Search results for: chemical doping

Authors: Suresh Vanguri, Suresh Palla, Prasad G., Ramaswamy V., Kalyani K. V., Chaturvedi S. K., Mohapatra B. N., Sunder Rao TBVN

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The utilization of industrial waste materials and by-products in the cement industry helps in the conservation of natural resources besides avoiding the problems arising due to waste dumping. The use of non-carbonated materials as raw mix components in clinker manufacturing is identified as one of the key areas to reduce Green House Gas (GHG) emissions. Chrome sludge is a waste material generated from the manufacturing process of sodium dichromate. This paper aims to present studies on the use of chrome sludge in clinker manufacturing, its impact on the development of clinker mineral phases and on the cement properties. Chrome sludge was found to contain substantial amounts of CaO, Fe2O3 and Al2O3 and therefore was used to replace some conventional sources of alumina and iron in the raw mix. Different mixes were prepared by varying the chrome sludge content from 0 to 5 % and the mixes were evaluated for burnability. Laboratory prepared clinker samples were evaluated for qualitative and quantitative mineralogy using X-ray Diffraction Studies (XRD). Optical microscopy was employed to study the distribution of clinker phases, their granulometry and mineralogy. Since chrome sludge also contains considerable amounts of chromium, studies were conducted on the leachability of heavy elements in the chrome sludge as well as in the resultant cement samples. Estimation of heavy elements, including chromium was carried out using ICP-OES. Further, the state of chromium valence, Cr (III) & Cr (VI), was studied using conventional chemical analysis methods coupled with UV-VIS spectroscopy. Assimilation of chromium in the clinker phases was investigated using SEM-EDXA studies. Bulk cement was prepared from the clinker to study the effect of chromium sludge on the cement properties such as setting time, soundness, strength development against the control cement. Studies indicated that chrome sludge can be successfully utilized and its content needs to be optimized based on raw material characteristics.

Keywords: chrome sludge, leaching, mineralogy, non-carbonate materials

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Authors: Juan Alfredo Guevara Carrio, Swamy Toolahalli Thipperudra, Riddhi Naik Dharmeshbhai, Sergio Graniero Echeverrigaray, Jose Vitorio Emiliano, Antonio Helio Castro

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In order to advance the hydrogen economy, several industrial sectors can potentially benefit from the trillions of stimulus spending for post-coronavirus. Blending hydrogen into natural gas pipeline networks has been proposed as a means of delivering it during the early market development phase, using separation and purification technologies downstream to extract the pure H₂ close to the point of end-use. This first step has been mentioned around the world as an opportunity to use existing infrastructures for immediate decarbonisation pathways. Among current technologies used to extract hydrogen from mixtures in pipelines or liquid carriers, membrane separation can achieve the highest selectivity. The most efficient approach for the separation of H₂ from other substances by membranes is offered from the research of 2D layered materials due to their exceptional physical and chemical properties. Graphene-based membranes, with their distribution of pore sizes in nanometers and angstrom range, have shown fundamental and economic advantages over other materials. Their combination with the structure of ceramic and geopolymeric materials enabled the synthesis of nanocomposites and the fabrication of membranes with long-term stability and robustness in a relevant range of physical and chemical conditions. Versatile separation modules have been developed for hydrogen separation, which adaptability allows their integration in industrial prototypes for applications in heavy transport, steel, and cement production, as well as small installations at end-user stations of pipeline networks. The developed membranes and prototypes are a practical contribution to the technological challenge of supply pure H₂ for the mentioned industries as well as hydrogen energy-based fuel cells.

Keywords: graphene nano-composite membranes, hydrogen separation and purification, separation modules, indsutrial prototype

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Authors: Barun Chakrabarti, Evangelos Kalamaras, Vladimir Yufit, Xinhua Liu, Billy Wu, Nigel Brandon, C. T. John Low

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In this work, we perform electrophoretic deposition of activated carbon on a number of substrates to prepare symmetrical coin cells for supercapacitor applications. From several recipes that involve the evaluation of a few solvents such as isopropyl alcohol, N-Methyl-2-pyrrolidone (NMP), or acetone to binders such as polyvinylidene fluoride (PVDF) and charging agents such as magnesium chloride, we display a working means for achieving supercapacitors that can achieve 100 F/g in a consistent manner. We then adapt this EPD method to deposit reduced graphene oxide on SGL 10AA carbon paper to achieve cathodic materials for testing in a hydrogen/vanadium flow battery. In addition, a self-supported hierarchical carbon nano-fibre is prepared by means of electrospray deposition of an iron phthalocyanine solution onto a temporary substrate followed by carbonisation to remove heteroatoms. This process also induces a degree of nitrogen doping on the carbon nano-fibres (CNFs), which allows its catalytic performance to improve significantly as detailed in other publications. The CNFs are then used as catalysts by attaching them to graphite felt electrodes facing the membrane inside an all-vanadium flow battery (Scribner cell using serpentine flow distribution channels) and efficiencies as high as 60% is noted at high current densities of 150 mA/cm². About 20 charge and discharge cycling show that the CNF catalysts consistently perform better than pristine graphite felt electrodes. Following this, we also test the CNF as an electro-catalyst in the hydrogen/vanadium flow battery (cathodic side as mentioned briefly in the first paragraph) facing the membrane, based upon past studies from our group. Once again, we note consistently good efficiencies of 85% and above for CNF modified graphite felt electrodes in comparison to 60% for pristine felts at low current density of 50 mA/cm² (this reports 20 charge and discharge cycles of the battery). From this preliminary investigation, we conclude that the CNFs may be used as catalysts for other systems such as vanadium/manganese, manganese/manganese and manganese/hydrogen flow batteries in the future. We are generating data for such systems at present, and further publications are expected.

Keywords: electrospinning, carbon nano-fibres, all-vanadium redox flow battery, hydrogen-vanadium fuel cell, electrocatalysis

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Authors: H. A. Jawan

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This review describes the models of environmental-related crack propagation of aluminum alloys (7xxx) during the last few decades. Acknowledge on effects of different factors on the susceptibility to SCC permits to propose valuable mechanisms on crack advancement. The reliable mechanism of cracking give a possibility to propose the optimum chemical composition and thermal treatment conditions resulting in microstructure the most suitable for real environmental condition and stress state.

Keywords: microstructure, environmental, propagation, mechanism

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Authors: Rashida Rahmat Zohra, Afsheen Aman, Shah Ali Ul Qader

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Commercially important biopolymer, dextran, is enzymatically degraded into lower molecular weight fractions of vast industrial potential. Various organisms are associated with dextranase production, among which fungal, yeast and bacterial origins are used for commercial production. Dextranases are used to remove contaminating dextran in sugar processing industry and also used in oral care products for efficient removal of dental plaque. Among the hydrolytic products of dextran, isomaltooligosaccharides have prebiotic effect in humans and reduces the cariogenic effect of sucrose in oral cavity. Dextran derivatives produced by hydrolysis of high molecular polymer are also conjugated with other chemical and metallic compounds for usage in pharmaceutical, fine chemical industry, cosmetics, and food industry. Owing to the vast application of dextran and dextranases, current study focused on purification and analysis of kinetic parameters of dextranase from a newly isolated strain of Bacillus licheniformis KIBGE-IB25. Dextranase was purified up to 35.75 folds with specific activity of 1405 U/mg and molecular weight of 158 kDa. Analysis of kinetic parameters revealed that dextranase performs optimum cleavage of low molecular weight dextran (5000 Da, 0.5%) at 35ºC in 15 min at pH 4.5 with a Km and Vmax of 0.3738 mg/ml and 182.0 µmol/min, respectively. Thermal stability profiling of dextranase showed that it retained 80% activity up to 6 hours at 30-35ºC and remains 90% active at pH 4.5. In short, the dextranase reported here performs rapid cleavage of substrate at mild operational conditions which makes it an ideal candidate for dextran removal in sugar processing industry and for commercial production of low molecular weight oligosaccharides.

Keywords: Bacillus licheniformis, dextranase, gel permeation chromatograpy, enzyme purification, enzyme kinetics

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Authors: Ramadan Ali Bawa, Ebtisam Mohammed Alzaraide

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The spectroscopic study on 4-(9-anthrylazo) phenol has revealed that the azo dye under study exists in two tautomeric forms which are azo phenol and hydrazo keto forms in ratio of almost (1:1). The azo hydrazone tautomerism was confirmed by the use of IR spectroscopy and HNMR in which the characteristic absorption bands and chemical shifts for both tautomers were assigned.

Keywords: spectroscopic, tautomeric forms, azo hydrazone tautomerism, IR spectroscopy, HNMR

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Authors: P. Hari Prasad Reddy, Shimna Paulose, V. Sai Kumar, C. H. Rama Vara Prasad

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Soil environment gets contaminated due to rapid industrialisation, agricultural-chemical application and improper disposal of waste generated by the society. Unexpected volume changes can occur in soil in the presence of certain contaminants usually after the long duration of interaction. Alkali is one of the major soil contaminant that has a considerable effect on behaviour of soils and capable of inducing swelling potential in soil. Chemical heaving of clayey soils occurs when they are wetted by aqueous solutions of alkalis. Mineralogical composition of the soil is one of the main factors influencing soil- alkali interaction. In the present work, studies are carried out to understand the swell potential of soils due to soil-alkali interaction with different concentrations of NaOH solution. Locally available soil, namely, red earth containing kaolinite which is of non-swelling nature is selected for the study. In addition to this, two commercially available clayey soils, namely ball clay and china clay containing mainly of kaolinite are selected to understand the effect of alkali interaction in various kaolinitic soils. Non-swelling red earth shows maximum swell at lower concentrations of alkali solution (0.1N) and a slightly decreasing trend of swelling with further increase in concentration (1N, 4N, and 8N). Marginal decrease in swell potential with increase in concentration indicates that the increased concentration of alkali solution exists as free solution in case of red earth. China clay and ball clay both falling under kaolinite group of clay minerals, show swelling with alkaline solution. At lower concentrations of alkali solution both the soils shows similar swell behaviour, but at higher concentration of alkali solution ball clay shows high swell potential compared to china clay which may be due to lack of well ordered crystallinity in ball clay compared to china clay. The variations in the results obtained were corroborated by carrying XRD and SEM studies.

Keywords: alkali, kaolinite, swell potential, XRD, SEM

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Authors: Cyril Deroy, Agata Rumianek, David R. Greaves, Peter R. Cook, Edmond J. Walsh

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Various microfluidic platforms have been developed in the past couple of decades offering experimental methods for the study of cell migration; however, their implementation in the laboratory has remained limited. Some reasons cited for the lack of uptake include the technical complexity of the devices, high failure rate associated with gas-bubbles, biocompatibility concerns with the use of polydimethylsiloxane (PDMS) and equipment/time/expertise requirements for operation and manufacture. As sample handling remains challenging due to the closed format of microfluidic devices, open microfluidic systems have been developed offering versatility and simplicity of use. Rather than confining fluids by solid walls, samples can be accessed directly over the open platform, by removing at least one of the solid boundaries, such as the cover. In this paper, a method for the fabrication of open fluid-walled microfluidic circuits for cell migration studies is introduced, where only materials commonly used by the life-science community are required; tissue culture dishes and cell media. The simplicity of the method, and ability to retrieve cells of interest are two key features of the method. Both passive and active flow-devices can be created in this way. To demonstrate the versatility of the method a cell migration assay is performed, which requires fabricating circuits for establishing chemical gradients, loading cells and incubating, creating chemical gradients, real time imaging of cell migration and finally retrieval of cells. The open architecture has high fidelity as it eliminates air bubble related failures and enables the precise control of gradients. The ability to fabricate custom microfluidic designs in minutes should make this method suitable for use in a wide range of cell migration studies.

Keywords: chemotaxis, fluid walls, gradient generation, open microfluidics

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Authors: Abayomi O. Adetuyi, Jamiu M. Jabar, Samuel O. Afolabi

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Vegetable fibres are classes of fibres of low density, biodegradable and non-abrasive that are largely abundant fibre materials with specific properties and mostly found/ obtained in plants on earth surface. They are classified into three categories, depending on the part of the plant from which they are gotten from namely: fruit, Blast and Leaf fibre. Ever since four/five millennium B.C, attention has been focussing on the commonest and highly utilized cotton fibre obtained from the fruit of cotton plants (Gossypium spp), for the production of cotton fabric used in every home today. The present study, therefore, focused on the ability of three underutilized vegetable (fruit) fibres namely: coir fiber (Eleas coniferus), palm kernel fiber and empty fruit bunch fiber (Elias guinensis) through chemical modifications for better composite value addition performance to polyurethane form and dye adsorption. These fibres were sourced from their parents’ plants, identified and cleansed with 2% hot detergent solution 1:100, rinsed in distilled water and oven-dried to constant weight, before been chemically modified through alkali bleaching, mercerization and acetylation. The alkali bleaching involves treating 0.5g of each fiber material with 100 mL of 2% H2O2 in 25 % NaOH solution with refluxing for 2 h. While that of mercerization and acetylation involves the use of 5% sodium hydroxide NaOH solution for 2 h and 10% acetic acid- acetic anhydride 1:1 (v/v) (CH3COOH) / (CH3CO)2O solution with conc. H2SO4 as catalyst for 1 h, respectively on the fibres. All were subsequently washed thoroughly with distilled water and oven dried at 105 0C for 1 h. These modified fibres were incorporated as composite into polyurethane form and used in dye adsorption study of indigo. The first two treatments led to fiber weight reduction, while the acidified acetic anhydride treatment gave the fibers weight increment. All the treated fibers were found to be of less hydrophilic nature, better mechanical properties, higher thermal stabilities as well as better adsorption surfaces/capacities than the untreated ones. These were confirmed by gravimetric analysis, Instron Universal Testing Machine, Thermogravimetric Analyser and the Scanning Electron Microscope (SEM) respectively. The fiber morphology of the modified fibers showed smoother surfaces than unmodified fibres.The empty fruit bunch fibre and the coconut coir fibre are better than the palm kernel fibres as reinforcers for composites or as adsorbents for waste-water treatment. Acetylation and alkaline bleaching treatment improve the potentials of the fibres more than mercerization treatment. Conclusively, vegetable fibres, especially empty fruit bunch fibre and the coconut coir fibre, which are cheap, abundant and underutilized, can replace the very costly powdered activated carbon in wastewater treatment and as reinforcer in foam.

Keywords: chemical modification, industrial application, value addition, vegetable fibre

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Authors: Golam Saklayen, Sheikh Rashel al Ahmed, Ferdous Rahman, Ismail Abu Bakar

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Investigation on Lanthanum Fluoride LaF3 layer embedding Silicon Nanocrystals (Si-NCs) fabricated using a novel one-step chemical method has been reported in this presentation. Application of this material has been tested for low-voltage operating non-volatile memory and Schottkey-junction solar cell. Colloidal solution of Si-NCs in hydrofluoric acid (HF) was prepared from meso-porous silicon by ultrasonic vibration (sonication). This solution prevents the Si-NCs to be oxidized. On a silicon (Si) substrate, LaCl3 solution in HCl is allowed to react with the colloidal solution of prepared Si-NCs. Since this solution contains HF, LaCl3 reacts with HF and produces LaF3 crystals that deposits on the silicon substrate as a layer embedding Si-NCs. This a novel single step chemical way of depositing LaF3 insulating layer embedding Si-NCs. The X-Ray diffraction of the deposited layer shows a polycrystalline LaF3 deposition on silicon. A non-stoichiometric LaF3 layer embedding Si-NCs was found by EDX analysis. The presence of Si-NCs was confirmed by SEM. FTIR spectroscopy of the deposited LaF3 powder also confirmed the presence of Si-NCs. The size of Si-NCs was found to be inversely proportional to the ultrasonic power. After depositing proper contacts on the back of Si and LaF3, the devices have been tested as a non-volatile memory and solar cell. A memory window of 525 mV was obtained at a programming and erasing bias of 2V. The LaF3 films with Si NCs showed strong absorption and was also found to decrease optical transmittance than pure LaF3 film of same thickness. The I-V characteristics of the films showed a dependency on the incident light intensity where current changed under various light illumination. Experimental results show a lot of promise for Si-NCs-embedded LaF3 layer to be used as an insulating layer in MIS devices as well as an photoactive material in Schottkey junction solar cells.

Keywords: silicon nanocrystals (Si NCs), LaF3, colloidal solution, Schottky junction solar cell

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Authors: David A. Olasehinde, Peter I. Olasehinde, Segun M. A. Adelana, Dapo O. Olasehinde

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An investigation was carried out on underground water system dynamics within Ilorin metropolis to monitor the subsurface flow and its corresponding pollution. Africa population growth rate is the highest among the regions of the world, especially in urban areas. A corresponding increase in waste generation and a change in waste composition from predominantly organic to non-organic waste has also been observed. Percolation of leachate from non-engineered landfills, the chief means of waste disposal in many of its cities, constitutes a threat to the underground water bodies. Ilorin city, a transboundary town in southwestern Nigeria, is a ready microcosm of Africa’s unique challenge. In spite of the fact that groundwater is naturally protected from common contaminants such as bacteria as the subsurface provides natural attenuation process, groundwater samples have been noted to however possesses relatively higher dissolved chemical contaminants such as bicarbonate, sodium, and chloride which poses a great threat to environmental receptors and human consumption. The Geographic Information System (GIS) was used as a tool to illustrate, subsurface dynamics and the corresponding pollutant indicators. Forty-four sampling points were selected around known groundwater pollutant, major old dumpsites without landfill liners. The results of the groundwater flow directions and the corresponding contaminant transport were presented using expert geospatial software. The experimental results were subjected to four descriptive statistical analyses, namely: principal component analysis, Pearson correlation analysis, scree plot analysis, and Ward cluster analysis. Regression model was also developed aimed at finding functional relationships that can adequately relate or describe the behaviour of water qualities and the hypothetical factors landfill characteristics that may influence them namely; distance of source of water body from dumpsites, static water level of groundwater, subsurface permeability (inferred from hydraulic gradient), and soil infiltration. The regression equations developed were validated using the graphical approach. Underground water seems to flow from the northern portion of Ilorin metropolis down southwards transporting contaminants. Pollution pattern in the study area generally assumed a bimodal pattern with the major concentration of the chemical pollutants in the underground watershed and the recharge. The correlation between contaminant concentrations and the spread of pollution indicates that areas of lower subsurface permeability display a higher concentration of dissolved chemical content. The principal component analysis showed that conductivity, suspended solids, calcium hardness, total dissolved solids, total coliforms, and coliforms were the chief contaminant indicators in the underground water system in the study area. Pearson correlation revealed a high correlation of electrical conductivity for many parameters analyzed. In the same vein, the regression models suggest that the heavier the molecular weight of a chemical contaminant of a pollutant from a point source, the greater the pollution of the underground water system at a short distance. The study concludes that the associative properties of landfill have a significant effect on groundwater quality in the study area.

Keywords: dumpsite, leachate, groundwater pollution, linear regression, principal component

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Authors: N. A. Hamizi, M. R. Johan, Y. H. Hor, A. N. Sabri, Y. Y. A. Yong

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In this research, Mn-doped CdSe QDs is synthesized by using paraffin liquid as the reacting solvent and oleic acid as the ligands for Cd in order to produce Mn-doped CdSe QDs in zinc-blende crystal structure. Characterization studies for synthesized Mn-doped CdSe QDs are carried out using UV-visible and photoluminescence spectroscopy. The absorption wavelengths in UV-vis test and emission wavelengths in PL test were increase with the increases in the ripening temperature and time respectively.

Keywords: semiconductor, chemical synthesis, optical properties, ripening

Procedia PDF Downloads 366

Authors: H. Jawan

Abstract:

This review describes the models of environmental-related crack propagation of aluminum alloys (7xxx) during the last few decades. Acknowledge on effects of different factors on the susceptibility to SCC permits to propose valuable mechanisms on crack advancement. The reliable mechanism of cracking give a possibility to propose the optimum chemical composition and thermal treatment conditions resulting in microstructure the most suitable for real environmental condition and stress state.

Keywords: microstructure, environmental, propagation, mechanism

Procedia PDF Downloads 392

Authors: Aditya Kumar

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One of the most fascinating properties of various insects and plant surfaces in nature is their water-repellent (superhydrophobicity) capability. The nature offers new insights to learn and replicate the same in designing artificial superhydrophobic structures for a wide range of applications such as micro-fluidics, micro-electronics, textiles, self-cleaning surfaces, anti-corrosion, anti-fingerprint, oil/water separation, etc. In general, artificial superhydrophobic surfaces are synthesized by creating roughness and then treating the surface with low surface energy materials. In this work, various super-hydrophobic coatings on metallic surfaces (aluminum, steel, copper, steel mesh) were synthesized by chemical etching process using different etchants and fatty acid. Also, SiO2 nano/micro-particles embedded polyethylene, polystyrene, and poly(methyl methacrylate) superhydrophobic coatings were synthesized on glass substrates. Also, the effect of process parameters such as etching time, etchant concentration, and particle concentration on wettability was studied. To know the applications of the coatings, surface morphology, contact angle, self-cleaning, corrosion-resistance, and water-repellent characteristics were investigated at various conditions. Furthermore, durabilities of coatings were also studied by performing thermal, ultra-violet, and mechanical stability tests. The surface morphology confirms the creation of rough microstructures by chemical etching or by embedding particles, and the contact angle measurements reveal the superhydrophobic nature. Experimentally it is found that the coatings have excellent self-cleaning, anti-corrosion and water-repellent nature. These coatings also withstand mechanical disturbances such surface bending, adhesive peeling, and abrasion. Coatings are also found to be thermal and ultra-violet stable. Additionally, coatings are also reproducible. Hence aforesaid durable superhydrophobic surfaces have many potential industrial applications.

Keywords: superhydrophobic, water-repellent, anti-corrosion, self-cleaning

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Authors: Julian Sandoval, Philipp Schober

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Lahar sand (lahars) is a material that originates from volcanic debris flows. During and after a volcano eruption, the lahars can move at speeds up to 22 meters per hour or more, so they can easily cover extensive areas and destroy any structure in their path. Mount Pinatubo eruption (1991) brought lahars to its vicinities, and its use has been a matter of research ever since. Lahars are often disposed of for land reclamation projects in the Manila Bay, Philippines. After reclamation, some deep loss deposits may still present and they are prone to liquefaction. To mitigate the risk of liquefaction of such deposits, Vibro compaction has been proposed and used as a ground improvement technique. Cone penetration testing (CPT) campaigns are usually initiated to monitor the effectiveness of the ground improvement works by vibro compaction. The CPT cone resistance is used to analyses the in-situ relative density of the reclaimed sand before and after compaction. Available correlations between the CPT cone resistance and the relative density are only valid for non-crushable sands. Due to the partially crushable nature of lahars, the CPT data requires to be adjusted to allow for a correct interpretation of the CPT data. The objective of this paper is to characterize the chemical and mechanical properties of the lahar sands used for an ongoing project in the Port of Manila, which comprises reclamation activities using lahars from the east of Mount Pinatubo, it investigates their effect in the proposed correction factor. Additionally, numerous CPTs were carried out in a test trial and during the execution of the project. Based on this data, the influence of the grid spacing, compaction steps and the holding time on the compaction results are analyzed. Moreover, the so-called “aging effect” of the lahars is studied by comparing the results of the CPT testing campaign at different times after the vibro compaction activities. A considerable increase in the tip resistance of the CPT was observed over time.

Keywords: vibro compaction, CPT, lahar sands, correction factor, chemical composition

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Authors: H. Saikouk, D. Laux, Emmanuel Le Clézio, B. Lacroix, K. Audic, R. Largenton, E. Federici, G. Despaux

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Pressurized Water Reactor (PWR) fuel rods are made of ceramic pellets (e.g. UO2 or (U,Pu) O2) assembled in a zirconium cladding tube. By design, an initial gap exists between these two elements. During irradiation, they both undergo transformations leading progressively to the closure of this gap. A local and non destructive examination of the pellet/cladding interface could constitute a useful help to identify the zones where the two materials are in contact, particularly at high burnups when a strong chemical bonding occurs under nominal operating conditions in PWR fuel rods. The evolution of the pellet/cladding bonding during irradiation is also an area of interest. In this context, the Institute of Electronic and Systems (IES- UMR CNRS 5214), in collaboration with the Alternative Energies and Atomic Energy Commission (CEA), is developing a high frequency acoustic microscope adapted to the control and imaging of the pellet/cladding interface with high resolution. Because the geometrical, chemical and mechanical nature of the contact interface is neither axially nor radially homogeneous, 2D images of this interface need to be acquired via this ultrasonic system with a highly performing processing signal and by means of controlled displacement of the sample rod along both its axis and its circumference. Modeling the multi-layer system (water, cladding, fuel etc.) is necessary in this present study and aims to take into account all the parameters that have an influence on the resolution of the acquired images. The first prototype of this microscope and the first results of the visualization of the inner face of the cladding will be presented in a poster in order to highlight the potentials of the system, whose final objective is to be introduced in the existing bench MEGAFOX dedicated to the non-destructive examination of irradiated fuel rods at LECA-STAR facility in CEA-Cadarache.

Keywords: high-frequency acoustic microscopy, multi-layer model, non-destructive testing, nuclear fuel rod, pellet/cladding interface, signal processing

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Authors: M. Salama, K. Haggag, H. El-Sayed

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An environmentally and ecologically acceptable method for eradication of wool fabrics based on microwave irradiation (MWI) was described. The process would be a suitable alternative for mothproofing of wool using toxic degradative chemical or biological methods. The effect of microwave irradiation and exposure time on the extent of eradication of wool fabrics from moth larvae was monitored. The inherent properties of the MW-irradiated wool fabrics; viz. tensile properties, alkali solubility, and yellowing index, were not adversely altered.

Keywords: microwave, wool, fabric, moth, eradication, resistance

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Authors: M. S. Stepanova, V. V. Zakharov, P. D. Khavlyuk, I. D. Skurlov, A. Y. Dubovik, A. L. Rogach

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Carbon dots are small carbon-based spherical nanoparticles, which are typically less than 10 nm in size that can be modified with surface passivation and heteroatoms doping. The light-absorbing ability of carbon dots has attracted a significant amount of attention in photoluminescence for bioimaging and fluorescence sensing applications owing to their advantages, such as tunable fluorescence emission, photo- and thermostability and low toxicity. In this study, carbon dots were synthesized by the solvothermal method from citric acid and ethylenediamine dissolved in water. The solution was heated for 5 hours at 200°C and then cooled down to room temperature. The carbon dots films were obtained by evaporation from a high-concentration aqueous solution. The increase of both luminescence intensity and light transmission was obtained as a result of a 405 nm laser exposure to a part of the carbon dots film, which was detected using a confocal laser scanning microscope (LSM 710, Zeiss). Blueshift up to 35 nm of the luminescence spectrum is observed as luminescence intensity, which is increased more than twofold. The exact value of the shift depends on the time of the laser exposure. This shift can be caused by the modification of surface groups at the carbon dots, which are responsible for long-wavelength luminescence. In addition, a shift of the absorption peak by 10 nm and a decrease in the optical density at the wavelength of 350 nm is detected, which is responsible for the absorption of surface groups. The obtained sample was also studied with time-resolved confocal fluorescence microscope (MicroTime 100, PicoQuant), which made it possible to receive a time-resolved photoluminescence image and construct emission decays of the laser-exposed and non-exposed areas. 5 MHz pulse rate impulse laser has been used as a photoluminescence excitation source. Photoluminescence decay was approximated by two exhibitors. The laser-exposed area has the amplitude of the first-lifetime component (A1) twice as much as before, with increasing τ1. At the same time, the second-lifetime component (A2) decreases. These changes evidence a modification of the surface groups of carbon dots. The detected effect can be used to create thermostable fluorescent marks, the physical size of which is bounded by the diffraction limit of the optics (~ 200-300 nm) used for exposure and to improve the optical properties of carbon dots or in the field of optical encryption. Acknowledgements: This work was supported by the Ministry of Science and Higher Education of Russian Federation, goszadanie no. 2019-1080 and financially supported by Government of Russian Federation, Grant 08-08.

Keywords: carbon dots, photoactivation, optical properties, photoluminescence and absorption spectra

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Authors: Pinar Erturk, Sevde Altuntas, Fatih Buyukserin

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In order to obtain an effective integration between an implant and a bone, implant surfaces should have similar properties to bone tissue surfaces. Especially mimicry of the chemical, mechanical and topographic properties of the implant to the bone is crucial for fast and effective osseointegration. Titanium-based biomaterials are more preferred in clinical use, and there are studies of coating these implants with oxide layers that have chemical/nanotopographic properties stimulating cell interactions for enhanced osseointegration. There are low success rates of current implantations, especially in craniofacial implant applications, which are large and vital zones, and the oxide layer coating increases bone-implant integration providing long-lasting implants without requiring revision surgery. Our aim in this study is to examine bone-cell behavior on titanium implants with an aluminum oxide layer (AAO) on effective osseointegration potential in the deformation of large zones with difficult spontaneous healing. In our study, aluminum layer coated titanium surfaces were anodized in sulfuric, phosphoric, and oxalic acid, which are the most common used AAO anodization electrolytes. After morphologic, chemical, and mechanical tests on AAO coated Ti substrates, viability, adhesion, and mineralization of adult bone cells on these substrates were analyzed. Besides with atomic layer deposition (ALD) as a sensitive and conformal technique, these surfaces were coated with pure alumina (5 nm); thus, cell studies were performed on ALD-coated nanoporous oxide layers with suppressed ionic content too. Lastly, in order to investigate the effect of the topography on the cell behavior, flat non-porous alumina layers on silicon wafers formed by ALD were compared with the porous ones. Cell viability ratio was similar between anodized surfaces, but pure alumina coated titanium and anodized surfaces showed a higher viability ratio compared to bare titanium and bare anodized ones. Alumina coated titanium surfaces, which anodized in phosphoric acid, showed significantly different mineralization ratios after 21 days over other bare titanium and titanium surfaces which anodized in other electrolytes. Bare titanium was the second surface that had the highest mineralization ratio. Otherwise, titanium, which is anodized in oxalic acid electrolyte, demonstrated the lowest mineralization. No significant difference was shown between bare titanium and anodized surfaces except AAO titanium surface anodized in phosphoric acid. Currently, osteogenic activities of these cells on the genetic level are investigated by quantitative real-time polymerase chain reaction (qRT-PCR) analysis results of RUNX-2, VEGF, OPG, and osteopontin genes. Also, as a result of the activities of the genes mentioned before, Western Blot will be used for protein detection. Acknowledgment: The project is supported by The Scientific and Technological Research Council of Turkey.

Keywords: alumina, craniofacial implant, MG-63 cell line, osseointegration, oxalic acid, phosphoric acid, sulphuric acid, titanium

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Authors: G. Olamiti; TK. Takalani; D. Beswa, AIO Jideani

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The study investigated the effects of malting and fermentation times on some chemical, functional properties and microstructural behaviour of Agrigreen, Babala pearl millet cultivars and sorghum flours using response surface methodology (RSM). Central Composite Rotatable Design (CCRD) was performed on two independent variables: malting and fermentation times (h), at intervals of 24, 48, and 72, respectively. The results of dependent parameters such as pH, titratable acidity (TTA), Water absorption capacity (WAC), Oil absorption capacity (OAC), bulk density (BD), dispersibility and microstructural behaviour of the flours studied showed a significant difference in p < 0.05 upon malting and fermentation time. Babala flour exhibited a higher pH value at 4.78 at 48 h malted and 81.9 fermentation times. Agrigreen flour showed a higher TTA value at 0.159% at 81.94 h malted and 48 h fermentation times. WAC content was also higher in malted and fermented Babala flour at 2.37 ml g-1 for 81.94 h malted and 48 h fermentation time. Sorghum flour exhibited the least OAC content at 1.67 ml g-1 at 14 h malted and 48 h fermentation times. Agrigreen flour recorded the least bulk density, at 0.53 g ml-1 for 72 h malted and 24 h fermentation time. Sorghum flour exhibited a higher content of dispersibility, at 56.34%, after 24 h malted and 72 h fermented time. The response surface plots showed that increased malting and fermentation time influenced the dependent parameters. The microstructure behaviour of malting and fermentation times of pearl millet varieties and sorghum flours showed isolated, oval, spherical, or polygonal to smooth surfaces. The optimal processing conditions, such as malting and fermentation time for Agrigreen, were 32.24 h and 63.32 h; 35.18 h and 34.58 h for Babala; and 36.75 h and 47.88 h for sorghum with high desirability of 1.00. The validation of the optimum processing malting and fermentation times (h) on the dependent improved the experimented values. Food processing companies can use the study's findings to improve food processing and quality.

Keywords: Pearl millet, malting, fermentation, microstructural behaviour

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Authors: Elizabeth R. LaFave, Grayson Sink, Anna Vassallo, Samantha Mills, Eli G. Hvastkovs

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Throughout history and into modern times, the continuation of male influence over female healthcare has created inadequacies in availability and access to treatments, often further limited in rural communities. The historical plight of women in healthcare can be understood by studying the advancements made by women in the field, both through their career arcs and by delving into the treatments they offer. An early example is the case of Martha Ballard (1735-1812), a midwife in New York who practiced when female practitioners were dismissed in favor of less educated male physicians, which was a well-accepted practice into the twentieth century. In order to overcome these setbacks, a strategy used by some female practitioners was to develop and market their own remedies in an attempt to better serve female patients. By highlighting the compromises and social manipulation of female entrepreneurs, in comparison with the medicines they developed and used, we can map their ability to carve a specific niche for themselves and their targeted customers. The application of modern chemical approaches in a historical context serves to enhance a variety of perspectives within the museum sphere necessary for the comprehension and understanding of the female plight in both medical care and service. In order to further examine the overall bias and scrutiny for women in the medical field, specifically those undertaking entrepreneurial roles, examples of alternative remedies from female founders will be analyzed utilizing these approaches. Modern analytical chemistry techniques, specifically mass spectrometry (MS), have been successful in offering compositional analyses for both labeled and unlabeled ingredients in old medicines. Previously, we have analyzed two forms of alternative treatment options created by male medical professionals to address lingering historical questions of purity and validity. Although primarily sugar based, both Humphreys’ Specifics and Boericke & Tafel remedies also contained unique ingredients, albeit in small quantities, with medicinal properties. Here, we applied the same methodology to study another highly politicized 19th-century debate surrounding the contribution and role of women in the medical profession through analyzing three remedies, each from a different female-led manufacturing company; Mrs. Joe Persons, Lydia Pinkham, and Winslow’s Syrups. Following MS analyses for both labeled and unlabeled ingredients, both Winslow’s and Pinkham’s remedies were similar to their male counterparts in advertisement strategy, targeted customer base, and overall composition of remedy (primarily sugar-based with small amounts of unique ingredients). In effect, these unbiased chemical assessments are used to dissect the rationality of both market and physician criticism for each individual manufacturer through assessment of authenticity, benefaction, and comparison among female entrepreneurs and their aims to enter the medical community (i.e., geographic location, market size). Our work aims to increase collaboration between STEM (Science, Technology, Engineering, Mathematics)-based fields and historical museum studies on a larger scale while also answering questions of potential bias towards females in the medical community as means of comparison to their male counterparts and in-depth historical analyses to unravel individual strategies to overcome the setback.

Keywords: nineteenth-century medicine, alternative remedies, female healthcare, chemical analyses, mass spectrometry

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Authors: Apoorva Bamal, Agnieszka Indiana Olbert

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Floods are known to be one of the most devastating hydro-climatic events, impacting a wide range of stakeholders in terms of environmental, social and economic losses. With difference in inundation durations and level of impact, flood hazards are of different degrees and strength. Amongst various set of domains being impacted by floods, environmental degradation in terms of water quality deterioration is one of the majorly effected but less highlighted domains across the world. The degraded water quality is caused by numerous natural and anthropogenic factors that are both point and non-point sources of pollution. Therefore, it is essential to understand the nature and source of the water pollution due to flooding. The major impact of floods is not only on the physico-chemical water quality parameters, but also on the biological elements leading to a vivid influence on the aquatic ecosystem. This deteriorated water quality is impacting many water categories viz. agriculture, drinking water, aquatic habitat, and miscellaneous services requiring an appropriate water quality to survive. This study identifies, reviews, evaluates and assesses multiple researches done across the world to determine the impact of floods on water quality. With a detailed statistical analysis of top relevant researches, this study is a synopsis of the methods used in assessment of impact of floods on water quality in different geographies, and identifying the gaps for further abridgement. As per majority of the studies, different flood magnitudes have varied impact on the water quality parameters leading to either increased or decreased values as compared to the recommended values for various categories. There is also an evident shift of the biological elements in the impacted waters leading to a change in its phenology and inhabitants of the specified water body. This physical, chemical and biological water quality degradation by floods is dependent upon its duration, extent, magnitude and flow direction. Therefore, this research provides an overview into the multiple impacts of floods on water quality, along with a roadmap of way forward to an efficient and uniform linkage of floods and impacted water quality dynamics.

Keywords: floods, statistical analysis, water pollution, water quality

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Authors: O. A. Apampa, Y. A. Jimoh

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The paper reports the investigation of Corn Cob Ash as a chemical stabilizing agent for laterite soils. Corn cob feedstock was obtained from Maya, a rural community in the derived savannah agro-ecological zone of South-Western Nigeria and burnt to ashes of pozzolanic quality. Reddish brown silty clayey sand material characterized as AASHTO A-2-6(3) lateritic material was obtained from a borrow pit in Abeokuta and subjected to strength characterization tests according to BS 1377: 2000. The soil was subsequently mixed with CCA in varying percentages of 0-7.5% at 1.5% intervals. The influence of CCA stabilized soil was determined for the Atterberg limits, compaction characteristics, CBR and the unconfined compression strength. The tests were repeated on laterite cement-soil mixture in order to establish a basis for comparison. The result shows a similarity in the compaction characteristics of soil-cement and soil-CCA. With increasing addition of binder from 1.5% to 7.5%, Maximum Dry Density progressively declined while the OMC steadily increased. For the CBR, the maximum positive impact was observed at 1.5% CCA addition at a value of 85% compared to the control value of 65% for the cement stabilization, but declined steadily thereafter with increasing addition of CCA, while that of soil-cement continued to increase with increasing addition of cement beyond 1.5% though at a relatively slow rate. Similar behavior was observed in the UCS values for the soil-CCA mix, increasing from a control value of 0.4 MN/m2 to 1.0 MN/m2 at 1.5% CCA and declining thereafter, while that for soil-cement continued to increase with increasing cement addition, but at a slower rate. This paper demonstrates that CCA is effective for chemical stabilization of a typical Nigerian AASHTO A-2-6 lateritic soil at maximum stabilizer content limit of 1.5% and therefore recommends its use as a way of finding further application for agricultural waste products and achievement of environmental sustainability in line with the ideals of the millennium development goals because of the economic and technical feasibility of the processing of the cobs from corn.

Keywords: corn cob ash, pozzolan, cement, laterite, stabilizing agent, cation exchange capacity

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Authors: Xiaoqing Liu, Kurt Friese, Karsten Rinke

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Lacustrine sediment archives rich paleoenvironmental information in lake and surrounding environment. Additionally, modern sediment is used as an effective medium for the monitoring of lake. Organic carbon in sediment is a heterogeneous mixture with varying turnover times and qualities which result from the different biogeochemical processes in the deposition of organic material. Therefore, the isolation of different carbon pools is important for the research of lacustrine condition in the lake. However, the numeric available fractionation procedures can hardly yield homogeneous carbon pools on terms of stability and age. In this work, a multi-step fractionation protocol that treated sediment with hot water, HCl, H2O2 and Na2S2O8 in sequence was adopted, the treated sediment from each step were analyzed for the isotopic and structural compositions with Isotope Ratio Mass Spectrometer coupled with element analyzer (IRMS-EA) and Solid-state 13C Nuclear Magnetic Resonance (NMR), respectively. The sequential extractions with hot-water, HCl, and H2O2 yielded a more homogeneous and C3 plant-originating OC fraction, which was characterized with an atomic C/N ratio shift from 12.0 to 20.8, and 13C and 15N isotopic signatures were 0.9‰ and 1.9‰ more depleted than the original bulk sediment, respectively. Additionally, the H2O2- resistant residue was dominated with stable components, such as the lignins, waxes, cutans, tannins, steroids and aliphatic proteins and complex carbohydrates. 6M HCl in the acid hydrolysis step was much more effective than 1M HCl to isolate a sedimentary OC fraction with higher degree of homogeneity. Owing to the extremely high removal rate of organic matter, the step of a Na2S2O8 oxidation is only suggested if the isolation of the most refractory OC pool is mandatory. We conclude that this multi-step chemical fractionation procedure is effective to isolate more homogeneous OC pools in terms of stability and functional structure, and it can be used as a promising method for OC pools fractionation of sediment or soil in future lake research.

Keywords: 13C-CPMAS-NMR, 13C signature, lake sediment, OC fractionation

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Authors: Vanessa Morgado, Ricardo Bettencourt da Silva, Carla Palma

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The environmental pollution by microplastics is well recognized. Microplastics were already detected in various matrices from distinct environmental compartments worldwide, some from remote areas. Various methodologies and techniques have been used to determine microplastic in such matrices, for instance, sediment samples from the ocean bottom. In order to determine microplastics in a sediment matrix, the sample is typically sieved through a 5 mm mesh, digested to remove the organic matter, and density separated to isolate microplastics from the denser part of the sediment. The physical analysis of microplastic consists of visual analysis under a stereomicroscope to determine particle size, colour, and shape. The chemical analysis is performed by an infrared spectrometer coupled to a microscope (micro-FTIR), allowing to the identification of the chemical composition of microplastic, i.e., the type of polymer. Creating legislation and policies to control and manage (micro)plastic pollution is essential to protect the environment, namely the coastal areas. The regulation is defined from the known relevance and trends of the pollution type. This work discusses the assessment of contamination trends of a 700 km² oceanic area affected by contamination heterogeneity, sampling representativeness, and the uncertainty of the analysis of collected samples. The methodology developed consists of objectively identifying meaningful variations of microplastic contamination by the Monte Carlo simulation of all uncertainty sources. This work allowed us to unequivocally conclude that the contamination level of the studied area did not vary significantly between two consecutive years (2018 and 2019) and that PET microplastics are the major type of polymer. The comparison of contamination levels was performed for a 99% confidence level. The developed know-how is crucial for the objective and binding determination of microplastic contamination in relevant environmental compartments.

Keywords: measurement uncertainty, micro-ATR-FTIR, microplastics, ocean contamination, sampling uncertainty

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Authors: I.K.Bedaida, A.Reguig

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Propolis is a complex resinous hive product, collected by bees from plants sources. Its chemical and constituents composition depends on its floral origin, and varies according to climatic and geographical conditions. Its strong antibacterial activity was correlated to the highest concentration of phenols. Staphylococcus aureus is the most significant human pathogen often carried asymptomatically on the bodies of both humans and animals, and has been implicated as causing severe morbidity and mortality worldwide. S. aureus has the ability to produce several exoenzymes that contribute to virulence such as coagulase, hemolysin, protease, and lipase and enterotoxin. It is considered also as one of the most important food safety concerns for the food industry. The aim of the study was to analyze propolis extracts' phytochemical and to study the cytoplasmic membrane damage of crude ethanol extract of propolis against Staphylococcus aureus ATCC 25923 by observing the changes of cell microstructure using scanning electron microscope and cell permeability damages. Propolis Ethanolic extract was analyzed by ultra-high-performance liquid chromatography coupled with a diode array detector and an electrospray mass spectrometer (UHPLC-DAD-ESI/MS). Additionally, polyphenols and volatile compounds of EEP was analyzed by gas chromatography–mass spectrometry GC-MS. Staphylococcus aureus ATCC 25923 was subjected to agar dilution method to determine the minimum inhibitory concentration (MIC) and potassium and protein leakages were performed to detect permeability damages. The results showed that the minimum inhibitory concentration (MIC) of EEP against Staphylococcus aureus ATCC 25923 was 39 µg/ml. Adding EEP at MIC level, there were obvious changes in the morphology of bacteria cells indicating cell damage. When EEP were added at (2MIC) levels, the cells were destroyed. EEP cause rapid increase the concentration of proteins and potassium in cell suspension.

Keywords: antimicrobial, GC-MS, HPLC, propolis, time kill effect

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Authors: M. Meddi, A. Boufekane

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The Mitidja coastal groundwater which extends over an area of 1450 km2 is a strategic resource in the Algiers region. The high dependence of the regional economy on the use of this groundwater forces us to have recourse to its artificial recharge from the Wadi El Harrach in its upstream part. This system of artificial recharge has shown its effectiveness in the development of water resource mentioned in the succeeding works in several regions of the world. The objective of this study is to: Increase the reserves of water inputs by infiltration, raise the water level and its good quality in wells and boreholes, reduce losses to the sea, and address seawater intrusion by maintaining balance in the freshwater-saltwater interface in the downstream part of the groundwater basin. After analyzing the situation, it was noticed that a qualitative monitoring of the Wadi water for the groundwater recharge has to be done. For this purpose, we proceeded during three successive years (2010, 2011, and 2012) to the monthly sampling of water in the upstream part of the Wadi El Harrach for chemical analysis. The variation of the sediment transport concentration will be also measured. This monitoring aims to characterize the water quality and avoid clogging in the proposed recharge area. The results of these analyses showed the good chemical quality according to the analyses we performed in the laboratory during the three years, but they are too loaded with suspended matters. We noticed that these fine particles come from the grinding of limestone of sandpit located upstream of the area of the proposed recharge system. This problem can be solved by a water supply upstream of sandpit. For the recharge, we propose the method of using two wells for dual use, which means that it can be used for water supply and extraction. This solution is inexpensive in our case and could easily be used as wells are already drilled in the upstream part. This solution increases over time the piezometric level and also reduce groundwater contamination by saltwater in the downstream part.

Keywords: water quality, artificial groundwater recharge, Mitidja, North Algeria

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Authors: Mst. Nilufa Sultana, Shatirah Akib, Muhammad Aqeel Ashraf, Mohamed Roseli Zainal Abidin

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Most people today are aware that global Climate change, is not just a scientific theory but also a fact with worldwide consequences. Global climate change is due to rapid urbanization, industrialization, high population growth and current vulnerability of the climatic condition. Water is becoming scarce as a result of global climate change. To mitigate the problem arising due to global climate change and its drought effect, harvesting rainwater from green roofs, an environmentally-friendly and versatile technology, is becoming one of the best assessment criteria and gaining attention in Malaysia. This paper addresses the sustainability of green roofs and examines the quality of water harvested from green roofs in comparison to rainwater. The factors that affect the quality of such water, taking into account, for example, roofing materials, climatic conditions, the frequency of rainfall frequency and the first flush. A green roof was installed on the Humid Tropic Centre (HTC) is a place of the study on monitoring program for urban Stormwater Management Manual for Malaysia (MSMA), Eco-Hydrological Project in Kualalumpur, and the rainwater was harvested and evaluated on the basis of four parameters i.e., conductivity, dissolved oxygen (DO), pH and temperature. These parameters were found to fall between Class I and Class III of the Interim National Water Quality Standards (INWQS) and the Water Quality Index (WQI). Some preliminary treatment such as disinfection and filtration could likely to improve the value of these parameters to class I. This review paper clearly indicates that there is a need for more research to address other microbiological and chemical quality parameters to ensure that the harvested water is suitable for use potable water for domestic purposes. The change in all physical, chemical and microbiological parameters with respect to storage time will be a major focus of future studies in this field.

Keywords: Green roofs, INWQS, MSMA-SME, rainwater harvesting, water treatment, water quality parameter, WQI

Procedia PDF Downloads 534

Authors: Danielle C. B. Honorato, Rafael H. Carvalho, Adriana L. Soares, Ana Paula F. R. L. Bracarense, Paulo D. Guarnieri, Massami Shimokomaki, Elza I. Ida

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Over the past decade, the Brazilian production of turkey meat increased by more than 50%, indicating that the turkey meat is considered a great potential for the Brazilian economy contributing to the growth of agribusiness at the marketing international scenario. However, significant color changes may occur during its processing leading to the pale, soft and exudative (PSE) appearance on the surface of breast meat due to the low water holding capacity (WHC). Changes in PSE meat functional properties occur due to the myofibrils proteins denaturation caused by a rapid postmortem glycolysis resulting in a rapid pH decline while the carcass temperature is still warm. The aim of this study was to analyze the physical, chemical and histological characteristics of PSE turkey meat obtained from a Brazilian commercial processing plant. The turkey breasts samples were collected (n=64) at the processing line and classified as PSE at L* ≥ 53 value. The pH was also analyzed after L* measurement. In sequence, PSE meat samples were evaluated for WHC, cooking loss (CL), shear force (SF), myofibril fragmentation index (MFI), protein denaturation (PD) and histological evaluation. The abnormal color samples presented lower pH values, 16% lower fiber diameter, 11% lower SF and 2% lower WHC than those classified as normal. The CL, PD and MFI were, respectively, 9%, 18% and 4% higher in PSE samples. The Pearson correlation between the L* values and CL, PD and MFI was positive, while that SF and pH values presented negative correlation. Under light microscopy, a shrinking of PSE muscle cell diameter was approximately 16% shorter in relation to normal samples and an extracellular enlargement of endomysium and perimysium sheaths as the consequence of higher water contents lost as observed previously by lower WHC values. Thus, the results showed that PSE turkey breast meat presented significant changes in their physical, chemical and histological characteristics that may impair its functional properties.

Keywords: functional properties, histological evaluation, meat quality, PSE

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Authors: Lucia Steenkamp, Chris V. D. Westhuyzen, Kgama Mathiba

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Ambergris, and more specifically its oxidation product (–)-ambrafuran, is a scarce, valuable, and sought-after perfumery ingredient. The material is used as a fixative agent to stabilise perfumes in formulations by reducing the evaporation rate of volatile substances. Ambergris is a metabolic product of the sperm whale (Physeter macrocephatus L.), resulting from intestinal irritation. Chemically, (–)-ambrafuran is produced from the natural product sclareol in eight synthetic steps – in the process using harsh and often toxic chemicals to do so. An overall yield of no more than 76% can be achieved in some routes, but generally, this is lower. A new 'green' route has been developed in our laboratory in which sclareol, extracted from the Clary sage plant, is converted to (–)-ambrafuran in two steps with an overall yield in excess of 80%. The first step uses a microorganism, Hyphozyma roseoniger, to bioconvert sclareol to an intermediate diol using substrate concentrations up to 50g/L. The yield varies between 90 and 67% depending on the substrate concentration used. The purity of the diol product is 95%, and the diol is used without further purification in the next step. The intermediate diol is then cyclodehydrated to the final product (–)-ambrafuran using a zeolite, which is not harmful to the environment and is readily recycled. The yield of the product is 96%, and following a single recrystallization, the purity of the product is > 99.5%. A preliminary LC-MS study of the bioconversion identified several intermediates produced in the fermentation broth under oxygen-restricted conditions. Initially, a short-lived ketone is produced in equilibrium with a more stable pyranol, a key intermediate in the process. The latter is oxidised under Norrish type I cleavage conditions to yield an acetate, which is hydrolysed either chemically or under lipase action to afford the primary fermentation product, an intermediate diol. All the intermediates identified point to the likely CYP450 action as the key enzyme(s) in the mechanism. This invention is an exceptional example of how the power of biocatalysis, combined with a mild, benign chemical step, can be deployed to replace a total chemical synthesis of a specific chiral antipode of a commercially relevant material.

Keywords: ambrafuran, biocatalysis, fragrance, microorganism

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