Search results for: in situ FTIR

Authors: Azuraida Amat, Halimah Mohamed Kamari, Che Azurahanim Che Abdullah, Ishak Mansor

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The changes of the optical and structural properties of Bismuth-Boro-Tellurite glasses pre and post gamma irradiation were studied. Six glass samples, with different compositions [(TeO2)0.7 (B2O3)0.3]1-x (Bi2O3)x prepared by melt quenching method were irradiated with 25kGy gamma radiation at room temperature. The Fourier Transform Infrared Spectroscopy (FTIR) was used to explore the structural bonding in the prepared glass samples due to exposure, while UV-VIS Spectrophotometer was used to evaluate the changes in the optical properties before and after irradiation. Gamma irradiation causes a profound changes in the peak intensity as shown by FTIR spectra which is due to the breaking of the network bonding. Before gamma irradiation, the optical band gap, Eg value decreased from 2.44 eV to 2.15 eV with the addition of Bismuth content. The value kept decreasing (from 2.18 eV to 2.00 eV) following exposure to gamma radiation due to the increase of non-bridging oxygen (NBO) and the increase of defects in the glass. In conclusion, the glass with high content of Bi2O3 (0.30Bi) give the smallest Eg and show less changes in FTIR spectra after gamma irradiation, which indicate that this glass is more resistant to gamma radiation compared to other glasses.

Keywords: boro-tellurite, bismuth, gamma radiation, optical properties

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Authors: Deepak Kumar, Jahangeer, Brijesh Kumar Yadav, Shashi Mathur

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In-situ remediation is a technique which can remediate either surface or groundwater at the site of contamination. In the present study, simulation optimization approach has been used to develop management strategy for remediating LNAPL (Light Non-Aqueous Phase Liquid) contaminated aquifers. Benzene, toluene, ethyl benzene and xylene are the main component of LNAPL contaminant. Collectively, these contaminants are known as BTEX. In in-situ bioremediation process, a set of injection and extraction wells are installed. Injection wells supply oxygen and other nutrient which convert BTEX into carbon dioxide and water with the help of indigenous soil bacteria. On the other hand, extraction wells check the movement of plume along downstream. In this study, optimal design of the system has been done using PSO (Particle Swarm Optimization) algorithm. A comprehensive management strategy for pumping of injection and extraction wells has been done to attain a maximum allowable concentration of 5 ppm and 4.5 ppm. The management strategy comprises determination of pumping rates, the total pumping volume and the total running cost incurred for each potential injection and extraction well. The results indicate a high pumping rate for injection wells during the initial management period since it facilitates the availability of oxygen and other nutrients necessary for biodegradation, however it is low during the third year on account of sufficient oxygen availability. This is because the contaminant is assumed to have biodegraded by the end of the third year when the concentration drops to a permissible level.

Keywords: groundwater, in-situ bioremediation, light non-aqueous phase liquid, BTEX, particle swarm optimization

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Authors: Lixin Zhao, Genmao Zhou

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Traditional acid in-situ leaching (ISL) is not suitable for the sandstone uranium deposit with low permeability and high content of carbonate minerals, because of the blocking of calcium sulfate precipitates. Another factor influences the uranium acid in-situ leaching is that the pyrite in ore rocks will react with oxidation reagent and produce lots of sulfate ions which may speed up the precipitation process of calcium sulphate and consume lots of oxidation reagent. Due to the advantages such as less chemical reagent consumption and groundwater pollution, CO₂+O₂ in-situ leaching method has become one of the important research areas in uranium mining. China is the second country where CO₂+O₂ ISL has been adopted in industrial uranium production of the world. It is shown that the CO₂+O₂ ISL in China has been successfully developed. The reaction principle, technical process, well field design and drilling engineering, uranium-bearing solution processing, etc. have been fully studied. At current stage, several uranium mines use CO₂+O₂ ISL method to extract uranium from the ore-bearing aquifers. The industrial application and development potential of CO₂+O₂ ISL method in China are summarized. By using CO₂+O₂ neutral leaching technology, the problem of calcium carbonate and calcium sulfate precipitation have been solved during uranium mining. By reasonably regulating the amount of CO₂ and O₂, related ions and hydro-chemical conditions can be controlled within the limited extent for avoiding the occurrence of calcium sulfate and calcium carbonate precipitation. Based on this premise, the demand of CO₂+O₂ uranium leaching has been met to the maximum extent, which not only realizes the effective leaching of uranium, but also avoids the occurrence and precipitation of calcium carbonate and calcium sulfate, realizing the industrial development of the sandstone type uranium deposit.

Keywords: CO₂+O₂ ISL, industrial production, well field layout, uranium processing

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Authors: Nurshafika Adira Bt Audi Ashraf, Habsah Alwi

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This study describes the series of analysis conducted after the use of Vacuum far Infra Red. Parameter including the constant drying temperature at 40°C with pressure difference (-400 bar, -500 bar and -600 bar) and constant drying pressure at -400 bar with difference temperature (40°C, 50°C and 60°C). The dried leaves with constant temperature and constant pressure is compared with the fresh leaves via several analysis including TGA, FTIR and Chromameter. Results indicated that the fresh leaves shows three degradation stages while temperature constant shows four stages of degradation and at constant pressure of -400 bar, five stages of degradation is shown. However, at the temperature constant with pressure -500 bar, five degradation stages are identified and at constant pressure with temperature 40°C, three stage of degradation is presence. It is assumed that it is due to the difference size of the sample as the particle size is decrease, the peak temperature shown in TG curves is also decrease which lead to the rapid ignition. Based on the FTIR analysis, fresh leaves gives the high presence of O-H and C=O group where both of the constant parameters give the absence of those due to the drying effects. In color analysis, the constant drying parameters (pressure and temperature) both shows that as the temperature increases, the average total of color change is also increases.

Keywords: chromameter, FTIR, TGA, Vaccum far infrared dying

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Authors: Nor Khaizan Anuar, Nur Karimah Aziz, Tin Wui Wong, Ahmad Sazali Hamzah, Wan Rozita Wan Engah

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The physicochemical attributes and wound healing activity of pectin hydrogel in rat models, following partial thickness thermal injury were investigated. The pectin hydrogel was prepared by solvent evaporation method with the aid of glutaraldehyde as crosslinking agent and glycerol as plasticizer. The physicochemical properties were mainly evaluated using differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR) spectroscopy, while the wound healing activity was examined by the macroscopic images, wound size reduction and histological evaluation using haematoxylin and eosin (H&E) stain for 14 days. The DSC and FTIR analysis suggested that pectin hydrogel exhibited higher extent of polymer-polymer interaction at O-H functional group in comparison to the unprocessed pectin. This was indicated by the increase of endothermic enthalpy values from 139.35 ± 13.06 J/g of unprocessed pectin to 156.23 ± 2.86 J/g of pectin hydrogel, as well as the decrease of FTIR wavenumber corresponding to O-H at 3432.07 ± 0.49 cm-1 of unprocessed pectin to 3412.62 ± 13.06 cm-1 of pectin hydrogel. Rats treated with pectin hydrogel had significantly smaller wound size (Student’s t-test, p<0.05) when compared to the untreated group starting from day 7 until day 14. H&E staining indicated that wounds received pectin hydrogel had more fibroblasts, blood vessels and collagen bundles on day 14 in comparison to the untreated rats.

Keywords: pectin, physicochemical, rats, wound

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Authors: Aram Yakoby, Yossef H. Hatzor, Shmulik Pinkert

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This work presents an applied engineering method for evaluating the stability of underground openings under conditions of uncertainty. The developed method is demonstrated by a comprehensive parametric study on a case of large-diameter vertical borehole stability analysis, with uncertainties regarding the in-situ stress distribution. To this aim, a safety factor analysis is performed for the stability of both supported and unsupported boreholes. In the analysis, we used analytic geomechanical calculations and advanced numerical modeling to evaluate the estimated stress field. In addition, the work presents the development of a boundary condition for the numerical model that fits the nature of the problem and yields excellent accuracy. The borehole stability analysis is studied in terms of (1) the stress ratio in the vertical and horizontal directions, (2) the mechanical properties and geometry of the support system, and (3) the parametric sensitivity. The method's results are studied in light of a real case study of an underground waste disposal site. The conclusions of this study focus on the developed method for capturing the parametric uncertainty, the definition of critical geological depths, the criteria for implementing structural support, and the effectiveness of further in-situ investigations.

Keywords: borehole stability, in-situ stress, parametric study, factor of safety

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Authors: Reza Ziaie Moayed, Ehsan Azini

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Jet grouting (JG) is one of the methods of improving and increasing the strength and bearing of soil in which the high pressure water or grout is injected through the nozzles into the soil. During this process, a part of the soil and grout particles comes out of the drill borehole, and the other part is mixed up with the grout in place, as a result of this process, a mass of modified soil is created. The purpose of this method is to change the soil into a mixture of soil and cement, commonly known as "soil-cement". In this paper, first, the principles of high pressure injection and then the effective parameters in the JG method are described. Then, the tests on the samples taken from the columns formed from the excavation around the soil-cement columns, as well as the static loading test on the created column, are discussed. In the other part of this paper, the soil behavior models for numerical modeling in PLAXIS software are mentioned. The purpose of this paper is to evaluate the results of numerical modeling based on in-situ static loading tests. The results indicate an acceptable agreement between the results of the tests mentioned and the modeling results. Also, modeling with this software as an appropriate option for technical feasibility can be used to soil improvement using JG.

Keywords: jet grouting column, soil improvement, numerical modeling, in-situ loading test

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Authors: Esther Lorrayne M. Pereira, Adriana Souza M. Batista, Fabíola A. S. Ribeiro, Adelina P. Santos, Clascídia A. Furtado, Luiz O. Faria

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The combination of multi–walled carbon nanotubes (MWCNTs) with polymers offers an attractive route to reinforce the macromolecular compounds as well as the introduction of new properties based on morphological modifications or electronic interactions between the two constituents. As they are only a few nanometers in dimension, it offers ultra-large interfacial area per volume between the nano-element and polymer matrix. Nevertheless, the use of MWCNTs as a rough material in different applications has been largely limited by their poor processability, insolubility, and infusibility. Studies concerning the nanofiller reinforced polymer composites are justified in an attempt to overcome these limitations. This work presents one preliminary study of MWCNTs dispersion into the PVDF homopolymer. For preparation, the composite components were diluted in n,n-dimethylacetamide (DMAc) with mechanical agitation assistance. After complete dilution, followed by slow evaporation of the solvent at 60°C, the samples were dried. Films of about 80 μm were obtained. FTIR and UV-Vis spectroscopic techniques were used to characterize the nanocomposites. The appearance of absorption bands in the FTIR spectra of nanofilled samples, when compared to the spectrum of pristine PVDF samples, are discussed and compared with the UV-Vis measurements.

Keywords: composites materials, FTIR, MWNTs, PVDF, UV-vis

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Authors: Rana Th. A. Al-rubaye

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A novel chromium-free protective coating films based on a zeolite coating was growing onto a FeCrAlloy metal using in –situ hydrothermal method. The zeolite film was obtained using in-situ crystallization process that is capable of coating large surfaces with complex shape and in confined spaces has been developed. The zeolite coating offers an advantage of a high mechanical stability and thermal stability. The physico-chemical properties were investigated using X-ray diffraction (XRD), Electron microscopy (SEM), Energy Dispersive X–ray analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550°C).

Keywords: fecralloy, zsm-5 zeolite, zeolite coatings, hydrothermal method

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Authors: Justice Zakhele Msomi

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Nanoparticles of CdFe2O4 with particle size of about 10 nm have been synthesized by high energy ball milling and co-precipitation processes. The synthesis route appears to have some effects on the properties. The compounds have been characterized by X-ray diffraction, Fourier Transform Infrared (FTIR), transmission electron microscopy (TEM), Mössbauer and magnetization measurements. The XRD pattern of CdFe2O4 provides information about single-phase formation of spinel structure with cubic symmetry. The FTIR measurements between 400 and 4000 cm-1 indicate intrinsic cation vibration of the spinel structure. The Mössbauer spectra were recorded at 4 K and 300 K. The hyperfine fields appear to be highly sensitive on particle size. The evolution of the properties as a function of particle size is also presented.

Keywords: ferrite, nanoparticles, magnetization, Mössbauer

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Authors: Surabhi Pandey, Pavuluri Srinivasa Rao

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Extrusion processing is a high-temperature short time (HTST) treatment which can improve protein quality and digestibility together with retaining active nutrients. In-vitro protein digestibility of plant protein-based foods is generally enhanced by extrusion. The current study aimed to investigate the effect of extrusion cooking on in-vitro protein digestibility (IVPD) and conformational modification of protein in green banana flour extrudates. Green banana flour was extruded through a co-rotating twin-screw extruder varying the moisture content, barrel temperature, screw speed in the range of 10-20 %, 60-80 °C, 200-300 rpm, respectively, at constant feed rate. Response surface methodology was used to optimise the result for IVPD. Fourier-transform infrared spectroscopy (FTIR) analysis provided a convenient and powerful means to monitor interactions and changes in functional and conformational properties of extrudates. Results showed that protein digestibility was highest in extrudate produced at 80°C, 250 rpm and 15% feed moisture. FTIR analysis was done for the optimised sample having highest IVPD. FTIR analysis showed that there were no changes in primary structure of protein while the secondary protein structure changed. In order to explain this behaviour, infrared spectroscopy analysis was carried out, mainly in the amide I and II regions. Moreover, curve fitting analysis showed the conformational changes produced in the flour due to protein denaturation. The quantitative analysis of the changes in the amide I and II regions provided information about the modifications produced in banana flour extrudates.

Keywords: extrusion, FTIR, protein conformation, raw banana flour, SDS-PAGE method

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Authors: Ravi Raj, Louis Chiu, Deepak Marla, Aijun Huang

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Hybridization of the directed laser deposition (DLD) process using an in-situ micro-roller to impart a vertical compressive load on the deposited bead at elevated temperatures can relieve tensile residual stresses incurred in the process. To investigate this stress relief mechanism and its relationship with the in-situ rolling parameters, a fully coupled dynamic thermo-mechanical model is presented in this study. A single bead deposition of Ti-6Al-4V alloy with an in-situ roller made of mild steel moving at a constant speed with a fixed nominal bead reduction is simulated using the explicit solver of the finite element software, Abaqus. The thermal model includes laser heating during the deposition process and the heat transfer between the roller and the deposited bead. The laser heating is modeled using a moving heat source with a Gaussian distribution, applied along the pre-formed bead’s surface using the VDFLUX Fortran subroutine. The bead’s cross-section is assumed to be semi-elliptical. The interfacial heat transfer between the roller and the bead is considered in the model. Besides, the roller is cooled internally using axial water flow, considered in the model using convective heat transfer. The mechanical model for the bead and substrate includes the effects of rolling along with the deposition process, and their elastoplastic material behavior is captured using the J2 plasticity theory. The model accounts for strain, strain rate, and temperature effects on the yield stress based on Johnson-Cook’s theory. Various aspects of this material behavior are captured in the FE software using the subroutines -VUMAT for elastoplastic behavior, VUHARD for yield stress, and VUEXPAN for thermal strain. The roller is assumed to be elastic and does not undergo any plastic deformation. Also, contact friction at the roller-bead interface is considered in the model. Based on the thermal results of the bead, the distance between the roller and the deposition nozzle (roller o set) can be determined to ensure rolling occurs around the beta-transus temperature for the Ti-6Al-4V alloy. It is identified that roller offset and the nominal bead height reduction are crucial parameters that influence the residual stresses in the hybrid process. The results obtained from a simulation at roller offset of 20 mm and nominal bead height reduction of 7% reveal that the tensile residual stresses decrease to about 52% due to in-situ rolling throughout the deposited bead. This model can be used to optimize the rolling parameters to minimize the residual stresses in the hybrid DLD process with in-situ micro-rolling.

Keywords: directed laser deposition, finite element analysis, hybrid in-situ rolling, thermo-mechanical model

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Authors: Babak Sadeghi, Rony Snyders, Marie-Paule.Delplancke-Ogletree

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Nitrogen fixation (NF) is one of the crucial industrial processes. Many attempts have been made in order to artificially fix nitrogen, and among them, the Haber-Bosch’s (H-B) process is widely used. However, it presents two major drawbacks: huge fossil feedstock consumption and noticeable greenhouse gases emission. It is, therefore, necessary to develop alternatives. Plasma technology, as an inherent “green” technology, is considered to have a great potential for reducing the environmental impacts and improving the energy efficiency of the NF process. In this work, we have studied the catalyst assisted microwave plasma for NF application. Heterogeneous catalysts of MoO₃, with various loads 0, 5, 10, 20, and 30 wt%, supported on γ-alumina were prepared by conventional wet impregnation. Crystallinity, surface area, pore size, and microstructure were obtained by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) adsorption isotherm, Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The XRD patterns of calcined alumina confirm the γ- phase. Characteristic picks of MoO₃ could not be observed for low loads (< 20 wt%), likely indicating a high dispersion of metal oxide over the support. The specific surface area along with pores size are decreasing with increasing calcination temperature and MoO₃ loading. The MoO₃ loading does not modify the microstructure. TEM and SEM results for loading inferior to 20 wt% are coherent with a monolayer of MoO₃ on the support as proposed elsewhere. For loading of 20 wt% and more, TEM and Electron diffraction (ED) show nanocrystalline ₃-D MoO₃ particles. The catalytic performances of these catalysts were investigated in the post-discharge of a microwave plasma for NOx formation from N₂/O₂ mixtures. The plasma is sustained by a surface wave launched in a quartz tube via a surfaguide supplied by a 2.45 GHz microwave generator in pulse mode. In-situ identification and quantification of the products were carried out by Fourier-transform infrared spectroscopy (FTIR) in the post-discharge region. FTIR analysis of the exhausted gas reveal NO and NO₂ bands in presence of catalyst while only NO band were assigned without catalyst. On the other hand, in presence of catalyst, a 10% increase of NOₓ formation and of 20% increase in energy efficiency are observed.

Keywords: γ-Al2O₃-MoO₃, µ-waveplasma, N2 fixation, Plasma-catalysis, Plasma diagnostic

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Authors: Sonalee Das, Smita Mohanty, S. K. Nayak

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Recent years has witnessed the increasing demand for natural resources and products in polyurethane synthesis because of global warming, sustainable development and oil crisis. For this purpose, different plant oils such as soybean oil, castor oil and linseed oil are extensively used. Moreover, the isocyanate used for the synthesis of polyurethane is derived from petroleum resources. In this present work attempts have been made for the successful synthesis of biobased isocyanate from castor oil with partially biobased isocyanate in presence of catalyst dibutyltin dilaurate (DBTDL). The goal of the present study was to investigate the thermal, mechanical, morphological and chemical properties of the synthesized polyurethane in terms of castor oil modification. The transesterified polyol shows broad and higher hydroxyl value as compared to castor oil which was confirmed by FTIR studies. The FTIR studies also revealed the successful synthesis of bio based polyurethane by showing characteristic peaks at 3300cm-1, 1715cm-1 and 1532cm-1 respectively. The TGA results showed three step degradation mechanism for the synthesized polyurethane from modified and unmodified castor oil. However, the modified polyurethane exhibited higher degradation temperature as compared to unmodified one. The mechanical properties also demonstrated higher tensile strength for modified polyurethane as compared to unmodified one.

Keywords: castor oil, partially biobased Isocyanate, polyurethane synthesis, FTIR

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Authors: Seyfullah Madakbas, Emrah Cakmakci

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Polyaniline (PANI), the most studied member of the conductive polymers, has a wide range of uses from several electronic devices to various conductive high-technology applications. Boron nitride (BN) is a boron and nitrogen containing compound with superior chemical and thermal resistance and thermal conductivity. Even though several composites of PANI was prepared in literature, the preparation of h-BN/PANI composites is rare. In this work PANI was polymerized in the presence of different amounts of h-BN (1, 3 and 5% with respect to PANI) by using 0.1 M solution of NH4S2O8 in HCl as the oxidizing agent and conductive composites were prepared. Composites were structurally characterized with FTIR spectroscopy and X-Ray Diffraction (XRD). Thermal properties of conductive composites were determined by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric measurements were performed in the frequency range of 106–108 Hz at room temperature. The corresponding bands for the benzenoid and quinoid rings at around 1593 and 1496 cm-1 in the FTIR spectra of the composites proved the formation of polyaniline. Together with the FTIR spectra, XRD analysis also revealed the existence of the interactions between PANI and h-BN. Glass transition temperatures (Tg) of the composites increased with the increasing amount of PANI (from 87 to 101). TGA revealed that the char yield of the composites increased as the amount of h-BN was increased in the composites. Finally the dielectric permittivity of 3 wt.%h-BN-containing composite was measured and found as approximately 17. This work was supported by Marmara University, Commission of Scientific Research Project.

Keywords: dielectric permittivity, h-BN, PANI, thermal analysis

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Authors: A. Adelhafidhi, I. M. Babaghayou, S. F. Chabira, M. Sebaa

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This study deals with the photodegradation of unformulated polyethylene films for greenhouse covering. The UV range of solar light appears as the most deleterious factor of plastic degradation in outdoor exposure. The reasons of this photosensitivity are structural defects which are light-absorbing. The use of FTIR as an investigation tool has revealed that the material reacts with surrounding oxygen via a photooxidation process. Although the photochemical process is quite complex, it appears through this study than crosslinking and chain scissions are the most important events taking place during aging These two key reactions change irremediably the average molecular weight affecting thus drastically the mechanical properties and reducing, in the same way, the service lifetime of the films.

Keywords: polyethylene, films, unformulated, FTIR, ageing

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Authors: Shivani A. Singh, Pravin S. More

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In the present inspection, we indicate the falsification of Fe-doped graphene nanoparticles by modified Hummers method. Structural and physiochemical properties of the resulting pallets were explored with the help of ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), Photoluminescence spectroscopy (PL) for graphene sample exhibits absorption peaks ~248nm. Pure graphene shows PL peak at 348 nm. After doping of Fe with graphene the PL peak shifted from 348 nm to 332 nm. The oxidation degree, i.e. the relative amount of oxygen functional groups was estimated from the relative intensities of the oxygen related bands (ORB) in the FTIR measurements. These analyses show that this modified material can be useful for gas sensing applications and to be used in diverse areas.

Keywords: chemical doping, graphene, gas sensing, sensing

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Authors: L. N. Shubha, P. Madhusudana Rao

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The Polyaniline / Copper Oxide(PANI / CuO) nanocomposite was prepared by solution mixing of prepared Polyaniline and copper Oxide in Dimethyl sulfoxide (DMSO). The synthesis involved the formation of dark green colored Polyaniline-Copper Oxide nanocomposite. The synthesized polymer nano composites were characterized by XRD, FTIR, SEM and UV-Visible Spectroscopy. The characteristic peaks in XRD, FTIR and UV-Visible spectra confirmed the presence of CuO in the polymer structure. SEM analysis revealed formation of PANI/CuO nano composite The D.C. conductivity measurements were performed using two probe method for various temperatures.

Keywords: polyaniline/copper oxide (PANI/CuO) nanocomposite, XRD, SEM, FTIRand DC- conductivity, UV-visible spectra

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Authors: Mohamed Izzharif Abdul Halim, Niamh Nic Daeid

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Determining the source of pen inks used on a variety of documents is impartial for forensic document examiners. The examination of inks is often performed to differentiate between inks in order to evaluate the authenticity of a document. A ballpoint pen ink consists of synthetic dyes in (acidic and/or basic), pigments (organic and/or inorganic) and a range of additives. Inks of similar color may consist of different composition and are frequently the subjects of forensic examinations. This study emphasizes on blue ballpoint pen inks available in the market because it is reported that approximately 80% of questioned documents analysis involving ballpoint pen ink. Analytical techniques such as thin layer chromatography, high-performance liquid chromatography, UV-vis spectroscopy, luminescence spectroscopy and infrared spectroscopy have been used in the analysis of ink samples. In this study, application of Diamond Attenuated Total Reflectance (ATR) FTIR is straightforward but preferable in forensic science as it offers no sample preparation and minimal analysis time. The data obtained from these techniques were further analyzed using multivariate chemometric methods which enable extraction of more information based on the similarities and differences among samples in a dataset. It was indicated that some pens from the same manufactures can be similar in composition, however, discrete types can be significantly different.

Keywords: ATR FTIR, ballpoint, multivariate chemometric, PCA

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Authors: Raphaelle Guillou, Matthieu Le Saux, Jean-Christophe Brachet, Thomas Guilbert, Elodie Rouesne, Denis Menut, Caroline Toffolon-Masclet, Dominique Thiaudiere

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In some hypothetical accidental situations, such as during a Loss Of Coolant Accident (LOCA) in pressurized water reactors, fuel cladding tubes made of zirconium alloys can be exposed for a few minutes to steam at High Temperature (HT up to 1200°C) before being cooled and then quenched in water. Under LOCA-like conditions, the cladding undergoes a number of metallurgical changes (phase transformations, oxygen diffusion and growth of an oxide layer...) and is consequently submitted to internal stresses whose state evolves during the transient. These stresses can have an effect on the oxide structure and the oxidation kinetics of the material. They evolve during cooling, owing to differences between the thermal expansion coefficients of the various phases and phase transformations of the metal and the oxide. These stresses may result in the failure of the cladding during quenching, once the material is embrittled by oxidation. In order to progress in the evaluation of these internal stresses, X-ray diffraction experiments were performed in-situ under synchrotron radiation during HT oxidation and subsequent cooling on Zircaloy-4 sheet samples. First, structural evolutions, such as phase transformations, have been studied as a function of temperature for both the oxide layer and the metallic substrate. Then, internal stresses generated within the material oxidized at temperatures between 700 and 900°C have been evaluated thanks to the 2θ diffraction peak position shift measured during the in-situ experiments. Electron backscatter diffraction (EBSD) analysis was performed on the samples after cooling in order to characterize their crystallographic texture. Furthermore, macroscopic strains induced by oxidation in the conditions investigated during the in-situ X-ray diffraction experiments were measured in-situ in a dilatometer.

Keywords: APRP, stains measurements, synchrotron diffraction, zirconium allows

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Authors: Christine Fräulin, Daniela Schurr, Hamed Shahidi Rad, Gerrit Waters, Günter Rinke, Roland Dittmeyer, Michael Nilles

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The reaction mechanisms of many liquid-phase reactions in organic chemistry have not yet been sufficiently clarified. Process conditions of several hundred degrees celsius and pressures to ten megapascals complicate the sampling and the determination of kinetic data. Space resolved in-situ measurements promises new insights. A non-invasive in-situ measurement technique has the advantages that no sample preparation is necessary, there is no change in sample mixture before analysis and the sampling do no lead to interventions in the flow. Thus, the goal of our research was the development of a contact-free spatially resolved measurement technique for kinetic studies of liquid phase reaction under process conditions. Therefore we used laser Raman spectroscopy combined with an optical transparent microchannel reactor. To show the performance of the system we choose the oxidation of cyclohexane as sample reaction. Cyclohexane oxidation is an economically important process. The products are intermediates for caprolactam and adipic acid, which are starting materials for polyamide 6 and 6.6 production. To maintain high selectivities of 70 to 90 %, the reaction is performed in industry at a low conversion of about six percent. As Raman spectroscopy is usually very selective but not very sensitive the detection of the small product concentration in cyclohexane oxidation is quite challenging. To meet these requirements, an optical experimental setup was optimized to determine the concentrations by laser Raman spectroscopy with respect to good detection sensitivity. With this measurement technique space resolved kinetic studies of uncatalysed and homogeneous catalyzed cyclohexane oxidation were carried out to obtain details about the reaction mechanism.

Keywords: in-situ laser raman spectroscopy, space resolved kinetic measurements, homogeneous catalysis, chemistry

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Authors: Ashraf Eid

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Many formulas are set to estimate the pile load capacity based on the in-situ pile load tests. However, discrepancy is obvious between the results of these applications. Some formulas are more adequate than others with respect to soil formation and its characteristics. In this research, attempts were undertaken to evaluate the adequacy of the most well-known formulas based on a series of pile load tests carried out in Port Said city in the northeast of Egypt for major residential projects. Comparisons were undertaken between the different formulas supported by the results of in-situ Cone Penetration Tests (CPT). Based on this study, a guide for engineers for using the proper formula can be adopted with consideration of soil type and characteristics. The Egyptian Code which relies on the results of some formulas is involved in the study as a guiding aspect in the pile design.

Keywords: pile load formula, load test of piles, CPT, Egyptian code

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Authors: Kaiyi Zhang, Wenlong Li, Haicheng Li, Yifei Luo, Zheng Li, Xiaoshi Wang, Xiaodong Chen

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Plant wearable sensors facilitate the real-time monitoring of plant physiological status. In situ monitoring of the plant chlorophyll content over days could provide valuable information on the photosynthetic capacity, nitrogen content, and general plant health. However, it cannot be achieved by current chlorophyll measuring methods. Here, a miniaturized and plant-wearable chlorophyll meter was developed for rapid, non-destructive, in situ, and long-term chlorophyll monitoring. This reflectance-based chlorophyll sensor with 1.5 mm thickness and 0.2 g weight (1000 times lighter than the commercial chlorophyll meter), includes a light emitting diode (LED) and two symmetric photodetectors (PDs) on a flexible substrate and is patched onto the leaf upper epidermis with a conformal light guiding layer. A chlorophyll content index (CCI) calculated based on this sensor shows a better linear relationship with the leaf chlorophyll content (r² > 0.9) than the traditional chlorophyll meter. This meter can wirelessly communicate with a smartphone to monitor the leaf chlorophyll change under various stresses and indicate the unhealthy status of plants for long-term application of plants under various stresses earlier than chlorophyll meter and naked-eye observation. This wearable chlorophyll sensing patch is promising in smart and precision agriculture.

Keywords: plant wearable sensors, reflectance-based measurements, chlorophyll content monitoring, smart agriculture

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Authors: Chinh Nguyen Nhu Bao, Hien To Thi, Norimichi Takenaka

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Formaldehyde (HCHO) concentrations in rainwater including in tropical storms in Sakai City, Osaka, Japan have been measured continuously during rain event by developed chemiluminescence method. The level of formaldehyde was ranged from 15 µg/L to 500 µg/L. The high concentration of HCHO in rainwater is related to the wind direction from the south and west sides of Sakai City where manufactures related to chemicals, oil-refinery, and steel. The in-situ irradiated experiment on rainwater sample was conducted to prove the aqueous phase photo-production of HCHO and the degradation of HCHO. In the daytime, the aqueous phase photolysis is the source of HCHO in rainwater (4.52 ± 5.74 µg/L/h for UV light source in-situ condition, 2.84-8.96 µg/L/h under sunlight). However, in the night time, the degradation is the function of microorganism.

Keywords: chemiluminescence, formaldehyde, rainwater, typhoon

Procedia PDF Downloads 141

Authors: Avoseh Funmilola, Osman Khalid, Wayne Nelson, Paramespri Naidoo, Deresh Ramjugernath

Abstract:

The increasing global atmospheric temperature is of great concern and this has led to the development of technologies to reduce the emission of greenhouse gases into the atmosphere. Flue gas emissions from fossil fuel combustion are major sources of greenhouse gases. One of the ways to reduce the emission of CO₂ from flue gases is by post combustion capture process and this can be done by absorbing the gas into suitable chemical solvents before emitting the gas into the atmosphere. Alkanolamines are promising solvents for this capture process. Vapour liquid equilibrium of CO₂-alkanolamine systems is often represented by CO₂ loading and partial pressure of CO₂ without considering the liquid phase. The liquid phase of this system is a complex one comprising of 9 species. Online analysis of the process is important to monitor the concentrations of the liquid phase reacting and product species. Liquid phase analysis of CO₂-diethanolamine (DEA) solution was performed by attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. A robust Calibration was performed for the CO₂-aqueous DEA system prior to an online monitoring experiment. The partial least square regression method was used for the analysis of the calibration spectra obtained. The models obtained were used for prediction of DEA and CO₂ concentrations in the online monitoring experiment. The experiment was performed with a newly built recirculating experimental set up in the laboratory. The set up consist of a 750 ml equilibrium cell and ATR-FTIR liquid flow cell. Measurements were performed at 400°C. The results obtained indicated that the FTIR spectroscopy combined with Partial least square method is an effective tool for online monitoring of speciation.

Keywords: ATR-FTIR, CO₂ capture, online analysis, PLS regression

Procedia PDF Downloads 171

Authors: Saad S. Alrwashdeh, Henning Markötter, Handri Ammari, Jan Haußmann, Tobias Arlt, Joachim Scholta, Ingo Manke

Abstract:

In this investigation, synchrotron X-ray imaging is used to study water transport inside polymer electrolyte membrane fuel cells. Two measurement techniques are used, namely in-situ radiography and quasi-in-situ tomography combining together in order to reveal the relationship between the structures of the microporous layers (MPLs) and the gas diffusion layers (GDLs), the operation temperature and the water flow. The developed cell is equipped with a thick GDL and a high back pressure MPL. It is found that these modifications strongly influence the overall water transport in the whole adjacent GDM.

Keywords: polymer electrolyte membrane fuel cell, microporous layer, water transport, radiography, tomography

Procedia PDF Downloads 153

Authors: Salihu Takuma

Abstract:

Neem seed oil has high contents of unsaturated fatty acids which can be converted to epoxy fatty acids. The vegetable oil – based epoxy material are sustainable, renewable and biodegradable materials replacing petrochemical – based epoxy materials in some applications. Polystyrene is highly brittle with limited mechanical applications. Raw neem seed oil was obtained from National Research Institute for Chemical Technology (NARICT), Zaria, Nigeria. The oil was epoxidized at 60 0C for three (3) hours using formic acid generated in situ. The epoxidized oil was characterized using Fourier Transform Infrared spectroscopy (FTIR). The disappearance of C = C stretching peak around 3011.7 cm-1and formation of a new absorption peak around 943 cm-1 indicate the success of epoxidation. The epoxidized oil was blended with pure polystyrene in different weight percent compositions using solution casting in chloroform. The tensile properties of the blends demonstrated that the addition of 5 wt % ENO to PS led to an increase in elongation at break, but a decrease in tensile strength and modulus. This is in accordance with the common rule that plasticizers can decrease the tensile strength of the polymer.

Keywords: biodegradable, elongation at break, epoxidation, epoxy fatty acids, sustainable, tensile strength and modulus

Procedia PDF Downloads 207

Authors: N. Zoghi, Laleh Maleknia , M. E. Olya

Abstract:

The nano-Cu particles were produced on cotton fabric substrate by ink-jet printing technology with water-soluble ink, which was based on copper. The surface tension and viscosity of the prepared inks were evaluated. The ink-jet printing process was repeated 1, 3, and 5 times in order to evaluate variations in the optical properties by changing thickness of printed film. Following initial drying of the printed film, the samples were annealed at different temperatures (150 °C, 200 °C and 250 °C) to determine the optimum temperature for the parameters set out in this experiment. The prepared nano-Cu particles were characterized by XRD and UV spectroscopy. The appearance of printed image and the nano-Cu particles morphology were observed by SEM. The results demonstrated that the ink-jet printing technology can be used to produce nano-particles on the cotton fabrics surface.

Keywords: ink-jet printing, nano-cu, fabric ink, in situ production, cotton fabric, water-soluble ink, morphology

Procedia PDF Downloads 393

Authors: Pravina Gurjar, Bothiraja Pour, Vijay Kumbhar, Ganesh Dama

Abstract:

Andrographolide (AG), a bioactive phytoconstituent, has a wider range of pharmacological action. However, due to the intestinal degradation, shows low oral bioavailability. The aim of the present work was to develop Floating In-situ gelling Gastro retentive System (FISGS) for AG in order to enhance its site specific absorption and minimize pH dependent hydrolysis in alkaline environment. Further to increase its therapeutic efficacy for peptic ulcer disease caused by H. pyroli. Gellan based floating in situ gelling system of AG were prepared by using sodium citrate and calcium carbonate. The 32 factorial designs was used to study the effect of gellan and calcium carbonate concentration (independent variables) on dependent variable such as viscosity, floating lag time and drug release. Developed system was evaluated for drug content, floating lag time, viscosity, and drug release studies. Drug content, viscosity, and floating lag time was found to be 81-99%, 67-117 Cps, and 3-5 sec, respectively. The obtained system showed good in vitro floating ability for more than 12 h using 0.1 N HCl as dissolution medium with initial burst release followed by the controlled zero order drug release up to 24 hrs. In vivo testing of FISGS of AG to rats demonstrated significant antiulcer activity that were evaluated by various parameters like pH, volume, total acidity, millimole equivalent of H+ ions/30 min, and protein content of gastric content. The densities of all the formulation batches were found to be near about 0.9 and floating duration above 12 hr. It was observed that with the increase in conc. of gellan there was increase in the viscosity of formulation but all formulations were in optimum range. The drug content of optimized batch was found to be 99.23. In histopathology study of stomach, the villi at the mucosal surface, the intercellular junction, the intestinal lumen were intact; no destruction of the epithelium, and submucosal gland in formulation treated and control group animals as compared to pure drug AG and standard ranitidine. Gellan-based in situ gastro retentive floating system could be advantageous in terms of increased bioavailability of AG to maintain an effective drug conc. in gastric fluid as well as in serum for longer period of time.

Keywords: andrographolide, floating drug delivery, in situ gelling system, gastroretentive system

Procedia PDF Downloads 340

Authors: M. Rouhani, F. C. N. Hong, Y. R. Jeng

Abstract:

The tribological performance of DLC films is limited by graphitization at elevated temperatures. Despite of numerous studies on the thermal stability of DLC films, a comprehensive in-situ characterization at elevated temperature is still lacking. In this study, DLC films were deposited using filtered cathodic arc vacuum method. Thermal stability of the films was characterized in-situally using a synchronized technique integrating Raman spectroscopy and depth-sensing measurements. Tests were performed in a high temperature chamber coupled with feedback control to make it possible to study the temperature effects in the range of 21 – 450 ̊C. Co-located SPM and Raman microscopy maps at different temperature over a specific area on the surface of the film were prepared. The results show that the thermal stability of the DLC films depends on their sp3 content. Films with lower sp3 content endure graphitization during the temperature-course used in this study. The graphitization is accompanied with significant changes in surface roughness and Raman spectrum of the film. Surface roughness of the films start to change even before graphitization transformation could be detected using Raman spectroscopy. Depth-sensing tests (nanoindentation, nano-scratch and wear) endorse the surface roughness change seen before graphitization occurrence. This in-situ study showed that the surface of the films is more sensitive to temperature rise compared to the bulk. We presume the changes observed in films hardness, surface roughness and scratch resistance with temperature rise, before graphitization occurrence, is due to surface relaxation.

Keywords: DLC film, nanoindentation, Raman spectroscopy, thermal stability

Procedia PDF Downloads 171