Search results for: in situ FTIR

Authors: Yogesh S. Patel

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Novel polyimides were synthesized by Diels–Alder polymerization. Bisfuran was reacted with a couple of bismaleimides containing diglycidyl ether of bisphenol-A and F (epoxy) segment to obtain Diels–Alder polyadducts. Polyadducts were then aromatized and imidized (i.e. cyclized) through carboxylic and amide groups to afford polyimides. Synthesized polyadducts and polyimides were characterized by elemental analysis, spectral features, the number of average molecular weight (Mn) and thermal analysis. The ‘in situ’ glass fiber reinforced composites were prepared and characterized by mechanical, electrical, and chemical properties. These properties were compared with the other reported polyimides. All the composites showed good mechanical and electrical properties and good resistance to organic solvents and mineral acids.

Keywords: Diels-Alder reaction, bisfuran, bismaleimides, polyimide

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Authors: Shimaa M. Elsaeed, Reem K. Farag, Ibrahim M. Nassar

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Hydrogel conductive polymer nanocomposite fabricated via in-situ polymerization of polyaniline (PANI) inside thermosensitive hydrogels based on hydroxy ethyl meth acrylate (HEMA) copolymer with 2-acrylamido-2-methyl propane sulfonic acid (AMPS). SEM micrographs show the nanometric size of the conductive material (polyaniline, PANI) dispersed in the hydrogel matrix. The swelling parameters of hydrogel are measured. The incorporation of PANI improves the mechanical properties and swelling up to 30,000% without breaking. X-ray diffraction shows that typical polyaniline crystallization is formed in composite, which is advantageous to increase the electrical conductivity of the composite hydrogel. Open-circuit voltage (I-V) curve fill factor of the highest photo-conversion efficiency and enhanced to use in solar cell.

Keywords: hydrogel, solar cell, conductive polymer, nanocomposite

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Authors: Nouf Alharbi

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The electrospray deposition technique became an important method that enables fragile, nonvolatile molecules to be deposited in situ in high vacuum environments. Furthermore, it is considered one of the ways to close the gap between basic surface science and molecular engineering, which represents a gradual change in the range of scientist research. Also, this paper talked about one of the most important techniques that have been developed and aimed for helping to further develop and characterize the electrospray by providing data collected using an image charge detection instrument. Image charge detection mass spectrometry (CDMS) is used to measure speed and charge distributions of the molecular ions. As well as, some data has been included using SIMION simulation to simulate the energies and masses of the molecular ions through the system in order to refine the mass-selection process.

Keywords: charge, deposition, electrospray, image, ions, molecules, SIMION

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Authors: Endalkachew Abebe Kebede, Bojin Bojinov, Andon Vasilev Andonov, Orhan Dengiz

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Remote sensing has a potential application in assessing and monitoring the plants' biophysical properties using the spectral responses of plants and soils within the electromagnetic spectrum. However, only a few reports compare the performance of different remote sensing sensors against in-situ field spectral measurement. The current study assessed the potential applications of open data source satellite images (Sentinel 2 and Landsat 9) in estimating the biophysical properties of the wheat crop on a study farm found in the village of OvchaMogila. A Landsat 9 (30 m resolution) and Sentinel-2 (10 m resolution) satellite images with less than 10% cloud cover have been extracted from the open data sources for the period of December 2021 to April 2022. An Unmanned Aerial Vehicle (UAV) has been used to capture the spectral response of plant leaves. In addition, SpectraVue 710s Leaf Spectrometer was used to measure the spectral response of the crop in April at five different locations within the same field. The ten most common vegetation indices have been selected and calculated based on the reflectance wavelength range of remote sensing tools used. The soil samples have been collected in eight different locations within the farm plot. The different physicochemical properties of the soil (pH, texture, N, P₂O₅, and K₂O) have been analyzed in the laboratory. The finer resolution images from the UAV and the Leaf Spectrometer have been used to validate the satellite images. The performance of different sensors has been compared based on the measured leaf spectral response and the extracted vegetation indices using the five sampling points. A scatter plot with the coefficient of determination (R2) and Root Mean Square Error (RMSE) and the correlation (r) matrix prepared using the corr and heatmap python libraries have been used for comparing the performance of Sentinel 2 and Landsat 9 VIs compared to the drone and SpectraVue 710s spectrophotometer. The soil analysis revealed the study farm plot is slightly alkaline (8.4 to 8.52). The soil texture of the study farm is dominantly Clay and Clay Loam.The vegetation indices (VIs) increased linearly with the growth of the plant. Both the scatter plot and the correlation matrix showed that Sentinel 2 vegetation indices have a relatively better correlation with the vegetation indices of the Buteo dronecompared to the Landsat 9. The Landsat 9 vegetation indices somewhat align better with the leaf spectrometer. Generally, the Sentinel 2 showed a better performance than the Landsat 9. Further study with enough field spectral sampling and repeated UAV imaging is required to improve the quality of the current study.

Keywords: landsat 9, leaf spectrometer, sentinel 2, UAV

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Authors: Samira Tlili, Amina Grairia, Sihem Benayache, Saida Bouyegh, Sabrina Ladjama, Abdelmoumen Guedri

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Phosphorites from Djebel Onk Tebessa/Algeria deposit contain a CaO of 50-52 wt. % and P₂O₅ level of ≥ 30.20 wt. %. The microstructure revealed using a spectroscopy electronic microscope (SEM) consists of phosphate granules with an ovular form. In this investigation, we have identified phosphate with varying particle sizes using mineralogical methods. The phosphogypsum formed by the mineralization of natural phosphate has also been discovered. This co-product was formed during the attack on natural phosphates by sulfuric acid. This study demonstrated the effectiveness of the thermoanalytical technique of differential scanning calorimetry (DSC), X-ray diffraction, and EDS/MEB analysis. FTIR analyses also validated the identification of mineral phases with the observation of bands from structural phosphate groups.

Keywords: phosphate, Djebel Onk deposit, mineralogy, valorization, phosphogypsum

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Authors: Haythem Barrak, Gaetan Laroche, Adel M’nif, Ahmed Hichem Hamzaoui

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The use of semiconductor oxides, as chemical or biological, requires their functionalization with appropriate dependent molecules of the substance to be detected. generally, the support materials used are TiO2 and SiO2. In the present work, we used zinc oxide (ZnO) known for its interesting physical properties. The synthesis of nano scale ZnO was performed by co-precipitation at low temperature (60 ° C).To our knowledge, the obtaining of this material at this temperature was carried out for the first time. This shows the low cost of this operation. On the other hand, the surface functionalization of ZnO was performed with (3-aminopropyl) triethoxysilane (APTES) by using a specific method using ethanol for the first time. In addition, the duration of this stage is very low compared to literature. The samples obtained were analyzed by XRD, TEM, DLS, FTIR, and TGA shows that XPS that the operation of grafting of APTES on our support was carried out with success.

Keywords: functionalization, nanoparticle, ZnO, APTES, caractérisation

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Authors: D. Majumdar, M. Baskey, S. K. Saha

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Graphene has already been identified as a promising material for future carbon based electronics. To develop graphene technology, the fabrication of a high quality P-N junction is a great challenge. In the present work, we have described a simple and general technique to grow single crystalline polyaniline (PANI) films on graphene sheets using in situ polymerization via the oxidation-reduction of aniline monomer and graphene oxide, respectively, to fabricate a high quality P-N junction, which shows diode-like behavior with a remarkably low turn-on voltage (60 mV) and high rectification ratio (1880:1) up to a voltage of 0.2 Volt. The origin of these superior electronic properties is the preferential growth of a highly crystalline PANI film as well as lattice matching between the d-values [~2.48 Å] of graphene and {120} planes of PANI.

Keywords: epitaxial growth, PANI, reduced graphene oxide, rectification ratio

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Authors: Rio Hirakawa, Christian Gundlach, Sven Hartwig

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In recent years, the use of aluminium has further expanded and is expected to replace steel in the future as vehicles become lighter and more recyclable in order to reduce greenhouse gas (GHG) emissions and improve fuel economy. In line with this, structures and components are becoming increasingly multi-material, with different materials, including aluminium, being used in combination to improve mechanical utility and performance. A common method of assembling dissimilar materials is mechanical fastening, but it has several drawbacks, such as increased manufacturing processes and the influence of substrate-specific mechanical properties. Adhesive bonding and fusion bonding are methods that overcome the above disadvantages. In these two joining methods, surface pre-treatment of the substrate is always necessary to ensure the strength and durability of the joint. Previous studies have shown that laser surface treatment improves the strength and durability of the joint. Yan et al. showed that laser surface treatment of aluminium alloys changes α-Al2O3 in the oxide layer to γ-Al2O3. As γ-Al2O3 has a large specific surface area, is very porous and chemically active, laser-treated aluminium surfaces are expected to undergo physico-chemical changes over time and adsorb moisture and organic substances from the air or storage atmosphere. The impurities accumulated on the laser-treated surface may be released at the adhesive and bonding interface by the heat input to the bonding system during the joining phase, affecting the strength and durability of the joint. However, only a few studies have discussed the effect of such storage periods on laser-treated surfaces. This paper, therefore, investigates the ageing of laser-treated aluminium alloy surfaces through thermal analysis, electrochemical analysis and microstructural observations.AlMg3 of 0.5 mm and 1.5 mm thickness was cut using a water-jet cutting machine, cleaned and degreased with isopropanol and surface pre-treated with a pulsed fibre laser at 1060 nm wavelength, 70 W maximum power and 55 kHz repetition frequency. The aluminium surface was then analysed using SEM, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR) and cyclic voltammetry (CV) after storage in air for various periods ranging from one day to several months TGA and FTIR analysed impurities adsorbed on the aluminium surface, while CV revealed changes in the true electrochemically active surface area. SEM also revealed visual changes on the treated surface. In summary, the changes in the laser-treated aluminium surface with storage time were investigated, and the final results were used to determine the appropriate storage period.

Keywords: laser surface treatment, pre-treatment, adhesion, bonding, corrosion, durability, dissimilar material interface, automotive, aluminium alloys

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Authors: Andrew J. Zacharias

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The forest garden approach (FGA) was established by Trees for the Future (TREES) over the organization’s 30 years of agroforestry projects in Sub-Saharan Africa. This method transforms traditional agricultural systems into highly managed gardens that produce food and marketable products year-round. The effects of the FGA on food security, dietary diversity, and economic resilience have been measured closely, and TREES has begun to closely monitor the environmental impacts through the use of sensors mounted on unmanned aerial vehicles, commonly known as 'drones'. These drones collect thousands of pictures to create 3-D models in both the visible and the near-infrared wavelengths. Analysis of these models provides TREES with quantitative and qualitative evidence of improvements to the annual above-ground biomass and leaf area indices, as measured in-situ using NDVI calculations.

Keywords: agroforestry, biomass, drones, NDVI

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Authors: Chunxiao Wu, Dongyun Jiang, Tao Jiang, Luxia Xu, Qian Xu, Meng Zhao, Qin Zhu, Zhigang Guo, Jinlan Pan, Suning Chen

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The stability and evolution of human genetics depends on chromosomes (and chromosome-chromosome interactions). We wish to understand the spatial location of chromosomes in dividing cells in order to understand the relationship between chromosome-chromosome interactions and to further investigate the role of chromosomes and their impact on cell biological behavior. In this study, we explored the relative spatial positional relationships of chromosomes [t (9;22) and t (15;17)] in B-ALL cells by using the three-dimensions DNA in situ fluorescent hybridization (3D-FISH) method. The results showed that chromosomes [t (9;22) and t (15;17)] showed relatively stable spatial relationships. The relative stability of the spatial location of chromosomes in dividing cells may be relevant to disease.

Keywords: chromosome, human genetics, chromosome territory, 3D-FISH

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Authors: Anton G. Kalmykov, Andrew Yu. Bychkov, Georgy A. Kalmykov

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Nowadays, most oil reserves in Russia and all over the world are hard to recover. That is the reason oil companies are searching for new sources for hydrocarbon production. One of the sources might be high-carbon formations with unconventional reservoirs. Bazhenov formation is a huge source rock formation located in West Siberia, which contains unconventional reservoirs on some of the areas. These reservoirs are formed by secondary processes with low predicting ratio. Only one of five wells is drilled through unconventional reservoirs, in others kerogen has low thermal maturity, and they are of low petroliferous. Therefore, there was a request for tertiary methods for in-situ cracking of kerogen and production of oil. Laboratory experiments of Bazhenov formation rock hydrous pyrolysis were used to investigate features of the oil generation process. Experiments on Bazhenov rocks with a different mineral composition (silica concentration from 15 to 90 wt.%, clays – 5-50 wt.%, carbonates – 0-30 wt.%, kerogen – 1-25 wt.%) and thermal maturity (from immature to late oil window kerogen) were performed in a retort under reservoir conditions. Rock samples of 50 g weight were placed in retort, covered with water and heated to the different temperature varied from 250 to 400°C with the durability of the experiments from several hours to one week. After the experiments, the retort was cooled to room temperature; generated hydrocarbons were extracted with hexane, then separated from the solvent and weighted. The molecular composition of this synthesized oil was then investigated via GC-MS chromatography Characteristics of rock samples after the heating was measured via the Rock-Eval method. It was found, that the amount of synthesized oil and its composition depending on the experimental conditions and composition of rocks. The highest amount of oil was produced at a temperature of 350°C after 12 hours of heating and was up to 12 wt.% of initial organic matter content in the rocks. At the higher temperatures and within longer heating time secondary cracking of generated hydrocarbons occurs, the mass of produced oil is lowering, and the composition contains more hydrocarbons that need to be recovered by catalytical processes. If the temperature is lower than 300°C, the amount of produced oil is too low for the process to be economically effective. It was also found that silica and clay minerals work as catalysts. Selection of heating conditions allows producing synthesized oil with specified composition. Kerogen investigations after heating have shown that thermal maturity increases, but the yield is only up to 35% of the maximum amount of synthetic oil. This yield is the result of gaseous hydrocarbons formation due to secondary cracking and aromatization and coaling of kerogen. Future investigations will allow the increase in the yield of synthetic oil. The results are in a good agreement with theoretical data on kerogen maturation during oil production. Evaluated trends could be tooled up for in-situ oil generation by shale rocks thermal action.

Keywords: Bazhenov formation, fossil fuels, hydropyrolysis, synthetic oil

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Authors: Nesrin Köken, Esin A. Güvel, Nilgün Kızılcan

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This work presents synthesis of α,ω-dithienyl terminated poly(ethylene glycol) (PEGTh) capable for further chain extension by either chemical or electrochemical polymerization. PEGTh was characterized by FTIR and 1H-NMR. Further, copolymerization of PEGTh and pyrrole (Py) was performed by chemical oxidative polymerization using ceric (IV) salt as an oxidant (PPy-PEGTh). PEG without end group modification was used directly to prepare copolymers with Py by Ce (IV) salt (PPy-PEG). Block copolymers with mole ratio of pyrrole to PEGTh (PEG) 50:1 and 10:1 were synthesized. The electrical conductivities of copolymers PPy-PEGTh and PPy-PEG were determined by four-point probe technique. Influence of the synthetic route and content of the insulating segment on conductivity and yield of the copolymers were investigated.

Keywords: chemical oxidative polymerization, conducting polymer, poly(ethylene glycol), polypyrrole

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Authors: Evgeny A. Ermakov, Lyudmila P. Smirnova, Valentina N. Buneva

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Schizophrenia associated with dysregulation of neurotransmitter processes in the central nervous system and disturbances in the humoral immune system resulting in the formation of antibodies (Abs) to the various components of the nervous tissue. Abs to different neuronal receptors and DNA were detected in the blood of patients with schizophrenia. Abs hydrolyzing DNA were detected in pool of polyclonal autoantibodies in autoimmune and infectious diseases, such catalytic Abs were named abzymes. It is believed that DNA-hydrolyzing abzymes are cytotoxic, cause nuclear DNA fragmentation and induce cell death by apoptosis. Abzymes with DNAase activity are interesting because of the mechanism of formation and the possibility of use as diagnostic markers. Therefore, in our work we have set following goals: to determine the level anti-DNA Abs in the serum of patients with schizophrenia and to study DNA-hydrolyzing activity of IgG of patients with schizophrenia. Materials and methods: In our study there were included 41 patients with a verified diagnosis of paranoid or simple schizophrenia and 24 healthy donors. Electrophoretically and immunologically homogeneous IgGs were obtained by sequential affinity chromatography of the serum proteins on protein G-Sepharose and gel filtration. The levels of anti-DNA Abs were determined using ELISA. DNA-hydrolyzing activity was detected as the level of supercoiled pBluescript DNA transition in circular and linear forms, the hydrolysis products were analyzed by agarose electrophoresis followed by ethidium bromide stain. To correspond the registered catalytic activity directly to the antibodies we carried out a number of strict criteria: electrophoretic homogeneity of the antibodies, gel filtration (acid shock analysis) and in situ activity. Statistical analysis was performed in ‘Statistica 9.0’ using the non-parametric Mann-Whitney test. Results: The sera of approximately 30% of schizophrenia patients displayed a higher level of Abs interacting with single-stranded (ssDNA) and double-stranded DNA (dsDNA) compared with healthy donors. The average level of Abs interacting with ssDNA was only 1.1-fold lower than that for interacting with dsDNA. IgG of patient with schizophrenia were shown to possess DNA hydrolyzing activity. Using affinity chromatography, electrophoretic analysis of isolated IgG homogeneity, gel filtration in acid shock conditions and in situ DNAse activity analysis we proved that the observed activity is intrinsic property of studied antibodies. We have shown that the relative DNAase activity of IgG in patients with schizophrenia averaged 55.4±32.5%, IgG of healthy donors showed much lower activity (average of 9.1±6.5%). It should be noted that DNAase activity of IgG in patients with schizophrenia with a negative symptoms was significantly higher (73.3±23.8%), than in patients with positive symptoms (43.3±33.1%). Conclusion: Anti-DNA Abs of patients with schizophrenia not only bind DNA, but quite efficiently hydrolyze the substrate. The data show a correlation with the level of DNase activity and leading symptoms of patients with schizophrenia.

Keywords: anti-DNA antibodies, abzymes, DNA hydrolysis, schizophrenia

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Authors: Esther Acha, Jose Cambra, De Chen

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Hydrogen is considered an important energy vector for the 21st century. Nowadays there are some difficulties for hydrogen economy implantation, and one of them is the high purity required for hydrogen. This energy vector is still being mainly produced from fuels, from wich hydrogen is produced as a component of a mixture containing other gases, such as CO, CO2 and H2O. A forthcoming sustainable pathway for hydrogen is steam-reforming of bio-oils derived from biomass, e.g. via fast pyrolysis. Bio-oils are a mixture of acids, alcohols, aldehydes, esters, ketones, sugars phenols, guaiacols, syringols, furans, multi-functional compounds and also up to a 30 wt% of water. The sorption enhanced steam reforming (SESR) process is attracting a great deal of attention due to the fact that it combines both hydrogen production and CO2 separation. In the SESR process, carbon dioxide is captured by an in situ sorbent, which shifts the reversible reforming and water gas shift reactions to the product side, beyond their conventional thermodynamic limits, giving rise to a higher hydrogen production and lower cost. The hydrogen containing mixture has been obtained from the SESR of bio-oil type compounds. Different types of catalysts have been tested. All of them contain Ni at around a 30 wt %. Two samples have been prepared with the wet impregnation technique over conventional (gamma alumina) and non-conventional (olivine) supports. And a third catalysts has been prepared over a hydrotalcite-like material (HT). The employed sorbent is a commercial dolomite. The activity tests were performed in a bench-scale plant (PID Eng&Tech), using a stainless steel fixed bed reactor. The catalysts were reduced in situ in the reactor, before the activity tests. The effluent stream was cooled down, thus condensed liquid was collected and weighed, and the gas phase was analysed online by a microGC. The hydrogen yield, and process behavior was analysed without the sorbent (the traditional SR where a second purification step will be needed but that operates in steady state) and the SESR (where the purification step could be avoided but that operates in batch state). The influence of the support type and preparation method will be observed in the produced hydrogen yield. Additionally, the stability of the catalysts is critical, due to the fact that in SESR process sorption-desorption steps are required. The produced hydrogen yield and hydrogen purity has to be high and also stable, even after several sorption-desorption cycles. The prepared catalysts were characterized employing different techniques to determine the physicochemical properties of the fresh-reduced and used (after the activity tests) materials. The characterization results, together with the activity results show the influence of the catalysts preparation method, calcination temperature, or can even explain the observed yield and conversion.

Keywords: CO2 sorbent, enhanced steam reforming, hydrogen

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Authors: Guido Trautmann-Sáez, Mario Pérez-Won, Vilbett Briones, María José Bugueño, Gipsy Tabilo-Munizaga, Luis Gonzáles-Cavieres

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Shrimp by-products are a valuable source of protein. However, traditional protein extraction methods have limitations in terms of their efficiency. Protein extraction from shrimp (Pleuroncodes monodon) industrial by-products assisted with ohmic heating (OH), microwave (MW) and pulsed electric field (PEF). It was performed by chemical method (using NaOH and HCl 2M) assisted with OH, MW and PEF in a continuous flow system (5 ml/s). Protein determination, differential scanning calorimetry (DSC) and Fourier-transform infrared (FTIR). Results indicate a 19.25% (PEF) 3.65% (OH) and 28.19% (MW) improvement in protein extraction efficiency. The most efficient method was selected for the electrospinning process and obtaining fiber.

Keywords: electrospinning process, emerging technology, protein extraction, shrimp by-products

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Authors: S. E. Mohmad-Saberi, W. Song, N. Oliver, M. Adrian, T.C. Hsu, A. Darbyshire

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Biodegradable polyurethane (PU) has emerged as a potential material to promote repair and regeneration of damaged/diseased tissues in heart valve regeneration due to its excellent biomechanical profile. Understanding the effects of sterilization on their properties is vital since they are more sensitive and more critical of porous structures compared to bulk ones. In this study, the effects of low concentration of hydrogen peroxide (H₂O₂) solution sterilization has been investigated to determine whether the procedure would be efficient and non-destructive to porous three-dimensional (3D) elastomeric nanocomposite, polyhedral oligomeric silsesquioxane-terminated poly (ethylene-diethylene glycol succinate-sebacate) urea-urethane (POSS-EDSS-PU) scaffold. All the samples were tested for sterility following sterilization using phosphate buffer saline (PBS) as control and 5 % v/v H₂O₂ solution. The samples were incubated in tryptic soy broth for the cultivation of microorganisms under agitation at 37˚C for 72 hours. The effects of the 5 % v/v H₂O₂ solution sterilization were evaluated in terms of morphology, chemical and mechanical properties using scanning electron microscopy (SEM), Fourier transform infrared (FTIR) and tensile tester apparatus. Toxicity effects of the 5 % v/v H₂O₂ solution decontamination were studied by in vitro cytotoxicity test, where the cellular responses of human dermal fibroblast (HDF) were examined. A clear, uncontaminated broth using 5 % v/v H₂O₂ solution method indicated efficient sterilization after 3 days, while the non-sterilized control shows clouding broth indicated contamination. The morphology of 3D POSS-EDSS-PU scaffold appeared to have similar morphology after sterilization with 5 % v/v H₂O₂ solution regarding of pore size and surface. FTIR results show that the sterilized samples and non-sterilized control share the same spectra pattern, confirming no significant alterations over the surface chemistry. For the mechanical properties of the H₂O₂ solution-treated scaffolds, the tensile strain was not significantly decreased, however, become significantly stiffer after the sterilization. No cytotoxic effects were observed after the 5 % v/v H₂O₂ solution sterilization as confirmed by cell viability assessed by Alamar Blue assay. The results suggest that low concentration of 5 % v/v hydrogen peroxide solution can be used as an alternative method for sterilizing biodegradable 3D porous scaffold with micro/nano-architecture without structural deformation. This study provides the understanding of the sterilization effects on biomechanical profile and cell proliferation of 3D POSS-EDSS-PU scaffolds.

Keywords: biodegradable, hydrogen peroxide solution, POSS-EDSS-PU, sterilization

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Authors: Tariku Nefo Duke

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Herein, we synthesized three PIs/h-boron nitride composite films for corrosion resistance of mild steel material. The structures of these three polyimide/h-boron nitride composite films were confirmed using (FTIR, 1H NMR, 13C NMR, and 2D NMR) spectroscopy techniques. The synthesized PIs composite films have high mechanical properties, thermal stability, high glass-transition temperature (Tg), and insulating properties. It has been shown that the presence of electroactive TiO2, SiO2, and h-BN, in polymer coatings effectively inhibits corrosion. The h-BN displays an admirable anti-corrosion barrier for the 6F-OD and BT-OD films. PI/ h-BN composite films of 6F-OD exhibited better resistance to water vapor, high corrosion resistance, and positive corrosion voltage. Only four wt. percentage of h-BN in the composite is adequate.

Keywords: polyimide, corrosion resistance, electroactive, Tg

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Authors: Nitin Jadhav, Pradeep R. Vavia

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Poor water soluble drugs are difficult to promote for oral drug delivery as they demonstrate poor and variable bioavailability because of its poor solubility and dissolution in GIT fluid. Nowadays lipid based formulations especially self microemulsifying drug delivery system (SMEDDS) is found as the most effective technique. With all the impressive advantages, the need of high amount of surfactant (50% - 80%) is the major drawback of SMEDDS. High concentration of synthetic surfactant is known for irritation in GIT and also interference with the function of intestinal transporters causes changes in drug absorption. Surfactant may also reduce drug activity and subsequently bioavailability due to the enhanced entrapment of drug in micelles. In chronic treatment these issues are very conspicuous due to the long exposure. In addition the liquid self microemulsifying system also suffers from stability issues. Recently one novel approach of solid stabilized micro and nano emulsion (Pickering emulsion) has very admirable properties such as high stability, absence or very less concentration of surfactant and easily converts into the dry form. So here we are exploring pickering dry emulsion system for dissolution enhancement of anti-lipemic, extremely poorly water soluble drug (Fenofibrate). Oil moiety for emulsion preparation was selected mainly on the basis of higher solubility of drug. Captex 300 was showed higher solubility for fenofibrate, hence selected as oil for emulsion. With Silica (solid stabilizer); Span 20 was selected to improve the wetting property of it. Emulsion formed by Silica and Span20 as stabilizer at the ratio 2.5:1 (silica: span 20) was found very stable at the particle size 410 nm. The prepared emulsion was further preceded for spray drying and formed microcapsule evaluated for in-vitro dissolution study, in-vivo pharmacodynamic study and characterized for DSC, XRD, FTIR, SEM, optical microscopy etc. The in vitro study exhibits significant dissolution enhancement of formulation (85 % in 45 minutes) as compared to plain drug (14 % in 45 minutes). In-vivo study (Triton based hyperlipidaemia model) exhibits significant reduction in triglyceride and cholesterol with formulation as compared to plain drug indicating increasing in fenofibrate bioavailability. DSC and XRD study exhibit loss of crystallinity of drug in microcapsule form. FTIR study exhibit chemical stability of fenofibrate. SEM and optical microscopy study exhibit spherical structure of globule coated with solid particles.

Keywords: captex 300, fenofibrate, pickering dry emulsion, silica, span20, stability, surfactant

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Authors: Alberto Sanchidrián, José A. Parra, Jesús Alonso, Julián Pecharromán, Antonia Pacios, Consuelo Huerta

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Glass is a commonly used material in building; there is not a unique design solution as plates with a different number of layers and interlayers may be used. In most façades, a security glazing have to be used according to its performance in the impact pendulum. The European Standard EN 12600 establishes an impact test procedure for classification under the point of view of the human security, of flat plates with different thickness, using a pendulum of two tires and 50 kg mass that impacts against the plate from different heights. However, this test does not replicate the actual dimensions and border conditions used in building configurations and so the real stress distribution is not determined with this test. The influence of different boundary conditions, as the ones employed in construction sites, is not well taking into account when testing the behaviour of safety glazing and there is not a detailed procedure and criteria to determinate the glass resistance against human impact. To reproduce the actual boundary conditions on site, when needed, the pendulum test is arranged to be used "in situ", with no account for load control, stiffness, and without a standard procedure. Fracture stress of small and large glass plates fit a Weibull distribution with quite a big dispersion so conservative values are adopted for admissible fracture stress under static loads. In fact, test performed for human impact gives a fracture strength two or three times higher, and many times without a total fracture of the glass plate. Newest standards, as for example DIN 18008-4, states for an admissible fracture stress 2.5 times higher than the ones used for static and wing loads. Now two working areas are open: a) to define a standard for the ‘in situ’ test; b) to prepare a laboratory procedure that allows testing with more real stress distribution. To work on both research lines a laboratory that allows to test medium size specimens with different border conditions, has been developed. A special steel frame allows reproducing the stiffness of the glass support substructure, including a rigid condition used as reference. The dynamic behaviour of the glass plate and its support substructure have been characterized with finite elements models updated with modal tests results. In addition, a new portable impact machine is being used to get enough force and direction control during the impact test. Impact based on 100 J is used. To avoid problems with broken glass plates, the test have been done using an aluminium plate of 1000 mm x 700 mm size and 10 mm thickness supported on four sides; three different substructure stiffness conditions are used. A detailed control of the dynamic stiffness and the behaviour of the plate is done with modal tests. Repeatability of the test and reproducibility of results prove that procedure to control both, stiffness of the plate and the impact level, is necessary.

Keywords: glass plates, human impact test, modal test, plate boundary conditions

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Authors: Marivane Turim Koschevic, Maycon dos Santos, Marcello Lima Bertuci, Farayde Matta Fakhouri, Silvia Maria Martelli

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Natural fibers are rich raw materials in cellulose and abundant in the world, its use for the cellulose nanocrystals extraction is promising as an example cited is the cattail, macrophyte native weed in South America. This study deals with the pre-treatment cattail of crushed fibers, at six different methods of mercerization, followed by the use of bleaching. As a result, have found The positive effects of treating fibers by means of optical microscopy and spectroscopy, Fourier transform (FTIR). The sample selected for future testing of cellulose nanocrystals extraction was treated in 2.5% NaOH for 2 h, 60 °C in the first stage and 30vol H2O2, NaOH 5% in the proportion 30/70% (v/v) for 1 hour 60 °C, followed by treatment at 50/50% (v/v) 15 minutes, 50°C, with the same constituents of the solution.

Keywords: cellulose nanocrystal, chemical treatment, mercerization, natural fibers

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Authors: Duygu Çimen, Nilay Bereli, Adil Denizli

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In this study is to synthesis magnetic nanoparticles for purify protein C. For this aim, N-Methacryloyl-(L)-histidine methyl ester (MAH) containing 2-hydroxyethyl methacrylate (HEMA) based magnetic nanoparticles were synthesized by using micro-emulsion polymerization technique for templating protein C via metal chelation. The obtained nanoparticles were characterized with Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), zeta-size analysis and electron spin resonance (ESR) spectroscopy. After that, they were used for protein C purification from aqueous solution to evaluate/optimize the adsorption condition. Hereby, the effecting factors such as concentration, pH, ionic strength, temperature, and reusability were evaluated. As the last step, protein C was determined with sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

Keywords: immobilized metal affinity chromatography (IMAC), magnetic nanoparticle, protein C, hydroxyethyl methacrylate (HEMA)

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Authors: Xiaoling Ren, Guidong Yang

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Ammonia, as one of the largest-volume industrial chemicals, is mostly produced by century-old Haber-Bosch process with extreme conditionsand high-cost. Under the circumstance, researchersarededicated in finding new ways to replace the Haber-Bosch process. Photocatalytic nitrogen fixation is a promising sustainable, clear and green strategy for ammonia synthesis, butit is still a big challenge due to the high activation energy for nitrogen. It is essential to develop an efficient photocatalyst for making this approach industrial application. Constructing chemisorption active sites through defect engineering can be defined as an effective and reliable means to improve nitrogen activation by forming the extraordinary coordination environment and electronic structure. Besides, the construction of three-dimensionally orderdmacroporous (3DOM) structured photocatalyst is considered to be one of effectivestrategiesto improve the activity due to it canincrease the diffusion rate of reactants in the interior, which isbeneficial to the mass transfer process of nitrogen molecules in photocatalytic nitrogen reduction. Herein, Fe doped 3DOM WO₃(Fe-3DOM WO₃) without noble metal cocatalysts is synthesized by a polystyrene-template strategy, which is firstly used for photocatalytic nitrogen fixation. To elucidate the chemical nature of the dopant, the X-ray diffraction (XRD) analysiswas conducted. The pure 3DOM WO₃ has a monoclinic type crystal structure. And no additional peak is observed in Fe doped 3DOM WO₃, indicating that the incorporation of Fe atoms did not result in a secondary phase formation. In order to confirm the morphologies of Fe-3DOM WO₃and 3DOM WO₃, scanning electron microscopy (SEM) was employed. The synthesized Fe-3DOM WO₃and 3DOM WO₃ both exhibit a highly ordered three dimensional inverse opal structure with interconnected pores. From high-resolution TEM image of Fe-3DOM WO₃, the ordered lattice fringes with a spacing of 3.84 Å can be assigned to the (001) plane of WO₃, which is consistent with the XRD results. Finally, the photocatalytic nitrogen reduction performance of 3DOM WO₃ and Fe doped 3DOM WO₃with various Fe contents were examined. As a result, both Fe-3DOM WO₃ samples achieve higher ammonia production rate than that of pure 3DOM WO₃, indicating that the doped Fe plays a critical role in the photocatalytic nitrogen fixation performance. To verify the reaction process upon N2 reduction on the Fe-3DOM WO₃, in-situ diffuse reflectance infrared Fourier-transform spectroscopy was employed to monitor the intermediates. The in-situ DRIFTS spectra of Fe-3DOM WO₃ exhibit the increased signals with the irradiation time from 0–60min in the N2 atmosphere. The above results prove that nitrogen is gradually hydrogenated to produce ammonia over Fe-3DOM WO₃. Thiswork would enrich our knowledge in designing efficient photocatalystsfor photocatalytic nitrogen reduction.

Keywords: ammonia, photocatalytic, nitrogen fixation, Fe doped 3DOM WO₃

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Authors: Tallal Abdel Karim Bouzir, Nourdinne Zemmouri, Djihed Berkouk

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In this research, a quantitative assessment of the urban sound environment of the city of Biskra, Algeria, was conducted. To determine the quality of the soundscape based on in-situ measurement, using a Landtek SL5868P sound level meter in 47 points, which have been identified to represent the whole city. The result shows that the urban noise level varies from 55.3 dB to 75.8 dB during the weekdays and from 51.7 dB to 74.3 dB during the weekend. On the other hand, we can also note that 70.20% of the results of the weekday measurements and 55.30% of the results of the weekend measurements have levels of sound intensity that exceed the levels allowed by Algerian law and the recommendations of the World Health Organization. These very high urban noise levels affect the quality of life, the acoustic comfort and may even pose multiple risks to people's health.

Keywords: road traffic, noise pollution, sound intensity, public health

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Authors: O. Hanita, S. A. Ainnul Hamidah, A. H. Yang Zalila, M. R. Siti Nadiah, M. H. Najihah, M. A. Hapipah

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The crude extract of the leaves of Actinodaphne sesquipedalis Hook. F. Var. Glabra (Kochummen), was taken under phytochemical investigation. The crude methanolic extract was partitioned with a different solvent system by increasing their polarities (n-hexane, dichloromethane, and methanol). The compounds were fractionated and isolated from n-hexane partition by using column chromatography with silica gel 60 or Sephadex LH-20 as a stationary phase and preparative thin layer chromatographic technique. Isolates were characterized using TLC, FTIR, UV spectrophotometer and NMR spectroscopy. The n-hexane fractionates yielded a total of four compounds namely N-methyllaurotetanine (1), dicentrine (2), β-sitosterol (3), and stigmasterol (4). The result indicates that the leaves of Actinodaphne sesquipedalis may provide a rich source of alkaloids and triterpenoids.

Keywords: actinodaphne sesquipedalis, alkaloids, phytochemical investigation, triterpenoids

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Authors: Ayla Roberta Galaco, Juliana Fonseca De Lima, Osvaldo Antonio Serra

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Coordination polymers, also known as metal-organic frameworks (MOFs) or lanthanoide organic frameworks (LOFs) have been reported due of their promising applications in gas storage, separation, catalysis, luminescence, magnetism, drug delivery, and so on. As a type of organic–inorganic hybrid materials, the properties of coordination polymers could be chosen by deliberately selecting the organic and inorganic components. LOFs have received considerable attention because of their properties such as porosity, luminescence, and magnetism. Methods such as solvothermal synthesis are important as a strategy to control the structural and morphological properties as well as the composition of the target compounds. In this work the first solvothermal synthesis was employed to obtain the compound [Y0.4,Yb0.4,Er0.2(dmf)(for)(H2O)(tft)], by using terephthalic acid (tft) and oxalic acid, decomposed in formate (for), as ligands; Yttrium, Ytterbium and, Erbium as metal centers, in DMF and water for 4 days under 160 °C. The semi-rigid terephthalic acid (dicarboxylic) coordinates with Ln3+ ions and also is possible to form a polyfunctional bridge. On the other hand, oxalate anion has no high-energy vibrational groups, which benefits the excitation of Yb3+ in upconversion process. It was observed that the compounds with water molecules in the coordination sphere of the lanthanoide ions cause lower crystalline properties and change the structure of the LOF (1D, 2D, 3D). In the FTIR, the bands at 1589 and 1500 cm-1 correspond to the asymmetric stretching vibration of –COO. The band at 1383 cm-1 is assigned to the symmetric stretching vibration of –COO. Single crystal X-ray diffraction study reveals an infinite 3D coordination framework that crystalizes in space group P21/c. The other three products, [TR(chel)(ofd)0,5(H2O)2], where TR= Eu3+, Y3, and Yb3+/Er3+ were obtained by using 1, 2-phenylenedioxydiacetic acid (ofd) and chelidonic acid (chel) as organic ligands. Thermal analysis shows that the lanthanoide organic frameworks do not collapse at temperatures below 250 °C. By the polycrystalline X-ray diffraction patterns (PXRD) it was observed that the compounds with Eu3+, Y3+, and Yb3+/Er3+ ions are isostructural. From PXRD patterns, high crystallinity can be noticed for the complexes. The final products were characterized by single X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), energy dispersive spectroscopy (EDS) and thermogravimetric analysis (TGA). The X-ray diffraction (XRD) is an effective method to investigate crystalline properties of synthesized materials. The solid crystal obtained in the synthesis show peaks at 2θ < 10°, indicating the MOF formation. The chemical composition of LOFs was also confirmed by EDS.

Keywords: isostructural, lanthanoids, lanthanoids organic frameworks (LOFs), metal organic frameworks (MOFs), thermogravimetry, X-Ray diffraction

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Authors: Adriana Garcia G., Alberto A. Escobar P., Amira D. Calvo L., Gabriel Lizama U., Alejandro Zepeda P., Fernando Martínez B., Susana Rincón A.

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Different studies have recently been focused on the use of antioxidants such as polyphenols because of to its anticarcinogenic capacity. However, these compounds are highly sensible to environmental factors such as light and heat, so lose its long-term stability, besides possess an astringent and bitter taste. Nevertheless, the polyphenols can be protected by microcapsule formulation. In this sense, a rich source of polyphenols is sorghum, besides presenting a high starch content. Due to the above, the aim of this work was to obtain modified starches from sorghum by extrusion to encapsulate polyphenols the sorghum by spray drying. Polyphenols were extracted by ethanol solution from sorghum (Pajarero/red) and determined by the method of Folin-Ciocalteu, obtaining GAE at 30 mg/g. Moreover, was extracted starch of sorghum (Sinaloense/white) through wet milling (yield 32 %). The hydrolyzed starch was modified with three treatments: acetic anhydride (2.5g/100g), sodium tripolyphosphate (4g/100g), and sodium tripolyphosphate/ acetic anhydride (2g/1.25g by each 100 g) by extrusion. Processing conditions of extrusion were as follows: barrel temperatures were of 60, 130 and 170 °C at the feeding, transition, and high-pressure extrusion zones, respectively. Analysis of Fourier Transform Infrared spectroscopy (FTIR), showed bands exhibited of acetyl groups (1735 cm-1) and phosphates (1170 cm-1, 910 cm-1 and 525 cm-1), indicating the respective modification of starch. Besides, all modified starches not developed viscosity, which is a characteristic required for use in the encapsulation of polyphenols using the spray drying technique. As result of the modification starch, was obtained a water solubility index (WSI) from 33.8 to 44.8 %, and crystallinity from 8 to 11 %, indicating the destruction of the starch granule. Afterwards, microencapsulation of polyphenols was developed by spray drying, with a blend of 10 g of modified starch, 60 ml polyphenol extract and 30 ml of distilled water. Drying conditions were as follows: inlet air temperature 150 °C ± 1, outlet air temperature 80°C ± 5. As result of the microencapsulation: were obtained yields of 56.8 to 77.4 % and an efficiency of encapsulation from 84.6 to 91.4 %. The FTIR analysis showed evidence of microcapsules loaded with polyphenols in bands 1042 cm-1, 1038 cm-1 and 1148 cm-1. Analysis Differential scanning calorimetry (DSC) showed transition temperatures from 144.1 to 173.9 °C. For the order hand, analysis of Scanning Electron Microscopy (SEM), were observed rounded surfaces with concavities, typical feature of microcapsules produced by spray drying, how result of rapid evaporation of water. Finally, the modified starches were obtained by extrusion with good characteristics for use as cover materials by spray drying, where the phosphorylated starch was the best treatment in this work, according to the encapsulation yield, efficiency, and transition temperature.

Keywords: encapsulation, extrusion, modified starch, polyphenols, spray drying

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Authors: Muhammad Bello Ibrahim, M. Auwal Zakari, Aliyu Usman

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Hybrid concrete construction (HCC) combines all the benefits of pre-casting with the advantages of cast in-situ construction. Merging the two, as a hybrid structure, results in even greater construction speed, value, and the overall economy. Its variety of uses has gained popularity in the United States and in Europe due to its distinctive benefits. However, the increase of its application in some countries (including Nigeria) has been relatively slow. Several researches have shown that hybrid construction offers an ultra-high performance concrete that offers superior strength, durability and aesthetics with design flexibility and within sustainability credentials, based on the available and economically visible technologies. This paper examines and documents the criterion that will help inform the process of deciding whether or not to adopt hybrid concrete construction (HCC) technology rather than more traditional alternatives. It also the present situation of design, construction and research on hybrid structures.

Keywords: hybrid concrete construction, Nigeria, sustainable infrastructure development, design flexibility

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Authors: Pallab Bhattacharya, C. K. Das

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Development of microwave absorbing material is a growing field of research in both the commercial and defense sector, and also to enrich the field of stealth technology. The recent work is attentive to the preparation of nanocomposite based on acid modified MWCNT, hexagonal shaped magnetic M-type hexaferrite (CuFe10Al2O19) and polyaniline. CuFe10Al2O19 was prepared by a facile chemical co-precipitation method. An in-situ approach was employed for the coating of polyaniline on MWCNT/CuFe10Al2O19 nanocomposite. The final fabrication of this nanocomposite for microwave measurements was done suitably in the matrix of thermoplastic polyurethane with 10% filler content. The nanocomposites showed the maximum reflection loss of -60.2 dB (in X-band) at the thickness of 2.5 mm with a broad absorption range in contrast to the pristine MWCNT and CuFe10Al2O19. Addition of PANI improves the microwave absorption property of the nanocomposites. The thermal stability of the prepared nanocomposites is also very high.

Keywords: magnetic materials, microwave absorption, MWCNT, nanocomposites

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Authors: A. D. Rao, Sachiko Mohanty, R. Gayathri, V. Ranga Rao

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Modeling on coupled physical and biogeochemical processes of coastal waters is vital to identify the primary production status under different natural and anthropogenic conditions. About 7, 500 km length of Indian coastline is occupied with number of semi enclosed coastal bodies such as estuaries, inlets, bays, lagoons, and other near shore, offshore shelf waters, etc. This coastline is also rich in wide varieties of ecosystem flora and fauna. Directly/indirectly extensive domestic and industrial sewage enter into these coastal water bodies affecting the ecosystem character and create environment problems such as water quality degradation, hypoxia, anoxia, harmful algal blooms, etc. lead to decline in fishery and other related biological production. The present study is focused on the southeast coast of India, starting from Pulicat to Gulf of Mannar, which is rich in marine diversity such as lagoon, mangrove and coral ecosystem. Three dimensional Massachusetts Institute of Technology general circulation model (MITgcm) along with Darwin biogeochemical module is configured for the western Bay of Bengal (BoB) to study the biogeochemistry over this region. The biogeochemical module resolves the cycling of carbon, phosphorous, nitrogen, silica, iron and oxygen through inorganic, living, dissolved and particulate organic phases. The model domain extends from 4°N-16.5°N and 77°E-86°E with a horizontal resolution of 1 km. The bathymetry is derived from General Bathymetric Chart of the Oceans (GEBCO), which has a resolution of 30 sec. The model is initialized by using the temperature, salinity filed from the World Ocean Atlas (WOA2013) of National Oceanographic Data Centre with a resolution of 0.25°. The model is forced by the surface wind stress from ASCAT and the photosynthetically active radiation from the MODIS-Aqua satellite. Seasonal climatology of nutrients (phosphate, nitrate and silicate) for the southwest BoB region are prepared using available National Institute of Oceanography (NIO) in-situ data sets and compared with the WOA2013 seasonal climatology data. The model simulations with the two different initial conditions viz., WOA2013 and the generated NIO climatology, showed evident changes in the concentration and the evolution of the nutrients in the study region. It is observed that the availability of nutrients is more in NIO data compared to WOA in the model domain. The model simulated primary productivity is compared with the spatially distributed satellite derived chlorophyll data and at various locations with the in-situ data. The seasonal variability of the model simulated primary productivity is also studied.

Keywords: Bay of Bengal, Massachusetts Institute of Technology general circulation model, MITgcm, biogeochemistry, primary productivity

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Authors: Thirawudh Pongprayoon, Watcharin Rassamee

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Silica-filled natural rubber compounds were prepared from unmodified and surface-modified silica. The modified silica was coated by ultrathin film of polyisoprene by admicellar polymerization. FTIR and SEM were applied to characterize the modified silica. The cure, mechanic, and dynamics properties were investigated with the comparison of the compounds. Cure characterization of modified silica rubber compound was shorter than that of unmodified silica compound. Strength and abrasion resistance of modified silica compound were better than those of unmodified silica rubber compound. Wet grip and rolling resistance analyzed by DMA from tanδ at 0°C and 60°C using 5 Hz were also better than those of unmodified silica rubber compound.

Keywords: silica, admicellar polymerization, rubber compounds, mechanical properties, dynamic properties

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