Search results for: in-situ laser raman spectroscopy
Commenced in January 2007
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Edition: International
Paper Count: 2851

Search results for: in-situ laser raman spectroscopy

421 Oil-Oil Correlation Using Polar and Non-Polar Fractions of Crude Oil: A Case Study in Iranian Oil Fields

Authors: Morteza Taherinezhad, Ahmad Reza Rabbani, Morteza Asemani, Rudy Swennen

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Oil-oil correlation is one of the most important issues in geochemical studies that enables to classify oils genetically. Oil-oil correlation is generally estimated based on non-polar fractions of crude oil (e.g., saturate and aromatic compounds). Despite several advantages, the drawback of using these compounds is their susceptibility of being affected by secondary processes. The polar fraction of crude oil (e.g., asphaltenes) has similar characteristics to kerogen, and this structural similarity is preserved during migration, thermal maturation, biodegradation, and water washing. Therefore, these structural characteristics can be considered as a useful correlation parameter, and it can be concluded that asphaltenes from different reservoirs with the same genetic signatures have a similar origin. Hence in this contribution, an integrated study by using both non-polar and polar fractions of oil was performed to use the merits of both fractions. Therefore, five oil samples from oil fields in the Persian Gulf were studied. Structural characteristics of extracted asphaltenes were investigated by Fourier transform infrared (FTIR) spectroscopy. Graphs based on aliphatic and aromatic compounds (predominant compounds in asphaltenes structure) and sulphoxide and carbonyl functional groups (which are representatives of sulphur and oxygen abundance in asphaltenes) were used for comparison of asphaltenes structures in different samples. Non-polar fractions were analyzed by GC-MS. The study of asphaltenes showed the studied oil samples comprise two oil families with distinct genetic characteristics. The first oil family consists of Salman and Reshadat oil samples, and the second oil family consists of Resalat, Siri E, and Siri D oil samples. To validate our results, biomarker parameters were employed, and this approach completely confirmed previous results. Based on biomarker analyses, both oil families have a marine source rock, whereby marl and carbonate source rocks are the source rock for the first and the second oil family, respectively.

Keywords: biomarker, non-polar fraction, oil-oil correlation, petroleum geochemistry, polar fraction

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420 Advanced Bio-Composite Materials Based on Biopolymer Blends and Cellulose Nanocrystals

Authors: Zineb Kassab, Nassima El Miri, A. Aboulkas, Abdellatif Barakat, Mounir El Achaby

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Recently, more attention has been given to biopolymers with a focus on sustainable development and environmental preservation. Following this tendency, the attempt has been made to replace polymers derived from petroleum with superior biodegradable polymers (biopolymers). In this context, biopolymers are considered potential replacements for conventional plastic materials. However, some of their properties must be improved for better competitiveness, especially regarding their mechanical, thermal and barrier properties. Bio-nanocomposite technology using nanofillers has already been proven as an effective way to produce new materials with specific properties and high performances. With the emergence of nanostructured bio-composite materials, incorporating elongated rod-like cellulose nanocrystals (CNC) has attracted more and more attention in the field of nanotechnology. This study is aimed to develop bio-composite films of biopolymer matrices [Carboxymethyle cellulose (CMC), Starch (ST), Chitosan (CS) and Polyvinyl alcohol (PVA)] reinforced with cellulose nanocrystals (CNC) using the solution casting method. The CNC were extracted at a nanometric scale from lignocellulosic fibers via sulfuric acid hydrolysis and then characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), confocal microscopy, infrared spectroscopy (IR), atomic force and transmission electron microscopies (AFM and TEM) techniques. The as extracted CNC were used as a reinforcing phase to produce a variety of bio-composite films at different CNC loading (0.5-10 wt %) with specific properties. The rheological properties of film-forming solutions (FFS) of bio-composites were studied, and their relation to the casting process was evaluated. Then, the structural, optical transparency, water vapor permeability, thermal stability and mechanical properties of all prepared bio-composite films were evaluated and studied in this report. The high performances of these bio-composite films are expected to have potential in biomaterials or packaging applications.

Keywords: biopolymer composites, cellulose nanocrystals, food packaging, lignocellulosic fibers

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419 Evaluation of Chitin Filled Epoxy Coating for Corrosion Protection of Q235 Steel in Saline Environment

Authors: Innocent O. Arukalam, Emeka E. Oguzie

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Interest in the development of eco-friendly anti-corrosion coatings using bio-based renewable materials is gaining momentum recently. To this effect, chitin biopolymer, which is non-toxic, biodegradable, and inherently possesses anti-microbial property, was successfully synthesized from snail shells and used as a filler in the preparation of epoxy coating. The chitin particles were characterized with contact angle goniometer, scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectrophotometer, and X-ray diffractometer (XRD). The performance of the coatings was evaluated by immersion and electrochemical impedance spectroscopy (EIS) tests. Electronic structure properties of the coating ingredients and molecular level interaction of the corrodent and coated Q235 steel were appraised by quantum chemical computations (QCC) and molecular dynamics (MD) simulation techniques, respectively. The water contact angle (WCA) measurement of chitin particles was found to be 129.3o while that of chitin particles modified with amino trimethoxy silane (ATMS) was 149.6o, suggesting it is highly hydrophobic. Immersion and EIS analyses revealed that epoxy coating containing silane-modified chitin exhibited lowest water absorption and highest barrier as well as anti-corrosion performances. The QCC showed that quantum parameters for the coating containing silane-modified chitin are optimum and therefore corresponds to high corrosion protection. The high negative value of adsorption energies (Eads) for the coating containing silane-modified chitin indicates the coating molecules interacted and adsorbed strongly on the steel surface. The observed results have shown that silane-modified epoxy-chitin coating would perform satisfactorily for surface protection of metal structures in saline environment.

Keywords: chitin, EIS, epoxy coating, hydrophobic, molecular dynamics simulation, quantum chemical computation

Procedia PDF Downloads 98
418 A Method against Obsolescence of Three-Dimensional Archaeological Collection. Two Cases of Study from Qubbet El-Hawa Necropolis, Aswan, Egypt

Authors: L. Serrano-Lara, J.M Alba-Gómez

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Qubbet el–Hawa Project has been documented archaeological artifacts as 3d models by laser scanning technique since 2015. Currently, research has obtained the right methodology to develop a high accuracy photographic texture for each geometrical 3D model. Furthermore, the right methodology to attach the complete digital surrogate into a 3DPDF document has been obtained; it is used as a catalogue worksheet that brings archaeological data and, at the same time, allows us to obtain precise measurements, volume calculations and cross-section mapping of each scanned artifact. This validated archaeological documentation is the first step for dissemination, application as Qubbet el-Hawa Virtual Museum, and, moreover, multi-sensory experience through 3D print archaeological artifacts. Material culture from four funerary complexes constructed in West Aswan has become physical replicas opening the archaeological research process itself and offering creative possibilities on museology or educational projects. This paper shares a method of acquiring texture for scanning´s output product in order to achieve a 3DPDF archaeological cataloguing, and, on the other hand, to allow the colorfully 3D printing of singular archaeological artifacts. The proposed method has undergone two concrete cases, a polychrome wooden ushabti, and, a cartonnage mask belonging to a lady, bought recovered on intact tomb QH34aa. Both 3D model results have been implemented on three main applications, archaeological 3D catalogue, public dissemination activities, and the 3D artifact model in a bachelor education program. Due to those three already mentioned applications, productive interaction among spectator and three-dimensional artifact have been increased; moreover, functionality as archaeological documentation has been consolidated. Finding the right methodology to assign a specific color to each vector on the geometric 3D model, we had been achieved two essential archaeological applications. Firstly, 3DPDF as a display document for an archaeological catalogue, secondly, the possibility to obtain a colored 3d printed object to be displayed in public exhibitions. Obsolescences 3D models have become updated archaeological documentation of QH43aa tomb cultural material. Therefore, Qubbet el-Hawa Project has been actualized the educational potential of its results thanks to a multi-sensory experience that arose from 3d scanned´s archaeological artifacts.

Keywords: 3D printed, 3D scanner, Middle Kingdom, Qubbet el-Hawa necropolis, virtual archaeology

Procedia PDF Downloads 141
417 Dwindling the Stability of DNA Sequence by Base Substitution at Intersection of COMT and MIR4761 Gene

Authors: Srishty Gulati, Anju Singh, Shrikant Kukreti

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The manifestation of structural polymorphism in DNA depends on the sequence and surrounding environment. Ample of folded DNA structures have been found in the cellular system out of which DNA hairpins are very common, however, are indispensable due to their role in the replication initiation sites, recombination, transcription regulation, and protein recognition. We enumerate this approach in our study, where the two base substitutions and change in temperature embark destabilization of DNA structure and misbalance the equilibrium between two structures of a sequence present at the overlapping region of the human COMT gene and MIR4761 gene. COMT and MIR4761 gene encodes for catechol-O-methyltransferase (COMT) enzyme and microRNAs (miRNAs), respectively. Environmental changes and errors during cell division lead to genetic abnormalities. The COMT gene entailed in dopamine regulation fosters neurological diseases like Parkinson's disease, schizophrenia, velocardiofacial syndrome, etc. A 19-mer deoxyoligonucleotide sequence 5'-AGGACAAGGTGTGCATGCC-3' (COMT19) is located at exon-4 on chromosome 22 and band q11.2 at the intersection of COMT and MIR4761 gene. Bioinformatics studies suggest that this sequence is conserved in humans and few other organisms and is involved in recognition of transcription factors in the vicinity of 3'-end. Non-denaturating gel electrophoresis and CD spectroscopy of COMT sequences indicate the formation of hairpin type DNA structures. Temperature-dependent CD studies revealed an unusual shift in the slipped DNA-Hairpin DNA equilibrium with the change in temperature. Also, UV-thermal melting techniques suggest that the two base substitutions on the complementary strand of COMT19 did not affect the structure but reduces the stability of duplex. This study gives insight about the possibility of existing structurally polymorphic transient states within DNA segments present at the intersection of COMT and MIR4761 gene.

Keywords: base-substitution, catechol-o-methyltransferase (COMT), hairpin-DNA, structural polymorphism

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416 Enhanced Exchange Bias in Poly-crystalline Compounds through Oxygen Vacancy and B-site Disorder

Authors: Koustav Pal, Indranil Das

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In recent times, perovskite and double perovskite (DP) systems attracts lot of interest as they provide a rich material platform for studying emergent functionalities like near-room-temperature ferromagnetic (FM) insulators, exchange bias (EB), magnetocaloric effects, colossal magnetoresistance, anisotropy, etc. These interesting phenomena emerge because of complex couplings between spin, charge, orbital, and lattice degrees of freedom in these systems. Various magnetic phenomena such as exchange bias, spin glass, memory effect, colossal magneto-resistance, etc. can be modified and controlled through antisite (B-site) disorder or controlling oxygen concentration of the material. By controlling oxygen concentration in SrFe0.5Co0.5O3 – δ (SFCO) (δ ∼ 0.3), we achieve intrinsic exchange bias effect with a large exchange bias field (∼1.482 Tesla) and giant coercive field (∼1.454 Tesla). Now we modified the B-site by introducing 10% iridium in the system. This modification give rise to the exchange bias field as high as 1.865 tesla and coercive field 1.863 tesla. Our work aims to investigate the effect of oxygen deficiency and B-site effect on exchange bias in oxide materials for potential technological applications. Structural characterization techniques including X-ray diffraction, scanning tunneling microscopy, and transmission electron microscopy were utilized to determine crystal structure and particle size. X-ray photoelectron spectroscopy was used to identify valence states of the ions. Magnetic analysis revealed that oxygen deficiency resulted in a large exchange bias due to a significant number of ionic mixtures. Iridium doping was found to break interaction paths, resulting in various antiferromagnetic and ferromagnetic surfaces that enhance exchange bias.

Keywords: coercive field, disorder, exchange bias, spin glass

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415 Inhibition Effect of Natural Junipers Extract towards Steel Corrosion in HCl Solution

Authors: L. Bammou, M. Belkhaouda R. Salghi, L. Bazzi, B. Hammouti

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Steel and steel-based alloys of different grades steel are extensively used in numerous applications where acid solutions are widely applied such as industrial acid pickling, industrial acid cleaning and oil-well acidizing. The use of chemical inhibitors is one of the most practical methods for the protection against corrosion in acidic media. Most of the excellent acid inhibitors are organic compounds containing nitrogen, oxygen, phosphorus and sulphur. The use of non-toxic inhibitors called green or eco-friendly environmental inhibitors is one of the solutions possible to prevent the corrosion of the material. These advantages have incited us to draw a large part of program of our laboratory to examine natural substances as corrosion inhibitors such as: prickly pear seed oil, Argan oil, Argan extract, Fennel oil, Rosemary oil, Thymus oil, Lavender oil, Jojoba oil, Pennyroyal Mint oil, and Artemisia. In the present work, we investigate the corrosion inhibition of steel in 1 M HCl by junipers extract using weight loss, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) methods. The result obtained of junipers extract (JE) shows excellent inhibition properties for the corrosion of C38 steel in 1M HCl at 298K, and the inhibition efficiency increases with increasing of the JE concentration. The inhibitor efficiencies determined by weight loss, Tafel polarisation and EIS methods are in reasonable agreement. Based on the polarisation results, the investigated junipers extract can be classified as mixed inhibitor. The calculated structural parameters show increase of the obtained Rct values and decrease of the capacitance, Cdl, with JE concentration increase. It is suggested to attribute this to the increase of the thickness of the adsorption layer at steel surface. The adsorption model obeys to the Langmuir adsorption isotherm. The adsorption process is a spontaneous and exothermic process.

Keywords: corrosion inhibition, steel, friendly inhibitors, Tafel polarisation

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414 Synthesis, Characterization, Optical and Photophysical Properties of Pyrene-Labeled Ruthenium(Ii) Trisbipyridine Complex Cored Dendrimers

Authors: Mireille Vonlanthen, Pasquale Porcu, Ernesto Rivera

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Dendritic macromolecules are presenting unique physical and chemical properties. One of them is the faculty of transferring energy from a donor moiety introduced at the periphery to an acceptor moiety at the core, mimicking the antenna effect of the process of photosynthesis. The mechanism of energy transfer is based on the Förster resonance energy exchange and requires some overlap between the emission spectrum of the donor and the absorption spectrum of the acceptor. Since it requires a coupling of transition dipole but no overlap of the physical wavefunctions, the energy transfer by Förster mechanism can occur over quite long distances from 1 to a maximum of 10 nm. However, the efficiency of the transfer depends strongly on distance. The Förster radius is the distance at which 50% of the donor’s emission is deactivated by FRET. In this work, we synthesized and characterized a novel series of dendrimers bearing pyrene moieties at the periphery and a Ru (II) complex at the core. The optical and photophysical properties of these compounds were studied by absorption and fluorescence spectroscopy. Pyrene is a well-studied chromophore that has the particularity to present monomer as well as excimer fluorescence emission. The coordination compounds of Ru (II) are red emitters with low quantum yield and long excited lifetime. We observed an efficient singulet to singulet energy transfer in such constructs. Moreover, it is known that the energy of the MLCT emitting state of Ru (II) can be tuned to become almost isoenegetic with respect to the triplet state of pyrene, leading to an extended phosphorescence lifetime. Using dendrimers bearing pyrene moieties as ligands for Ru (II), we could combine the antenna effect of dendrimers as well as its protection effect to the quenching by dioxygen with lifetime increase due to triplet-triplet equilibrium.

Keywords: dendritic molecules, energy transfer, pyrene, ru-trisbipyridine complex

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413 A Semi-Automated GIS-Based Implementation of Slope Angle Design Reconciliation Process at Debswana Jwaneng Mine, Botswana

Authors: K. Mokatse, O. M. Barei, K. Gabanakgosi, P. Matlhabaphiri

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The mining of pit slopes is often associated with some level of deviation from design recommendations, and this may translate to associated changes in the stability of the excavated pit slopes. Therefore slope angle design reconciliations are essential for assessing and monitoring compliance of excavated pit slopes to accepted slope designs. These associated changes in slope stability may be reflected by changes in the calculated factors of safety and/or probabilities of failure. Reconciliations of as-mined and slope design profiles are conducted periodically to assess the implications of these deviations on pit slope stability. Currently, the slope design reconciliation process being implemented in Jwaneng Mine involves the measurement of as-mined and design slope angles along vertical sections cut along the established geotechnical design section lines on the GEOVIA GEMS™ software. Bench retentions are calculated as a percentage of the available catchment area, less over-mined and under-mined areas, to that of the designed catchment area. This process has proven to be both tedious and requires a lot of manual effort and time to execute. Consequently, a new semi-automated mine-to-design reconciliation approach that utilizes laser scanning and GIS-based tools is being proposed at Jwaneng Mine. This method involves high-resolution scanning of targeted bench walls, subsequent creation of 3D surfaces from point cloud data and the derivation of slope toe lines and crest lines on the Maptek I-Site Studio software. The toe lines and crest lines are then exported to the ArcGIS software where distance offsets between the design and actual bench toe lines and crest lines are calculated. Retained bench catchment capacity is measured as distances between the toe lines and crest lines on the same bench elevations. The assessment of the performance of the inter-ramp and overall slopes entails the measurement of excavated and design slope angles along vertical sections on the ArcGIS software. Excavated and design toe-to-toe or crest-to-crest slope angles are measured for inter-ramp stack slope reconciliations. Crest-to-toe slope angles are also measured for overall slope angle design reconciliations. The proposed approach allows for a more automated, accurate, quick and easier workflow for carrying out slope angle design reconciliations. This process has proved highly effective and timeous in the assessment of slope performance in Jwaneng Mine. This paper presents a newly proposed process for assessing compliance to slope angle designs for Jwaneng Mine.

Keywords: slope angle designs, slope design recommendations, slope performance, slope stability

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412 Influence of the Adsorption of Anionic–Nonionic Surfactants/Silica Nanoparticles Mixture on Clay Rock Minerals in Chemical Enhanced Oil Recovery

Authors: C. Mendoza Ramírez, M. Gambús Ordaz, R. Mercado Ojeda.

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Chemical solutions flooding with surfactants, based on their property of reducing the interfacial tension between crude oil and water, is a potential application of chemical enhanced oil recovery (CEOR), however, the high-rate retention of surfactants associated with adsorption in the porous medium and the complexity of the mineralogical composition of the reservoir rock generates a limitation in the efficiency of displacement of crude oil. This study evaluates the effect of the concentration of a mixture of anionic-non-ionic surfactants with silica nanoparticles, in a rock sample composed of 25.14% clay minerals of the kaolinite, chlorite, halloysite and montmorillonite type, according to the results of X-Ray Diffraction analysis and Scanning Electron Spectrometry (XRD and SEM, respectively). The amount of the surfactant mixture adsorbed on the clay rock minerals was analyzed from the construction of its calibration curve and the 4-Region Isotherm Model in a UV-Visible spectroscopy. The adsorption rate of the surfactant in the clay rock averages 32% across all concentrations, influenced by the presence of the surface area of the substrate with a value of 1.6 m2/g and by the mineralogical composition of the clay that increases the cation exchange capacity (CEC). In addition, on Region I and II a final concentration measurement is not evident in the UV-VIS, due to its ionic nature, its high affinity with the clay rock and its low concentration. Finally, for potential CEOR applications, the adsorption of these mixed surfactant systems is considered due to their industrial relevance and it is concluded that it is possible to use concentrations in Region III and IV; initially the adsorption has an increasing slope and then reaches zero in the equilibrium where interfacial tension values are reached in the order of x10-1 mN/m.

Keywords: anionic–nonionic surfactants, clay rock, adsorption, 4-region isotherm model, cation exchange capacity, critical micelle concentration, enhanced oil recovery

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411 Measurement of Radon Exhalation Rate, Natural Radioactivity, and Radiation Hazard Assessment in Soil Samples from the Surrounding Area of Kasimpur Thermal Power Plant Kasimpur (U. P.), India

Authors: Anil Sharma, Ajay Kumar Mahur, R. G. Sonkawade, A. C. Sharma, R. Prasad

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In coal fired thermal power stations, large amount of fly ash is produced after burning of coal. Fly ash is spread and distributed in the surrounding area by air and may be deposited on the soil of the region surrounding the power plant. Coal contains increased levels of these radionuclides and fly ash may increase the radioactivity in the soil around the power plant. Radon atoms entering into the pore space from the mineral grain are transported by diffusion and advection through this space until they in turn decay or are released into the atmosphere. In the present study, Soil samples were collected from the region around a Kasimpur Thermal Power Plant, Kasimpur, Aligarh (U.P.). Radon activity, radon surface exhalation and mass exhalation rates were measured using “sealed can technique” using LR 115-type II nuclear track detectors. Radon activities vary from 92.9 to 556.8 Bq m-3 with mean value of 279.8 Bq m-3. Surface exhalation rates (EX) in these samples are found to vary from 33.4 to 200.2 mBq m-2 h-1 with an average value of 100.5 mBq m-2 h-1 whereas, Mass exhalation rates (EM) vary from 1.2 to 7.7 mBq kg-1 h-1 with an average value of 3.8 mBq kg-1 h-1. Activity concentrations of radionuclides were measured in these samples by using a low level NaI (Tl) based gamma ray spectrometer. Activity concentrations of 226Ra 232Th and 40K vary from 12 to 49 Bq kg-1, 24 to 49 Bq kg-1 and 135 to 546 Bq kg-1 with overall mean values of 30.3 Bq kg-1, 38.5 Bq kg-1 and 317.8 Bq kg-1, respectively. Radium equivalent activity has been found to vary from 80.0 to 143.7 Bq kg-1 with an average value of 109.7 Bq kg-1. Absorbed dose rate varies from 36.1 to 66.4 nGy h-1 with an average value of 50.4 nGy h-1 and corresponding outdoor annual effective dose varies from 0.044 to 0.081 mSv with an average value of 0.061 mSv. Values of external and internal hazard index Hex, Hin in this study vary from 0.21 to 0.38 and 0.27 to 0.50 with an average value of 0.29 and 0.37, Respectively. The results will be discussed in light of various factors.

Keywords: natural radioactivity, radium equivalent activity, absorbed dose rate, gamma ray spectroscopy

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410 Evaluation of Ficus racemosa (Moraceae) as a Potential Source for Drug Formulation Against Coccidiosis

Authors: Naveeda Akhtar Qureshi, Wajiha

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Coccidiosis is a protozoan parasitic disease of genus Eimeria. It is an avian infection causing a great economic loss of 3 billion USD per year globally. A number of anticoccidial drugs are in use however many of them have side effects and cost effective. With increase in poultry demand throughout the world there is a need of more drugs and vaccines against coccidiosis. The present study is based upon the use of F. racemosa a medicinal plant to be a potential source of anticoccidial agents. The methanolic leaves extract was fractionated by column and thin layer chromatography and got nineteen fractions. Each fraction different concentrations was evaluated for its anticoccidial properties in an invitro experiment against E. tenella, E. necatrix and E. mitis. The anticoccidial active fractions were further characterized by spectroscopy (UV-Vis, FTIR) and GC-MS analysis. The in silico molecular docking of active fractions identified compounds were carried out. Among all fractions significantly maximum sporulation inhibition efficacy was shown by F-19 (67.11±2.18) followed by F-15 (65.21±1.34) at concentration of 30mg/ml against E. tenella. The significantly highest sporozoites viability inhibition was shown by F-19 (69.23±2.11) followed by F-15 (67.14±1.52) against E. necatrix at concentration 30mg/ml. Anticoccidial active fractions 15 and 19 showed peak spectrum at 207 and 202nm respectively by UV analysis. Their FTIR analysis confirmed the presence of carboxylic acid, amines, phenols, etc. Anticoccidial active compounds like Cyclododecane methanol, oleic acid, Octadecanoic acid, etc were identified by GC-MS analysis. Identified compounds in silico molecular docking study showed that cyclododecane methanol of F-19 and oleic acid of F-15 showed highest binding affinity with target S-Adenosylmethionine synthase. Hence for further authentication in vivo anticoccidial studies are recommended.

Keywords: ficus racemosa, cluster fig, column chromatography, anticoccidial fractions, GC-MS, molecular docking., s-adenosylmethionine synthase

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409 Spherical Organic Particle (SOP) Emissions from Fixed-Bed Residential Coal-Burning Devices

Authors: Tafadzwa Makonese, Harold Annegarn, Patricia Forbes

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Residential coal combustion is one of the largest sources of carbonaceous aerosols in the Highveld region of South Africa, significantly affecting the local and regional climate. In this study, we investigated single coal burning particles emitted when using different fire-ignition techniques (top-lit up-draft vs bottom-lit up-draft) and air ventilation rates (defined by the number of air holes above and below the fire grate) in selected informal braziers. Aerosol samples were collected on nucleopore filters at the SeTAR Centre Laboratory, University of Johannesburg. Individual particles (~700) were investigated using a scanning electron microscope equipped with an energy-dispersive X-ray spectroscopy (EDS). Two distinct forms of spherical organic particles (SOPs) were identified, one less oxidized than the other. The particles were further classified into "electronically" dark and bright, according to China et al. [2014]. EDS analysis showed that 70% of the dark spherical organic particles balls had higher (~60%) relative oxygen content than in the bright SOPs. We quantify the morphology of spherical organic particles and classify them into four categories: ~50% are bare single particles; ~35% particles are aggregated and form diffusion accretion chains; 10% have inclusions; and 5% are deformed due to impaction on filter material during sampling. We conclude that there are two distinct kinds of coal burning spherical organic particles and that dark SOPs are less volatile than bright SOPs. We also show that these spherical organic particles are similar in nature and characteristics to tar balls observed in biomass combustion, and that they have the potential to absorb sunlight thereby affecting the earth’s radiative budget and climate. This study provides insights on the mixing states, morphology, and possible formation mechanisms of these organic particles from residential coal combustion in informal stoves.

Keywords: spherical organic particles, residential coal combustion, fixed-bed, aerosols, morphology, stoves

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408 Boron Nitride Nanoparticle Enhanced Prepreg Composite Laminates

Authors: Qiong Tian, Lifeng Zhang, Demei Yu, Ajit D. Kelkar

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Low specific weight and high strength is the basic requirement for aerospace materials. Fiber-reinforced epoxy resin composites are attractive materials for this purpose. Boron nitride nanoparticles (BNNPs) have good radiation shielding capacity, which is very important to aerospace materials. Herein a processing route for an advanced hybrid composite material is demonstrated by introducing dispersed BNNPs in standard prepreg manufacturing. The hybrid materials contain three parts: E-fiberglass, an aerospace-grade epoxy resin system, and BNNPs. A vacuum assisted resin transfer molding (VARTM) was utilized in this processing. Two BNNP functionalization approaches are presented in this study: (a) covalent functionalization with 3-aminopropyltriethoxysilane (KH-550); (b) non-covalent functionalization with cetyltrimethylammonium bromide (CTAB). The functionalized BNNPs were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction(XRD) and scanning electron microscope (SEM). The results showed that BN powder was successfully functionalized via the covalent and non-covalent approaches without any crystal structure change and big agglomerate particles were broken into platelet-like nanoparticles (BNNPs) after functionalization. Compared to pristine BN powder, surface modified BNNPs could result in significant improvement in mechanical properties such as tensile, flexural and compressive strength and modulus. CTAB functionalized BNNPs (CTAB-BNNPs) showed higher tensile and flexural strength but lower compressive strength than KH-550 functionalized BNNPs (KH550-BNNPs). These reinforcements are mainly attributed to good BNNPs dispersion and interfacial adhesion between epoxy matrix and BNNPs. This study reveals the potential in improving mechanical properties of BNNPs-containing composites laminates through surface functionalization of BNNPs.

Keywords: boron nitride, epoxy, functionalization, prepreg, composite

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407 Hyperspectral Imaging and Nonlinear Fukunaga-Koontz Transform Based Food Inspection

Authors: Hamidullah Binol, Abdullah Bal

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Nowadays, food safety is a great public concern; therefore, robust and effective techniques are required for detecting the safety situation of goods. Hyperspectral Imaging (HSI) is an attractive material for researchers to inspect food quality and safety estimation such as meat quality assessment, automated poultry carcass inspection, quality evaluation of fish, bruise detection of apples, quality analysis and grading of citrus fruits, bruise detection of strawberry, visualization of sugar distribution of melons, measuring ripening of tomatoes, defect detection of pickling cucumber, and classification of wheat kernels. HSI can be used to concurrently collect large amounts of spatial and spectral data on the objects being observed. This technique yields with exceptional detection skills, which otherwise cannot be achieved with either imaging or spectroscopy alone. This paper presents a nonlinear technique based on kernel Fukunaga-Koontz transform (KFKT) for detection of fat content in ground meat using HSI. The KFKT which is the nonlinear version of FKT is one of the most effective techniques for solving problems involving two-pattern nature. The conventional FKT method has been improved with kernel machines for increasing the nonlinear discrimination ability and capturing higher order of statistics of data. The proposed approach in this paper aims to segment the fat content of the ground meat by regarding the fat as target class which is tried to be separated from the remaining classes (as clutter). We have applied the KFKT on visible and nearinfrared (VNIR) hyperspectral images of ground meat to determine fat percentage. The experimental studies indicate that the proposed technique produces high detection performance for fat ratio in ground meat.

Keywords: food (ground meat) inspection, Fukunaga-Koontz transform, hyperspectral imaging, kernel methods

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406 Magnetic Nano-Composite of Self-Doped Polyaniline Nanofibers for Magnetic Dispersive Micro Solid Phase Extraction Applications

Authors: Hatem I. Mokhtar, Randa A. Abd-El-Salam, Ghada M. Hadad

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An improved nano-composite of self-doped polyaniline nanofibers and silica-coated magnetite nanoparticles were prepared and evaluated for suitability to magnetic dispersive micro solid-phase extraction. The work focused on optimization of the composite capacity to extract four fluoroquinolones (FQs) antibiotics, ciprofloxacin, enrofloxacin, danofloxacin, and difloxacin from water and improvement of composite stability towards acid and atmospheric degradation. Self-doped polyaniline nanofibers were prepared by oxidative co-polymerization of aniline with anthranilic acid. Magnetite nanopariticles were prepared by alkaline co-precipitation and coated with silica by silicate hydrolysis on magnetite nanoparticles surface at pH 6.5. The composite was formed by self-assembly by mixing self-doped polyaniline nanofibers with silica-coated magnetite nanoparticles dispersions in ethanol. The composite structure was confirmed by transmission electron microscopy (TEM). Self-doped polyaniline nanofibers and magnetite chemical structures were confirmed by FT-IR while silica coating of the magnetite was confirmed by Energy Dispersion X-ray Spectroscopy (EDS). Improved stability of the composite magnetic component was evidenced by resistance to degrade in 2N HCl solution. The adsorption capacity of self-doped polyaniline nanofibers based composite was higher than previously reported corresponding composite prepared from polyaniline nanofibers instead of self-doped polyaniline nanofibers. Adsorption-pH profile for the studied FQs on the prepared composite revealed that the best pH for adsorption was in range of 6.5 to 7. Best extraction recovery values were obtained at pH 7 using phosphate buffer. The best solvent for FQs desorption was found to be 0.1N HCl in methanol:water (8:2; v/v) mixture. 20 mL of Spiked water sample with studied FQs were preconcentrated using 4.8 mg of composite and resulting extracts were analysed by HPLC-UV method. The prepared composite represented a suitable adsorbent phase for magnetic dispersive micro-solid phase application.

Keywords: fluoroquinolones, magnetic dispersive micro extraction, nano-composite, self-doped polyaniline nanofibers

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405 Chikungunya Virus Detection Utilizing an Origami Based Electrochemical Paper Analytical Device

Authors: Pradakshina Sharma, Jagriti Narang

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Due to the critical significance in the early identification of infectious diseases, electrochemical sensors have garnered considerable interest. Here, we develop a detection platform for the chikungunya virus by rationally implementing the extremely high charge-transfer efficiency of a ternary nanocomposite of graphene oxide, silver, and gold (G/Ag/Au) (CHIKV). Because paper is an inexpensive substrate and can be produced in large quantities, the use of electrochemical paper analytical device (EPAD) origami further enhances the sensor's appealing qualities. A cost-effective platform for point-of-care diagnostics is provided by paper-based testing. These types of sensors are referred to as eco-designed analytical tools due to their efficient production, usage of the eco-friendly substrate, and potential to reduce waste management after measuring by incinerating the sensor. In this research, the paper's foldability property has been used to develop and create 3D multifaceted biosensors that can specifically detect the CHIKVX-ray diffraction, scanning electron microscopy, UV-vis spectroscopy, and transmission electron microscopy (TEM) were used to characterize the produced nanoparticles. In this work, aptamers are used since they are thought to be a unique and sensitive tool for use in rapid diagnostic methods. Cyclic voltammetry (CV) and linear sweep voltammetry (LSV), which were both validated with a potentiostat, were used to measure the analytical response of the biosensor. The target CHIKV antigen was hybridized with using the aptamer-modified electrode as a signal modulation platform, and its presence was determined by a decline in the current produced by its interaction with an anionic mediator, Methylene Blue (MB). Additionally, a detection limit of 1ng/ml and a broad linear range of 1ng/ml-10µg/ml for the CHIKV antigen were reported.

Keywords: biosensors, ePAD, arboviral infections, point of care

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404 Performance and Structural Evaluation of the Torrefaction of Bamboo under a High Gravity (Higee) Environment Using a Rotating Packed Bed

Authors: Mark Daniel De Luna, Ma. Katreena Pillejera, Wei-Hsin Chen

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The raw bamboo (Phyllostachys mankinoi), with a moisture content of 13.54 % and a higher heating value (HHV) of 17.657 MJ/kg, was subjected to torrefaction under a high gravity (higee) environment using a rotating packed bed. The performance of the higee torrefaction was explored in two parts: (1) effect of rotation and temperature and (2) effect of duration on the solid yield, HHV and energy yield. By statistical analyses, the results indicated that the rotation, temperature and their interaction has a significant effect on the three responses. Same remarks on the effect of duration where when the duration (temperature and rotation) increases, the HHV increases, while the solid yield and energy yield decreases. Graphical interpretations showed that at 300 °C, the rotating speed has no evident effect on the responses. At 30-min holding time, the highest HHV reached (28.389 MJ/kg) was obtained in the most severe torrefaction condition (the rotating speed at 1800 rpm and temperature at 300 °C) with an enhancement factor of HHV corresponding to 1.61 and an energy yield of 63.51%. Upon inspection, the recommended operating condition under a 30-min holding time is at 255 °C-1800 rpm since the enhancement factor of HHV (1.53), HHV (26.988 MJ/kg), and energy yield (65.21%) values are relatively close to that of the aforementioned torrefaction condition. The Van Krevelen diagram of the torrefied biomass showed that the ratios decrease as the torrefaction intensifies, hence improving the hydrophobicity of the product. The spreads of the results of the solid yield, enhancement factor (EF) of HHV, energy yield, and H/C and O/C ratios were in accordance with the trends of the responses. Overall, from the results presented, it can be concluded that the quality of the product from the process is at par to that of coal (i.e. HHV of coal is 21-35 MJ/kg). The Fourier transform infrared (FTIR) spectroscopy results indicated that cellulose and lignin may have been degraded at a lower temperature accompanied with a high rotating speed. The results suggested that torrefaction under higee environment indicates promising process for the utilization of bamboo.

Keywords: heat transfer, high gravity environment, FTIR, rotation, rotating speed, torrefaction

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403 Synthesis and Properties of Chitosan-Graft-Polyacrylamide/Gelatin Superabsorbent Composites for Wastewater Purification

Authors: Hafida Ferfera-Harrar, Nacera Aiouaz, Nassima Dairi

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Super absorbents polymers received much attention and are used in many fields because of their superior characters to traditional absorbents, e.g., sponge and cotton. So, it is very important but challenging to prepare highly and fast-swelling super absorbents. A reliable, efficient and low-cost technique for removing heavy metal ions from waste water is the adsorption using bio-adsorbents obtained from biological materials, such as polysaccharides-based hydrogels super absorbents. In this study, novel multi-functional super absorbent composites type semi-interpenetrating polymer networks (Semi-IPNs) were prepared via graft polymerization of acrylamide onto chitosan backbone in presence of gelatin, CTS-g-PAAm/Ge, using potassium persulfate and N,N’ -methylenebisacrylamide as initiator and cross linker, respectively. These hydrogels were also partially hydrolyzed to achieve superabsorbents with ampholytic properties and uppermost swelling capacity. The formation of the grafted network was evidenced by Fourier Transform Infrared Spectroscopy (ATR-FTIR) and thermo gravimetric Analysis (TGA). The porous structures were observed by Scanning Electron Microscope (SEM). From TGA analysis, it was concluded that the incorporation of the Ge in the CTS-g-PAAm network has marginally affected its thermal stability. The effect of gelatin content on the swelling capacities of these super absorbent composites was examined in various media (distilled water, saline and pH-solutions).The water absorbency was enhanced by adding Ge in the network, where the optimum value was reached at 2 wt. % of Ge. Their hydrolysis has not only greatly optimized their absorption capacity but also improved the swelling kinetic. These materials have also showed reswelling ability. We believe that these super-absorbing materials would be very effective for the adsorption of harmful metal ions from waste water.

Keywords: chitosan, gelatin, superabsorbent, water absorbency

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402 Calculating Asphaltenes Precipitation Onset Pressure by Using Cardanol as Precipitation Inhibitor: A Strategy to Increment the Oil Well Production

Authors: Camilo A. Guerrero-Martin, Erik Montes Paez, Marcia C. K. Oliveira, Jonathan Campos, Elizabete F. Lucas

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Asphaltenes precipitation is considered as a formation damage problem, which can reduce the oil recovery factor. It fouls piping and surface installations, as well as cause serious flow assurance complications and decline oil well production. Therefore, researchers have shown an interest in chemical treatments to control this phenomenon. The aim of this paper is to assess the asphaltenes precipitation onset of crude oils in the presence of cardanol, by titrating the crude with n-heptane. Moreover, based on this results obtained at atmosphere pressure, the asphaltenes precipitation onset pressure were calculated to predict asphaltenes precipitation in the reservoir, by using differential liberation and refractive index data of the oils. The influence of cardanol concentrations in the asphaltenes stabilization of three Brazilian crude oils samples (with similar API densities) was studied. Therefore, four formulations of cardanol in toluene were prepared: 0, 3, 5, 10 and 15 m/m%. The formulations were added to the crude at 2:98 ratio. The petroleum samples were characterized by API density, elemental analysis and differential liberation test. The asphaltenes precipitation onset (APO) was determined by titrating with n-heptane and monitoring with near-infrared (NIR). UV-Vis spectroscopy experiments were also done to assess the precipitate asphaltenes content. The asphaltenes precipitation envelopes (APE) were also determined by numerical simulation (Multiflash). In addition, the adequate artificial lift systems (ALS) for the oils were selected. It was based on the downhole well profile and a screening methodology. Finally, the oil flowrates were modelling by NODAL analysis production system in the PIPESIM software. The results of this study show that the asphaltenes precipitation onset of the crude oils were 2.2, 2.3 and 6.0 mL of n-heptane/g of oil. The cardanol was an effective inhibitor of asphaltenes precipitation for the crude oils used in this study, since it displaces the precipitation pressure of the oil to lower values. This indicates that cardanol can increase the oil wells productivity.

Keywords: asphaltenes, NODAL analysis production system, precipitation pressure onset, inhibitory molecule

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401 Understanding the Impact of Li- bis(trifluoromethanesulfonyl)imide Doping on Spiro-OMeTAD Properties and Perovskite Solar Cell Performance

Authors: Martin C. Eze, Gao Min

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Lithium bis(trifluoromethanesulfonyl)imide (Li-TFSI) dopant is beneficial in improving the properties of 2,2′,7,7′-Tetrakis (N, N-di-p-methoxyphenylamino)-9,9′-spiro-bifluorene (Spiro-OMETAD) transport layer used in perovskite solar cells (PSCs). Properties such as electrical conductivity, band energy mismatch, and refractive index of Spiro-OMETAD layers are believed to play key roles in PSCs performance but only the dependence of electrical conductivity on Li-TFSI doping has been extensively studied. In this work, the effect of Li-TFSI doping level on highest occupied molecular orbital (HOMO) energy, electrical conductivity, and refractive index of Spiro-OMETAD film and PSC performance was demonstrated. The Spiro-OMETAD films were spin-coated at 4000 rpm for 30 seconds from solutions containing 73.4 mM of Spiro-OMeTAD, 23.6 mM of 4-tert-butylpyridine, 7.6 mM of tris(2-(1H-pyrazol-1-yl)-4-tert-butylpyridine) cobalt(III) tri[bis(trifluoromethane) sulfonimide] (FK209) dopant and Li-TFSI dopant varying from 37 to 62 mM in 1 ml of chlorobenzene. From ultraviolet photoelectron spectroscopy (UPS), ellipsometry, and 4-probe studies, the results show that films deposition from Spiro-OMETAD solution doped with 40 mM of Li-TFSI shows the highest electrical conductivity of 6.35×10-6 S/cm, the refractive index of 1.87 at 632.32 nm, HOMO energy of -5.22 eV and the lowest HOMO energy mismatch of 0.21 eV compared to HOMO energy of perovskite layer. The PSCs fabricated show the best power conversion efficiency, open-circuit voltage, and fill factor of 17.10 %, 1.1 V, and 70.12%, respectively, for devices based on Spiro-OMETAD solution doped with 40 mM of Li-TFSI. This study demonstrates that the optimum Spiro-OMETAD/ Li-TFSI doping ratio of 1.84 is the optimum doping level for Spiro-OMETAD layer preparation.

Keywords: electrical conductivity, homo energy mismatch, lithium bis(trifluoromethanesulfonyl)imide, power conversion efficiency, refractive index

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400 Synthesis, Characterization, and Catalytic Application of Modified Hierarchical Zeolites

Authors: A. Feliczak Guzik, I. Nowak

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Zeolites, classified as microporous materials, are a large group of crystalline aluminosilicate materials commonly used in the chemical industry. These materials are characterized by large specific surface area, high adsorption capacity, hydrothermal and thermal stability. However, the micropores present in them impose strong mass transfer limitations, resulting in low catalytic performance. Consequently, mesoporous (hierarchical) zeolites have attracted considerable attention from researchers. These materials possess additional porosity in the mesopore size region (2-50 nm according to IUPAC). Mesoporous zeolites, based on commercial MFI-type zeolites modified with silver, were synthesized as follows: 0.5 g of zeolite was dispersed in a mixture containing CTABr (template), water, ethanol, and ammonia under ultrasound for 30 min at 65°C. The silicon source, which was tetraethyl orthosilicate, was then added and stirred for 4 h. After this time, silver(I) nitrate was added. In a further step, the whole mixture was filtered and washed with water: ethanol mixture. The template was removed by calcination at 550°C for 5h. All the materials obtained were characterized by the following techniques: X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), nitrogen adsorption/desorption isotherms, FTIR spectroscopy. X-ray diffraction and low-temperature nitrogen adsorption/desorption isotherms revealed additional secondary porosity. Moreover, the structure of the commercial zeolite was preserved during most of the material syntheses. The aforementioned materials were used in the epoxidation reaction of cyclohexene using conventional heating and microwave radiation heating. The composition of the reaction mixture was analyzed every 1 h by gas chromatography. As a result, about 60% conversion of cyclohexene and high selectivity to the desired reaction products i.e., 1,2-epoxy cyclohexane and 1,2-cyclohexane diol, were obtained.

Keywords: catalytic application, characterization, epoxidation, hierarchical zeolites, synthesis

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399 Optical Assessment of Marginal Sealing Performance around Restorations Using Swept-Source Optical Coherence Tomography

Authors: Rima Zakzouk, Yasushi Shimada, Yasunori Sumi, Junji Tagami

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Background and purpose: The resin composite has become the main material for the restorations of caries in recent years due to aesthetic characteristics, especially with the development of the adhesive techniques. The quality of adhesion to tooth structures is depending on an exchange process between inorganic tooth material and synthetic resin and a micromechanical retention promoted by resin infiltration in partially demineralized dentin. Optical coherence tomography (OCT) is a noninvasive diagnostic method for obtaining cross-sectional images that produce high-resolution of the biological tissue at the micron scale. The aim of this study was to evaluate the gap formation at adhesive/tooth interface of two-step self-etch adhesives that are preceded with or without phosphoric acid pre-etching in different regions of teeth using SS-OCT. Materials and methods: Round tapered cavities (2×2 mm) were prepared in cervical part of bovine incisors teeth and divided into 2 groups (n=10): first group self-etch adhesive (Clearfil SE Bond) was applied for SE group and second group treated with acid etching before applying the self-etch adhesive for PA group. Subsequently, both groups were restored with Estelite Flow Quick Flowable Composite Resin and observed under OCT. Following 5000 thermal cycles, the same section was obtained again for each cavity using OCT at 1310-nm wavelength. Scanning was repeated after two months to monitor the gap progress. Then the gap length was measured using image analysis software, and the statistics analysis were done between both groups using SPSS software. After that, the cavities were sectioned and observed under Confocal Laser Scanning Microscope (CLSM) to confirm the result of OCT. Results: Gaps formed at the bottom of the cavity was longer than the gap formed at the margin and dento-enamel junction in both groups. On the other hand, pre-etching treatment led to damage the DEJ regions creating longer gap. After 2 months the results showed almost progress in the gap length significantly at the bottom regions in both groups. In conclusions, phosphoric acid etching treatment did not reduce the gap lrngth in most regions of the cavity. Significance: The bottom region of tooth was more exposed to gap formation than margin and DEJ regions, The DEJ damaged with phosphoric acid treatment.

Keywords: optical coherence tomography, self-etch adhesives, bottom, dento enamel junction

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398 Lightweight Ceramics from Clay and Ground Corncobs

Authors: N.Quaranta, M. Caligaris, R. Varoli, A. Cristobal, M. Unsen, H. López

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Corncobs are agricultural wastes and they can be used as fuel or as raw material in different industrial processes like cement manufacture, contaminant adsorption, chemical compound synthesis, etc. The aim of this work is to characterize this waste and analyze the feasibility of its use as a pore-forming material in the manufacture of lightweight ceramics for the civil construction industry. The characterization of raw materials is carried out by using various techniques: electron diffraction analysis X-ray, differential and gravimetric thermal analyses, FTIR spectroscopy, ecotoxicity evaluation, among others. The ground corncobs, particle size less than 2 mm, are mixed with clay up to 30% in volume and shaped by uniaxial pressure of 25 MPa, with 6% humidity, in moulds of 70mm x 40mm x 18mm. Then the green bodies are heat treated at 950°C for two hours following the treatment curves used in ceramic industry. The ceramic probes are characterized by several techniques: density, porosity and water absorption, permanent volumetric variation, loss on ignition, microscopies analysis, and mechanical properties. DTA-TGA analysis of corncobs shows in the range 20°-250°C a small loss in TGA curve and exothermic peaks at 250°-500°C. FTIR spectrum of the corncobs sample shows the characteristic pattern of this kind of organic matter with stretching vibration bands of adsorbed water, methyl groups, C–O and C–C bonds, and the complex form of the cellulose and hemicellulose glycosidic bonds. The obtained ceramic bodies present external good characteristics without loose edges and adequate properties for the market requirements. The porosity values of the sintered pieces are higher than those of the reference sample without waste addition. The results generally indicate that it is possible to use corncobs as porosity former in ceramic bodies without modifying the usual sintering temperatures employed in the industry.

Keywords: ceramic industry, biomass, recycling, hemicellulose glycosidic bonds

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397 Effects of pH, Load Capacity and Contact Time in the Sulphate Sorption onto a Functionalized Mesoporous Structure

Authors: Jaime Pizarro, Ximena Castillo

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The intensive use of water in agriculture, industry, human consumption and increasing pollution are factors that reduce the availability of water for future generations; the challenge is to advance in sustainable and low-cost solutions to reuse water and to facilitate the availability of the resource in quality and quantity. The use of new low-cost materials with sorbent capacity for pollutants is a solution that contributes to the improvement and expansion of water treatment and reuse systems. Fly ash, a residue from the combustion of coal in power plants that is produced in large quantities in newly industrialized countries, contains a high amount of silicon oxides and aluminum oxides, whose properties can be used for the synthesis of mesoporous materials. Properly functionalized, this material allows obtaining matrixes with high sorption capacity. The mesoporous materials have a large surface area, thermal and mechanical stability, uniform porous structure, and high sorption and functionalization capacities. The goal of this study was to develop hexagonal mesoporous siliceous material (HMS) for the adsorption of sulphate from industrial and mining waters. The silica was extracted from fly ash after calcination at 850 ° C, followed by the addition of water. The mesoporous structure has a surface area of 282 m2 g-1 and a size of 5.7 nm and was functionalized with ethylene diamine through of a self-assembly method. The material was characterized by Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS). The capacity of sulphate sorption was evaluated according to pH, maximum load capacity and contact time. The sulphate maximum adsorption capacity was 146.1 mg g-1, which is three times higher than commercial sorbents. The kinetic data were fitted according to a pseudo-second order model with a high coefficient of linear regression at different initial concentrations. The adsorption isotherm that best fitted the experimental data was the Freundlich model.

Keywords: fly ash, mesoporous siliceous, sorption, sulphate

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396 Characterization of Dota-Girentuximab Conjugates for Radioimmunotherapy

Authors: Tais Basaco, Stefanie Pektor, Josue A. Moreno, Matthias Miederer, Andreas Türler

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Radiopharmaceuticals based in monoclonal anti-body (mAb) via chemical linkers have become a potential tool in nuclear medicine because of their specificity and the large variability and availability of therapeutic radiometals. It is important to identify the conjugation sites and number of attached chelator to mAb to obtain radioimmunoconjugates with required immunoreactivity and radiostability. Girentuximab antibody (G250) is a potential candidate for radioimmunotherapy of clear cell carcinomas (RCCs) because it is reactive with CAIX antigen, a transmembrane glycoprotein overexpressed on the cell surface of most ( > 90%) (RCCs). G250 was conjugated with the bifunctional chelating agent DOTA (1,4,7,10-Tetraazacyclododecane-N,N’,N’’,N’’’-tetraacetic acid) via a benzyl-thiocyano group as a linker (p-SCN-Bn-DOTA). DOTA-G250 conjugates were analyzed by size exclusion chromatography (SE-HPLC) and by electrophoresis (SDS-PAGE). The potential site-specific conjugation was identified by liquid chromatography–mass spectrometry (LC/MS-MS) and the number of linkers per molecule of mAb was calculated using the molecular weight (MW) measured by matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). The average number obtained in the conjugates in non-reduced conditions was between 8-10 molecules of DOTA per molecule of mAb. The average number obtained in the conjugates in reduced conditions was between 1-2 and 3-4 molecules of DOTA per molecule of mAb in the light chain (LC) and heavy chain (HC) respectively. Potential DOTA modification sites of the chelator were identified in lysine residues. The biological activity of the conjugates was evaluated by flow cytometry (FACS) using CAIX negative (SKRC-18) and CAIX positive (SKRC-52). The DOTA-G250 conjugates were labelled with 177Lu with a radiochemical yield > 95% reaching specific activities of 12 MBq/µg. The stability in vitro of different types of radioconstructs was analyzed in human serum albumin (HSA). The radiostability of 177Lu-DOTA-G250 at high specific activity was increased by addition of sodium ascorbate after the labelling. The immunoreactivity was evaluated in vitro and in vivo. Binding to CAIX positive cells (SK-RC-52) at different specific activities was higher for conjugates with less DOTA content. Protein dose was optimized in mice with subcutaneously growing SK-RC-52 tumors using different amounts of 177Lu- DOTA-G250.

Keywords: mass spectrometry, monoclonal antibody, radiopharmaceuticals, radioimmunotheray, renal cancer

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395 Oxide Based Memristor and Its Potential Application in Analog-Digital Electronics

Authors: P. Michael Preetam Raj, Souri Banerjee, Souvik Kundu

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Oxide based memristors were fabricated in order to establish its potential applications in analog/digital electronics. BaTiO₃-BiFeO₃ (BT-BFO) was employed as an active material, whereas platinum (Pt) and Nb-doped SrTiO₃ (Nb:STO) were served as a top and bottom electrodes, respectively. Piezoelectric force microscopy (PFM) was utilized to present the ferroelectricity and repeatable polarization inversion in the BT-BFO, demonstrating its effectiveness for resistive switching. The fabricated memristors exhibited excellent electrical characteristics, such as hysteresis current-voltage (I-V), high on/off ratio, high retention time, cyclic endurance, and low operating voltages. The band-alignment between the active material BT-BFO and the substrate Nb:STO was experimentally investigated using X-Ray photoelectron spectroscopy, and it attributed to staggered heterojunction alignment. An energy band diagram was proposed in order to understand the electrical transport in BT-BFO/Nb:STO heterojunction. It was identified that the I-V curves of these memristors have several discontinuities. Curve fitting technique was utilized to analyse the I-V characteristic, and the obtained I-V equations were found to be parabolic. Utilizing this analysis, a non-linear BT-BFO memristors equivalent circuit model was developed. Interestingly, the obtained equivalent circuit of the BT-BFO memristors mimics the identical electrical performance, those obtained in the fabricated devices. Based on the developed equivalent circuit, a finite state machine (FSM) design was proposed. Efforts were devoted to fabricate the same FSM, and the results were well matched with those in the simulated FSM devices. Its multilevel noise filtering and immunity to external noise characteristics were also studied. Further, the feature of variable negative resistance was established by controlling the current through the memristor.

Keywords: band alignment, finite state machine, polarization inversion, resistive switching

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394 Improving the Corrosion Resistance of Magnesium by Application of TiO₂-MgO Coatings

Authors: Eric Noe Hernandez Rodriguez, Cristian Esneider Penuela Cruz

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Magnesium is a biocompatible and biodegradable material that has gained increased interest for application in resorbable orthopedic implants. However, to date, much research is being conducted to overcome the main disadvantage: its low corrosion resistance. In this work, we report our findings on the development and application of TiO₂-MgO coatings to improve and modulate the corrosion resistance of magnesium pieces. The plasma electrolytic oxidation (PEO) technique was employed to obtain the TiO₂-MgO coatings. The effect of the experimental parameters on the modulation of the TiO₂:MgO ratio was investigated. The most critical parameters were the chemical composition of the precursor electrolytic solution and the current density. According to scanning electron microscopy (SEM) observations, the coatings were porous; however, they become more compact as the current density increases. XRD measurements showed that the coatings are formed by a composite consisting of TiO₂ and MgO oxides, whose ratio can be changed by the experimental conditions. TiO₂ had the anatase crystalline structure, while the MgO had the FCC crystalline structure. The corrosion resistance was evaluated through the corrosion current (Icorr) measured at room temperature by the polarization technique (Tafel). For doing it, Hank's solution was used in order to simulate the body fluids. Also, immersion tests were conducted. Tafel curves showed an improvement of the corrosion resistance at some coated magnesium pieces in contrast to control pieces (uncoated). Corrosion currents were lower, and the corrosion potential changed to positive values. It was observed that the experimental parameters allowed to modulate the protective capacity of the coatings by changing the TiO₂:MgO ratio. Coatings with a higher content of TiO₂ (measured by energy dispersive spectroscopy) showed higher corrosion resistance. Results showed that TiO₂-MgO coatings can be successfully applied to improve the corrosion resistance of Mg pieces in simulated body fluid; even more, the corrosion resistance can be tuned by changing the TiO₂:MgO ratio.

Keywords: biomaterials, PEO, corrosion resistance, magnesium

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393 Development of Structural Deterioration Models for Flexible Pavement Using Traffic Speed Deflectometer Data

Authors: Sittampalam Manoharan, Gary Chai, Sanaul Chowdhury, Andrew Golding

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The primary objective of this paper is to present a simplified approach to develop the structural deterioration model using traffic speed deflectometer data for flexible pavements. Maintaining assets to meet functional performance is not economical or sustainable in the long terms, and it would end up needing much more investments for road agencies and extra costs for road users. Performance models have to be included for structural and functional predicting capabilities, in order to assess the needs, and the time frame of those needs. As such structural modelling plays a vital role in the prediction of pavement performance. A structural condition is important for the prediction of remaining life and overall health of a road network and also major influence on the valuation of road pavement. Therefore, the structural deterioration model is a critical input into pavement management system for predicting pavement rehabilitation needs accurately. The Traffic Speed Deflectometer (TSD) is a vehicle-mounted Doppler laser system that is capable of continuously measuring the structural bearing capacity of a pavement whilst moving at traffic speeds. The device’s high accuracy, high speed, and continuous deflection profiles are useful for network-level applications such as predicting road rehabilitations needs and remaining structural service life. The methodology adopted in this model by utilizing time series TSD maximum deflection (D0) data in conjunction with rutting, rutting progression, pavement age, subgrade strength and equivalent standard axle (ESA) data. Then, regression analyses were undertaken to establish a correlation equation of structural deterioration as a function of rutting, pavement age, seal age and equivalent standard axle (ESA). This study developed a simple structural deterioration model which will enable to incorporate available TSD structural data in pavement management system for developing network-level pavement investment strategies. Therefore, the available funding can be used effectively to minimize the whole –of- life cost of the road asset and also improve pavement performance. This study will contribute to narrowing the knowledge gap in structural data usage in network level investment analysis and provide a simple methodology to use structural data effectively in investment decision-making process for road agencies to manage aging road assets.

Keywords: adjusted structural number (SNP), maximum deflection (D0), equant standard axle (ESA), traffic speed deflectometer (TSD)

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392 Structural and Functional Characterization of the Transcriptional Regulator Rv1176 of Mycobacterium tuberculosis H37Rv

Authors: Vikash Yadav, Ashish Arora

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Microorganisms have self-defense mechanisms to protect themselves from toxic environments. Phenolic acid decarboxylase(pad) is responsible for the defense against toxicity caused by phenolic acids, converting them into less toxic vinyl derivatives. The transcription of the pad gene is regulated by a negative transcription factor, phenolic acid decarboxylase regulators (PadR), in a substrate-inducible manner. The PadR family members share the conserved DNA-binding features and interact with the operator DNA using a winged helix-turn-helix (wHTH) motif, which contains a three-helix motif and a β-stranded wing. The members of this family function as transcriptional regulators that are involved in various cellular survival processes, such as toxin production, detoxification, multidrug resistance, antibiotic biosynthesis, and carbon catabolism. Rv1176 of Mycobacterium tuberculosis H37Rv has been assigned to the PadR family protein that remains to be structurally and functionally uncharacterized. To reveal the structural mechanism by which Rv1176 could regulates effector-responsive transcription, several experiments were performed, including Electrophoretic Mobility Shift Assay (EMSA) for DNA protein interaction, differential scanning calorimetry (DSC) and Differential Scanning Fluorimetry (DSF) for temperature and ligand-dependent protein stability, Circular Dichroism (CD) spectroscopy for secondary structure analysis. Further, to evaluate the functional role of Rv1176, the intracellular survival of recombinant M. smegmatis was examined in murine macrophage cell line J774A.1 and different stressed conditions like oxidative, pH, and nutritive stress. All these studies demonstrated that Rv1176 could behave as a transcription regulator and its expression in recombinant M. smegmatis increases intracellular survival.

Keywords: EMSA, Mycobacterium tuberculosis, PadR family protein, transcriptional regulator

Procedia PDF Downloads 78