Search results for: chemical composition

Authors: Małgorzata Golonka, Jadwiga Laska

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Among self-healing materials, the most unexplored group are thermoplastic polymers. These polymers are used not only to produce packaging with a relatively short life but also to obtain coatings, insulation, casings, or parts of machines and devices. Due to its exceptional resistance to weather conditions, hydrophobicity, sufficient mechanical strength, and ease of extrusion, polyethylene is used in the production of polymer pipelines and as an insulating layer for steel pipelines. Polyethylene or PE coated steel pipelines can be used in difficult conditions such as underground or underwater installations. Both installation and use under such conditions are associated with high stresses and consequently the formation of microdamages in the structure of the material, loss of its integrity and final applicability. The ideal solution would be to include a self-healing system in the polymer material. In the presented study the behavior of resin-coated microcapsules in the extrusion process of low-density polyethylene was examined. Microcapsules are a convenient element of the repair system because they can be filled with appropriate reactive substances to ensure the repair process, but the main problem is their durability under processing conditions. Rapeseed oil, which has a relatively high boiling point of 240⁰C and low volatility, was used as the core material that simulates the reactive agents. The capsule shell, which is a key element responsible for its mechanical strength, was obtained by in situ polymerising urea-formaldehyde, melamine-urea-formaldehyde or melamine-formaldehyde resin on the surface of oil droplets dispersed in water. The strength of the capsules was compared based on the shell material, and in addition, microcapsules with single- and multilayer shells were obtained using different combinations of the chemical composition of the resins. For example, the first layer of appropriate tightness and stiffness was made of melamine-urea-formaldehyde resin, and the second layer was a melamine-formaldehyde reinforcing layer. The size, shape, distribution of capsule diameters and shell thickness were determined using digital optical microscopy and electron microscopy. The efficiency of encapsulation (i.e., the presence of rapeseed oil as the core) and the tightness of the shell were determined by FTIR spectroscopic examination. The mechanical strength and distribution of microcapsules in polyethylene were tested by extruding samples of crushed low-density polyethylene mixed with microcapsules in a ratio of 1 and 2.5% by weight. The extrusion process was carried out in a mini extruder at a temperature of 150⁰C. The capsules obtained had a diameter range of 70-200 µm. FTIR analysis confirmed the presence of rapeseed oil in both single- and multilayer shell microcapsules. Microscopic observations of cross sections of the extrudates confirmed the presence of both intact and cracked microcapsules. However, the melamine-formaldehyde resin shells showed higher processing strength compared to that of the melamine-urea-formaldehyde coating and the urea-formaldehyde coating. Capsules with a urea-formaldehyde shell work very well in resin coating systems and cement composites, i.e., in pressureless processing and moulding conditions. The addition of another layer of melamine-formaldehyde coating to both the melamine-urea-formaldehyde and melamine-formaldehyde resin layers significantly increased the number of microcapsules undamaged during the extrusion process. The properties of multilayer coatings were also determined and compared with each other using computer modelling.

Keywords: self-healing polymers, polyethylene, microcapsules, extrusion

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Authors: Chen Jiang, Eric Jordan, Maurice Gell, Balakrishnan Nair

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Nuclear fusion, one of the most promising options for reliably generating large amounts of carbon-free energy in the future, has seen a plethora of ground-breaking technological advances in recent years. An efficient and durable “breeding blanket”, needed to ensure a reactor’s self-sufficiency by maintaining the optimal coolant temperature as well as by minimizing radiation dosage behind the blanket, still remains a technological challenge for the various reactor designs for commercial fusion power plants. A relatively new dual-coolant lead-lithium (DCLL) breeder design has exhibited great potential for high-temperature (>700oC), high-thermal-efficiency (>40%) fusion reactor operation. However, the structural material, namely reduced activation ferritic-martensitic (RAFM) steel, is not chemically stable in contact with molten Pb-17%Li coolant. Thus, to utilize this new promising reactor design, the demand for effective corrosion-resistant coatings on RAFM steels represents a pressing need. Solution Spray Technologies LLC (SST) is developing a double-layer ceramic coating design to address the corrosion protection of RAFM steels, using a novel solution and solution/suspension plasma spray technology through a US Department of Energy-funded project. Plasma spray is a coating deposition method widely used in many energy applications. Novel derivatives of the conventional powder plasma spray process, known as the solution-precursor and solution/suspension-hybrid plasma spray process, are powerful methods to fabricate thin, dense ceramic coatings with complex compositions necessary for the corrosion protection in DCLL breeders. These processes can be used to produce ultra-fine molten splats and to allow fine adjustment of coating chemistry. Thin, dense ceramic coatings with chosen chemistry for superior chemical stability in molten Pb-Li, low activation properties, and good radiation tolerance, is ideal for corrosion-protection of RAFM steels. A key challenge is to accommodate its CTE mismatch with the RAFM substrate through the selection and incorporation of appropriate bond layers, thus allowing for enhanced coating durability and robustness. Systematic process optimization is being used to define the optimal plasma spray conditions for both the topcoat and bond-layer, and X-ray diffraction and SEM-EDS are applied to successfully validate the chemistry and phase composition of the coatings. The plasma-sprayed double-layer corrosion resistant coatings were also deposited onto simulated RAFM steel substrates, which are being tested separately under thermal cycling, high-temperature moist air oxidation as well as molten Pb-Li capsule corrosion conditions. Results from this testing on coated samples, and comparisons with bare RAFM reference samples will be presented and conclusions will be presented assessing the viability of the new ceramic coatings to be viable corrosion prevention systems for DCLL breeders in commercial nuclear fusion reactors.

Keywords: breeding blanket, corrosion protection, coating, plasma spray

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Authors: M. Al Azri, M. Elzain, K. Bouziane, S. M. Chérif

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n-Type 6H-SiC(0001) substrates were implanted with three fluencies of Mn+ 5x1015 Mn/cm2 (Mn content: 0.7%), 1x1016 (~2 %), and 5x1016 cm–2 (7%) with implantation energy of 80 keV and substrate temperature of 365ºC. The samples were characterized using Rutherford Backscattering and Channeling Spectroscopy (RBS/C), High-Resolution X-Ray Diffraction technique (HRXRD), micro-Raman Spectroscopy (μRS), and Superconducting Quantum Interference Device (SQUID) techniques. The aim of our work is to investigate implantation induced defects with dose and to study any correlation between disorder-composition and magnetic properties. In addition, ab-initio calculations were used to investigate the structural and magnetic properties of Mn-doped 6H-SiC. Various configurations of Mn sites and vacancy types were considered. The calculations showed that a substitutional Mn atom at Si site possesses larger magnetic moment than Mn atom at C site. A model is introduced to explain the dependence of the magnetic structure on site occupation. The magnetic properties of ferromagnetically (FM) and antiferromagnetically (AFM) coupled pairs of Mn atoms with and without neighboring vacancies have also been explored.

Keywords: ab-initio calculations, diluted magnetic semiconductors, magnetic properties, silicon carbide

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Authors: Malory Jonata

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Chlordecone (CLD) is an organochlorine pesticide used between 1971 and 1993 in both Guadeloupe and Martinique for the control of banana black weevil. The bishomocubane structure which characterizes this chemical compound led to high stability in organic matter and high persistence in the environment. Recently, researchers found that CLD can be degraded by isolated bacteria consortiums and, particularly, by bacteria such as Citrobacter sp 86 and Delsulfovibrio sp 86. Actually, six transformation product families of CLD are known. Moreover, the latest discovery showed that CLD was disappearing faster than first predicted in highly contaminated soil in Guadeloupe. However, the toxicity of transformation products is still unknown, and knowledge has to be deepened on the degradation ways and chemical characteristics of chlordecone and its transformation products. Microbial fuel cells (MFC) are electrochemical systems that can convert organic matter into electricity thanks to electroactive bacteria. These bacteria can exchange electrons through their membranes to solid surfaces or molecules. MFC have proven their efficiency as bioremediation systems in water and soils. They are already used for the bioremediation of several organochlorine compounds such as perchlorate, trichlorophenol or hexachlorobenzene. In this study, a three-electrodes system, inspired by MFC, is used to try to degrade chlordecone using bacteria from a mangrove swamp in Martinique. As we know, some mangrove bacteria are electroactive. Furthermore, the CLD rate seems to decline in mangrove swamp sediments. This study aims to prove that electroactive bacteria from a mangrove swamp in Martinique can degrade CLD thanks to a three-electrodes bioelectrochemical system. To achieve this goal, the tree-electrodes assembly has been connected to a potentiostat. The substrate used is mangrove water and sediments sampled in the mangrove swamp of La Trinité, a coastal city in Martinique, where CLD contamination has already been studied. Electroactive biofilms are formed by imposing a potential relative to Saturated Calomel Electrode using chronoamperometry. Moreover, their comportment has been studied by using cyclic voltametry. Biofilms have been studied under different imposed potentials, several conditions of the substrate and with or without CLD. In order to quantify the evolution of CLD rates in the substrate’s system, gas chromatography coupled with mass spectrometry (GC-MS) was performed on pre-treated samples of water and sediments after short, medium and long-term contact with the electroactive biofilms. Results showed that between -0,8V and -0,2V, the three-electrodes system was able to reduce the chemical in the substrate solution. The first GC-MS analysis result of samples spiked with CLD seems to reveal decreased CLD concentration over time. In conclusion, the designed bioelectrochemical system can provide the necessary conditions for chlordecone degradation. However, it is necessary to improve three-electrodes control settings in order to increase degradation rates. The biological pathways are yet to enlighten by biologicals analysis of electroactive biofilms formed in this system. Moreover, the electrochemical study of mangrove substrate gives new informations on the potential use of this substrate for bioremediation. But further studies are needed to a better understanding of the electrochemical potential of this environment.

Keywords: bioelectrochemistry, bioremediation, chlordecone, mangrove swamp

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Authors: Temesgen Geremew

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ZnO is currently receiving a lot of attention in the semiconductor industry due to its unique characteristics. ZnO is widely used in solar cells, heat-reflecting glasses, optoelectronic bias, and detectors. In this composition, we provide an overview of the ZnO thin flicks' packages, methods of characterization, and implicit operations. They consist of Transmission spectroscopy, Raman spectroscopy, Field emigration surveying electron microscopy, and X-ray diffraction. This review content also demonstrates how ZnO thin flicks function in electrical components for piezoelectric bias, optoelectronics, detectors, and renewable energy sources. Zinc oxide (ZnO) thin films offer a captivating tapestry of possibilities due to their unique blend of electrical, optical, and mechanical properties. This review delves into the realm of their potential applications and future prospects, highlighting the pivotal contributions of research endeavors aimed at tailoring their functionalities.

Keywords: Zinc oxide, raman spectroscopy, thin films, piezoelectric devices

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Authors: M. Bellakhal, M. Bellakhal, L. Aleya

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The specific composition and abundance of dinoflagellate resistance cysts in relation to environmental factors were studied from the superficial sediment at 123 stations in the Bizerte lagoon. 48 morphotypes of dinoflagellate cysts were identified, mainly dominated by Brigantidinium simplex, Votadinum spinosum, Alexandrium pacificum, Alexandrium pseudogonyaulax, and Lingulodinum machaerophorum. The density of cysts ranged from 1276 to 20126 cysts g⁻¹ dry sediment. Significant differences in the distribution pattern of the cysts were recorded, which allowed us to distinguish two areas; thus the inner areas of the lagoon have an abundance of cysts greater than the areas with marine influence. Ballast water discharges and shellfish culture may be incriminated as potential sources of introduction of species, particularly potentially toxic ones such as A. pacificum and Polysphaeridium zoharyi, without neglecting the role of currents in cyst distribution. Cyst mapping can be used as an indicator of potential foci of future toxic species blooms in this ecosystem.

Keywords: Bizerta Lagoon, cysts, dinoflagellates, mapping

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Authors: Gyeongbeom Yi

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The purpose of this study is to introduce the analytic solution for determining the optimal capacity (lot-size) of a multiproduct, multistage production and inventory system to meet the finished product demand. Reasonable decision-making about the capacity of processes and storage units is an important subject for industry. The industrial solution for this subject is to use the classical economic lot sizing method, EOQ/EPQ (Economic Order Quantity/Economic Production Quantity) model, incorporated with practical experience. However, the unrealistic material flow assumption of the EOQ/EPQ model is not suitable for chemical plant design with highly interlinked processes and storage units. This study overcomes the limitation of the classical lot sizing method developed on the basis of the single product and single stage assumption. The superstructure of the plant considered consists of a network of serially and/or parallelly interlinked processes and storage units. The processes involve chemical reactions with multiple feedstock materials and multiple products as well as mixing, splitting or transportation of materials. The objective function for optimization is minimizing the total cost composed of setup and inventory holding costs as well as the capital costs of constructing processes and storage units. A novel production and inventory analysis method, PSW (Periodic Square Wave) model, is applied. The advantage of the PSW model comes from the fact that the model provides a set of simple analytic solutions in spite of a realistic description of the material flow between processes and storage units. The resulting simple analytic solution can greatly enhance the proper and quick investment decision for plant design and operation problem confronted in diverse economic situations.

Keywords: analytic solution, optimal design, process-storage network

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Authors: N. S. Achour, M. Hamdaoui, S. Ben Nasrallah, A. Perwuelz

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The main idea of this work is to investigate the effect of knitted fabrics characteristics on moisture management properties. Wetting and transport properties of single jersey, Rib 1&1 and English Rib fabrics made out of cotton and blended Cotton/Polyester yarns were studied. The dynamic water sorption of fabrics was investigated under same isothermal and terrestrial conditions at 20±2°C-65±2% by using the Moisture Management Tester (MMT) which can be used to quantitatively measure liquid moisture transfer in one step in a fabric in multi directions: Absorption rate, moisture absorbing time of the fabric's inner and outer surfaces, one-way transportation capability, the spreading/drying rate, the speed of liquid moisture spreading on fabric's inner and outer surfaces are measured, recorded and discussed. The results show that fabric’s composition and knit’s structure have a significant influence on those phenomena.

Keywords: knitted fabrics characteristics, moisture management properties, multi directions, the moisture management tester

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Authors: Dilip K. Paul

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The most popular mesoporous molecular sieves, Mobil Composition of Matter (MCM) are keenly studied by researchers because of these materials possess amorphous silica wall and have a long range of ordered framework with uniform mesopores. These materials also possess large surface area, which can be up to more than 1000 m2g−1. Herein the investigation is focused upon the synthesis and characterization of chromium and aluminum doped MCM-41 using XRD and FTIR. Acid-base properties of Cr-Al-MCM 41 was investigated by molecularly sensitive transmission FT-IR spectroscopy by adsorbing pyridine. In addition, these MCM nanomaterial was used to catalyze C-C bond formation from acetaldehyde adsorption. The assignment of all infrared peaks during adsorption of pyridine provided detail information on the presence of acid-base sites which in turn helped us to explain the roles of these in the condensation reaction of aldehyde. Reaction mechanisms of C-C bond formation is therefore explored to shed some light on this elusive reaction detail.

Keywords: mesoporous nanomaterial, MCM 41, FTIR studies, acid-base studies

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Authors: Anuj Tyagi, Balwinder Singh, Naveen Kumar B. T., Niraj K. Singh

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Characterization of diverse microbial communities in specific environment plays a crucial role in the better understanding of their functional relationship with the ecosystem. It is now well established that gut microbiome of fish is not the simple replication of microbiota of surrounding local habitat, and extensive species, dietary, physiological and metabolic variations in fishes may have a significant impact on its composition. Moreover, overuse of antibiotics in human, veterinary and aquaculture medicine has led to rapid emergence and propagation of antibiotic resistance genes (ARGs) in the aquatic environment. Microbial communities harboring specific ARGs not only get a preferential edge during selective antibiotic exposure but also possess the significant risk of ARGs transfer to other non-resistance bacteria within the confined environments. This phenomenon may lead to the emergence of habitat-specific microbial resistomes and subsequent emergence of virulent antibiotic-resistant pathogens with severe fish and consumer health consequences. In this study, gut microbiota of freshwater carp (Labeo rohita) was investigated by shotgun metagenomics to understand its taxonomic composition and functional capabilities. Metagenomic DNA, extracted from the fish gut, was subjected to sequencing on Illumina NextSeq to generate paired-end (PE) 2 x 150 bp sequencing reads. After the QC of raw sequencing data by Trimmomatic, taxonomic analysis by Kraken2 taxonomic sequence classification system revealed the presence of 36 phyla, 326 families and 985 genera in the fish gut microbiome. At phylum level, Proteobacteria accounted for more than three-fourths of total bacterial populations followed by Actinobacteria (14%) and Cyanobacteria (3%). Commonly used probiotic bacteria (Bacillus, Lactobacillus, Streptococcus, and Lactococcus) were found to be very less prevalent in fish gut. After sequencing data assembly by MEGAHIT v1.1.2 assembler and PROKKA automated analysis pipeline, pathway analysis revealed the presence of 1,608 Metacyc pathways in the fish gut microbiome. Biosynthesis pathways were found to be the most dominant (51%) followed by degradation (39%), energy-metabolism (4%) and fermentation (2%). Almost one-third (33%) of biosynthesis pathways were involved in the synthesis of secondary metabolites. Metabolic pathways for the biosynthesis of 35 antibiotic types were also present, and these accounted for 5% of overall metabolic pathways in the fish gut microbiome. Fifty-one different types of antibiotic resistance genes (ARGs) belonging to 15 antimicrobial resistance (AMR) gene families and conferring resistance against 24 antibiotic types were detected in fish gut. More than 90% ARGs in fish gut microbiome were against beta-lactams (penicillins, cephalosporins, penems, and monobactams). Resistance against tetracycline, macrolides, fluoroquinolones, and phenicols ranged from 0.7% to 1.3%. Some of the ARGs for multi-drug resistance were also found to be located on sequences of plasmid origin. The presence of pathogenic bacteria and ARGs on plasmid sequences suggested the potential risk due to horizontal gene transfer in the confined gut environment.

Keywords: antibiotic resistance, fish gut, metabolic pathways, microbial diversity

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Authors: Emmanuel Ogundimu, Esther Akinlabi, Mutiu Erinosho

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The aim of this paper is to study the effect of welding current on the microstructure and the mechanical properties. Material characterizations were conducted on a 6 mm thick plates of type-304 austenite stainless steel, welded by TIG welding process at two different welding currents of 150 A (Sample F3) and 170 A (Sample F4). The tensile strength and the elongation obtained from sample F4 weld were approximately 584 MPa and 19.3 %; which were higher than sample F3 weld. The average microhardness value of sample F4 weld was found to be 235.7 HV, while that of sample F3 weld was 233.4 HV respectively. Homogenous distribution of iron (Fe), chromium (Cr) and nickel (Ni) were observed at the welded joint of the two samples. The energy dispersive spectroscopy (EDS) analysis revealed that Fe, Cr, and Ni made up the composition formed in the weld zone. The optimum welding current of 170 A for TIG welding of type-304 austenite stainless steel can be recommended for high-tech industrial applications.

Keywords: microhardness, microstructure, tensile, MIG welding, process, tensile, shear stress TIG welding, TIG-MIG welding

Procedia PDF Downloads 188

Authors: Anahita Izadyar

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Using a recombinant enzyme derived from corn and a simple modification, we are fabricating a facile, fast, and cost-beneficial novel biosensor to measure glucose. We are applying Plant Produced Mn Peroxidase (PPMP), glucose oxidase (GOx), polyaniline (PANI) as conductive polymer and gold nanoparticles (AuNPs) on Au electrode using electrochemical response to detect glucose. We applied the entrapment method of enzyme composition, which is generally used to immobilize conductive polymer and facilitate electron transfer from the enzyme oxidation-reduction center to the sample solution. In this work, the oxidation of glucose on the modified gold electrode was quantified with Linear Sweep Voltammetry(LSV). We expect that the modified biosensor has the potential for monitoring various biofluids.

Keywords: plant-produced manganese peroxidase, enzyme-based biosensors, glucose, modified gold nanoparticles electrode, polyaniline

Procedia PDF Downloads 189

Authors: M. Naveed Yasin, Robert Brooke, Andrew Chan, Geoffrey I. N. Waterhouse, Drew Evans, Darren Svirskis, Ilva D. Rupenthal

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Poly(3,4-ethylenedioxythiophene) (PEDOT) is a robust conducting polymer (CP) exhibiting high conductivity and environmental stability. It can be synthesized by either chemical, electrochemical or vapour phase polymerization (VPP). Dexamethasone sodium phosphate (dexP) is an anionic drug molecule which has previously been loaded onto PEDOT as a dopant via electrochemical polymerisation; however this technique requires conductive surfaces from which polymerization is initiated. On the other hand, VPP produces highly organized biocompatible CP structures while polymerization can be achieved onto a range of surfaces with a relatively straight forward scale-up process. Following VPP of PEDOT, dexP can be loaded and subsequently released via ion-exchange. This study aimed at preparing and characterising both non-porous and porous VPP PEDOT structures including examining drug loading and release via ion-exchange. Porous PEDOT structures were prepared by first depositing a sacrificial polystyrene (PS) colloidal template on a substrate, heat curing this deposition and then spin coating it with the oxidant solution (iron tosylate) at 1500 rpm for 20 sec. VPP of both porous and non-porous PEDOT was achieved by exposing to monomer vapours in a vacuum oven at 40 mbar and 40 °C for 3 hrs. Non-porous structures were prepared similarly on the same substrate but without any sacrificial template. Surface morphology, compositions and behaviour were then characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV) respectively. Drug loading was achieved by 50 CV cycles in a 0.1 M dexP aqueous solution. For drug release, each sample was exposed to 20 mL of phosphate buffer saline (PBS) placed in a water bath operating at 37 °C and 100 rpm. Film was stimulated (continuous pulse of ± 1 V at 0.5 Hz for 17 mins) while immersed into PBS. Samples were collected at 1, 2, 6, 23, 24, 26 and 27 hrs and were analysed for dexP by high performance liquid chromatography (HPLC Agilent 1200 series). AFM and SEM revealed the honey comb nature of prepared porous structures. XPS data showed the elemental composition of the dexP loaded film surface, which related well with that of PEDOT and also showed that one dexP molecule was present per almost three EDOT monomer units. The reproducible electroactive nature was shown by several cycles of reduction and oxidation via CV. Drug release revealed success in drug loading via ion-exchange, with stimulated porous and non-porous structures exhibiting a proof of concept burst release upon application of an electrical stimulus. A similar drug release pattern was observed for porous and non-porous structures without any significant statistical difference, possibly due to the thin nature of these structures. To our knowledge, this is the first report to explore the potential of VPP prepared PEDOT for stimuli-responsive drug delivery via ion-exchange. The produced porous structures were ordered and highly porous as indicated by AFM and SEM. These porous structures exhibited good electroactivity as shown by CV. Future work will investigate porous structures as nano-reservoirs to increase drug loading while sealing these structures to minimize spontaneous drug leakage.

Keywords: PEDOT for ion-exchange drug delivery, stimuli-responsive drug delivery, template based porous PEDOT structures, vapour phase polymerization of PEDOT

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Authors: R. Mickiene, A. Friese, U. Rosler, A. Maruska, O. Ragazinskiene

Abstract:

This research focuses on phytochemistry and antimicrobial activities of compounds isolated and identified from three species of Eryngium. The antimicrobial activity of extracts from Eryngiumplanum L., Eryngium maritimum L., Eryngium campestre L. grown in Lithuania, were tested by the method of series dilutions, against different bacteria species: Escherichia coli, Proteus vulgaris and Staphylococcus aureus with and without antibiotic resistances, originating from livestock. The antimicrobial activity of extracts was described by determination of the minimal inhibitory concentration. Preliminary results show that the minimal inhibitory concentration range between 8.0 % and 17.0 % for the different Eryngium extracts and bacterial species.The total amounts ofphenolic compounds and total amounts of flavonoids were tested in the methanolic extracts of the plants. Identification and evaluation of the phenolic compounds were performed by liquid chromatography. The essential oils were analyzed by gas chromatography mass spectrometry.

Keywords: antimicrobial activities, Eryngium L. species, essential oils, gas chromatography mass spectrometry

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Authors: Filip Varga, Nina Jeran, Martina Biosic, Zlatko Satovic, Martina Grdisa

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Dalmatian pyrethrum (Tanacetum cinerariifolium /Trevir./ Sch. Bip.), a species endemic to the eastern Adriatic coastline, is the source of natural insecticide pyrethrin. Pyrethrin is a mixture of six compounds (pyrethrin I and II, cinerin I and II, jasmolin I and II) that exhibits high insecticidal activity with no detrimental effects to the environment. A recently optimized matrix-solid phase dispersion method (MSPD), using florisil as the sorbent, acetone-ethyl acetate (1:1, v/v) as the elution solvent, and sodium sulfate anhydrous as the drying agent was utilized to extract the pyrethrins from 10 wild populations (20 individuals per population) distributed along the Croatian coast. All six components in the extracts were qualitatively and quantitatively determined by high-performance liquid chromatography with a diode array detector (HPLC-DAD). Pearson’s correlation index was calculated between pyrethrin compounds, and differences between the populations using the analysis of variance were tested. Additionally, the correlation of each pyrethrin component with spatio-ecological variables (bioclimate, soil properties, elevation, solar radiation, and distance from the coastline) was calculated. Total pyrethrin content ranged from 0.10% to 1.35% of dry flower weight, averaging 0.58% across all individuals. Analysis of variance revealed significant differences between populations based on all six pyrethrin compounds and total pyrethrin content. On average, the lowest total pyrethrin content was found in the population from Pelješac peninsula (0.22% of dry flower weight) in which total pyrethrin content lower than 0.18% was detected in 55% of the individuals. The highest average total pyrethrin content was observed in the population from island Zlarin (0.87% of dry flower weight), in which total pyrethrin content higher than 1.00% was recorded in only 30% of the individuals. Pyrethrin I/pyrethrin II ratio as a measure of extract quality ranged from 0.21 (population from the island Čiovo) to 5.88 (population from island Mali Lošinj) with an average of 1.77 across all individuals. By far, the lowest quality of extracts was found in the population from Mt. Biokovo (pyrethrin I/II ratio lower than 0.72 in 40% of individuals) due to the high pyrethrin II content typical for this population. Pearson’s correlation index revealed a highly significant positive correlation between pyrethrin I content and total pyrethrin content and a strong negative correlation between pyrethrin I and pyrethrin II. The results of this research clearly indicate high intra- and interpopulation diversity of Dalmatian pyrethrum with regards to pyrethrin content and composition. The information obtained has potential use in plant genetic resources conservation and biodiversity monitoring. Possibly the largest potential lies in designing breeding programs aimed at increasing pyrethrin content in commercial breeding lines and reintroduction in agriculture in Croatia. Acknowledgment: This work has been fully supported by the Croatian Science Foundation under the project ‘Genetic background of Dalmatian pyrethrum (Tanacetum cinerariifolium /Trevir/ Sch. Bip.) insecticidal potential’ - (PyrDiv) (IP-06-2016-9034).

Keywords: Dalmatian pyrethrum, HPLC, MSPD, pyrethrin

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Authors: Hien Thi Dieu Truong, Mahmoud Al-Sarayreh, Pullanagari Reddy, Marlon M. Reis, Richard Archer

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New Zealand mānuka honey is a honeybee product derived mainly from Leptospermum scoparium nectar. The potent antibacterial activity of mānuka honey derives principally from methylglyoxal (MGO), in addition to the hydrogen peroxide and other lesser activities present in all honey. MGO is formed from dihydroxyacetone (DHA) unique to L. scoparium nectar. Mānuka honey also has an idiosyncratic phenolic profile that is useful as a chemical maker. Authentic mānuka honey is highly valuable, but almost all honey is formed from natural mixtures of nectars harvested by a hive over a time period. Once diluted by other nectars, mānuka honey irrevocably loses value. We aimed to apply hyperspectral imaging to honey frames before bulk extraction to minimise the dilution of genuine mānuka by other honey and ensure authenticity at the source. This technology is non-destructive and suitable for an industrial setting. Chemometrics using linear Partial Least Squares (PLS) and Support Vector Machine (SVM) showed limited efficacy in interpreting chemical footprints due to large non-linear relationships between predictor and predictand in a large sample set, likely due to honey quality variability across geographic regions. Therefore, an advanced modelling approach, one-dimensional convolutional neural networks (1D-CNN), was investigated for analysing hyperspectral data for extraction of biochemical information from honey. The 1D-CNN model showed superior prediction of honey quality (R² = 0.73, RMSE = 2.346, RPD= 2.56) to PLS (R² = 0.66, RMSE = 2.607, RPD= 1.91) and SVM (R² = 0.67, RMSE = 2.559, RPD=1.98). Classification of mono-floral manuka honey from multi-floral and non-manuka honey exceeded 90% accuracy for all models tried. Overall, this study reveals the potential of HSI and deep learning modelling for automating the evaluation of honey quality in frames.

Keywords: mānuka honey, quality, purity, potency, deep learning, 1D-CNN, chemometrics

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Authors: Reza M. Rudd, Ali Saeedi, Colin Wood

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In this article, the latest advancements made in the applications of polymers in the enhanced hydrocarbon recovery technologies are investigated. For this purpose, different classes of polymers are reviewed and the latest progresses made in making them suitable for application under harsh reservoir conditions are discussed. The main reservoir conditions whose effects are taken into account include the temperature, rock mineralogy and brine salinity and composition. For profile modification and blocking the thief zones, polymers are used in the form of nanocomposite hydrogels. Polymers are also used as thickeners during CO2 flooding. Also, they are used in enhanced gas recovery, to inhibit the mixing of injection gas with the in-situ natural gas. This review covers the main types of polymers, their functions and the challenges in their applications, some of which are mentioned above. Included in this review are also the latest progresses made in the development of new polymeric surfactants used for surfactant flooding.

Keywords: EOR, EGR, polymer flooding, profile modification, mobility control, nanocomposite hydrogels, CO2 flooding, polymeric surfactants

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Authors: Beenish Saba, Ann D. Christy

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Modern day municipal solid waste landfills are operated and controlled to protect the environment from contaminants during the biological stabilization and degradation of the solid waste. They are equipped with liners, caps, gas and leachate collection systems. Landfill gas is passively or actively collected and can be used as bio fuel after necessary purification, but leachate treatment is the more difficult challenge. Leachate, if not recirculated in a bioreactor landfill system, is typically transported to a local wastewater treatment plant for treatment. These plants are designed for sewage treatment, and often charge additional fees for higher strength wastewaters such as leachate if they accept them at all. Different biological, chemical, physical and integrated techniques can be used to treat the leachate. Treating that leachate with simultaneous power production using microbial fuel cells (MFC) technology has been a recent innovation, reported its application in its earliest starting phase. High chemical oxygen demand (COD), ionic strength and salt concentration are some of the characteristics which make leachate an excellent substrate for power production in MFCs. Different materials of electrodes, microbial communities, carbon co-substrates and temperature conditions are some factors that can be optimized to achieve simultaneous power production and treatment. The advantage of the MFC is its dual functionality but lower power production and high costs are the hurdles in its commercialization and more widespread application. The studies so far suggest that landfill leachate MFCs can produce 1.8 mW/m2 with 79% COD removal, while amendment with food leachate or domestic wastewater can increase performance up to 18W/m3 with 90% COD removal. The columbic efficiency is reported to vary between 2-60%. However efforts towards biofilm optimization, efficient electron transport system studies and use of genetic tools can increase the efficiency of the MFC and can determine its future potential in treating landfill leachate.

Keywords: microbial fuel cell, landfill leachate, power generation, MFC

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Authors: I. Farid, K. Zouari

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An attempt has been made to examine the effect of water storage structures on groundwater recharge in a semi-arid agroclimatic setting in Jeloula Basin (Central Tunisia). In this area, surface water in rivers is seasonal, and therefore groundwater is the perennial source of water supply for domestic and agricultural purposes. Three pumped storage water power plants (PSWPP) have been built to increase the overall water availability in the basin and support agricultural livelihoods of rural smallholders. The scale and geographical dispersion of these multiple lakes restrict the understanding of these coupled human-water systems and the identification of adequate strategies to support riparian farmers. In the present review, hydrochemistry and isotopic tools were combined to get an insight into the processes controlling mineralization and recharge conditions in the investigated aquifer system. This study showed a slight increase in the groundwater level, especially after the artificial recharge operations and a decline when the water volume moves down during drought periods. Chemical data indicate that the main sources of salinity in the waters are related to water-rock interactions. Data inferred from stable isotopes in groundwater samples indicated recharge with modern rainfall. The investigated surface water samples collected from the PSWPP are affected by a significant evaporation and reveal large seasonal variations, which could be controlled by the water volume changes in the open surface reservoirs and the meteorological conditions during evaporation, condensation, and precipitation. The geochemical information is comparable to the isotopic results and illustrates that the chemical and isotopic signatures of reservoir waters differ clearly from those of groundwaters. These data confirm that the contribution of the artificial recharge operations from the PSWPP is very limited.

Keywords: Jeloula basin, recharge, hydrochemistry, isotopes

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Authors: Graham Hancox, Saydia Razak, Sue Hignett, Jo Barnes, Jyri Silmari, Florian Kading

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In the event of a Chemical, Biological, Radiological and Nuclear (CBRN) incident rapidly gaining, situational awareness is of paramount importance and advanced technologies have an important role to play in improving detection, identification, monitoring (DIM) and patient tracking. Understanding how these advanced technologies can fit into current response systems is essential to ensure they are optimally designed, usable and meet end-users’ needs. For this reason, Human Factors (Ergonomics) methods have been used within an EU Horizon 2020 project (TOXI-Triage) to firstly describe (map) the hierarchical structure in a CBRN response with adapted Accident Map (AcciMap) methodology. Secondly, Hierarchical Task Analysis (HTA) has been used to describe and review the sequence of steps (sub-tasks) in a CBRN scenario response as a task system. HTA methodology was then used to map one advanced technology, ‘Tag and Trace’, which tags an element (people, sample and equipment) with a Near Field Communication (NFC) chip in the Hot Zone to allow tracing of (monitoring), for example casualty progress through the response. This HTA mapping of the Tag and Trace system showed how the provider envisaged the technology being used, allowing for review and fit with the current CBRN response systems. These methodologies have been found to be very effective in promoting and supporting a dialogue between end-users and technology providers. The Human Factors methods have given clear diagrammatic (visual) representations of how providers see their technology being used and how end users would actually use it in the field; allowing for a more user centered approach to the design process. For CBRN events usability is critical as sub-optimum design of technology could add to a responders’ workload in what is already a chaotic, ambiguous and safety critical environment.

Keywords: AcciMap, CBRN, ergonomics, hierarchical task analysis, human factors

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Authors: J. P. Makwana, A. K. Joshi, Rajesh N. Patel, Darshil Patel

Abstract:

Recently, fluidized bed gasification becomes an attractive technology for power generation due to its higher efficiency. The main objective pursued in this work is to investigate the producer gas production potential from sized biomass (sawdust and pigeon pea) by applying the air gasification technique. The size of the biomass selected for the study was in the range of 0.40-0.84 mm. An experimental study was conducted using a fluidized bed gasifier with 210 mm diameter and 1600 mm height. During the experiments, the fuel properties and the effects of operating parameters such as gasification temperatures 700 to 900 °C, equivalence ratio 0.16 to 0.46 were studied. It was concluded that substantial amounts of producer gas (up to 1110 kcal/m3) could be produced utilizing biomass such as sawdust and pigeon pea by applying this fluidization technique. For both samples, the rise of temperature till 900 °C and equivalence ratio of 0.4 favored further gasification reactions and resulted into producer gas with calorific value 1110 kcal/m3.

Keywords: sized biomass, fluidized bed gasifier, equivalence ratio, temperature profile, gas composition

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Authors: Aleksandr Kavetskiy, Galina Yakubova, Nikolay Sargsyan, Stephen A. Prior, H. Allen Torbert

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The carbon sequestration question of modern times requires the development of an in-situ method of measuring soil carbon over large landmasses. Traditional chemical analytical methods used to evaluate large land areas require extensive soil sampling prior to processing for laboratory analysis; collectively, this is labor-intensive and time-consuming. An alternative method is to apply nuclear physics analysis, primarily in the form of pulsed fast-thermal neutron-gamma soil carbon analysis. This method is based on measuring the gamma-ray response that appears upon neutron irradiation of soil. Specific gamma lines with energies of 4.438 MeV appearing from neutron irradiation can be attributed to soil carbon nuclei. Based on measuring gamma line intensity, assessments of soil carbon concentration can be made. This method can be done directly in the field using a specially developed pulsed fast-thermal neutron-gamma system (PFTNA system). This system conducts in-situ analysis in a scanning mode coupled with GPS, which provides soil carbon concentration and distribution over large fields. The system has radiation shielding to minimize the dose rate (within radiation safety guidelines) for safe operator usage. Questions concerning the effect of neutron irradiation on soil health will be addressed. Information regarding absorbed neutron and gamma dose received by soil and its distribution with depth will be discussed in this study. This information was generated based on Monte-Carlo simulations (MCNP6.2 code) of neutron and gamma propagation in soil. Received data were used for the analysis of possible induced irradiation effects. The physical, chemical and biological effects of neutron soil irradiation were considered. From a physical aspect, we considered neutron (produced by the PFTNA system) induction of new isotopes and estimated the possibility of increasing the post-irradiation gamma background by comparisons to the natural background. An insignificant increase in gamma background appeared immediately after irradiation but returned to original values after several minutes due to the decay of short-lived new isotopes. From a chemical aspect, possible radiolysis of water (presented in soil) was considered. Based on stimulations of radiolysis of water, we concluded that the gamma dose rate used cannot produce gamma rays of notable rates. Possible effects of neutron irradiation (by the PFTNA system) on soil biota were also assessed experimentally. No notable changes were noted at the taxonomic level, nor was functional soil diversity affected. Our assessment suggested that the use of a PFTNA system with a neutron flux of 1e7 n/s for soil carbon analysis does not notably affect soil properties or soil health.

Keywords: carbon sequestration, neutron gamma analysis, radiation effect on soil, Monte-Carlo simulation

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Authors: Ravi Prakash

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The effects of Zr addition on kinetics and hydrogen absorption characteristics of BCC alloy 52Ti-12V-36Cr doped with x wt% of Zr (x = 0, 4, 8 & 12) was investigated. The samples have been characterized by X-ray diffraction, and activation study were made at four different temperatures- 100 oC, 200 oC, 300 oC and 400 oC. First hydrogenation kinetics of alloys were studied at 20 bar of hydrogen pressure and room temperature after giving heat treatment at different temperatures for 6 hours. Among the various Zr doped alloys studied, the composition 52Ti-12V-36Cr + 4wt% Zr shows maximum hydrogen storage capacity of 3.6wt%. Small amount of Zr shows advantageous effects on kinetics of alloy. It was also found out that alloys with the higher Zr concentration can be activated by giving heat treatment at lower temperatures. There is reduction in hydrogen storage capacity with increasing Zr content in the alloy primarily due to increasing abundance of secondary phase as established by X-Ray Diffraction and Scanning Electron Microscope results.

Keywords: hydrogen storage, metal hydrides, bcc alloy, heat treatment

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Authors: Juergen Junk, Franz Ronellenfitsch, Michael Eickermann

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An appropriate weed management in autumn is a prerequisite for an economically successful harvest in the following year. In Luxembourg oilseed rape, wheat and barley is sown from August until October, accompanied by a chemical weed control with soil active herbicides, depending on the state of the weeds and the meteorological conditions. Based on regular ground and surface water-analysis, high levels of contamination by transformation products of respective herbicide compounds have been found in Luxembourg. The most ideal conditions for incorporating soil active herbicides are single rain events. Weed control may be reduced if application is made when weeds are under drought stress or if repeated light rain events followed by dry spells, because the herbicides tend to bind tightly to the soil particles. These effects have been frequently reported for Luxembourg throughout the last years. In the framework of a multisite long-term field experiment (EFFO) weed monitoring, plants observations and corresponding meteorological measurements were conducted. Long-term time series (1947-2016) from the SYNOP station Findel-Airport (WMO ID = 06590) showed a decrease in the number of days with precipitation. As the total precipitation amount has not significantly changed, this indicates a trend towards rain events with higher intensity. All analyses are based on decades (10-day periods) for September and October of each individual year. To assess the future meteorological conditions for Luxembourg, two different approaches were applied. First, multi-model ensembles from the CORDEX experiments (spatial resolution ~12.5 km; transient projections until 2100) were analysed for two different Representative Concentration Pathways (RCP8.5 and RCP4.5), covering the time span from 2005 until 2100. The multi-model ensemble approach allows for the quantification of the uncertainties and also to assess the differences between the two emission scenarios. Second, to assess smaller scale differences within the country a high resolution model projection using the COSMO-LM model was used (spatial resolution 1.3 km). To account for the higher computational demands, caused by the increased spatial resolution, only 10-year time slices have been simulated (reference period 1991-2000; near future 2041-2050 and far future 2091-2100). Statistically significant trends towards higher air temperatures, +1.6 K for September (+5.3 K far future) and +1.3 K for October (+4.3 K), were predicted for the near future compared to the reference period. Precipitation simultaneously decreased by 9.4 mm (September) and 5.0 mm (October) for the near future and -49 mm (September) and -10 mm (October) in the far future. Beside the monthly values also decades were analyzed for the two future time periods of the CLM model. For all decades of September and October the number of days with precipitation decreased for the projected near and far future. Changes in meteorological variables such as air temperature and precipitation did already induce transformations in weed societies (composition, late-emerging etc.) of arable ecosystems in Europe. Therefore, adaptations of agronomic practices as well as effective weed control strategies must be developed to maintain crop yield.

Keywords: CORDEX projections, dry spells, ensembles, weed management

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Authors: J. Gomez-Caturla, L. Quiles-Carrillo, J. Ivorra-Martinez, D. Garcia-Garcia, R. Balart

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The present work reports on the development of wood plastic composites based on biopolypropylene (BioPP) and mango peel flour (MPF) by extrusion and injection moulding processes. PP-g-IA and DCP have been used as a compatibilizer and as free radical initiators for reactive extrusion, respectively. Mechanical and morphological properties have been characterized in order to study the compatibility of the blends. The obtained results showed that DCP and PP-g-IA improved the stiffness of BioPP in terms of elastic modulus. Moreover, they positively increased the tensile strength and elongation at the break of the blends in comparison with the sample that only had BioPP and MPF in its composition, improving the affinity between both compounds. DCP and PP-g-IA even seem to have certain synergy, which was corroborated through FESEM analysis. Images showed that the MPF particles had greater adhesion to the polymer matrix when PP-g-IA and DCP were added. This effect was more intense when both elements were added, observing an almost inexistent gap between MPF particles and the BioPP matrix.

Keywords: biopolyproylene, compatibilization, mango peel flour, wood plastic composite

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Authors: Monica Jong, Antonios Banos, Tom Scott, Chris Webster, David Fletcher

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Hydrogen, as a clean alternative to methane, is relatively easy to make, either from water using electrolysis or from methane using steam reformation. However, hydrogen is much trickier to store than methane, and without effective storage, it simply won’t pass muster as a suitable methane substitute. Physical storage of hydrogen is quite inefficient. Storing hydrogen as a compressed gas at pressures up to 900 times atmospheric is volumetrically inefficient and carries safety implications, whilst storing it as a liquid requires costly and constant cryogenic cooling to minus 253°C. This is where DU steps in as a possible solution. Across the periodic table, there are many different metallic elements that will react with hydrogen to form a chemical compound known as a hydride (or metal hydride). From a chemical perspective, the ‘king’ of the hydride forming metals is palladium because it offers the highest hydrogen storage volumetric capacity. However, this material is simply too expensive and scarce to be used in a scaled-up bulk hydrogen storage solution. Depleted Uranium is the second most volumetrically efficient hydride-forming metal after palladium. The UK has accrued a significant amount of DU because of manufacturing nuclear fuel for many decades, and that is currently without real commercial use. Uranium trihydride (UH3) contains three hydrogen atoms for every uranium atom and can chemically store hydrogen at ambient pressure and temperature at more than twice the density of pure liquid hydrogen for the same volume. To release the hydrogen from the hydride, all you do is heat it up. At temperatures above 250°C, the hydride starts to thermally decompose, releasing hydrogen as a gas and leaving the Uranium as a metal again. The reversible nature of this reaction allows the hydride to be formed and unformed again and again, enabling its use as a high-density hydrogen storage material which is already available in large quantities because of its stockpiling as a ‘waste’ by-product. Whilst the tritium storage credentials of Uranium have been rigorously proven at the laboratory scale and at the fusion demonstrator JET for over 30 years, there is a need to prove the concept for depleted uranium hydrogen storage (HyDUS) at scales towards that which is needed to flexibly supply our national power grid with energy. This is exactly the purpose of the HyDUS project, a collaborative venture involving EDF as the interested energy vendor, Urenco as the owner of the waste DU, and the University of Bristol with the UKAEA as the architects of the technology. The team will embark on building and proving the world’s first pilot scale demonstrator of bulk chemical hydrogen storage using depleted Uranium. Within 24 months, the team will attempt to prove both the technical and commercial viability of this technology as a longer duration energy storage solution for the UK. The HyDUS project seeks to enable a true by-product to wonder material story for depleted Uranium, demonstrating that we can think sustainably about unlocking the potential value trapped inside nuclear waste materials.

Keywords: hydrogen, long duration storage, storage, depleted uranium, HyDUS

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Authors: Ashish Dhamaniya, Satish Chandra

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Speed and traffic volume data are collected on different sections of four lane and six lane roads in three metropolitan cities in India. Speed data are analyzed to fit the statistical distribution to individual vehicle speed data and all vehicles speed data. It is noted that speed data of individual vehicle generally follows a normal distribution but speed data of all vehicle combined at a section of urban road may or may not follow the normal distribution depending upon the composition of traffic stream. A new term Speed Spread Ratio (SSR) is introduced in this paper which is the ratio of difference in 85^th and 50^th percentile speed to the difference in 50^th and 15^th percentile speed. If SSR is unity then speed data are truly normally distributed. It is noted that on six lane urban roads, speed data follow a normal distribution only when SSR is in the range of 0.86 – 1.11. The range of SSR is validated on four lane roads also.

Keywords: normal distribution, percentile speed, speed spread ratio, traffic volume

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Authors: Adane Gebresilassie Hailemariam, Belete Yilma Hirpaye

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The enhanced concentrations of heavy metals, especially in sediments, may indicate human-induced perturbations rather than natural enrichment through geological weathering. Heavy metals are non-biodegradable, persist in the environment, and are concentrated up to the food chain, leading to enhanced levels in the liver and muscle tissues of fishes, aquatic bryophytes, and aquatic biota. Marine organisms, in general fish in particular, accumulate metals to concentrations many times higher than present in water or sediment as they can take up metals in their organs and concentrate at different levels. Thus, metals acquired through the food chain due to pollution are potential chemical hazards, threatening consumers. The Nile tilapia (oreochromic niloticus), catfish (clarius garpinus), and water samples were collected from five sampling sites, namely, inlet-1, inlet-2, center, outlet-1 and outlet-2 of Lake Chamo. The concentration of major and trace metals Na, K, Mg, Ca, Cr, Co, Ni, Mn and Cu in the two fish muscles, gill and liver, was determined using an atomic absorption spectrometer (AAS) and flame photometer (FP). Metal concentrations in the water have also been evaluated within the two consecutive seasons, winter (dry) and spring (wet). The results revealed that the concentration of those metals in Tilapia’s (O. niloticus) muscle, gill, and liver were Na 44.5, 35.1, 28, Mg 2.8, 8.41, 4.61, K 43, 32, 30, Ca 1.5, 6.0, 5.5, Cr 0.91, 1.2, 3.5, Co 3.0, 2.89, 2.62, Ni 0.94, 1.99, 2.2, Mn 1.23, 1.51, 1.6 and Cu 1.1, 1.99, 3.5 mg kg-1 respectively and in catfish’s muscle, gill and liver Na 25, 39, 41.5, Mg 4.8, 2.87, 6, K 29, 38, 40, Ca 2.5, 8.10, 3.0, Cr 0.65, 3.5, 5.0, Co 2.62, 1.86, 1.73, Ni 1.10, 2.3, 3.1, Mn 1.54, 1.57, 1.59 and Cu 1.01, 1.10, 3.70 mg kg-1 respectively. The highest accumulation of Na and K were observed for tilapia muscle and catfish gill, Mg and Ca got higher in tilapia gill and catfish liver, while Co is higher in muscle of the two fish. The Cr, Ni, Mn and Cu levels were higher in the livers of the two fish species. In conculusion, metal toxicity through food chain is the current dangerous issue for human and othe animals. This needs deep focus to promot the health of living animals. The Details of the work are going to be discussed at the conference.

Keywords: bioaccumulation, catfish, essential metals, nile tilapia

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Authors: Zakia Fatima, Liu Lu, Donghao Li

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The analysis of biological fluid metabolites holds significant importance in various areas, such as medical research, food science, and public health. Investigating the levels and distribution of nutrients and their metabolites in biological samples allows researchers and healthcare professionals to determine nutritional status, find hypovitaminosis or hypervitaminosis, and monitor the effectiveness of interventions such as dietary supplementation. Moreover, analysis of nutrient metabolites provides insight into their metabolism, bioavailability, and physiological processes, aiding in the clarification of their health roles. Hence, the exploration of a distinct, efficient, eco-friendly, and simpler methodology is of great importance to evaluate the metabolic content of complex biological samples. In this work, a green and rapid analytical method based on an automated online two-dimensional microscale carbon fiber/activated carbon fiber fractionation system and time-of-flight mass spectrometry (2DμCFs-TOF-MS) was used to evaluate metabolites of urine samples after oral administration of food supplements. The automated 2DμCFs instrument consisted of a microcolumn system with bare carbon fibers and modified carbon fiber coatings. Carbon fibers and modified carbon fibers exhibit different surface characteristics and retain different compounds accordingly. Three kinds of mobile-phase solvents were used to elute the compounds of varied chemical heterogeneities. The 2DμCFs separation system has the ability to effectively separate different compounds based on their polarity and solubility characteristics. No complicated sample preparation method was used prior to analysis, which makes the strategy more eco-friendly, practical, and faster than traditional analysis methods. For optimum analysis results, mobile phase composition, flow rate, and sample diluent were optimized. Water-soluble vitamins, fat-soluble vitamins, and amino acids, as well as 22 vitamin metabolites and 11 vitamin metabolic pathway-related metabolites, were found in urine samples. All water-soluble vitamins except vitamin B12 and vitamin B9 were detected in urine samples. However, no fat-soluble vitamin was detected, and only one metabolite of Vitamin A was found. The comparison with a blank urine sample showed a considerable difference in metabolite content. For example, vitamin metabolites and three related metabolites were not detected in blank urine. The complete single-run screening was carried out in 5.5 minutes with the minimum consumption of toxic organic solvent (0.5 ml). The analytical method was evaluated in terms of greenness, with an analytical greenness (AGREE) score of 0.72. The method’s practicality has been investigated using the Blue Applicability Grade Index (BAGI) tool, obtaining a score of 77. The findings in this work illustrated that the 2DµCFs-TOF-MS approach could emerge as a fast, sustainable, practical, high-throughput, and promising analytical tool for screening and accurate detection of various metabolites, pharmaceuticals, and ingredients in dietary supplements as well as biological fluids.

Keywords: metabolite analysis, sustainability, carbon fibers, urine.

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Authors: Reza Vakili, Xiaolei Fan, Alex Walton

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The first near ambient pressure (NAP)-XPS study of CO oxidation over Pt nanoparticles (NPs) incorporated into Zr-based UiO (UiO for Universitetet i Oslo) MOFs was carried out. For this purpose, the MOF-based Catalysts were prepared by wetness impregnation (WI-PtNPs@UiO-67) and linker design (LD-PtNPs@UiO-67) methods along with PtNPs@ZrO₂ as the control catalyst. Firstly, the as-synthesized catalysts were reduced in situ prior to the operando XPS analysis. The existence of Pt(II) species was proved in UiO-67 by observing Pt 4f core level peaks at a high binding energy of 72.6 ± 0.1 eV. However, by heating the WI-PtNPs@UiO-67 catalyst in situ to 200 °C under vacuum, the higher BE components disappear, leaving only the metallic Pt 4f doublet, confirming the formation of Pt NPs. The complete reduction of LD-PtNPs@UiO-67 is achieved at 250 °C and 1 mbar H₂. To understand the chemical state of Pt NPs in UiO-67 during catalytic turnover, we analyzed the Pt 4f region using operando NAP-XPS in the temperature-programmed measurements (100-260 °C) with reference to PtNPs@ZrO₂ catalyst. CO conversion during NAP-XPS experiments with the stoichiometric mixture shows that LD-PtNPs@UiO-67 has a better CO turnover frequency (TOF, 0.066 s⁻¹ at 260 °C) than the other two (ca. 0.055 s⁻¹). Pt 4f peaks only show one chemical species present at all temperatures, but the core level BE shifts change as a function of reaction temperature, i.e., Pt 4f peak from 71.8 eV at T < 200 °C to 71.2 eV at T > 200 °C. As this higher BE state of 71.8 eV was not observed after in situ reductions of the catalysts and only once the CO/O₂ mixture was introduced, we attribute it to the surface saturation of Pt NPs with adsorbed CO. In general, the quantitative analysis of Pt 4f data from the operando NAP-XPS experiments shows that the surface chemistry of the Pt active phase in the two PtNPs@UiO-67 catalysts is the same, comparable to that of PtNPs@ZrO₂. The observed difference in the catalytic activity can be attributed to the particle sizes of Pt NPs, as well as the dispersion of active phase in the support, which are different in the three catalysts.

Keywords: CO oxidation, heterogeneous catalysis, MOFs, Metal Organic Frameworks, NAP-XPS, Near Ambient Pressure X-ray Photoelectron Spectroscopy

Procedia PDF Downloads 133