions due to the gradual transition from maltenes to asphaltenes, the electron density difference between the micelles and the surrounding mediums decreases, resulting in a decrease in the scattering contrast of asphalt SAXS. Finally, this paper correlates the macroscopic properties of asphalt with microstructural parameters, and the results show that the high-temperature rutting resistance of asphalt is enhanced and the low-temperature cracking resistance decreases due to the aggregation of micelles and the generation of new micelles. These results are useful for understanding the relationship between changes in microstructure and changes in properties during asphalt aging and provide theoretical guidance for the regeneration of aged asphalt.

Keywords: asphalt, Beaucage model, microstructure, SAXS

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434 Analogy in Microclimatic Parameters, Chemometric and Phytonutrient Profiles of Cultivated and Wild Ecotypes of Origanum vulgare L., across Kashmir Himalaya

Authors: Sumira Jan, Javid Iqbal Mir, Desh Beer Singh, Anil Sharma, Shafia Zaffar Faktoo

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Background and Aims: Climatic and edaphic factors immensely influence crop quality and proper development. Regardless of economic potential, Himalayan Oregano has not subjected to phytonutrient and chemometric evaluation and its relationship with environmental conditions are scarce. The central objective of this research was to investigate microclimatic variation among wild and cultivated populations located in a microclimatic gradient in north-western Himalaya, Kashmir and analyse if such disparity was related with diverse climatic and edaphic conditions. Methods: Micrometeorological, Atomic absorption spectroscopy for micro elemental analysis was carried for soil. HPLC was carried out to estimate variation in phytonutrients and phytochemicals. Results: Geographic variation in phytonutrient was observed among cultivated and wild populations and among populations diverse within regions. Cultivated populations exhibited comparatively lesser phytonutrient value than wild populations. Moreover, our results observed higher vegetative growth of O. vulgare L. with higher pH (6-7), elevated organic carbon (2.42%), high nitrogen (97.41Kg/ha) and manganese (10-12ppm) and zinc contents (0.39-0.50) produce higher phytonutrients. HPLC data of phytonutrients like quercetin, betacarotene, ascorbic acid, arbutin and catechin revealed direct relationship with UV-B flux (r2=0.82), potassium (r2=0.97) displaying parallel relationship with phytonutrient value. Conclusions: Catechin was found as predominant phytonutrient among all populations with maximum accumulation of 163.8 ppm while as quercetin exhibited lesser value. Maximum arbutin (53.42ppm) and quercetin (2.87ppm) accumulated in plants thriving under intense and high UV-B flux. Minimum variation was demonstrated by beta carotene and ascorbic acid.

Keywords: phytonutrient, ascorbic acid, beta carotene, quercetin, catechin

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433 Tri/Tetra-Block Copolymeric Nanocarriers as a Potential Ocular Delivery System of Lornoxicam: Experimental Design-Based Preparation, in-vitro Characterization and in-vivo Estimation of Transcorneal Permeation

Authors: Alaa Hamed Salama, Rehab Nabil Shamma

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Introduction: Polymeric micelles that can deliver drug to intended sites of the eye have attracted much scientific attention recently. The aim of this study was to review the aqueous-based formulation of drug-loaded polymeric micelles that hold significant promise for ophthalmic drug delivery. This study investigated the synergistic performance of mixed polymeric micelles made of linear and branched poly (ethylene oxide)-poly (propylene oxide) for the more effective encapsulation of Lornoxicam (LX) as a hydrophobic model drug. Methods: The co-micellization process of 10% binary systems combining different weight ratios of the highly hydrophilic poloxamers; Synperonic® PE/P84, and Synperonic® PE/F127 and the hydrophobic poloxamine counterpart (Tetronic® T701) was investigated by means of photon correlation spectroscopy and cloud point. The drug-loaded micelles were tested for their solubilizing capacity towards LX. Results: Results showed a sharp solubility increase from 0.46 mg/ml up to more than 4.34 mg/ml, representing about 136-fold increase. Optimized formulation was selected to achieve maximum drug solubilizing power and clarity with lowest possible particle size. The optimized formulation was characterized by 1HNMR analysis which revealed complete encapsulation of the drug within the micelles. Further investigations by histopathological and confocal laser studies revealed the non-irritant nature and good corneal penetrating power of the proposed nano-formulation. Conclusion: LX-loaded polymeric nanomicellar formulation was fabricated allowing easy application of the drug in the form of clear eye drops that do not cause blurred vision or discomfort, thus achieving high patient compliance.

Keywords: confocal laser scanning microscopy, Histopathological studies, Lornoxicam, micellar solubilization

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432 Degradation of Emerging Pharmaceuticals by Gamma Irradiation Process

Authors: W. Jahouach-Rabai, J. Aribi, Z. Azzouz-Berriche, R. Lahsni, F. Hosni

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Gamma irradiation applied in removing pharmaceutical contaminants from wastewater is an effective advanced oxidation process (AOP), considered as an alternative to conventional water treatment technologies. In this purpose, the degradation efficiency of several detected contaminants under gamma irradiation was evaluated. In fact, radiolysis of organic pollutants in aqueous solutions produces powerful reactive species, essentially hydroxyl radical ( ·OH), able to destroy recalcitrant pollutants in water. Pharmaceuticals considered in this study are aqueous solutions of paracetamol, ibuprofen, and diclofenac at different concentrations 0.1-1 mmol/L, which were treated with irradiation doses from 3 to 15 kGy. The catalytic oxidation of these compounds by gamma irradiation was investigated using hydrogen peroxide (H₂O₂) as a convenient oxidant. Optimization of the main parameters influencing irradiation process, namely irradiation doses, initial concentration and oxidant volume (H₂O₂) were investigated, in the aim to release high degradation efficiency of considered pharmaceuticals. Significant modifications attributed to these parameters appeared in the variation of degradation efficiency, chemical oxygen demand removal (COD) and concentration of radio-induced radicals, confirming them synergistic effect to attempt total mineralization. Pseudo-first-order reaction kinetics could be used to depict the degradation process of these compounds. A sophisticated analytical study was released to quantify the detected radio-induced radicals (electron paramagnetic resonance spectroscopy (EPR) and high performance liquid chromatography (HPLC)). All results showed that this process is effective for the degradation of many pharmaceutical products in aqueous solutions due to strong oxidative properties of generated radicals mainly hydroxyl radical. Furthermore, the addition of an optimal amount of H₂O₂ was efficient to improve the oxidative degradation and contribute to the high performance of this process at very low doses (0.5 and 1 kGy).

Keywords: AOP, COD, hydroxyl radical, EPR, gamma irradiation, HPLC, pharmaceuticals

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431 Polypyrrole Integrated MnCo2O4 Nanorods Hybrid as Electrode Material for High Performance Supercapacitor

Authors: Santimoy Khilari, Debabrata Pradhan

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Ever−increasing energy demand and growing energy crisis along with environmental issues emphasize the research on sustainable energy conversion and storage systems. Recently, supercapacitors or electrochemical capacitors emerge as a promising energy storage technology for future generation. The activity of supercapacitors generally depends on the efficiency of its electrode materials. So, the development of cost−effective efficient electrode materials for supercapacitors is one of the challenges to the scientific community. Transition metal oxides with spinel crystal structure receive much attention for different electrochemical applications in energy storage/conversion devices because of their improved performance as compared to simple oxides. In the present study, we have synthesized polypyrrole (PPy) supported manganese cobaltite nanorods (MnCo2O4 NRs) hybrid electrode material for supercapacitor application. The MnCo2O4 NRs were synthesized by a simple hydrothermal and calcination approach. The MnCo2O4 NRs/PPy hybrid was prepared by in situ impregnation of MnCo2O4 NRs during polymerization of pyrrole. The surface morphology and microstructure of as−synthesized samples was characterized by scanning electron microscopy and transmission electron microscopy, respectively. The crystallographic phase of MnCo2O4 NRs, PPy and hybrid was determined by X-ray diffraction. Electrochemical charge storage activity of MnCo2O4 NRs, PPy and MnCo2O4 NRs/PPy hybrid was evaluated from cyclic voltammetry, chronopotentiometry and electrochemical impedance spectroscopy. Significant improvement of specific capacitance was achieved in MnCo2O4 NRs/PPy hybrid as compared to the individual components. Furthermore, the mechanically mixed MnCo2O4 NRs, and PPy shows lower specific capacitance as compared to MnCo2O4 NRs/PPy hybrid suggesting the importance of in situ hybrid preparation. The stability of as prepared electrode materials was tested by cyclic charge-discharge measurement for 1000 cycles. Maximum 94% capacitance was retained with MnCo2O4 NRs/PPy hybrid electrode. This study suggests that MnCo2O4 NRs/PPy hybrid can be used as a low cost electrode material for charge storage in supercapacitors.

Keywords: supercapacitors, nanorods, spinel, MnCo2O4, polypyrrole

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430 A Radioprotective Effect of Nanoceria (CNPs), Magnetic Flower-Like Iron Oxide Microparticles (FIOMPs), and Vitamins C and E on Irradiated BSA Protein

Authors: Hajar Zarei, AliAkbar Zarenejadatashgah, Vuk Uskoković, Hiroshi Watabe

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The reactive oxygen species (ROS) generated by radiation in nuclear diagnostic imaging and radiotherapy could damage the structure of the proteins in noncancerous cells surrounding the tumor. The critical factor in many age-related diseases, such as Alzheimer, Parkinson, or Huntington diseases, is the oxidation of proteins by the ROS as molecular triggers of the given pathologies. Our studies by spectroscopic experiments showed doses close to therapeutic ones (1 to 5 Gy) could lead to changes of secondary and tertiary structures in BSA protein macromolecule as a protein model as well as the aggregation of polypeptide chain but without the fragmentation. For this reason, we investigated the radioprotective effects of natural (vitamin C and E) and synthetic materials (CNPs and FIOMPs) on the structural changes in BSA protein induced by gamma irradiation at a therapeutic dose (3Gy). In the presence of both vitamins and synthetic materials, the spectroscopic studies revealed that irradiated BSA was protected from the structural changes caused by ROS, according to in vitro research. The radioprotective property of CNPs and FIOMPs arises from enzyme mimetic activities (catalase, superoxide dismutase, and peroxidase) and their antioxidant capability against hydroxyl radicals. In the case of FIOMPs, a porous structure also leads to increased ROS recombination with each other in the same radiolytic track and subsequently decreased encounters with BSA. The hydrophilicity of vitamin C resulted in the major scavenging of ROS in the solvent, whereas hydrophobic vitamin E localized on the nonpolar patches of the BSA surface, where it did not only neutralize them thanks to the moderate BSA binding constant but also formed a barrier for diffusing ROS. To the best of our knowledge, there has been a persistent lack of studies investigating the radioactive effect of mentioned materials on proteins. Therefore, the results of our studies can open a new widow for application of these common dietary ingredients and new synthetic NPs in improving the safety of radiotherapy.

Keywords: reactive oxygen species, spectroscopy, bovine serum albumin, gamma radiation, radioprotection

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429 Selective Guest Accommodation in Zn(II) Bimetallic: Organic Coordination Frameworks

Authors: Bukunola K. Oguntade, Gareth M. Watkins

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The synthesis and characterization of metal-organic frameworks (MOFs) is an area of coordination chemistry which has grown rapidly in recent years. Worldwide there has been growing concerns about future energy supplies, and its environmental impacts. A good number of MOFs have been tested for the adsorption of small molecules in the vapour phase. An important issue for potential applications of MOFs for gas adsorption and storage materials is the stability of their structure upon sorption. Therefore, study on the thermal stability of MOFs upon adsorption is important. The incorporation of two or more transition metals in a coordination polymer is a current challenge for designed synthesis. This work focused on the synthesis, characterization and small molecule adsorption properties of three microporous (one zinc monometal and two bimetallics) complexes involving Cu(II), Zn(II) and 1,2,4,5-benzenetetracarboxylic acid using the ambient precipitation and solvothermal method. The complexes were characterized by elemental analysis, Infrared spectroscopy, Scanning Electron microscopy, Thermogravimetry analysis and X-ray Powder diffraction. The N2-adsorption Isotherm showed the complexes to be of TYPE III in reference to IUPAC classification, with very small pores only capable for small molecule sorption. All the synthesized compounds were observed to contain water as guest. Investigations of their inclusion properties for small molecules in the vapour phase showed water and methanol as the only possible inclusion candidates with 10.25H2O in the monometal complex [Zn4(H2B4C)2.5(OH)3(H2O)]·10H2O but not reusable after a complete structural collapse. The ambient precipitation bimetallic; [(CuZnB4C(H2O)2]·5H2O, was found to be reusable and recoverable from structure collapse after adsorption of 5.75H2O. In addition, Solvo-[CuZnB4C(H2O)2.5]·2H2O obtained from solvothermal method show two cycles of rehydration with 1.75H2O and 0.75MeOH inclusion while structure remains unaltered upon dehydration and adsorption.

Keywords: adsorption, characterization, copper, metal -organic frameworks, zinc

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428 Poly(L-Lactic Acid) Scaffolds for Bone Tissue Engineering

Authors: Aleksandra BužArovska, Gordana Bogoeva Gaceva

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Biodegradable polymers have received significant scientific attention in tissue engineering (TE) application, in particular their composites consisting of inorganic nanoparticles. In the last 15 years, they are subject of intensive research by many groups, aiming to develop polymer scaffolds with defined biodegradability, porosity and adequate mechanical stability. The most important characteristic making these materials attractive for TE is their biodegradability, a process that could be time controlled and long enough to enable generation of a new tissue as a replacement for the degraded polymer scaffold. In this work poly(L-lactic acid) scaffolds, filled with TiO2 nanoparticles functionalized with oleic acid, have been prepared by thermally induced phase separation method (TIPS). The functionalization of TiO2 nanoparticles with oleic acid was performed in order to improve the nanoparticles dispersibility within the polymer matrix and at the same time to inhibit the cytotoxicity of the nanofiller. The oleic acid was chosen as amphiphilic molecule belonging to the fatty acid family because of its non-toxicity and possibility for mediation between the hydrophilic TiO2 nanoparticles and hydrophobic PLA matrix. The produced scaffolds were characterized with thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and mechanical compression measurements. The bioactivity for bone tissue engineering application was tested in supersaturated simulated body fluid. The degradation process was followed by Fourier transform infrared spectroscopy (FTIR). The results showed anisotropic morphology with elongated open pores (100 µm), high porosity (around 92%) and perfectly dispersed nanofiller. The compression moduli up to 10 MPa were identified independent on the nanofiller content. Functionalized TiO2 nanoparticles induced formation of hydroxyapatite clusters as much as unfunctionalized TiO2. The prepared scaffolds showed properties ideal for scaffold vascularization, cell attachment, growth and proliferation.

Keywords: biodegradation, bone tissue engineering, mineralization, PLA scaffolds

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427 Enzyme Involvement in the Biosynthesis of Selenium Nanoparticles by Geobacillus wiegelii Strain GWE1 Isolated from a Drying Oven

Authors: Daniela N. Correa-Llantén, Sebastián A. Muñoz-Ibacache, Mathilde Maire, Jenny M. Blamey

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The biosynthesis of nanoparticles by microorganisms, on the contrary to chemical synthesis, is an environmentally-friendly process which has low energy requirements. In this investigation, we used the microorganism Geobacillus wiegelii, strain GWE1, an aerobic thermophile belonging to genus Geobacillus, isolated from a drying oven. This microorganism has the ability to reduce selenite evidenced by the change of color from colorless to red in the culture. Elemental analysis and composition of the particles were verified using transmission electron microscopy and energy-dispersive X-ray analysis. The nanoparticles have a defined spherical shape and a selenium elemental state. Previous experiments showed that the presence of the whole microorganism for the reduction of selenite was not necessary. The results strongly suggested that an intracellular NADPH/NADH-dependent reductase mediates selenium nanoparticles synthesis under aerobic conditions. The enzyme was purified and identified by mass spectroscopy MALDI-TOF TOF technique. The enzyme is a 1-pyrroline-5-carboxylate dehydrogenase. Histograms of nanoparticles sizes were obtained. Size distribution ranged from 40-160 nm, where 70% of nanoparticles have less than 100 nm in size. Spectroscopic analysis showed that the nanoparticles are composed of elemental selenium. To analyse the effect of pH in size and morphology of nanoparticles, the synthesis of them was carried out at different pHs (4.0, 5.0, 6.0, 7.0, 8.0). For thermostability studies samples were incubated at different temperatures (60, 80 and 100 ºC) for 1 h and 3 h. The size of all nanoparticles was less than 100 nm at pH 4.0; over 50% of nanoparticles have less than 100 nm at pH 5.0; at pH 6.0 and 8.0 over 90% of nanoparticles have less than 100 nm in size. At neutral pH (7.0) nanoparticles reach a size around 120 nm and only 20% of them were less than 100 nm. When looking at temperature effect, nanoparticles did not show a significant difference in size when they were incubated between 0 and 3 h at 60 ºC. Meanwhile at 80 °C the nanoparticles suspension lost its homogeneity. A change in size was observed from 0 h of incubation at 80ºC, observing a size range between 40-160 nm, with 20% of them over 100 nm. Meanwhile after 3 h of incubation at size range changed to 60-180 nm with 50% of them over 100 nm. At 100 °C the nanoparticles aggregate forming nanorod structures. In conclusion, these results indicate that is possible to modulate size and shape of biologically synthesized nanoparticles by modulating pH and temperature.

Keywords: genus Geobacillus, NADPH/NADH-dependent reductase, selenium nanoparticles, biosynthesis

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426 Redox-Mediated Supramolecular Radical Gel

Authors: Sonam Chorol, Sharvan Kumar, Pritam Mukhopadhyay

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In biology, supramolecular systems require the use of chemical fuels to stay in sustained nonequilibrium steady states termed dissipative self-assembly in contrast to synthetic self-assembly. Biomimicking these natural dynamic systems, some studies have demonstrated artificial self-assembly under nonequilibrium utilizing various forms of energies (fuel) such as chemical, redox, and pH. Naphthalene diimides (NDIs) are well-known organic molecules in supramolecular architectures with high electron affinity and have applications in controlled electron transfer (ET) reactions, etc. Herein, we report the endergonic ET from tetraphenylborate to highly electron-deficient phosphonium NDI²+ dication to generate NDI•+ radical. The formation of radicals was confirmed by UV-Vis-NIR absorption spectroscopy. Electron-donor and electron-acceptor energy levels were calculated from experimental electrochemistry and theoretical DFT analysis. The HOMO of the electron donor locates below the LUMO of the electro-acceptor. This indicates that electron transfer is endergonic (ΔE°ET = negative). The endergonic ET from NaBPh₄ to NDI²+ dication was achieved thermodynamically by the formation of coupled biphenyl product confirmed by GC-MS analysis. NDI molecule bearing octyl phosphonium at the core and H-bond forming imide moieties at the axial position forms a gel. The rheological properties of purified radical ion NDI⦁+ gels were evaluated. The atomic force microscopy studies reveal the formation of large branching-type networks with a maximum height of 70-80 nm. The endergonic ET from NaBPh₄ to NDI²+ dication was used to design the assembly and disassembly redox reaction cycle using reducing (NaBPh₄) and oxidizing agents (Br₂) as chemical fuels. A part of NaBPh₄ is used to drive assembly, while a fraction of the NaBPh₄ is dissipated by forming a useful product. The system goes back to the disassembled NDI²+ dication state with the addition of Br₂. We think bioinspired dissipative self-assembly is the best approach to developing future lifelike materials with autonomous behavior.

Keywords: Ionic-gel, redox-cycle, self-assembly, useful product

Procedia PDF Downloads 84
425 Synthesis of Silver Nanoparticles Adsorbent from Phytolacca Dodecandra ‘Endod’ Leaf to Water Treatment, at Almeda Textile Factory, Tigray Ethiopia

Authors: Letemariam Gebreslassie Gebrekidan

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Water pollution is one of the most feared problems in modern societies, especially in developing countries like Ethiopia. Nanoparticles with controlled size and composition are of fundamental and technological interest as they provide solutions to technological and environmental challenges in the areas of solar energy conversion, catalysis, medicine, and water treatment. The synthesis of metallic nanoparticles is an active area of academic and, more importantly, application research in nanotechnology. Adsorption is a process in which pollutants are absorbed on a solid surface. A molecule (pollutant) adhered to the solid surface is called an adsorbate, and the solid surface is an adsorbent. Adsorption is controlled by various parameters such as temperature, the nature of the adsorbate and adsorbent, and the presence of other pollutants along with the experimental conditions (pH, concentration of pollutants, contact time, particle size, and temperature). Depending on the main problem of water pollution, this research is available on the adsorption of wastewater using silver nanoparticles extracted from phytolacca Dodecandra leaf. AgNP was synthesized from a 1mM aqueous solution of silver nitrate (AgNO3) and Phytolacca Dodecandra leaf extract at room temperature. The synthesized nanoparticles were characterized using UV/visible Spectrometer, FTIR and XRD. In the UV-Vis spectrum, The Surface Plasmon resonance (SPR) peak was observed at 414 nm, which confirmed the synthesis of AgNPs. FTIR spectroscopy, recorded from 4000 cm-1 to 400 cm-1, indicated the presence of a capping agent with the nanoparticles. From the XRD results, the average crystalline size was estimated to be 20 nm Confirming the nanoparticle nature of the obtained sample. Thus, the present method leads to the formation of silver nanoparticles with well-defined dimensions. The effects of different parameters like solution pH, adsorbent dose, contact time and initial concentration of dye were studied. The concentration of MB is 0.01 mg/L and 0.002 mg/L before and after adsorption, respectively. The wastewater containing MB was well purified using AgNP adsorbent.

Keywords: wastewater, silver nanoparticle, Characterization, adsorption, parameter

Procedia PDF Downloads 16
424 Parameter Estimation of Gumbel Distribution with Maximum-Likelihood Based on Broyden Fletcher Goldfarb Shanno Quasi-Newton

Authors: Dewi Retno Sari Saputro, Purnami Widyaningsih, Hendrika Handayani

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Extreme data on an observation can occur due to unusual circumstances in the observation. The data can provide important information that can’t be provided by other data so that its existence needs to be further investigated. The method for obtaining extreme data is one of them using maxima block method. The distribution of extreme data sets taken with the maxima block method is called the distribution of extreme values. Distribution of extreme values is Gumbel distribution with two parameters. The parameter estimation of Gumbel distribution with maximum likelihood method (ML) is difficult to determine its exact value so that it is necessary to solve the approach. The purpose of this study was to determine the parameter estimation of Gumbel distribution with quasi-Newton BFGS method. The quasi-Newton BFGS method is a numerical method used for nonlinear function optimization without constraint so that the method can be used for parameter estimation from Gumbel distribution whose distribution function is in the form of exponential doubel function. The quasi-New BFGS method is a development of the Newton method. The Newton method uses the second derivative to calculate the parameter value changes on each iteration. Newton's method is then modified with the addition of a step length to provide a guarantee of convergence when the second derivative requires complex calculations. In the quasi-Newton BFGS method, Newton's method is modified by updating both derivatives on each iteration. The parameter estimation of the Gumbel distribution by a numerical approach using the quasi-Newton BFGS method is done by calculating the parameter values that make the distribution function maximum. In this method, we need gradient vector and hessian matrix. This research is a theory research and application by studying several journals and textbooks. The results of this study obtained the quasi-Newton BFGS algorithm and estimation of Gumbel distribution parameters. The estimation method is then applied to daily rainfall data in Purworejo District to estimate the distribution parameters. This indicates that the high rainfall that occurred in Purworejo District decreased its intensity and the range of rainfall that occurred decreased.

Keywords: parameter estimation, Gumbel distribution, maximum likelihood, broyden fletcher goldfarb shanno (BFGS)quasi newton

Procedia PDF Downloads 324
423 Heavy Sulphide Material Characterization of Grasberg Block Cave Mine, Mimika, Papua: Implication for Tunnel Development and Mill Issue

Authors: Cahya Wimar Wicaksono, Reynara Davin Chen, Alvian Kristianto Santoso

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Grasberg Cu-Au ore deposit as one of the biggest porphyry deposits located in Papua Province, Indonesia produced by several intrusion that restricted by Heavy Sulphide Zone (HSZ) in peripheral. HSZ is the rock that becomes the contact between Grassberg Igneous Complex (GIC) with sedimentary and igneous rock outside, which is rich in sulphide minerals such as pyrite ± pyrrhotite. This research is to obtain the characteristic of HSZ based on geotechnical, geochemical and mineralogy aspect and those implication for daily mining operational activities. Method used in this research are geological and alteration mapping, core logging, FAA (Fire Assay Analysis), AAS (Atomic absorption spectroscopy), RQD (Rock Quality Designation) and rock water content. Data generated from methods among RQD data, mineral composition and grade, lithological and structural geology distribution in research area. The mapping data show that HSZ material characteristics divided into three type based on rocks association, there are near igneous rocks, sedimentary rocks and on HSZ area. And also divided based on its location, north and south part of research area. HSZ material characteristic consist of rock which rich of pyrite ± pyrrhotite, and RQD range valued about 25%-100%. Pyrite ± pyrrhotite which outcropped will react with H₂O and O₂ resulting acid that generates corrosive effect on steel wire and rockbolt. Whereas, pyrite precipitation proses in HSZ forming combustible H₂S gas which is harmful during blasting activities. Furthermore, the impact of H₂S gas in blasting activities is forming poison gas SO₂. Although HSZ high grade Cu-Au, however those high grade Cu-Au rich in sulphide components which is affected in flotation milling process. Pyrite ± pyrrhotite in HSZ will chemically react with Cu-Au that will settle in milling process instead of floating.

Keywords: combustible, corrosive, heavy sulphide zone, pyrite ± pyrrhotite

Procedia PDF Downloads 326
422 Evolutions of Structural Properties of Native Phospho Casein (NPC) Powder during Storage

Authors: Sarah Nasser, Anne Moreau, Alain Hedoux, Romain Jeantet, Guillaume Delaplace

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Background: Spray dryed powders containing some caseins are commonly produced in dairy industry. It is widely admitted that the structure of casein evolves during powder storage, inducing a loss of solubility. However few studies evaluate accurately the destabilization mechanisms at molecular and mesoscopic level, in particular for Native Phospho Casein powder (NPC). Consequently, at the state of the art, it is very difficult to assess which secondary structure change or crosslinks initiate insolubility during storage. To address this issue, controlled ageing conditions have been applied to a NPC powder (which was obtained by spray drying a concentrate containing a higher content of casein (90%), whey protein (8%) and lactose (few %)). Evolution of structure and loss of solubility, with the effects of temperature and time of storage were systematically reported. Methods: FTIR spectroscopy, Raman and Circular Dichroism were used to monitor changes of secondary structure in dry powder and in solution after rehydration. Besides, proteomic tools and electrophoresis have been performed after varying storage conditions for evaluating aggregation and post translational modifications, like lactosylation or phosphorylation. Finally, Tof Sims and MEB were used to follow in parallel evolution of structure in surface and skin formation due to storage. Results + conclusion: These results highlight the important role of storage temperature in the stability of NPC. It is shown that this is not lactosylation at the heart of formation of aggregates, as advanced in others publications This is almost the rise of multitude post translational modifications (chemical cross link), added to disulphide bridges (physical cross link) wich contribute to the destabilisation of structure and aggregation of casein. A relative quantification of each kind of cross link, source of aggregates, is proposed. In addition, it has been proved that migration of lipids and formation of skin in surface during the ageing also explains the evolution of structure casein and thus the alterations of functional properties of NPC powder.

Keywords: casein, cross link, powder, storage

Procedia PDF Downloads 379
421 Evaluation of the Effect of Lactose Derived Monosaccharide on Galactooligosaccharides Production by β-Galactosidase

Authors: Yenny Paola Morales Cortés, Fabián Rico Rodríguez, Juan Carlos Serrato Bermúdez, Carlos Arturo Martínez Riascos

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Numerous benefits of galactooligosaccharides (GOS) as prebiotics have motivated the study of enzymatic processes for their production. These processes have special complexities due to several factors that make difficult high productivity, such as enzyme type, reaction medium pH, substrate concentrations and presence of inhibitors, among others. In the present work the production of galactooligosaccharides (with different degrees of polymerization: two, three and four) from lactose was studied. The study considers the formulation of a mathematical model that predicts the production of GOS from lactose using the enzyme β-galactosidase. The effect of pH in the reaction was studied. For that, phosphate buffer was used and with this was evaluated three pH values (6.0.6.5 and 7.0). Thus it was observed that at pH 6.0 the enzymatic activity insignificant. On the other hand, at pH 7.0 the enzymatic activity was approximately 27 times greater than at 6.5. The last result differs from previously reported results. Therefore, pH 7.0 was chosen as working pH. Additionally, the enzyme concentration was analyzed, which allowed observing that the effect of the concentration depends on the pH and the concentration was set for the following studies in 0.272 mM. Afterwards, experiments were performed varying the lactose concentration to evaluate its effects on the process and to generate the data for the adjustment of the mathematical model parameters. The mathematical model considers the reactions of lactose hydrolysis and transgalactosylation for the production of disaccharides and trisaccharides, with their inverse reactions. The production of tetrasaccharides was negligible and, because of that, it was not included in the model. The reaction was monitored by HPLC and for the quantitative analysis of the experimental data the Matlab programming language was used, including solvers for differential equations systems integration (ode15s) and nonlinear problems optimization (fminunc). The results confirm that the transgalactosylation and hydrolysis reactions are reversible, additionally inhibition by glucose and galactose is observed on the production of GOS. In relation to the production process of galactooligosaccharides, the results show that it is necessary to have high initial concentrations of lactose considering that favors the transgalactosylation reaction, while low concentrations favor hydrolysis reactions.

Keywords: β-galactosidase, galactooligosaccharides, inhibition, lactose, Matlab, modeling

Procedia PDF Downloads 358
420 Evidence of Microplastics Ingestion in Two Commercial Cephalopod Species: Octopus Vulgaris and Sepia Officinalis

Authors: Federica Laface, Cristina Pedà, Francesco Longo, Francesca de Domenico, Riccardo Minichino, Pierpaolo Consoli, Pietro Battaglia, Silvestro Greco, Teresa Romeo

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Plastics pollution represents one of the most important threats to marine biodiversity. In the last decades, different species are investigated to evaluate the extent of the plastic ingestion phenomenon. Even if the cephalopods play an important role in the food chain, they are still poorly studied. The aim of this research was to investigate the plastic ingestion in two commercial cephalopod species from the southern Tyrrhenian Sea: the common octopus, Octopus vulgaris (n=6; mean mantle length ML 10.7 ± 1.8) and the common cuttlefish, Sepia officinalis (n=13; mean ML 13.2 ± 1.7). Plastics were extracted from the filters obtained by the chemical digestion of cephalopods gastrointestinal tracts (GITs), using 10% potassium hydroxide (KOH) solution in a 1:5 (w/v) ratio. Once isolated, particles were photographed, measured, and their size class, shape and color were recorded. A total of 81 items was isolated from 16 of the 19 examined GITs, representing a total occurrence (%O) of 84.2% with a mean value of 4.3 ± 8.6 particles per individual. In particular, 62 plastics were found in 6 specimens of O. vulgaris (%O=100) and 19 particles in 10 S. officinalis (%O=94.7). In both species, the microplastics size class was the most abundant (93.8%). Plastic items found in O. vulgaris were mainly fibers (61%) while fragments were the most frequent in S. officinalis (53%). Transparent was the most common color in both species. The analysis will be completed by Fourier transform infrared (FT-IR) spectroscopy technique in order to identify polymers nature. This study reports preliminary data on plastic ingestion events in two cephalopods species and represents the first record of plastic ingestion by the common octopus. Microplastic items detected in both common octopus and common cuttlefish could derive from secondary and/or accidental ingestion events, probably due to their behavior, feeding habits and anatomical features. Further studies will be required to assess the effect of marine litter pollution in these ecologically and commercially important species.

Keywords: cephalopods, GIT analysis, marine pollution, Mediterranean sea, microplastics

Procedia PDF Downloads 253
419 Seismic Behavior and Loss Assessment of High–Rise Buildings with Light Gauge Steel–Concrete Hybrid Structure

Authors: Bing Lu, Shuang Li, Hongyuan Zhou

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The steel–concrete hybrid structure has been extensively employed in high–rise buildings and super high–rise buildings. The light gauge steel–concrete hybrid structure, including light gauge steel structure and concrete hybrid structure, is a new–type steel–concrete hybrid structure, which possesses some advantages of light gauge steel structure and concrete hybrid structure. The seismic behavior and loss assessment of three high–rise buildings with three different concrete hybrid structures were investigated through finite element software, respectively. The three concrete hybrid structures are reinforced concrete column–steel beam (RC‒S) hybrid structure, concrete–filled steel tube column–steel beam (CFST‒S) hybrid structure, and tubed concrete column–steel beam (TC‒S) hybrid structure. The nonlinear time-history analysis of three high–rise buildings under 80 earthquakes was carried out. After simulation, it indicated that the seismic performances of three high–rise buildings were superior. Under extremely rare earthquakes, the maximum inter–storey drifts of three high–rise buildings are significantly lower than 1/50. The inter–storey drift and floor acceleration of high–rise building with CFST‒S hybrid structure were bigger than those of high–rise buildings with RC‒S hybrid structure, and smaller than those of high–rise building with TC‒S hybrid structure. Then, based on the time–history analysis results, the post-earthquake repair cost ratio and repair time of three high–rise buildings were predicted through an economic performance analysis method proposed in FEMA‒P58 report. Under frequent earthquakes, basic earthquakes and rare earthquakes, the repair cost ratio and repair time of three high-rise buildings were less than 5% and 15 days, respectively. Under extremely rare earthquakes, the repair cost ratio and repair time of high-rise buildings with TC‒S hybrid structure were the most among three high rise buildings. Due to the advantages of CFST-S hybrid structure, it could be extensively employed in high-rise buildings subjected to earthquake excitations.

Keywords: seismic behavior, loss assessment, light gauge steel–concrete hybrid structure, high–rise building, time–history analysis

Procedia PDF Downloads 185
418 Analysis and Design of Offshore Met Mast Supported on Jacket Substructure

Authors: Manu Manu, Pardha J. Saradhi, Ramana M. V. Murthy

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Wind Energy is accepted as one of the most developed, cost effective and proven renewable energy technologies to meet increasing electricity demands in a sustainable manner. Preliminary assessment studies along Indian Coastline by Ministry of New and Renewable Energy have indicated prospects for development of offshore wind power along Tamil Nadu Coast, India. The commercial viability of a wind project mainly depends on wind characteristics on site. Hence, it is internationally recommended to perform site-specific wind resource assessment based on two years’ wind profile as a part of the feasibility study. Conventionally, guy wire met mast are used onshore for the collection of wind profile. Installation of similar structure in offshore requires complex marine spread and are very expensive. In the present study, an attempt is made to develop 120 m long lattice tower supported on the jacket, piled to the seabed at Rameshwaram, Tamil Nadu, India. Offshore met-masts are subjected to combined wind and hydrodynamic loads, and these lateral loads should be safely transferred to soil. The wind loads are estimated based on gust factor method, and the hydrodynamic loads are estimated by Morison’s equation along with suitable wave theory. The soil is modeled as three nonlinear orthogonal springs based on API standards. The structure configuration and optimum member sizes are obtained for extreme cyclone events. The dynamic behavior of mast under coupled wind and wave loads is also studied. The static responses of a mast with jacket type offshore platform have been studied using a frame model in SESAM. It is found from the study that the maximum displacement at the top of the mast for the random wave is 0.003 m and that of the tower for wind is 0.08 m during the steady state. The dynamic analysis results indicate that the structure is safe against coupled wind and wave loading.

Keywords: offshore wind, mast, static, aerodynamic load, hydrodynamic load

Procedia PDF Downloads 215
417 A New Co(II) Metal Complex Template with 4-dimethylaminopyridine Organic Cation: Structural, Hirshfeld Surface, Phase Transition, Electrical Study and Dielectric Behavior

Authors: Mohamed dammak

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Great attention has been paid to the design and synthesis of novel organic-inorganic compounds in recent decades because of their structural variety and the large diversity of atomic arrangements. In this work, the structure for the novel dimethyl aminopyridine tetrachlorocobaltate (C₇H₁₁N₂)₂CoCl₄ prepared by the slow evaporation method at room temperature has been successfully discussed. The X-ray diffraction results indicate that the hybrid material has a triclinic structure with a P space group and features a 0D structure containing isolated distorted [CoCl₄]2- tetrahedra interposed between [C7H11N²⁻]+ cations forming planes perpendicular to the c axis at z = 0 and z = ½. The effect of the synthesis conditions and the reactants used, the interactions between the cationic planes, and the isolated [CoCl4]2- tetrahedra are employing N-H...Cl and C-H…Cl hydrogen bonding contacts. The inspection of the Hirshfeld surface analysis helps to discuss the strength of hydrogen bonds and to quantify the inter-contacts. A phase transition was discovered by thermal analysis at 390 K, and comprehensive dielectric research was reported, showing a good agreement with thermal data. Impedance spectroscopy measurements were used to study the electrical and dielectric characteristics over a wide range of frequencies and temperatures, 40 Hz–10 MHz and 313–483 K, respectively. The Nyquist plot (Z" versus Z') from the complex impedance spectrum revealed semicircular arcs described by a Cole-Cole model. An electrical circuit consisting of a link of grain and grain boundary elements is employed. The real and imaginary parts of dielectric permittivity, as well as tg(δ) of (C₇H₁₁N₂)₂CoCl₄ at different frequencies, reveal a distribution of relaxation times. The presence of grain and grain boundaries is confirmed by the modulus investigations. Electric and dielectric analyses highlight the good protonic conduction of this material.

Keywords: organic-inorganic, phase transitions, complex impedance, protonic conduction, dielectric analysis

Procedia PDF Downloads 85
416 Bioavailability Enhancement of Ficus religiosa Extract by Solid Lipid Nanoparticles

Authors: Sanjay Singh, Karunanithi Priyanka, Ramoji Kosuru, Raju Prasad Sharma

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Herbal drugs are well known for their mixed pharmacological activities with the benefit of no harmful side effects. The use of herbal drugs is limited because of their higher dose requirement, frequent drug administration, poor bioavailability of phytochemicals and delayed onset of action. Ficus religiosa, a potent anti-oxidant plant useful in the treatment of diabetes and cancer was selected for the study. Solid lipid nanoparticles (SLN) of Ficus religiosa extract was developed for the enhancement in oral bioavailability of stigmasterol and β-sitosterol-d-glucoside, principal components present in the extract. Hot homogenization followed by ultrasonication method was used to develop extract loaded SLN. Developed extract loaded SLN were characterized for particle size, PDI, zeta potential, entrapment efficiency, in vitro drug release and kinetics, fourier transform infra-red spectroscopy, differential scanning calorimetry, powder X-ray diffractrometry and stability studies. Entrapment efficiency of optimized extract loaded SLN was found to be 68.46 % (56.13 % of stigmasterol and 12.33 % of β-sitosteryl-d-glucoside, respectively). RP HPLC method development was done for simultaneous estimation of stigmasterol and β-sitosterol-d-glucoside in Ficus religiosa extract in rat plasma. Bioavailability studies were carried out for extract in suspension form and optimized extract loaded SLN. AUC of stigmasterol and β-sitosterol-d-glucoside were increased by 6.7-folds by 9.2-folds, respectively in rats treated with extract loaded SLN compared to extract suspension. Also, Cmax of stigmasterol and β-sitosterol-d-glucoside were increased by 4.3-folds by 3.9-folds, respectively in rats treated with extract loaded SLN compared to extract suspension. Mean residence times (MRT) for stigmasterol were found to be 12.3 ± 0.67 hours from extract and 7.4 ± 2.1 hours from SLN and for β-sitosterol-d-glucoside, 10.49 ± 2.9 hours from extract and 6.4 ± 0.3 hours from SLN. Hence, it was concluded that SLN enhanced the bioavailability and reduced the MRT of stigmasterol and β-sitosterol-d-glucoside in Ficus religiosa extract which in turn may lead to reduction in dose of Ficus religiosa extract, prolonged duration of action and also enhanced therapeutic efficacy.

Keywords: Ficus religiosa, phytosterolins, bioavailability, solid lipid nanoparticles, stigmasterol and β-sitosteryl-d-glucoside

Procedia PDF Downloads 473
415 A Method for Solid-Liquid Separation of Cs+ from Radioactive Waste by Using Ionic Liquids and Extractants

Authors: J. W. Choi, S. Y. Cho, H. J. Lee, W. Z. Oh, S. J. Choi

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Ionic liquids (ILs), which is alternative to conventional organic solvent, were used for extraction of Cs ions. ILs, as useful environment friendly green solvents, have been recently applied as replacement for traditional volatile organic compounds (VOCs) in liquid/liquid extraction of heavy metal ions as well as organic and inorganic species and pollutants. Thus, Ionic liquids were used for extraction of Cs ions from the liquid radioactive waste. In most cases, Cs ions present in radioactive wastes in very low concentration, approximately less than 1ppm. Therefore, unlike established extraction system the required amount of ILs as extractant is comparatively very small. This extraction method involves cation exchange mechanism in which Cs ion transfers to the organic phase and binds to one crown ether by chelation in exchange of single ILs cation, IL_cation+, transfer to the aqueous phase. In this extraction system showed solid-liquid separation in which the Ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonly)imide (C2mimTf2N) and the crown ether Dicyclohexano-18-crown-6 (DCH18C6) both were used here in very little amount as solvent and as extractant, respectively. 30 mM of CsNO3 was used as simulated waste solution cesium ions. Generally, in liquid-liquid extraction, the molar ratio of CE:Cs+:ILs was 1:5~10:>100, while our applied molar ratio of CE:Cs+:ILs was 1:2:1~10. The quantity of CE and Cs ions were fixed to 0.6 and 1.2 mmol, respectively. The phenomenon of precipitation showed two kinds of separation: solid-liquid separation in the ratio of 1:2:1 and 1:2:2; solid-liquid-liquid separation (3 phase) in the ratio of 1:2:5 and 1:2:10. In the last system, 3 phases were precipitate-ionic liquids-aqueous. The precipitate was verified to consist of Cs+, DCH18C6, Tf2N- based on the cation exchange mechanism. We analyzed precipitate using scanning electron microscopy with X-ray microanalysis (SEM-EDS), an elemental analyser, Fourier transform infrared spectroscopy (FT-IR) and differential scanning calorimetry (DSC). The experimental results showed an easy extraction method and confirmed the composition of solid precipitate. We also obtained information that complex formation ratio of Cs+ to DCH18C6 is 0.88:1 regardless of C2mimTf2N quantities.

Keywords: extraction, precipitation, solid-liquid seperation, ionic liquid, precipitate

Procedia PDF Downloads 421
414 Modification of Titanium Surfaces with Micro/Nanospheres for Local Antibiotic Release

Authors: Burcu Doymus, Fatma N. Kok, Sakip Onder

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Titanium and titanium-based materials are commonly used to replace or regenerate the injured or lost tissues because of accidents or illnesses. Hospital infections and strong bond formation at the implant-tissue interface are directly affecting the success of the implantation as weak bonding with the native tissue and hospital infections lead to revision surgery. The purpose of the presented study is to modify the surface of the titanium substrates with nano/microspheres for local drug delivery and to prevent hospital infections. Firstly, titanium surfaces were silanized with APTES (3-Triethoxysilylpropylamine) following the negatively charged oxide layer formation. Then characterization studies using Scanning Electron Microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were done on the modified surfaces. Secondly, microspheres/nanospheres were prepared with chitosan that is a natural polymer and having valuable properties such as non-toxicity, high biocompatibility, low allergen city and biodegradability for biomedical applications. Antibiotic (ciprofloxacin) loaded micro/nanospheres have been fabricated using emulsion cross-linking method and have been immobilized onto the titanium surfaces with different immobilization techniques such as covalent bond and entrapment. Optimization studies on size and drug loading capacities of micro/nanospheres were conducted before the immobilization process. Light microscopy and SEM were used to visualize and measure the size of the produced micro/nanospheres. Loaded and released drug amounts were determined by using UV- spectrophotometer at 278 nm. Finally, SEM analysis and drug release studies on the micro/nanospheres coated Ti surfaces were done. As a conclusion, it was shown that micro/nanospheres were immobilized onto the surfaces successfully and drug release from these surfaces was in a controlled manner. Moreover, the density of the micro/nanospheres after the drug release studies was higher on the surfaces where the entrapment technique was used for immobilization. Acknowledgement: This work is financially supported by The Scientific and Technological Research Council Of Turkey (Project # 217M220)

Keywords: chitosan, controlled drug release, nanosphere, nosocomial infections, titanium

Procedia PDF Downloads 125
413 Structural Evolution of Na6Mn(SO4)4 from High-Pressure Synchrotron Powder X-ray Diffraction

Authors: Monalisa Pradhan, Ajana Dutta, Irshad Kariyattuparamb Abbas, Boby Joseph, T. N. Guru Row, Diptikanta Swain, Gopal K. Pradhan

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Compounds with the Vanthoffite crystal structure having general formula Na6M(SO₄)₄ (M= Mg, Mn, Ni , Co, Fe, Cu and Zn) display a variety of intriguing physical properties intimately related to their structural arrangements. The compound Na6Mn(SO4)4 shows antiferromagnetic ordering at low temperature where the in-plane Mn-O•••O-Mn interactions facilitates antiferromagnetic ordering via a super-exchange interaction between the Mn atoms through the oxygen atoms . The inter-atomic bond distances and angles can easily be tuned by applying external pressure and can be probed using high resolution X-ray diffraction. Moreover, because the magnetic interaction among the Mn atoms are super-exchange type via Mn-O•••O-Mn path, the variation of the Mn-O•••O-Mn dihedral angle and Mn-O bond distances under high pressure inevitably affects the magnetic properties. Therefore, it is evident that high pressure studies on the magnetically ordered materials would shed light on the interplay between their structural properties and magnetic ordering. This will indeed confirm the role of buckling of the Mn-O polyhedral in understanding the origin of anti-ferromagnetism. In this context, we carried out the pressure dependent X-ray diffraction measurement in a diamond anvil cell (DAC) up to a maximum pressure of 17 GPa to study the phase transition and determine equation of state from the volume compression data. Upon increasing the pressure, we didn’t observe any new diffraction peaks or sudden discontinuity in the pressure dependences of the d values up to the maximum achieved pressure of ~17 GPa. However, it is noticed that beyond 12 GPa the a and b lattice parameters become identical while there is a discontinuity in the β value around the same pressure. This indicates a subtle transition to a pseudo-monoclinic phase. Using the third order Birch-Murnaghan equation of state (EOS) to fit the volume compression data for the entire range, we found the bulk modulus (B0) to be 44 GPa. If we consider the subtle transition at 12 GPa, we tried to fit another equation state for the volume beyond 12 GPa using the second order Birch-Murnaghan EOS. This gives a bulk modulus of ~ 34 GPa for this phase.

Keywords: mineral, structural phase transition, high pressure XRD, spectroscopy

Procedia PDF Downloads 87
412 Methylglyoxal Induced Glycoxidation of Human Low Density Lipoprotein: A Biophysical Perspective and Its Role in Diabetes and Periodontitis

Authors: Minhal Abidi, Moinuddin

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Diabetes mellitus (DM) induced metabolic abnormalities causes oxidative stress which leads to the pathogenesis of complications associated with diabetes like retinopathy, nephropathy periodontitis etc. Combination of glycation and oxidation 'glycoxidation' occurs when oxidative reactions affect the early state of glycation products. Low density lipoprotein (LDL) is prone to glycoxidative attack by sugars and methylglyoxal (MGO) being a strong glycating agent may have severe impact on its structure and consequent role in diabetes. Pro-inflammatory cytokines like IL1β and TNFα produced by the action of gram negative bacteria in periodontits (PD) can in turn lead to insulin resistance. This work discusses modifications to LDL as a result of glycoxidation. The changes in the protein molecule have been characterized by various physicochemical techniques and the immunogenicity of the modified molecules was also evaluated as they presented neo-epitopes. Binding of antibodies present in diabetes patients to the native and glycated LDL has been evaluated. Role of modified epitopes in the generation of antibodies in diabetes and periodontitis has been discussed. The structural perturbations induced in LDL were analyzed by UV–Vis, fluorescence, circular dichroism and FTIR spectroscopy, molecular docking studies, thermal denaturation studies, Thioflavin T assay, isothermal titration calorimetry, comet assay. MALDI-TOF, ketoamine moieties, carbonyl content and HMF content were also quantitated in native and glycated LDL. IL1β and TNFα levels were also measured in the type 2 DM and PD patients. We report increased carbonyl content, ketoamine moieties and HMF content in glycated LDL as compared to native analogue. The results substantiate that in hyperglycemic state MGO modification of LDL causes structural perturbations making the protein antigenic which could obstruct normal physiological functions and might contribute in the development of secondary complications in diabetic patients like periodontitis.

Keywords: advanced glycation end products, diabetes mellitus, glycation, glycoxidation, low density lipoprotein, periodontitis

Procedia PDF Downloads 191