Search results for: physico-chemical characterization

Authors: Siti N. M. Rozali, A. H. J. Paterson, J. P. Hindmarsh

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Spray drying of fruit juices from liquid to powder is desirable as the powders are easier to handle, especially for storage and transportation. In this project, pomace fibres will be used as a drying aid during spray drying, replacing the commonly used maltodextrins. The main attraction of this drying aid is that the pomace fibres are originally derived from the fruit itself. However, the addition of micro-sized fibres to fruit juices is expected to affect the rheology and subsequent atomization behaviour during the spray drying process. This study focuses on the determination and characterization of the rheology of juice-fibre suspensions specifically inside a spray dryer nozzle. Results show that the juice-fibre suspensions exhibit shear thinning behaviour with a significant extensional viscosity. The shear and extensional viscosities depend on several factors which include fibre fraction, shape, size and aspect ratio. A commercial capillary rheometer is used to characterize the shear behaviour while a portable extensional rheometer has been designed and built to study the extensional behaviour. Methods and equipment will be presented along with the rheology results. Rheology or behaviour of the juice-fibre suspensions provides an insight into the limitations that will be faced during atomization, and in the future, this finding will assist in choosing the best nozzle design that can overcome the limitations introduced by the fibre particles thus resulting in successful spray drying of juice-fibre suspensions.

Keywords: extensional rheology, fibre suspensions, portable extensional rheometer, shear rheology

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

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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

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Authors: Alireza Rezagholilou

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Moisture susceptibility of bituminous mixes directly affect the stripping of asphalt layers. The majority of relevant test methods are mechanical methods with low repeatability and consistency of results. Thus, this research aims to evaluate the physicochemical interactions of bitumen and aggregates based on the wettability concept. As such, the surface energies of components at the interface are measured by contact angle method. That gives an opportunity to investigate the adhesion properties of multiple mineral fillers at various percentages to explore the best dosage in the mix. Three types of fillers, such as hydrated lime, ground lime and rock powder, are incorporated into the bitumen mix for a series of sessile drop tests for both aggregates and binders. Results show the variation of adhesion properties versus filler (%).

Keywords: adhesion, contact angle, filler, surface energy, moisture susceptibility

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Authors: M. Abderrahmane Mograne, Didier Laux, Jean-Yves Ferrandis

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Rheological characterizations of complex liquids like polymer solutions present an important scientific interest for a lot of researchers in many fields as biology, food industry, chemistry. In order to establish master curves (elastic moduli vs frequency) which can give information about microstructure, classical rheometers or viscometers (such as Couette systems) are used. For broadband characterization of the sample, temperature is modified in a very large range leading to equivalent frequency modifications applying the Time Temperature Superposition principle. For many liquids undergoing phase transitions, this approach is not applicable. That is the reason, why the development of broadband spectroscopic methods around room temperature becomes a major concern. In literature many solutions have been proposed but, to our knowledge, there is no experimental bench giving the whole rheological characterization for frequencies about a few Hz (Hertz) to many MHz (Mega Hertz). Consequently, our goal is to investigate in a nondestructive way in very broadband frequency (A few Hz – Hundreds of MHz) rheological properties using longitudinal ultrasonic waves (L waves), a unique experimental bench and a specific container for the liquid: a test tube. More specifically, we aim to estimate the three viscosities (longitudinal, shear and bulk) and the complex elastic moduli (M*, G* and K*) respectively longitudinal, shear and bulk moduli. We have decided to use only L waves conditioned in two ways: bulk L wave in the liquid or guided L waves in the tube test walls. In this paper, we will present first results for very low frequencies using the ultrasonic tracking of a falling ball in the test tube. This will lead to the estimation of shear viscosity from a few mPa.s to a few Pa.s (Pascal second). Corrections due to the small dimensions of the tube will be applied and discussed regarding the size of the falling ball. Then the use of bulk L wave’s propagation in the liquid and the development of a specific signal processing in order to assess longitudinal velocity and attenuation will conduct to the longitudinal viscosity evaluation in the MHz frequency range. At last, the first results concerning the propagation, the generation and the processing of guided compressional waves in the test tube walls will be discussed. All these approaches and results will be compared to standard methods available and already validated in our lab.

Keywords: nondestructive measurement for liquid, piezoelectric transducer, ultrasonic longitudinal waves, viscosities

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Authors: Matthias Walluch, José Alberto Rodríguez, Christopher Giehl, Gunther Arnold, Daniela Ehgartner

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Dynamic mechanical analysis (DMA) is a powerful method to characterize viscoelastic properties and phase transitions for a wide range of materials. It is often used to characterize polymers and their temperature-dependent behavior, including thermal transitions like the glass transition temperature Tg, via determination of storage and loss moduli in tension (Young’s modulus, E) and shear or torsion (shear modulus, G) or other testing modes. While production and application temperatures for polymers are often limited to several hundred degrees, material properties of glasses usually require characterization at temperatures exceeding 600 °C. This contribution highlights a high temperature setup for rotational and oscillatory rheometry as well as for DMA in different modes. The implemented standard convection oven enables the characterization of glass in different loading modes at temperatures up to 950 °C. Three-point bending, tension and torsional measurements on different glasses, with E and G moduli as a function of frequency and temperature, are presented. Additional tests include superimposing several frequencies in a single temperature sweep (“multiwave”). This type of test results in a considerable reduction of the experiment time and allows to evaluate structural changes of the material and their frequency dependence. Furthermore, DMA in torsion and tension was performed to determine the complex Poisson’s ratio as a function of frequency and temperature within a single test definition. Tests were performed in a frequency range from 0.1 to 10 Hz and temperatures up to the glass transition. While variations in the frequency did not reveal significant changes of the complex Poisson’s ratio of the glass, a monotonic increase of this parameter was observed when increasing the temperature. This contribution outlines the possibilities of DMA in bending, tension and torsion for an extended temperature range. It allows the precise mechanical characterization of material behavior from room temperature up to the glass transition and the softening temperature interval. Compared to other thermo-analytical methods, like Dynamic Scanning Calorimetry (DSC) where mechanical stress is neglected, the frequency-dependence links measurement results (e.g. relaxation times) to real applications

Keywords: dynamic mechanical analysis, oscillatory rheometry, Poisson's ratio, solid glass, viscoelasticity

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Authors: Lina Paola Orozco Marin, Yuliet Montoya Osorio, John Bustamante Osorno

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Ischemic events can culminate in acute myocardial infarction by irreversible cardiac lesions that cannot be restored due to the limited regenerative capacity of the heart. Cell therapy seeks to replace these injured or necrotic cells by transplanting healthy and functional cells. The therapeutic alternatives proposed by tissue engineering and cardiovascular regenerative medicine are the use of biomaterials to mimic the native extracellular medium, which is full of proteins, proteoglycans, and glycoproteins. The selected biomaterials must provide structural support to the encapsulated cells to avoid their migration and death in the host tissue. In this context, the present research work focused on developing a natural thermosensitive hydrogel, its physical and chemical characterization, and the determination of its biocompatibility in vitro. The hydrogel was developed by mixing hydrolyzed bovine and porcine collagen at 2% w/v, chitosan at 2.5% w/v, and beta-glycerolphosphate at 8.5% w/w and 10.5% w/w in magnetic stirring at 4°C. Once obtained, the thermosensitivity and gelation time were determined, incubating the samples at 37°C and evaluating them through the inverted tube method. The morphological characterization of the hydrogels was carried out through scanning electron microscopy. Chemical characterization was carried out employing infrared spectroscopy. The biocompatibility was determined using the MTT cytotoxicity test according to the ISO 10993-5 standard for the hydrogel’s precursors using the fetal human ventricular cardiomyocytes cell line RL-14. The RL-14 cells were also seeded on the top of the hydrogels, and the supernatants were subculture at different periods to their observation under a bright field microscope. Four types of thermosensitive hydrogels were obtained, which differ in their composition and concentration, called A1 (chitosan/bovine collagen/beta-glycerolphosphate 8.5%w/w), A2 (chitosan/porcine collagen/beta-glycerolphosphate 8.5%), B1 (chitosan/bovine collagen/beta-glycerolphosphate 10.5%) and B2 (chitosan/porcine collagen/beta-glycerolphosphate 10.5%). A1 and A2 had a gelation time of 40 minutes, and B1 and B2 had a gelation time of 30 minutes at 37°C. Electron micrographs revealed a three-dimensional internal structure with interconnected pores for the four types of hydrogels. This facilitates the exchange of nutrients, oxygen, and the exit of metabolites, allowing to preserve a microenvironment suitable for cell proliferation. In the infrared spectra, it was possible to observe the interaction that occurs between the amides of polymeric compounds with the phosphate groups of beta-glycerolphosphate. Finally, the biocompatibility tests indicated that cells in contact with the hydrogel or with each of its precursors are not affected in their proliferation capacity for a period of 16 days. These results show the potential of the hydrogel to increase the cell survival rate in the cardiac cell therapies under investigation. Moreover, the results lay the foundations for its characterization and biological evaluation in both in vitro and in vivo models.

Keywords: cardiac cell therapy, cardiac ischemia, natural polymers, thermosensitive hydrogel

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Authors: Harsha B. R., K. S. Anil Kumar

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Land characterization, classification, and soil suitability evaluation of grapes-growing pedons were assessed at fifteen taluks covering four agro climatic zones of Karnataka. Study on problems and potentials of grapes cultivation in selected agro-climatic zones was carried out along with the plant sample analysis. Twenty soil profiles were excavated as study site based on the dominance of area falling under grapes production and existing spatial variability of soils. The detailed information of profiles and horizon wise soil samples were collected to study the morphological, physical, chemical, and fertility characteristics. Climatic analysis and water retention characteristics of soils of major grapes-growing areas were also done. Based on the characterisation and classification study, it was revealed that soils of Doddaballapur (Bangalore Blue and Wine grapes), Bangalore North (GKVK Farm, Rajankunte, and IIHR Farm), Devanahalli, Magadi, Hoskote, Chikkaballapur (Dilkush and Red globe), Yelaburga, Hagari Bommanahalli, Bagalkot (UHS farm) and Indi fall under the soil order Alfisol. Vijaypur pedon of northern dry zone was keyed out as Vertisols whereas, Jamkhandi and Athani as Inceptisols. Properties of Aridisols were observed in B. Bagewadi (Manikchaman and Thompson Seedless) and Afzalpur. Soil fertility status and its mapping using GIS technique revealed that all the nutrients were found to be in adequate range except nitrogen, potassium, zinc, iron, and boron, which indicated the need for application along with organic matter to improve the SOC status. Varieties differed among themselves in yield and plant nutrient composition depending on their age, climatic, soil, and management requirements. Bangalore North (GKVK farm) and Jamkhandi are having medium soil organic carbon stocks of 6.21 and 6.55 kg m⁻³, respectively. Soils of Bangalore North (Rajankunte) were highly suitable (S1) for grapes cultivation. Under northern Karnataka, Vijayapura, B. Bagewadi, Indi, and Afzalpur vineyards were good performers despite the limitations of fertility and free lime content.

Keywords: land characterization, suitability, soil orders, soil organic carbon stock

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Authors: Djiazet Stève, Mezajoug Kenfack Laurette Blandine, Ravi Pullakhandam, Bethala L. A. Prabhavathi Devi, Tchiegang Clergé, Prathapkumar Halady Shetty

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The nutritional potential of a developed spice formulation for nah poh was evaluated. It was found that when spices were used for the formulation for nah poh, the concentration of some nutrients is diluted while that of some of them increases. The proportion of unsaturated fats was estimated to be 76.2% of the total fat content while the chemical score varied between 31 to 39%. The contents of some essential minerals of nutritional interest in mg are as follows for 100g of spice: 2372.474 ± 0.007 for potassium, 16.447 ± 0.010 for iron, 4.772 ± 0.005 for zinc, 0.537 ± 0.001 for cupper, 0.138 ± 0.005 for selenium, and 112.954 ± 0.003 for manganese. This study shows that the consumption of these spices in the form of formulation significantly contributes to meet the mineral requirements of the populations whose food habits regularly require these spices.

Keywords: spice formulation, characterisation, nutritional potential, nah poh, techno functional properties

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Authors: K. Melouk, M. Dellakrachaï

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Analytical formula for the optical gain based on a simple parabolic-band by introducing theoretical expressions for the quantized energy is presented. The model used in this treatment take into account the effects of intraband relaxation. It is shown, as a result, that the gain for the TE mode is larger than that for TM mode and the presence of acceptor impurity increase the peak gain.

Keywords: InGaAsP, laser, quantum well, semiconductor

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Authors: L. F. Tamele Jr., G. Buonocore, H. F. Muiambo

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Asphalt binders play an essential role in the performance and properties of asphalt mixtures. The increase in heavy loads, greater traffic volume, and high tire pressure, combined with a substantial variation in daily and seasonal pavement temperatures, are the main responsible for the failure of asphalt pavements. To avoid or mitigate these failures, the present research proposes the use of thermoplastic polymers, HDPE and LLDPE, and nanoclay Dellite 43B for modification of asphalt in order to improve its thermomechanical and rheological properties. The nanocomposites were prepared by the solution intercalation method in a high shear mixer for a mixing time of 2 h, at 180℃ and 5000 rpm. The addition of Dellite 43B improved the physical, rheological, and thermal properties of asphalt, either separated or in the form of polymer/bitumen blends. The results of the physical characterization showed a decrease in penetration and an increase in softening point, thermal susceptibility, viscosity, and stiffness. On the other hand, thermal characterization showed that the nanocomposites have greater stability at higher temperatures by exhibiting greater amounts of residues and improved initial and final decomposition temperatures. Thus, the modification of asphalt by polymers and nanoclays seems to be a suitable solution for road pavement in countries which experiment with high temperatures combined with long heavy rain seasons.

Keywords: asphalt, nanoclay dellite 43B, polymer modified asphalt, thermal and rheological properties

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Authors: P. S. Rajinikanth, Shobana Mariappan, Jestin Chellian

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The objective of the study was to prepare and characterize a water-in-oil nano emulsion of 5-Fluorouracil (5FU) to enhance the skin penetration. The present study describes a nano emulsion of 5FU using Capyrol PGMC, Transcutol HP and PEG 400 as oil, surfactant and co-surfactant, respectively. The optimized formulations were further evaluated for heating cooling cycle, centrifugation studies, freeze thaw cycling, particle size distribution and zeta potential in order to confirm the stability of the optimized nano emulsions. The in-vitro characterization results showed that the droplets of prepared formulation were ~100 nm with ± 15 zeta potential. In vitro skin permeation studies was conducted in albino mice skin. Significant increase in permeability parameters was also observed in nano emulsion formulations (P<0.05). The steady-state flux (Jss), enhancement ration and permeability coefficient (Kp) for optimized nano emulsion formulation (FU2, FU1, 1:1 S mix were found to be 24.21 ±2.45 μg/cm2/h, 3.28±0.87 & 19.52±1.87 cm/h, respectively), which were significant compared with conventional gel. The in vitro and in vivo skin deposition studies in rat indicated that the amount of drug deposited from the nano emulsion (292.45 µg/cm2) in skin was significant (P<0.05) an increased as compared to a conventional 5FU gel (121.42 µg/cm2). The skin irritation study using rat skin showed that the mean irritation index of the nano emulsion reduced significantly (P<0.05) as compared with conventional gel contain 1% 5FU. The results from this study suggest that a water-in-oil nano emulsion could be safely used to promote skin penetration of 5FU following topical application.

Keywords: nano emulsion, controlled release, 5 fluorouracil, skin penetration, skin irritation

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Authors: Muhammad Arshad, Ghulam Hussain Bhatti, Abdul Qayyum

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Zinc-doped silica oxide nanoparticles having size 7.93nm were synthesized by the deposition precipitation method by using different solvents (acetonitrile, n-hexane, isoamylalchol). Biological potential such as antibacterial activities against Bacillussubtilusand Escherichia coli, and antifungal activities against Candida parapsilosis and Aspergilusniger were also investigated by Disc diffusion method. Different characterizations techniques including Fournier Transmission Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Thermo-gravimeteric Analysis (TGA), Atomic forced microscopy (AFM), and Dynamic Light Scattering (DLS) were used. FT-IR characterization confirmed the presence of metal oxide bond (SiO2) while XRD showed the hexagonal structure. SEM and TEM characterization showed the morphology of nanoparticles. AFM study showed good particle size distribution as depicted by a histogram. DLS study showed the gradual decease in the size of nanoparticles from 24.86nm to 13.24 nm. Highest antibacterial activities revealed by acetonitrile solvents (6%and 4.5%) followed by isoamylalchol (3% and 2.4%) while n-hexane solvent showed the lowest activity (2%and 1%) respectively. Higher antifungal activities exhibited by n-hexane (0.34 % and 0.43%) followed by isoamylalchol (0.27% and 0.19%) solvent while acetonitrile (0.21% and 0.17%) showed least activity respectively. Statistical analysis by using one-way ANOVA also indicated the significant results of both biological activities.

Keywords: nanoparticles, precipitation methods, antibacterial, antifungal, characterizations

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Authors: Belete B. Beyene, Ayenew M. Mihirteu, Misganaw T. Ayana, Amogne W. Yibeltal

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Modification of synthetic porphyrins is one of the promising strategies in an attempt to get molecules with desired properties and applications. Here in, we report synthesis, photophysical characterization and antibacterial activity of 5, 10, 15, 20-tetrakis-(4- methoxy carbonyl phenyl) porphyrin M(II); where M = Co, Fe, Ni, Zn. Metallation of the ligand was confirmed by using UV–Vis spectroscopy and ESI-Ms measurement, in which the number of Q bands in absorption spectra of the ligand decreased from four to one or two as a result of metal insertion to the porphyrin core. The antibacterial activity study of the complexes toward two Gram-positive (Staphylococcus aureus (S. aureus) and Streptococcus pyogenes (s. pyogenes)) and two Gram-negative (Escherichia coli (E. coli) and Klebsiella pneumoniae (K. pneumoniae)) bacteria by disc diffusion method showed a promising inhibitory activity. The complexes exhibited highest activities at highest concentration and were better than the activity of free base ligand, the salts, and blank solution. This could be explained on the basis of Overton's concept of cell permeability and Tweed's Chelation theory. An increased lipo-solubility enhances the penetration of the complexes into the lipid membrane and interferes with the normal activities of the bacteria. Our study, therefore, showed that the growth inhibitory effect of these metalloporphyrins is generally in order of ZnTPPCOOMe > NiTPPCOOMe > CoTPPCOOMe> FeTPPCOOMe, which may be attributed to the better lipophilicity and binding of the complex with the cellular components.

Keywords: porphyrins, metalloporphyrins, spectral property, antibacterial activity, synthesis

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Authors: Malek Mahmoudi, Jonas Keruckas, Dmytro Volyniuk, Jurate Simokaitiene, Juozas V. Grazulevicius

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Host materials have been discovered as one of the most appealing methods for harvesting triplet states in organic materials for application in organic light-emitting diodes (OLEDs). The ideal host-guest system for emission in thermally delayed fluorescence OLEDs with 20% guest concentration for efficient energy transfer has been demonstrated in the present investigation. In this work, 3,3'-bis[9-(4-fluorophenyl) carbazole] (bFPC) has been used as the host, which induces balanced charge carrier transport for high-efficiency OLEDs.For providing a complete characterization of the synthesized compound, photophysical, photoelectrical, charge-transporting, and electrochemical properties of the compound have been examined. Excited-state lifetimes and singlet-triplet energy gaps were measured for characterization of photophysical properties, while thermogravimetric analysis, as well as differential scanning calorimetry measurements, were performed for probing of electrochemical and thermal properties of the compound. The electrochemical properties of this compound were investigated by cyclic voltammetry (CV) method, and ionization potential (IPCV) value of 5.68 eV was observed. UV–Vis absorption and photoluminescence spectrum of a solution of the compound in toluene (10-5 M) showed maxima at 302 and 405 nm, respectively. Photoelectron emission spectrometry was used for the characterization of charge-injection properties of the studied compound in solid. The ionization potential of this material was found to be 5.78 eV, and time-of-flight measurement was used for testing charge-transporting properties and hole mobility estimated using this technique in a vacuum-deposited layer reached 4×10-4 cm2 V-1s-1. Since the compound with high charge mobilities was tested as a host in an organic light-emitting diode. The device was fabricated by successive deposition onto a pre-cleaned indium tin oxide (ITO) coated glass substrate under a vacuum of 10-6 Torr and consisting of an indium-tin-oxide anode, hole injection and transporting layer(MoO3, NPB), emitting layer with bFPC as a host and 4CzIPN (2,4,5,6-tetra(9-carbazolyl)isophthalonitrile) which is a new highly efficient green thermally activated delayed fluorescence (TADF) material as an emitter, an electron transporting layer(TPBi) and lithium fluoride layer topped with aluminum layer as a cathode exhibited the highest maximum current efficiency and power efficiency of 33.9 cd/A and 23.5 lm/W, respectively and the electroluminescence spectrum showed only a peak at 512nm. Furthermore, the new bicarbazole-based compound was tested as a host in thermally activated delayed fluorescence organic light-emitting diodes are reaching luminance of 25300 cd m-2 and external quantum efficiency of 10.1%. Interestingly, the turn-on voltage was low enough (3.8 V), and such a device can be used for highly efficient light sources.

Keywords: thermally-activated delayed fluorescence, host material, ionization energy, charge mobility, electroluminescence

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Authors: N. Ouslimani, N. Hakimi, H. Aksas

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The reduction of oil reserves in the world makes that many countries are directed towards the study and the use of local and renewable energies. For this purpose, wood energy represents the material of choice. The energy production is primarily thermal and corresponds to a heating of comfort, auxiliary or principal. Wood is generally conditioned in the form of logs, of pellets, even of plates. In Algeria, this way of energy saving could contribute to the safeguarding of the environment, as to the recovery of under wood products (branches, barks and various wastes on the various transformation steps). This work is placed within the framework general of the search for new sources of energy starting from the recovery of the lignocellulosic matter. In this direction, we proposed various sources of products (biomass, under product and by-products) relating to the ‘Eucalyptus species’ being able to be developed, of which we carried out a preliminary physicochemical study, necessary to the development of the densified products with high calorific value.

Keywords: biomass, calorific value, combustion, energy recovery

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Authors: Jianshu Yang, Delphine Sordes, Marek Kolmer, Christian Joachim

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Nanoelectronics, for example the calculating circuits integrating at molecule scale logic gates, atomic scale circuits, has been constructed and investigated recently. A major challenge is their functional properties characterization because of the connecting problem from atomic scale to micrometer scale. New experimental instruments and new processes have been proposed therefore. To satisfy a precisely measurement at atomic scale and then connecting micrometer scale electrical integration controller, the technique improvement is kept on going. Our new machine, a low temperature high vacuum four scanning tunneling microscope, as a customer required instrument constructed by Omicron GmbH, is expected to be scaling down to atomic scale characterization. Here, we will present our first testified results about the performance of this new instrument. The sample we selected is Au(111) surface. The measurements have been taken at 4.2 K. The atomic resolution surface structure was observed with each of four scanners with noise level better than 3 pm. With a tip-sample distance calibration by I-z spectra, the sample conductance has been derived from its atomic locally I-V spectra. Furthermore, the surface conductance measurement has been performed using two methods, (1) by landing two STM tips on the surface with sample floating; and (2) by sample floating and one of the landed tips turned to be grounding. In addition, single atom manipulation has been achieved with a modified tip design, which is comparable to a conventional LT-STM.

Keywords: low temperature ultra-high vacuum four scanning tunneling microscope, nanoelectronics, point contact, single atom manipulation, tunneling resistance

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Authors: A. A Warra, S. Fatima

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The experimental investigation revealed that the hexane extract of onion seed oil has acid value, iodine value, peroxide value, saponification value, relative density and refractive index of 0.03±0.01 mgKOH/g, 129.80±0.21 gI2/100g, 3.00± 0.00 meq H2O2 203.00±0.71 mgKOH/g, 0.82±0.01and 1.44±0.00 respectively. The percentage yield was 50.28±0.01%. The colour of the oil was light green. We restricted our GC-MS spectra interpretation to compounds identification, particularly fatty acids and they are identified as palmitic acid, linolelaidic acid, oleic acid, stearic acid, behenic acid, linolenic acid and eicosatetraenoic acid. The pH , foam ability (cm³), total fatty matter, total alkali and percentage chloride of the onion oil soap were 11.03± 0.02, 75.13±0.15 (cm³), 36.66 ± 0.02 %, 0.92 ± 0.02% and 0.53 ± 0.15 % respectively. The texture was soft and the colour was lighter green. The results indicated that the hexane extract of the onion seed oil has potential for cosmetic industries.

Keywords: onion seeds, soxhlet extraction, physicochemical, GC-MS, cold saponification

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Authors: Ramzi Farra, Detre Teschner, Marc Willinger, Robert Schlögl

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Introduction: The conventional approach of characterizing solid catalysts under static conditions, i.e., before and after reaction, does not provide sufficient knowledge on the physicochemical processes occurring under dynamic conditions at the molecular level. Hence, the necessity of improving new in situ characterizing techniques with the potential of being used under real catalytic reaction conditions is highly desirable. In situ Prompt Gamma Activation Analysis (PGAA) is a rapidly developing chemical analytical technique that enables us experimentally to assess the coverage of surface species under catalytic turnover and correlate these with the reactivity. The catalytic HCl oxidation (Deacon reaction) over bulk ceria will serve as our example. Furthermore, the in situ Transmission Electron Microscopy is a powerful technique that can contribute to the study of atmosphere and temperature induced morphological or compositional changes of a catalyst at atomic resolution. The application of such techniques (PGAA and TEM) will pave the way to a greater and deeper understanding of the dynamic nature of active catalysts. Experimental/Methodology: In situ Prompt Gamma Activation Analysis (PGAA) experiments were carried out to determine the Cl uptake and the degree of surface chlorination under reaction conditions by varying p(O2), p(HCl), p(Cl2), and the reaction temperature. The abundance and dynamic evolution of OH groups on working catalyst under various steady-state conditions were studied by means of in situ FTIR with a specially designed homemade transmission cell. For real in situ TEM we use a commercial in situ holder with a home built gas feeding system and gas analytics. Conclusions: Two complimentary in situ techniques, namely in situ PGAA and in situ FTIR were utilities to investigate the surface coverage of the two most abundant species (Cl and OH). The OH density and Cl uptake were followed under multiple steady-state conditions as a function of p(O2), p(HCl), p(Cl2), and temperature. These experiments have shown that, the OH density positively correlates with the reactivity whereas Cl negatively. The p(HCl) experiments give rise to increased activity accompanied by Cl-coverage increase (opposite trend to p(O2) and T). Cl2 strongly inhibits the reaction, but no measurable increase of the Cl uptake was found. After considering all previous observations we conclude that only a minority of the available adsorption sites contribute to the reactivity. In addition, the mechanism of the catalysed reaction was proposed. The chlorine-oxygen competition for the available active sites renders re-oxidation as the rate-determining step of the catalysed reaction. Further investigations using in situ TEM are planned and will be conducted in the near future. Such experiments allow us to monitor active catalysts at the atomic scale under the most realistic conditions of temperature and pressure. The talk will shed a light on the potential and limitations of in situ PGAA and in situ TEM in the study of catalyst dynamics.

Keywords: CeO2, deacon process, in situ PGAA, in situ TEM, in situ FTIR

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Authors: Moncayo Donoso Miguelangel, Guevara Morales Johana, Kalenia Flores Kalenia, Barrera Avellaneda Luis Alejandro, Garzon Alvarado Diego Alexander

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In mammals, long bones are formed by ossification of a cartilage mold during early embryonic development, forming structures called secondary ossification centers (SOCs), a primary ossification center (POC) and growth plates. This last structure is responsible for long bone growth. During the femur growth, the morphology of the growth plate and the SOCs may vary during different developmental stages. So far there are no detailed morphological studies of the development process from embryonic to adult stages. In this work, we carried out a morphological characterization of femur development from embryonic period to adulthood in mice. 15, 17 and 19 days old embryos and 1, 7, 14, 35, 46 and 52 days old mice were used. Samples were analyzed by a computational approach, using 3D images obtained by micro-CT imaging. Results obtained in this study showed that femur, its growth plates and SOCs undergo morphological changes during different stages of development, including changes in shape, position and thickness. These variations may be related with a response to mechanical loads imposed for muscle development surrounding the femur and a high activity during early stages necessary to support the high growth rates during first weeks and years of development. This study is important to improve our knowledge about the ossification patterns on every stage of bone development and characterize the morphological changes of important structures in bone growth like SOCs and growth plates.

Keywords: development, femur, growth plate, mice

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Authors: Laura X. Martinez, Andrés F. Rodríguez, Ruth A. Catacoli

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One of the most important factors for air pollution is that the concentrations of PM₁₀ maintain a constant trend, with the exception of some places where that frequently surpasses the allowed ranges established by Colombian legislation. The community that surrounds the Universidad Libre Bogotá is inhabited by a considerable number of students and workers, all of whom are possibly being exposed to PM₁₀ for long periods of time while on campus. Thus, the chemical characterization of PM₁₀ found in the ambient air at the Universidad Libre Bogotá was identified as a problem. A Hi-Vol sampler and EPA Test Method 5 were used to determine if the quality of air is adequate for the human respiratory system. Additionally, quartz fiber filters were utilized during sampling. Samples were taken three days a week during a dry period throughout the months of November and December 2015. The gravimetric analysis method was used to determine PM₁₀ concentrations. The chemical characterization includes non-conventional carcinogenic pollutants. Atomic absorption spectrophotometry (AAS) was used for the determination of metals and VOCs were analyzed using the FTIR (Fourier transform infrared spectroscopy) method. In this way, concentrations of PM₁₀, ranging from values of 13 µg/m³ to 66 µg/m³, were obtained; these values were below standard conditions. This evidence concludes that the PM₁₀ concentrations during an exposure period of 24 hours are lower than the values established by Colombian law, Resolution 610 of 2010; however, when comparing these with the limits set by the World Health Organization (WHO), these concentrations could possibly exceed permissible levels.

Keywords: air quality, atomic absorption spectrophotometry, gas chromatography, particulate matter

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Authors: Sukhwinder K. Bhullar, M. B. G. Jun

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The developments in biomedical industry have demanded the development of biocompatible, high performance materials to meet higher engineering specifications. The general requirements of such materials are to provide a combination of high stiffness and strength with significant weight savings, resistance to corrosion, chemical resistance, low maintenance, and reduced costs. Auxetic materials which come under the category of smart materials offer huge potential through measured enhancements in mechanical properties. Unique deformation mechanism, providing cushioning on indentation, automatically adjustable with its strength and thickness in response to forces and having memory returns to its neutral state on dissipation of stresses make them good candidate in biomedical industry. As simple extension and compression of tissues is of fundamental importance in biomechanics, therefore, to study the elastic behaviour of auxetic soft tissues implant is targeted in this paper. Therefore development and characterization of auxetic soft tissue implant is studied in this paper. This represents a real life configuration where soft tissue such as meniscus in knee replacement, ligaments and tendons often are taken as transversely isotropic. Further, as composition of alternating polydisperse blocks of soft and stiff segments combined with excellent biocompatibility make polyurethanes one of the most promising synthetic biomaterials. Hence selecting auxetic polyurathylene foam functional characterization is performed and compared with conventional polyurathylene foam.

Keywords: auxetic materials, deformation mechanism, enhanced mechanical properties, soft tissues

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Authors: J. Subbalakshmi, G. Dhruvasamhith, S. M. Hussain

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Polyaniline (PANI) is one of the most extensively studied material among the conducting polymers due to its simple synthesis by chemical and electrochemical routes. PANIs have advantages of chemical stability and high conductivity making their commercial applications quite attractive. However, to our knowledge, very little work has been reported on the tensile strength properties of templated PANIs processed with polyvinyl alcohol and also, detailed study has not been carried out. We have investigated the effect of small molecule and polymers as templates on PANI. Stable aqueous colloidal suspensions of trisodium citrate (TSC), poly(ethylenedioxythiophene)-polystyrene sulfonate (PEDOT-PSS), and polyethylene glycol (PEG) templated PANIs were prepared through chemical synthesis, processed with polyvinyl alcohol (PVA) and were fabricated into films by solution casting. Absorption and infra-red spectra were studied to gain insight into the possible molecular interactions. Surface morphology was studied through scanning electron microscope and optical microscope. Interestingly, tensile testing studies revealed least strain for pure PVA when compared to the blends of templated PANI. Furthermore, among the blends, TSC templated PANI possessed maximum elasticity. The ultimate tensile strength for PVA processed, PEG-templated PANI was found to be five times more than other blends considered in this study. We establish structure–property correlation with morphology, spectral characterization and tensile testing studies.

Keywords: surface morphology, processed films, polyvinyl alcohol, templated polyanilines, tensile testing

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Authors: Nikola Góral, Piotr Mikołajczuk, Paweł Buczyński

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Much scientific research in the last 20 years has focused on the influence of global warming on the distribution and phenology of living organisms. Three potential responses to climate change are predicted: individual species may become extinct, adapt to new conditions in their existing range or change their range by migrating to places where climatic conditions are more favourable. It means not only migration to areas in other latitudes, but also different altitudes. In the case of dragonflies (Odonata), monitoring in Western Europe has shown that in response to global warming, dragonflies tend to change their range to a more northern one. The strongest response to global warming is observed in arctic and alpine species, as well as in species capable of migrating over long distances. The aim of the research was to assess whether the fauna of aquatic insects in high-mountain habitats has changed as a result of climate change and, if so, how big and what type these changes are. Dragonflies were chosen as a model organism because of their fast reaction to changes in the environment: they have high migration abilities and short life cycle. The state of the populations of boreal-mountain species and the extent to which lowland species entered high altitudes was assessed. The research was carried out on 20 sites in Western Sudetes, Southern Poland. They were located at an altitude of between 850 and 1250 m. The selected sites were representative of many types of valuable alpine habitats (subalpine raised bog, transitional spring bog, habitats associated with rivers and mountain streams). Several sites of anthropogenic origin were also selected. Thanks to this selection, a wide characterization of the fauna of the Karkonosze was made and it was compared whether the studied processes proceeded differently, depending on whether the habitat is primary or secondary. Both imagines and larvae were examined (by taking hydrobiological samples with a kick-net), and exuviae were also collected. Individual species dragonflies were characterized in terms of their reproductive, territorial and foraging behaviour. During each inspection, the basic physicochemical parameters of the water were measured. The population of the high-mountain dragonfly Somatochlora alpestris turned out to be in a good condition. This species was noted at several sites. Some of those sites were situated relatively low (995 m AMSL), which proves that the thermal conditions at the lower altitudes might be still optimal for this species. The protected by polish law species Somatochlora arctica, Aeshna subarctica and Leucorrhinia albifrons, as well as strongly associated with bogs Leucorrhinia dubia and Aeshna juncea bogs were observed. However, they were more frequent and more numerous in habitats of anthropogenic origin, which may suggest minor changes in the habitat preferences of dragonflies. The subject requires further research and observations over a longer time scale.

Keywords: alpine species, bioindication, global warming, habitat preferences, population dynamics

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Authors: Begüm Terzi, Özlem Ateş Sönmezoğlu, Ahmet Yildirim

Abstract:

Drought is the most important factor that limiting the production and productivity of wheat in the world. The yield of wheat, which is one of the most important crop in the world, reduced depend on drought. Researches to minimize effects of drought are one of the most important about breeding of drought resistant varieties. In recent years, benefiting from the drought resistance wild species and rapid advances in molecular biology studies, researches about drought have been accelerated and number of studies were made on molecular plant breeding which included the molecular mechanisms related to drought resistance. The aim of the present study was characterization of some bread wheat lines for drought tolerance which commonly cultivated in different location of Turkey. In this study, registered 9 bread wheat varieties which on the physiological tests about drought tolerance and 10 bread wheat line has been developed by Transitional Zone Agricultural Research Institute were used. SSR, STS, RAPD and SNP markers that associated with drought tolerance were used. The polymorphisms of the markers were determined by screening of two control varieties. For these purpose 40 molecular markers were used and 12 markers of them were polymorphic among the drought tolerance and the drought sensitive varieties. Control varieties were screened using polymorphic markers. All the DNAs on the genotypes will be searched for the presence of QTLs mapped to different chromosomes. Result of the research, the studied genotypes will be grouped according to drought tolerance and will be detected drought tolerance varieties by molecular markers. In addition, the results will be compared also with physiological tests. The drought tolerant wheat genotypes may be used in breeding studies related to drought stress.

Keywords: bread wheat, drought, molecular marker, Triticum aestivum

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Authors: A. Hassiba Zemmouri, B. Nabil Mameri, C. Hakim Lounici

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In this study, the effect of Fenton technology pretreatment on the anaerobic digestion of excess waste activated sludge (WAS) was investigated. The variation of physicochemical characteristics (TOC, DS, VSS, VS) and biogas volume (as form of value added products) were also evaluated. The preselected operator conditions of Fenton pretreatment were 0.01ml H2O2/g SS, 150 [H2O2]/[Fe2+], 25g/l TS, at 25 °C and 30, 60 and120 min as treatment duration. The main results show a Maximum solubilization and biodegradability (70%) obtained at 120 min of Fenton pretreatment duration. An increasing of TOC in soluble phase related obviously by releasing organic substances of sludge flocs was contested. Improving in biogas volume was also, increased. Fenton oxidation pretreatment may be a promising chemical pre-treatment for a benefic digestion, stabilization and volume reduction.

Keywords: waste activated sludge, fenton pre-treatment, biodegradability, biogas

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Authors: Ubeyd Toçoğlu, Miraç Alaf, Hatem Akbulut

Abstract:

We present a work which was conducted in order to improve the cycle life of silicon based lithium ion battery anodes by utilizing novel composite structure. In this study, carbon coated nano sized (50-100 nm) silicon particles were embedded into Graphene/MWCNT silicon matrix to produce free standing silicon based electrodes. Also, conventional Si powder anodes were produced from Si powder slurry on copper current collectors in order to make comparison of composite and conventional anode structures. Free –standing composite anodes (binder-free) were produced via vacuum filtration from a well dispersion of Graphene, MWCNT and carbon coated silicon powders. Carbon coating process of silicon powders was carried out via microwave reaction system. The certain amount of silicon powder and glucose was mixed under ultrasonication and then coating was conducted at 200 °C for two hours in Teflon lined autoclave reaction chamber. Graphene which was used in this study was synthesized from well-known Hummers method and hydrazine reduction of graphene oxide. X-Ray diffraction analysis and RAMAN spectroscopy techniques were used for phase characterization of anodes. Scanning electron microscopy analyses were conducted for morphological characterization. The electrochemical performance tests were carried out by means of galvanostatic charge/discharge, cyclic voltammetry and electrochemical impedance spectroscopy.

Keywords: graphene, Li-Ion, MWCNT, silicon

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Authors: Supreet Singh, Manpreet Kaur, Manoj Kumar

Abstract:

High temperature corrosion is an imperative material degradation method experienced in thermal power plants and other energy generation sectors. Metallic materials such as ferritic steels have special properties such as easy fabrication and machinibilty, low cost, but a serious drawback of these materials is the worsening in properties initiating from the interaction with the environments. The metallic materials do not endure higher temperatures for extensive period of time because of their poor corrosion resistance. Friction Stir Processing (FSP), has emerged as the potent surface modification means and control of microstructure in thermo mechanically heat affecting zones of various metal alloys. In the current research work, FSP was done on the boiler tube of SA 210 Grade A1 material which is regularly used by thermal power plants. The strengthening of SA210 Grade A1 boiler steel through microstructural refinement by Friction Stir Processing (FSP) and analyze the effect of the same on high temperature corrosion behavior. The high temperature corrosion performance of the unprocessed and the FSPed specimens were evaluated in the laboratory using molten salt environment of Na₂SO₄-82%Fe₂(SO₄). The unprocessed and FSPed low carbon steel Gr A1 evaluation was done in terms of microstructure, corrosion resistance, mechanical properties like hardness- tensile. The in-depth characterization was done by EBSD, SEM/EDS and X-ray mapping analyses with an aim to propose the mechanism behind high temperature corrosion behavior of the FSPed steel.

Keywords: boiler steel, characterization, corrosion, EBSD/SEM/EDS/XRD, friction stir processing

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Authors: Bouchra Wassate, Younes Karhat, Khadija El Falaki

Abstract:

Leachate is a source of surface water and groundwater contamination if it has not been pretreated. Indeed, due to its complex structure and its pollution load make its treatment extremely difficult to achieve the standard limits required. The objective of this work is to show the interest of advanced oxidation processes on leachate treatment of urban waste containing high concentrations of organic pollutants. The efficiency of Fenton (Fe2+ +H2O2 + H+) reagent for young leachate recovered from collection trucks household waste in the city of Casablanca, Morocco, was evaluated with the objectives of chemical oxygen demand (COD) and discoloration reductions. The optimization of certain physicochemical parameters (initial pH value, reaction time, and [Fe2+], [H2O2]/ [Fe2+] ratio) has yielded good results in terms of reduction of COD and discoloration of the leachate.

Keywords: COD removal, color removal, Fenton process, oxidation process, leachate

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Authors: Soumendu Monia, Vaibhav Jain, Hrishikesh Jugade, Manashi Adhikary, Goutam Mukhopadhyay

Abstract:

'Rolled in scale' (RIS) and 'Rolled in Scum' (RISc) are two superficial surface defects on cold rolled and annealed steel sheets which affect the aesthetics of surface and thereby that of the end-product. Both the defects are believed to be originating from distinctly different sources having different mechanisms of formation. However, due to their similar physical appearance, RIS and RISc are generally confused with each other and hence attaining the exact root cause for elimination of the defect becomes difficult. RIS appears irregular in shape, sometimes scattered, and always oriented in rolling direction. RISc is generally oval shaped, having identifiable pointed edges and mostly oriented in rolling direction. Visually, RIS appears to be greyish in colour whereas RISc is whitish in colour. Both the defects have quite random occurrence and do not leave any imprints on the reverse-side of the sheet. In the current study, an attempt has been made to differentiate these two similar looking surface defects using various metallographic and characterization techniques. Systematic experiments have been carried out to identify possible mechanisms of formation of these defects. Detailed characterization revealed basic differences between RIS and RISc with respect to their surface morphology. To summarize, RIS was observed as a residue of an otherwise under-pickled scale patch on surface, after it has been subjected to cold rolling and annealing in a batch/continuous furnace. Whereas RISc was found to be a localized rubbing of the surface, at the time of cold rolling itself, resulting in a rough surface texture.

Keywords: annealing, rolled in scale, rolled in scum, skin panel

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Authors: H. K. Esfahani, B. Datta

Abstract:

Groundwater is one of the most important natural resources in many parts of the world; however it is widely polluted due to human activities. Currently, effective and reliable groundwater management and remediation strategies are obtained using characterization of groundwater pollution sources, where the measured data in monitoring locations are utilized to estimate the unknown pollutant source location and magnitude. However, accurately identifying characteristics of contaminant sources is a challenging task due to uncertainties in terms of predicting source flux injection, hydro-geological and geo-chemical parameters, and the concentration field measurement. Reactive transport of chemical species in contaminated groundwater systems, especially with multiple species, is a complex and highly non-linear geochemical process. Although sufficient concentration measurement data is essential to accurately identify sources characteristics, available data are often sparse and limited in quantity. Therefore, this inverse problem-solving method for characterizing unknown groundwater pollution sources is often considered ill-posed, complex and non- unique. Different methods have been utilized to identify pollution sources; however, the linked simulation-optimization approach is one effective method to obtain acceptable results under uncertainties in complex real life scenarios. With this approach, the numerical flow and contaminant transport simulation models are externally linked to an optimization algorithm, with the objective of minimizing the difference between measured concentration and estimated pollutant concentration at observation locations. Concentration measurement data are very important to accurately estimate pollution source properties; therefore, optimal design of the monitoring network is essential to gather adequate measured data at desired times and locations. Due to budget and physical restrictions, an efficient and effective approach for groundwater pollutant source characterization is to design an optimal monitoring network, especially when only inadequate and arbitrary concentration measurement data are initially available. In this approach, preliminary concentration observation data are utilized for preliminary source location, magnitude and duration of source activity identification, and these results are utilized for monitoring network design. Further, feedback information from the monitoring network is used as inputs for sequential monitoring network design, to improve the identification of unknown source characteristics. To design an effective monitoring network of observation wells, optimization and interpolation techniques are used. A simulation model should be utilized to accurately describe the aquifer properties in terms of hydro-geochemical parameters and boundary conditions. However, the simulation of the transport processes becomes complex when the pollutants are chemically reactive. Three dimensional transient flow and reactive contaminant transport process is considered. The proposed methodology uses HYDROGEOCHEM 5.0 (HGCH) as the simulation model for flow and transport processes with chemically multiple reactive species. Adaptive Simulated Annealing (ASA) is used as optimization algorithm in linked simulation-optimization methodology to identify the unknown source characteristics. Therefore, the aim of the present study is to develop a methodology to optimally design an effective monitoring network for pollution source characterization with reactive species in polluted aquifers. The performance of the developed methodology will be evaluated for an illustrative polluted aquifer sites, for example an abandoned mine site in Queensland, Australia.

Keywords: monitoring network design, source characterization, chemical reactive transport process, contaminated mine site

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