Search results for: electron backscatter Diffraction
Commenced in January 2007
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Edition: International
Paper Count: 3030

Search results for: electron backscatter Diffraction

510 Preparation, Characterisation, and Measurement of the in vitro Cytotoxicity of Mesoporous Silica Nanoparticles Loaded with Cytotoxic Pt(II) Oxadiazoline Complexes

Authors: G. Wagner, R. Herrmann

Abstract:

Cytotoxic platinum compounds play a major role in the chemotherapy of a large number of human cancers. However, due to the severe side effects for the patient and other problems associated with their use, there is a need for the development of more efficient drugs and new methods for their selective delivery to the tumours. One way to achieve the latter could be in the use of nanoparticular substrates that can adsorb or chemically bind the drug. In the cell, the drug is supposed to be slowly released, either by physical desorption or by dissolution of the particle framework. Ideally, the cytotoxic properties of the platinum drug unfold only then, in the cancer cell and over a longer period of time due to the gradual release. In this paper, we report on our first steps in this direction. The binding properties of a series of cytotoxic Pt(II) oxadiazoline compounds to mesoporous silica particles has been studied by NMR and UV/vis spectroscopy. High loadings were achieved when the Pt(II) compound was relatively polar, and has been dissolved in a relatively nonpolar solvent before the silica was added. Typically, 6-10 hours were required for complete equilibration, suggesting the adsorption did not only occur to the outer surface but also to the interior of the pores. The untreated and Pt(II) loaded particles were characterised by C, H, N combustion analysis, BET/BJH nitrogen sorption, electron microscopy (REM and TEM) and EDX. With the latter methods we were able to demonstrate the homogenous distribution of the Pt(II) compound on and in the silica particles, and no Pt(II) bulk precipitate had formed. The in vitro cytotoxicity in a human cancer cell line (HeLa) has been determined for one of the new platinum compounds adsorbed to mesoporous silica particles of different size, and compared with the corresponding compound in solution. The IC50 data are similar in all cases, suggesting that the release of the Pt(II) compound was relatively fast and possibly occurred before the particles reached the cells. Overall, the platinum drug is chemically stable on silica and retained its activity upon prolonged storage.

Keywords: cytotoxicity, mesoporous silica, nanoparticles, platinum compounds

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509 Phenolic Composition and Antioxidant Property of Honey with Dried Apricots

Authors: Jasna Čanadanović-Brunet, Gordana Ćetković, Sonja Djilas, Vesna Tumbas-Šaponjac, Jelena Vulić, Sladjana Stajčić

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Honey, produced by the honeybee, is a natural saturated sugar solution, which is mainly composed of a complex mixture of carbohydrates. Besides this, it also contains certain minor constituents, proteins, enzymes, amino and organic acids, lipids, vitamins, phenolic acids, flavonoids and carotenoids. Honey serves as a source of natural antioxidants, which are effective in reducing the risk of heart disease, cancer, immune-system decline, cataracts, and different inflammatory processes. Honey is consumed in its natural form alone, but also in combination with nuts and various kinds of dried fruits (plums, figs, cranberries, apricots etc.). The aim of this research was to investigate the contribution of dried apricot addition to polyphenols and flavonoids contents and antioxidant activities of honey. Some individual phenolic compounds in Serbian polyfloral honey (PH), linden honey (LH) and also in their mixtures with dried apricot, in 40% mass concentrations (PH40; LH40), were identified and quantified by HPLC. The most dominant phenolic compound was: gallic acid in LH (11.14 mg/100g), LH40 (42.65 mg/100g), PH (7.24 mg/100g) and catehin in PH40 (11.83 mg/100g). The antioxidant activity of PH, LH, PH40 and LH40 was tested by measuring their ability to scavenge hydroxyl radicals (OH) by electron spin resonance spectroscopy (ESR). Honey samples with 40% dried apricot exhibited better antioxidant activity measured by hydroxyl radical scavenging activity. The EC50 values, the amount of antioxidant necessary to decrease the initial concentration of OH radicals by 50%, were: EC50PH=3.36 mg/ml, EC50LH=13.36 mg/ml, EC50PH40=2.29 mg/ml, EC50 LH40=7.78 mg/ml. Our results indicate that supplementation of polyfloral honey and linden honey with dried apricots improves antioxidant activity of honey by enriching the phenolic composition.

Keywords: honey, dried apricot, HPLC, hydroxyl radical

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508 Insights into Insect Vectors: Liberibacter Interactions

Authors: Murad Ghanim

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The citrus greening disease, also known as Huanglongbing, caused by the phloem-limited bacterium Candidatus Liberibacter asiaticus (CLas) has resulted in tremendous losses and the death of millions of citrus trees worldwide. CLas is transmitted by the Asian citrus psyllid (ACP) Diaphorina citri. The closely-related bacterium Candidatus Liberibacter solanacearum (CLso), which is associated with vegetative disorders in carrots and the zebra chips disease in potatoes, is transmitted by other psyllid species including Bactericera trigonica in carrots and B. ckockerelli in potatoes. Chemical sprays are currently the prevailing method for managing these diseases for limiting psyllid populations; however, they are limited in their effectiveness. A promising approach to prevent the transmission of these pathogens is to interfere with the vector-pathogen interactions, but our understanding of these processes is very limited. CLas induces changes in the nuclear architecture in the midgut of ACP and activates programmed cell death (apoptosis) in this organ. Strikingly, CLso displayed an opposite effect in the gut of B. trigonica, showing limited apoptosis, but widespread necrosis. Electron and fluorescent microscopy further showed that CLas induced the formation of Endoplasmic reticulum (ER) inclusion- and replication-like bodies, in which it increases and multiplies. ER involvement in bacterial replication is hypothesized to be the first stage of an immune response leading to the apoptotic and necrotic responses. ER exploitation and the subsequent events that lead to these cellular and stress responses might activate a cascade of molecular responses ending up with apoptosis and necrosis. Understanding the molecular interactions that underlay the necrotic/apoptotic responses to the bacteria will increase our knowledge of ACP-CLas, and BT-CLso interactions, and will set the foundation for developing novel, and efficient strategies to disturb these interactions and inhibit the transmission.

Keywords: Liberibacter, psyllid, transmission, apoptosis, necrosis

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507 Preparation, Characterization, and Antimicrobial Activity of Carboxymethyl Chitosan Schiff Bases with Different Benzaldehyde Derivatives

Authors: Nadia A. Mohamed, Magdy W. Sabaa, Ahmed H. H. El-Ghandour, Marwa M. Abdel-Aziz, Omayma F. Abdel-Gawad

Abstract:

Eighteen carboxymethyl chitosan (CMCh) schiff bases and their reduced derivatives have been synthesized. They were characterized by spectral analyses (FT-IR and H1-NMR) and scanning electron microscopy observation. Their antibacterial activities against Streptococcus pneumoniae (RCMB 010010), Bacillis subtilis (RCMB 010067), as Gram positive bacteria and Escherichia coli (RCMB 010052) as Gram negative bacteria and the antifungal activity against Aspergillus fumigatus (RCMB 02568), Geotricum candidum (RCMB 05097), and Candida albicans (RCMB 05031) were examined using agar disk diffusion method. The results demonstrate how the antibacterial and the antifungal activity are clearly affected by both the nature and position of the substituent groups in the aryl ring of the prepared derivatives. CMCh-4-nitroBenz Schiff base and its reduced form show higher antimicrobial activity comparing with other para substituted derivatives. CMCh-4-nitroBenz Schiff base: 18.3, 17, and 15.6 mm against Bacillis subtilis, Streptococcus pneumonia, and Escherichia coli respectively and 16.2, 17.3, and 16.4 mm against Aspergillus fumigates, Geotricum candidum, and Candida albicans respectively. CMCh-4-nitroBenz reduced form: 19.5, 18.7, and 16.2 mm against Bacillis subtilis, Streptococcus pneumonia, and Escherichia coli respectively and 17.5, 19.5, and 17.4 mm against Aspergillus fumigates, Geotricum candidum, and Candida albicans respectively. Also CMCh-3-bromoBenz show good results; CMCh-3-bromoBenz schiff base: 19.2, 16.9, and 14.6 mm Bacillis subtilis, Streptococcus pneumonia, and Escherichia coli respectively and 18.4, 17.6, and 15.9 mm against Aspergillus fumigates, Geotricum candidum, and Candida albicans respectively.

Keywords: chitosan, schiff base, minimum inhibition concentration, antimicrobial activity

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506 Mechanical and Physical Properties of Various Types of Dental Floss

Authors: Supanitayanon Lalita, Dechkunakorn Surachai, Anuwongnukroh Niwat, Srikhirin Toemsak, Roongrujimek Pitchaya, Tua-Ngam Peerapong

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Objective: To compare maximum load, percentage of elongation, physical characteristics of 4 types of dental floss: (1) Thai Silk Floss (silk, waxed), (2) Oral B® Essential Floss (nylon, waxed), (3) Experimental Floss Xu (nylon, unwaxed), (4) Experimental Floss Xw (nylon, waxed). Materials & method: Four types of floss were tested (n=30) with a Universal Testing Machine (Instron®). Each sample (30 cm long, 5 cm segment) was fixed, and pulled apart with load cell of 100 N and a test speed of 100 mm/min. Physical characteristics were investigated by digital microscope under 2.5×10 magnification, and scanning electron microscope under 1×100 and 5×100 magnification. The size of the filaments was measured in micron (μm) and the fineness were measured in Denier. Statistical analysis: For mechanical properties, the maximum load and the percentage of elongation were presented as mean ± SD. The distribution of the data was calculated by the Kolmogorov-Smirnov test. One-way ANOVA and multiple comparison (Tukey HSD) were used to analyze the differences among the groups with the level of a statistical difference at p < 0.05. Results: The maximum load of Floss Xu, Floss Xw, Oral B and Thai Silk were 47.39, 46.46, 25.38, and 23.70 N, respectively. The percentage of elongation of Oral B, Floss Xw, Floss Xu and Thai Silk were 72.43, 44.62, 31.25, and 16.44%, respectively. All 4 types of dental floss showed statistically differences in both the maximum load and percentage of elongation at p < 0.05, except for maximum load between Floss Xw and Floss Xu that showed no statistically significant difference. Physical characteristics of Thai silk revealed the most disintegrated, the smallest, and the least fine filaments. Conclusion: Floss Xu had the highest maximum load. Oral B had the highest percentage of elongation. Wax coating on Floss X increased the elongation but had no significant effect on the maximum load. The physical characteristics of Thai Silk resulted in the lowest mechanical properties values.

Keywords: dental floss, maximum load, mechanical property, percentage of elongation, physical property

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505 Evaluation of Elements Impurities in Drugs According to Pharmacopoeia by use FESEM-EDS Technique

Authors: Rafid Doulab

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Elemental Impurities in the Pharmaceuticals industryis are indispensable to ensure pharmaceuticalssafety for 24 elements. Although atomic absorption and inductively coupled plasma are used in the U.S Pharmacopeia and the European Pharmacopoeia, FESEM with energy dispersive spectrometers can be applied as an alternative analysis method for quantitative and qualitative results for a variety of elements without chemical pretreatment, unlike other techniques. This technique characterizes by shortest time, with more less contamination, no reagent consumption, and generation of minimal residue or waste, as well as sample preparations time limiting, with minimal analysis error. Simple dilution for powder or direct analysis for liquid, we analyzed the usefulness of EDS method in testing with field emission scanning electron microscopy (FESEM, SUPRA 55 Carl Zeiss Germany) with an X-ray energy dispersion (XFlash6l10 Bruker Germany). The samples analyzed directly without coating by applied 5µ of known concentrated diluted sample on carbon stub with accelerated voltage according to sample thickness, the result for this spot was in atomic percentage, and by Avogadro converted factor, the final result will be in microgram. Conclusion and recommendation: The conclusion of this study is application of FESEM-EDS in US pharmacopeia and ICH /Q3D guideline to reach a high-precision and accurate method in element impurities analysis of drugs or bulk materials to determine the permitted daily exposure PDE in liquid or solid specimens, and to obtain better results than other techniques, by the way it does not require complex methods or chemicals for digestion, which interfere with the final results with the possibility of to keep the sample at any time for re analysis. The recommendation is to use this technique in pharmacopeia as standard methods like inductively coupled plasma both ICP-AES, ICP-OES, and ICP-MS.

Keywords: pharmacopoeia, FESEM-EDS, element impurities, atomic concentration

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504 Aggregation-Induced-Active Stimuli-Responsive Based Nano-Objects for Wastewater Treatment Application

Authors: Parvaneh Eskandari, Rachel O'Reilly

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In the last years, controlling the self-assembly behavior of stimuli-responsive nano-objects, including micelles, vesicles, worm-like, etc., at different conditions is considered a pertinent challenge in the polymer community. The aim of the project was to synthesize aggregation-induced emission (AIE)-active stimuli-responsive polymeric nano-objects to control the self-assemblies morphologies of the prepared nano-objects. Two types of nanoobjects, micelle and vesicles, including PDMAEMA-b-P(BzMA-TPEMA) [PDMAEMA: poly(N,Ndimethylaminoethyl methacrylate); P(BzMA-TPEMA): poly[benzyl methacrylate-co- tetraphenylethene methacrylate]] were synthesized by using reversible addition−fragmentation chain-transfer (RAFT)- mediated polymerization-induced self-assembly (PISA), which combines polymerization and self-assembly in a single step. Transmission electron microscope and dynamic light scattering (DLS) analysis were used to confirm the formed self-assemblies morphologies. The controlled self-assemblies were applied as nitrophenolic compounds (NPCs) adsorbents from wastewater, thanks to their CO2-responsive part, PDMAEMA. Moreover, the fluorescence-active part of the prepared nano-objects, P(BzMA-TPEMA), played a key role in the detection of the NPCs at the aqueous solution. The optical properties of the prepared nano-objects were studied by UV/Vis and fluorescence spectroscopies. For responsivity investigations, the hydrodynamic diameter and Zeta-potential (ζ-potential) of the sample's aqueous solution were measured by DLS. In the end, the prepared nano-objects were used for the detection and adsorption of different NPCs.

Keywords: aggregation-induced emission polymers, stimuli-responsive polymers, reversible addition−fragmentation chain-transfer polymerization, polymerization-induced self-assembly, wastewater treatment

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503 Design and Development of High Strength Aluminium Alloy from Recycled 7xxx-Series Material Using Bayesian Optimisation

Authors: Alireza Vahid, Santu Rana, Sunil Gupta, Pratibha Vellanki, Svetha Venkatesh, Thomas Dorin

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Aluminum is the preferred material for lightweight applications and its alloys are constantly improving. The high strength 7xxx alloys have been extensively used for structural components in aerospace and automobile industries for the past 50 years. In the next decade, a great number of airplanes will be retired, providing an obvious source of valuable used metals and great demand for cost-effective methods to re-use these alloys. The design of proper aerospace alloys is primarily based on optimizing strength and ductility, both of which can be improved by controlling the additional alloying elements as well as heat treatment conditions. In this project, we explore the design of high-performance alloys with 7xxx as a base material. These designed alloys have to be optimized and improved to compare with modern 7xxx-series alloys and to remain competitive for aircraft manufacturing. Aerospace alloys are extremely complex with multiple alloying elements and numerous processing steps making optimization often intensive and costly. In the present study, we used Bayesian optimization algorithm, a well-known adaptive design strategy, to optimize this multi-variable system. An Al alloy was proposed and the relevant heat treatment schedules were optimized, using the tensile yield strength as the output to maximize. The designed alloy has a maximum yield strength and ultimate tensile strength of more than 730 and 760 MPa, respectively, and is thus comparable to the modern high strength 7xxx-series alloys. The microstructure of this alloy is characterized by electron microscopy, indicating that the increased strength of the alloy is due to the presence of a high number density of refined precipitates.

Keywords: aluminum alloys, Bayesian optimization, heat treatment, tensile properties

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502 Effect of Doping on Band Gap of Zinc Oxide and Degradation of Methylene Blue and Industrial Effluent

Authors: V. P. Borker, K. S. Rane, A. J. Bhobe, R. S. Karmali

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Effluent of dye industries contains chemicals and organic dyes. Sometimes they are thrown in the water bodies without any treatment. This leads to environmental pollution and is detrimental to flora and fauna. Semiconducting oxide zinc oxide with wide bandgap 3.37 eV is used as a photocatalyst in degrading organic dyes using UV radiations. It generates electron-hole pair on exposure to UV light. If degradation is aimed at solar radiations, bandgap of zinc oxide is to be reduced so as to utilize visible radiation. Thus, in present study, zinc oxide, ZnO is synthesized from zinc oxalate, N doped zinc oxide, ZnO₁₋ₓNₓ from hydrazinated zinc oxalate, cadmium doped zinc oxide Zn₀.₉Cd₀.₁₀ and magnesium-doped zinc oxide Zn₀.₉Mg₀.₁₀ from mixed metal oxalate and hydrazinated mixed metal oxalate. The precursors were characterized by FTIR. They were decomposed to form oxides and XRD were recorded. The compounds were monophasic. Bandgap was calculated using Diffuse Reflectance Spectrum. The bandgap of ZnO was reduced to 3.24 because of precursor method of synthesis leading large surface area. The bandgap of Zn₀.₉Cd₀.₁₀ was 3.11 eV and that of Zn₀.₉Mg₀.₁₀ 3.41 eV. The lowest value was of ZnO₁₋ₓNₓ 3.09 eV. These oxides were used to degrade methylene blue, a model dye in sunlight. ZnO₁₋ₓNₓ was also used to degrade effluent of industry manufacturing colours, crayons and markers. It was observed that ZnO₁₋ₓNₓ acts as a good photocatalyst for degradation of methylene blue. It can degrade the solution within 120 minutes. Similarly, diluted effluent was decolourised using this oxide. Some colours were degraded using ZnO. Thus, the use of these two oxides could mineralize effluent. Lesser bandgap leads to more electro hole pair thus helps in the formation of hydroxyl ion radicals. These radicals attack the dye molecule, fragmentation takes place and it is mineralised.

Keywords: cadmium doped zinc oxide, dye degradation, dye effluent degradation, N doped zinc oxide, zinc oxide

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501 Enhanced Photocatalytic H₂ Production from H₂S on Metal Modified Cds-Zns Semiconductors

Authors: Maali-Amel Mersel, Lajos Fodor, Otto Horvath

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Photocatalytic H₂ production by H₂S decomposition is regarded to be an environmentally friendly process to produce carbon-free energy through direct solar energy conversion. For this purpose, sulphide-based materials, as photocatalysts, were widely used due to their excellent solar spectrum responses and high photocatalytic activity. The loading of proper co-catalysts that are based on cheap and earth-abundant materials on those semiconductors was shown to play an important role in the improvement of their efficiency. In this research, CdS-ZnS composite was studied because of its controllable band gap and excellent performance for H₂ evolution under visible light irradiation. The effects of the modification of this photocatalyst with different types of materials and the influence of the preparation parameters on its H₂ production activity were investigated. The CdS-ZnS composite with an enhanced photocatalytic activity for H₂ production was synthesized from ammine complexes. Two types of modification were used: compounds of Ni-group metals (NiS, PdS, and Pt) were applied as co-catalyst on the surface of CdS-ZnS semiconductor, while NiS, MnS, CoS, Ag₂S, and CuS were used as a dopant in the bulk of the catalyst. It was found that 0.1% of noble metals didn’t remarkably influence the photocatalytic activity, while the modification with 0.5% of NiS was shown to be more efficient in the bulk than on the surface. The modification with other types of metals results in a decrease of the rate of H₂ production, while the co-doping seems to be more promising. The preparation parameters (such as the amount of ammonia to form the ammine complexes, the order of the preparation steps together with the hydrothermal treatment) were also found to highly influence the rate of H₂ production. SEM, EDS and DRS analyses were made to reveal the structure of the most efficient photocatalysts. Moreover, the detection of the conduction band electron on the surface of the catalyst was also investigated. The excellent photoactivity of the CdS-ZnS catalysts with and without modification encourages further investigations to enhance the hydrogen generation by optimization of the reaction conditions.

Keywords: H₂S, photoactivity, photocatalytic H₂ production, CdS-ZnS

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500 Glyco-Conjugated Gold Nanorods Based Biosensor for Optical Detection and Photothermal Ablation of Food Borne Bacteria

Authors: Shimayali Kaushal, Nitesh Priyadarshi, Nitin Kumar Singhal

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Food borne bacterial species have been identified as major pathogens in most of the severe pathogen-related diseases among humans which result in great loss to human health and food industry. Conventional methods like plating and enzyme-linked immune sorbent assay (ELISA) are time-consuming, laborious and require specialized instruments. Nanotechnology has emerged as a great field in case of rapid detection of pathogens in recent years. The AuNRs material has good electro-optical properties due to its larger light absorption band and scattering in surface plasmon resonance wavelength regions. By exploiting the sugar-based adhesion properties of microorganism, we can use the glycoconjugates capped gold nanorods as a potential nanobiosensor to detect the foodborne pathogen. In the present study, polyethylene glycol (PEG) coated gold nanorods (AuNRs) were prepared and functionalized with different types of carbohydrates and further characterized by UV-Visible spectrophotometry, dynamic light scattering (DLS), transmission electron microscopy (TEM). The reactivity of above said nano-biosensor was probed by lectin binding assay and also by different strains of foodborne bacteria by using spectrophotometric and microscopic techniques. Due to the specific interaction of probe with foodborne bacteria (Escherichia coli, Pseudomonas aeruginosa), our nanoprobe has shown significant and selective ablation of targeted bacteria. Our findings suggest that our nanoprobe can be an ideal candidate for selective optical detection of food pathogens and can reduce loss to the food industry.

Keywords: glyco-conjugates, gold nanorods, nanobiosensor, nanoprobe

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499 Validation of the Recovery of House Dust Mites from Fabrics by Means of Vacuum Sampling

Authors: A. Aljohani, D. Burke, D. Clarke, M. Gormally, M. Byrne, G. Fleming

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Introduction: House Dust Mites (HDMs) are a source of allergen particles embedded in textiles and furnishings. Vacuum sampling is commonly used to recover and determine the abundance of HDMs but the efficiency of this method is less than standardized. Here, the efficiency of recovery of HDMs was evaluated from home-associated textiles using vacuum sampling protocols.Methods/Approach: Living Mites (LMs) or dead Mites (DMs) House Dust Mites (Dermatophagoides pteronyssinus: FERA, UK) were separately seeded onto the surfaces of Smooth Cotton, Denim and Fleece (25 mites/10x10cm2 squares) and left for 10 minutes before vacuuming. Fabrics were vacuumed (SKC Flite 2 pump) at a flow rate of 14 L/min for 60, 90 or 120 seconds and the number of mites retained by the filter (0.4μm x 37mm) unit was determined. Vacuuming was carried out in a linear direction (Protocol 1) or in a multidirectional pattern (Protocol 2). Additional fabrics with LMs were also frozen and then thawed, thereby euthanizing live mites (now termed EMs). Results/Findings: While there was significantly greater (p=0.000) recovery of mites (76% greater) in fabrics seeded with DMs than LMs irrespective of vacuuming protocol or fabric type, the efficiency of recovery of DMs (72%-76%) did not vary significantly between fabrics. For fabrics containing EMs, recovery was greatest for Smooth Cotton and Denim (65-73% recovered) and least for Fleece (15% recovered). There was no significant difference (p=0.99) between the recovery of mites across all three mite categories from Smooth Cotton and Denim but significantly fewer (p=0.000) mites were recovered from Fleece. Scanning Electron Microscopy images of HMD-seeded fabrics showed that live mites burrowed deeply into the Fleece weave which reduced their efficiency of recovery by vacuuming. Research Implications: Results presented here have implications for the recovery of HDMs by vacuuming and the choice of fabric to ameliorate HDM-dust sensitization.

Keywords: allergy, asthma, dead, fabric, fleece, live mites, sampling

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498 The Effect of Mixing and Degassing Conditions on the Properties of Epoxy/Anhydride Resin System

Authors: Latha Krishnan, Andrew Cobley

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Epoxy resin is most widely used as matrices for composites of aerospace, automotive and electronic applications due to its outstanding mechanical properties. These properties are chiefly predetermined by the chemical structure of the prepolymer and type of hardener but can also be varied by the processing conditions such as prepolymer and hardener mixing, degassing and curing conditions. In this research, the effect of degassing on the curing behaviour and the void occurrence is experimentally evaluated for epoxy /anhydride resin system. The epoxy prepolymer was mixed with an anhydride hardener and accelerator in an appropriate quantity. In order to investigate the effect of degassing on the curing behaviour and void content of the resin, the uncured resin samples were prepared using three different methods: 1) no degassing 2) degassing on prepolymer and 3) degassing on mixed solution of prepolymer and hardener with an accelerator. The uncured resins were tested in differential scanning calorimeter (DSC) to observe the changes in curing behaviour of the above three resin samples by analysing factors such as gel temperature, peak cure temperature and heat of reaction/heat flow in curing. Additionally, the completely cured samples were tested in DSC to identify the changes in the glass transition temperature (Tg) between the three samples. In order to evaluate the effect of degassing on the void content and morphology changes in the cured epoxy resin, the fractured surfaces of cured epoxy resin were examined under the scanning electron microscope (SEM). Also, the changes in the mechanical properties of the cured resin were studied by three-point bending test. It was found that degassing at different stages of resin mixing had significant effects on properties such as glass transition temperature, the void content and void size of the epoxy/anhydride resin system. For example, degassing (vacuum applied on the mixed resin) has shown higher glass transition temperature (Tg) with lower void content.

Keywords: anhydride epoxy, curing behaviour, degassing, void occurrence

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497 Famotidine Loaded Solid Lipid Nanoparticles (SLN) for Oral Delivery System

Authors: Rachmat Mauludin, Novita R. Kusuma, Diky Mudhakir

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Famotidine (FMT) is one of used substances in the treatment of hiperacidity and peptic ulcer, administered orally and parenterally via intravenous injection. Oral administration, which is more favorable, has been reported to have many obstacles in the process of the treatment, includes decreasing the bioavailability of FMT. This research was aimed to prepare FMT in form of solid lipid nanoparticles (SLN) with size ranging between 100-200 nm. The research was carried out also by optimizing factors that may affect physical stability of SLN. Formulation of Famotidine SLN was carried out by optimizing factors, such as duration of homogenization and sonication, lipid concentration, stabilizer composition and stabilizer concentration. SLN physical stability was evaluated (particle size distribution) for 42 days in 3 diferent temperatures. Entrapment efficiency and drug loading was determined indirectly and directly. The morphology of SLN was visualized by transmission electron microscope (TEM). In vitro release study of FMT was conducted in 2 mediums, at pH of 1.2 and 7.4. Chemical stability of FMT was determined by quantifying the concentration of FMT within 42 days. Famotidin SLN consisted of GMS as lipid and poloxamer 188, lecithin, and polysorbate 80 as stabilizers. Homogenization and sonication was performed for 5 minutes and 10 minutes. Physyical stability of nanoparticles at 3 different temperatures was no significant difference. The best formula was physically stable until 42 days with mean particle size below 200 nm. Nanoparticles produced was able to entrap FMT until 86.6%. Evaluation by TEM showed that nanoparticles was spherical and solid. In medium pH of 1.2, FMT was released only 30% during 4 hour. On the other hand, within 4 hours SLN could release FMT completely in medium pH of 7.4. The FMT concentration in nanoparticles dispersion was maintained until 95% in 42 days (40oC, RH 75%). Famotidine SLN was able to be produced with mean particle size ranging between 100-200 nm and physically stable for 42 days. SLN could be loaded by 86,6% of FMT. Morphologically, obtained SLN was spheric and solid. During 4 hours in medium pH of 1.2 and 7.4, FMT was released until 30% and 100%, respectively.

Keywords: solid lipid nanoparticle (SLN), famotidine (FMT), physicochemical properties, release study

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496 AI Peer Review Challenge: Standard Model of Physics vs 4D GEM EOS

Authors: David A. Harness

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Natural evolution of ATP cognitive systems is to meet AI peer review standards. ATP process of axiom selection from Mizar to prove a conjecture would be further refined, as in all human and machine learning, by solving the real world problem of the proposed AI peer review challenge: Determine which conjecture forms the higher confidence level constructive proof between Standard Model of Physics SU(n) lattice gauge group operation vs. present non-standard 4D GEM EOS SU(n) lattice gauge group spatially extended operation in which the photon and electron are the first two trace angular momentum invariants of a gravitoelectromagnetic (GEM) energy momentum density tensor wavetrain integration spin-stress pressure-volume equation of state (EOS), initiated via 32 lines of Mathematica code. Resulting gravitoelectromagnetic spectrum ranges from compressive through rarefactive of the central cosmological constant vacuum energy density in units of pascals. Said self-adjoint group operation exclusively operates on the stress energy momentum tensor of the Einstein field equations, introducing quantization directly on the 4D spacetime level, essentially reformulating the Yang-Mills virtual superpositioned particle compounded lattice gauge groups quantization of the vacuum—into a single hyper-complex multi-valued GEM U(1) × SU(1,3) lattice gauge group Planck spacetime mesh quantization of the vacuum. Thus the Mizar corpus already contains all of the axioms required for relevant DeepMath premise selection and unambiguous formal natural language parsing in context deep learning.

Keywords: automated theorem proving, constructive quantum field theory, information theory, neural networks

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495 Formulation and Characterization of NaCS-PDMDAAC Capsules with Immobilized Chlorella vulgaris for Phycoremediation of Palm Oil Mill Effluent

Authors: Quin Emparan, Razif Harun, Dayang R. A. Biak, Rozita Omar, Michael K. Danquah

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Cultivation of immobilized microalgae cells is on the rise for biotechnological applications. In this study, cultivation of Chlorella vulgaris was carried out in the form of suspended free-cell and immobilized cells system. NaCS-PDMDAAC capsules were used to immobilize C. vulgaris. Initially, the synthesized NaCS with C. vulgaris culture were prepared at various concentration of 5- 20% (w/v) using a 6% hardening solution (PDMDAAC) to investigate the capsules' gel stability and suitability for microalgae cells growth. Then, the capsules produced from 15% NaCS with C. vulgaris culture were furthered investigated using 5%, 10%, and 15% (w/v) of PDMDAAC solution. The capsules' gel stability was evaluated through dissolution time and loss of uniform spherical shape of capsules, while suitability for microalgae cells growth was evaluated through the optical density of microalgae. In this study, the 15% NaCS-10% PDMDAAC capsules were found to be the most suitable to sustain the capsules' gel stability and microalgae cells growth in MLA. For that reason, the C. vulgaris immobilized in the 15% NaCS-10% PDMDAAC capsules were further characterized using physicochemical analysis in terms of morphological, carbon (C), hydrogen (H) and nitrogen (N), Fourier transform-infrared (FT-IR), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), zeta potential and Brunauer-Emmet-Teller (BET) analyses. The results revealed that the presence of sulfonates in the synthesized NaCS and NaCS-PDMDAAC capsules without and with C. vulgaris proves that cellulose alcohol group was successfully bonded by sulfo group. Besides that, immobilized microalgae cells have a smaller cell size of 6.29 ± 1.09 µm and zeta potential of -11.93 ± 0.91 mV than suspended free-cells microalgae culture. It can be summarized that immobilization of C. vulgaris in the 15% NaCS-10% PDMDAAC capsules are relevant as a bioremediator for wastewater treatment purposes due to its suitable size of pore and capsules as well as structural and compositional properties.

Keywords: biological capsules, immobilized cultivation, microalgae, physico-chemical analysis

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494 Uranium Migration Process: A Multi-Technique Investigation Strategy for a Better Understanding of the Role of Colloids

Authors: Emmanuelle Maria, Pierre Crançon, Gaëtane Lespes

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The knowledge of uranium migration processes within underground environments is a major issue in the environmental risk assessment associated with nuclear activities. This process is identified as strongly controlled by adsorption mechanisms, thus leading to strongly delayed migration paths. Colloidal ligands are likely to significantly increase the mobility of uranium in natural environments. The ability of colloids to mobilize and transport uranium depends on their origin, their nature, their structure, their stability and their reactivity with uranium. Thus, the colloidal mobilization and transport properties are often described as site-specific. In this work, the colloidal phases of two leachates obtained from two different horizons of the same podzolic soil were characterized with a speciation approach. For this purpose, a multi-technique strategy was used, based on Field-Flow Fractionation coupled to Ultraviolet, Multi-Angle Light Scattering and Inductively Coupled Plasma Mass Spectrometry (AF4-UV-MALS-ICPMS), Transmission Electron Microscopy (TEM), Electrospray Ionization Orbitrap Mass Spectrometry (ESI-Orbitrap), and Time-Resolved Laser Fluorescence Spectroscopy (TRLFS-EEM). Thus, elemental composition, size distribution, microscopic structure, colloidal stability and possible organic and/or inorganic content of colloids were determined, as well as their association with uranium. The leachates exhibit differences in their physical and chemical characteristics, mainly in the nature of organic matter constituents. The multi-technique investigation strategy used provides original data about colloidal phase structure and composition, offering a new vision of the way the uranium can be mobilized and transported in the considered soil. This information is a real significant contribution opening the way to our understanding and predicting of the colloidal transport.

Keywords: colloids, migration, multi-technique, speciation, transport, uranium

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

Authors: Innocent O. Arukalam, Emeka E. Oguzie

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

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

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492 The Evaluation of the Performance of CaCO3/Polymer Nano-Composites for the Preservation of Historic Limestone Monuments

Authors: Mohammed Badereldien, Rezk Diab, Mohamoud Ali, Ayman Aboelkassem

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The stone surfaces of historical architectural heritage in Egypt are under threat from of various environmental factors such as temperature fluctuation, humidity, pollution, and microbes. Due to these factors, the facades of buildings are deteriorating deformation and disfiguration of external decoration and the formation of black accretion also often from the stone works. The aim of this study is to evaluate the effectiveness of CaCO₃ nano-particles as consolidation and protection material for calcareous stone monuments. Selected tests were carried out in order to estimate the superficial consolidating and protective effect of the treatment. When applied the nanoparticles dispersed in the acrylic copolymer; poly ethylmethacrylate (EMA)/methylacrylate (MA) (70/30, respectively) (EMA)/methylacrylate (MA) (70/30, respectively). The synthesis process of CaCO₃ nanoparticles/polymer nano-composite was prepared using in situ emulsion polymerization system. The consolidation and protection were characterized by TEM, while the penetration depth, re-aggregating effects of the deposited phase, and the surface morphology before and after treatment were examined by SEM (Scanning Electron Microscopy). Improvement of the stones' mechanical properties was evaluated by compressive strength tests. Changes in water-interaction properties were evaluated by water absorption capillarity measurements, and colorimetric measurements were used to evaluate the optical appearance. Together the results appear to demonstrate that CaCO₃/polymer nanocomposite is an efficient material for the consolidation of limestone architecture and monuments. As compared with samples treated with pure acrylic copolymer without Calcium carbonate nanoparticles, for example, CaCO₃ nanoparticles are completely compatible, strengthening limestone against thermal aging and improving its mechanical properties.

Keywords: calcium carbonate nanoparticles, consolidation, nanocomposites, calcareous stone, colorimetric measurements, compressive strength

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491 Characterization of a Dentigerous Cyst Cell Line and Its Secretion of Metalloproteinases

Authors: Muñiz-Lino Marcos A.

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The ectomesenchymal tissues involved in tooth development and their remnants are the origin of different odontogenic lesions, including tumors and cysts of the jaws, with a wide range of clinical behaviors. A dentigerous cyst (DC) represents approximately 20% of all cases of odontogenic cysts, and it has been demonstrated that it can develop benign and malignant odontogenic tumors. DC is characterized by bone destruction of the area surrounding the crown of a tooth that has not erupted and contains liquid. The treatment of odontogenic tumors and cysts usually involves a partial or total removal of the jaw, causing important secondary co-morbidities. However, molecules implicated in DC pathogenesis, as well as in its development into odontogenic tumors, remain unknown. A cellular model may be useful to study these molecules, but that model has not been established yet. Here, we reported the establishment of a cell culture derived from a dentigerous cyst. This cell line was named DeCy-1. In spite of its ectomesenchymal morphology, DeCy-1 cells express epithelial markers such as cytokeratins 5, 6, and 8. Furthermore, these cells express the ODAM protein, which is present in odontogenesis and in dental follicles, indicating that DeCy-1 cells are derived from odontogenic epithelium. Analysis by electron microscopy of this cell line showed that it has a high vesicular activity, suggesting that DeCy-1 could secrete molecules that may be involved in DC pathogenesis. Thus, secreted proteins were analyzed by PAGE-SDS where we observed approximately 11 bands. In addition, the capacity of these secretions to degrade proteins was analyzed by gelatin substrate zymography. A degradation band of about 62 kDa was found in these assays. Western blot assays suggested that the matrix metalloproteinase 2 (MMP-2) is responsible for this protease activity. Thus, our results indicate that the establishment of a cell line derived from DC is a useful in vitro model to study the biology of this odontogenic lesion and its participation in the development of odontogenic tumors.

Keywords: dentigerous cyst, ameloblastoma, MMP-2, odontogenic tumors

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490 Treatment of Acid Mine Lake by Ultrasonically Modified Fly Ash at Different Frequencies

Authors: Burcu Ileri, Deniz Sanliyuksel Yucel, Onder Ayyildiz

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The oxidation of pyrite in water results in the formation of acid mine drainage, which typically forms extremely acid mine lake (AML) in the depression areas of abandoned Etili open-pit coal mine site, Northwest Turkey. Nine acid mine lakes of various sizes have been located in the Etili coal mine site. Hayirtepe AML is one of the oldest lake having a mean pH value of 2.9 and conductivity of 4550 μS/cm, and containing elevated concentrations of Al, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, and Zn. The water quality of the lake has been deteriorated due to its high chemical composition, in particular, increasing heavy metal pollution. In this study, fly ash (FA), a coal combustion by-product from fluidized bed thermal power plant in the northwestern part of Turkey, was used as an adsorbent for the treatment of Hayirtepe AML. The FA is a relatively abundant and cost effective material, but its use in adsorption processes usually require excessive adsorbent doses. To increase adsorption efficiency and lower the adsorbent dose, we modified the FA by means of ultrasonic treatment (20 kHz and 40 kHz). The images of scanning electron microscopy (SEM) have demonstrated that ultrasonic treatment not only decreased the size of ash particles but also created pits and cracks on their surfaces which in turn led to a significant increase in the BET surface area. Both FA and modified fly ash were later tested for the removal of heavy metals from the AML. The effect of various operating parameters such as ultrasonic power, pH, ash dose, and adsorption contact time were examined to obtain the optimum conditions for the treatment process. The results have demonstrated that removal of heavy metals by ultrasound-modified fly ash requires much shorter treatment times and lower adsorbent doses than those attained by the unmodified fly ash. This research was financially supported by the Scientific and Technological Research Council of Turkey (TUBITAK), (Project no: 116Y510).

Keywords: acid mine lake, heavy metal, modified fly ash, ultrasonic treatment

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489 Reinforcing Effects of Natural Micro-Particles on the Dynamic Impact Behaviour of Hybrid Bio-Composites Made of Short Kevlar Fibers Reinforced Thermoplastic Composite Armor

Authors: Edison E. Haro, Akindele G. Odeshi, Jerzy A. Szpunar

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Hybrid bio-composites are developed for use in protective armor through positive hybridization offered by reinforcement of high-density polyethylene (HDPE) with Kevlar short fibers and palm wood micro-fillers. The manufacturing process involved a combination of extrusion and compression molding techniques. The mechanical behavior of Kevlar fiber reinforced HDPE with and without palm wood filler additions are compared. The effect of the weight fraction of the added palm wood micro-fillers is also determined. The Young modulus was found to increase as the weight fraction of organic micro-particles increased. However, the flexural strength decreased with increasing weight fraction of added micro-fillers. The interfacial interactions between the components were investigated using scanning electron microscopy. The influence of the size, random alignment and distribution of the natural micro-particles was evaluated. Ballistic impact and dynamic shock loading tests were performed to determine the optimum proportion of Kevlar short fibers and organic micro-fillers needed to improve impact strength of the HDPE. These results indicate a positive hybridization by deposition of organic micro-fillers on the surface of short Kevlar fibers used in reinforcing the thermoplastic matrix leading to enhancement of the mechanical strength and dynamic impact behavior of these materials. Therefore, these hybrid bio-composites can be promising materials for different applications against high velocity impacts.

Keywords: hybrid bio-composites, organic nano-fillers, dynamic shocking loading, ballistic impacts, energy absorption

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488 Consequence of Multi-Templating of Closely Related Structural Analogues on a Chitosan-Methacryllic Acid Molecularly Imprinted Polymer Matrix-Thermal and Chromatographic Traits

Authors: O.Ofoegbu, S. Roongnapa, A.N. Eboatu

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Most polluted environments, most challengingly, aerosol types, contain a cocktail of different toxicants. Multi-templating of matrices have been the recent target by researchers in a bid to solving complex mixed-toxicant challenges using single or common remediation systems. This investigation looks at the effect of such multi-templated system vis-a-vis the synthesis by non-covalent interaction, of a molecularly imprinted polymer architecture using nicotine and its structural analogue Phenylalanine amide individually and, in the blend, (50:50), as template materials in a Chitosan-Methacrylic acid functional monomer matrix. The temperature for polymerization is 60OC and time for polymerization, 12hrs (water bath heating), 4mins for (microwave heating). The characteristic thermal properties of the molecularly imprinted materials are investigated using Simultaneous Thermal Analysis (STA) profiling, while the absorption and separation efficiencies based on the relative retention times and peak areas of templates were studied amongst other properties. Transmission Electron Microscopy (TEM) results obtained, show the creation of heterogeneous nanocavities, regardless, the introduction of Caffeine a close structural analogue presented near-zero perfusion. This confirms the selectivity and specificity of the templated polymers despite its dual-templated nature. The STA results presented the materials as having decomposition temperatures above 250OC and a relative loss in mass of less than19% over a period within 50mins of heating. Consequent to this outcome, multi-templated systems can be fabricated to sequester specifically and selectively targeted toxicants in a mixed toxicant populated system effectively.

Keywords: chitosan, dual-templated, methacrylic acid, mixed-toxicants, molecularly-imprinted-polymer

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487 Potentiodynamic Polarization Behavior of Surface Mechanical Attrition Treated AA7075

Authors: Vaibhav Pandey, K. Chattopadhyay, N. C. Santhi Srinivas, Vakil Singh

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Aluminium alloy 7075 consist of different intermetallic precipitate particles MgZn2, CuAl2, which result in heterogeneity of micro structure and influence the corrosion properties of the alloy. Artificial ageing was found to enhance the strength properties, but highly susceptible to stress-corrosion cracking. Various conventional surface modification techniques are developed for improving corrosion properties of aluminum alloys. This led to development of novel surface mechanical attrition treatment (SMAT) technique the so called ultrasonic shot peening which gives nano-grain structure at surface. In the present investigation the influence of surface mechanical attrition treatment on corrosion behavior of aluminum alloy 7075 was studied in 3.5wt% NaCl solution. Two different size of 1 mm and 3 mm steel balls are used as peening media and SMAT was carried out for different time intervals 5, 15 and 30 minutes. Surface nano-grains/nano-crystallization was observed after SMAT. The formation of nano-grain structure was observed for larger size balls with time of treatment and consequent increase in micro strain. As-SMATed sample with 1 mm balls exhibits better corrosion resistance as compared to that of un-SMATed sample. The enhancement in corrosion resistance may be due to formation of surface nano-grain structure which reduced the electron release rate. In contrast the samples treated with 3 mm balls showed very poor corrosion resistance. A decrease in corrosion resistance was observed with increase in the time of peening. The decrease in corrosion resistance in the shotpeened samples with larger diameter balls may due to increase in microstrain and defect density.

Keywords: aluminum alloy 7075, corrosion, SMAT, ultrasonic shot peening, surface nano-grains

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486 Soil Bioremediation Monitoring Systems Powered by Microbial Fuel Cells

Authors: András Fülöp, Lejla Heilmann, Zsolt Szabó, Ákos Koós

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Microbial fuel cells (MFCs) present a sustainable biotechnological solution to future energy demands. The aim of this study was to construct soil based, single cell, membrane-less MFC systems, operated without treatment to continuously power on-site monitoring and control systems during the soil bioremediation processes. Our Pseudomonas aeruginosa 541 isolate is an ideal choice for MFCs, because it is able to produce pyocyanin which behaves as electron-shuttle molecule, furthermore, it also has a significant antimicrobial effect. We tested several materials and structural configurations to obtain long term high power output. Comparing different configurations, a proton exchange membrane-less, 0.6 m long with 0.05 m diameter MFC tubes offered the best long-term performances. The long-term electricity production were tested from starch, yeast extract (YE), carboxymethyl cellulose (CMC) with humic acid (HA) as a mediator. In all cases, 3 kΩ external load have been used. The two best-operated systems were the Pseudomonas aeruginosa 541 containing MFCs with 1 % carboxymethyl cellulose and the MFCs with 1% yeast extract in the anode area and 35% hydrogel in the cathode chamber. The first had 3.3 ± 0.033 mW/m2 and the second had 4.1 ± 0.065 mW/m2 power density values. These systems have operated for 230 days without any treatment. The addition of 0.2 % HA and 1 % YE referred to the volume of the anode area resulted in 1.4 ± 0.035 mW/m2 power densities. The mixture of 1% starch with 0.2 % HA gave 1.82 ± 0.031 mW/m2. Using CMC as retard carbon source takes effect in the long-term bacterial survivor, thus enable the expression of the long term power output. The application of hydrogels in the cathode chamber significantly increased the performance of the MFC units due to their good water retention capacity.

Keywords: microbial fuel cell, bioremediation, Pseudomonas aeruginosa, biotechnological solution

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

Authors: Tafadzwa Makonese, Harold Annegarn, Patricia Forbes

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

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

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484 Modification of Aliphatic-Aromatic Copolyesters with Polyether Block for Segmented Copolymers with Elastothemoplastic Properties

Authors: I. Irska, S. Paszkiewicz, D. Pawlikowska, E. Piesowicz, A. Linares, T. A. Ezquerra

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Due to the number of advantages such as high tensile strength, sensitivity to hydrolytic degradation, and biocompatibility poly(lactic acid) (PLA) is one of the most common polyesters for biomedical and pharmaceutical applications. However, PLA is a rigid, brittle polymer with low heat distortion temperature and slow crystallization rate. In order to broaden the range of PLA applications, it is necessary to improve these properties. In recent years a number of new strategies have been evolved to obtain PLA-based materials with improved characteristics, including manipulation of crystallinity, plasticization, blending, and incorporation into block copolymers. Among the other methods, synthesis of aliphatic-aromatic copolyesters has been attracting considerable attention as they may combine the mechanical performance of aromatic polyesters with biodegradability known from aliphatic ones. Given the need for highly flexible biodegradable polymers, in this contribution, a series of aromatic-aliphatic based on poly(butylene terephthalate) and poly(lactic acid) (PBT-b-PLA) copolyesters exhibiting superior mechanical properties were copolymerized with an additional poly(tetramethylene oxide) (PTMO) soft block. The structure and properties of both series were characterized by means of attenuated total reflectance – Fourier transform infrared spectroscopy (ATR-FTIR), nuclear magnetic resonance spectroscopy (¹H NMR), differential scanning calorimetry (DSC), wide-angle X-ray scattering (WAXS) and dynamic mechanical, thermal analysis (DMTA). Moreover, the related changes in tensile properties have been evaluated and discussed. Lastly, the viscoelastic properties of synthesized poly(ester-ether) copolymers were investigated in detail by step cycle tensile tests. The block lengths decreased with the advance of treatment, and the block-random diblock terpolymers of (PBT-ran-PLA)-b-PTMO were obtained. DSC and DMTA analysis confirmed unambiguously that synthesized poly(ester-ether) copolymers are microphase-separated systems. The introduction of polyether co-units resulted in a decrease in crystallinity degree and melting temperature. X-ray diffraction patterns revealed that only PBT blocks are able to crystallize. The mechanical properties of (PBT-ran-PLA)-b-PTMO copolymers are a result of a unique arrangement of immiscible hard and soft blocks, providing both strength and elasticity.

Keywords: aliphatic-aromatic copolymers, multiblock copolymers, phase behavior, thermoplastic elastomers

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483 Aspirin Loaded Poly-L-Lactic Acid Nanofibers and Their Potentials as Small Diameter Vascular Grafts

Authors: Mahboubeh Kabiri, Saba Aslani

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Among various approaches used for the treatment of cardiovascular diseases, the occlusion of the small-diameter vascular graft (SDVG) is still an unresolved problem which seeks further research to address them. Though autografts are now the gold standards to be replaced for blocked coronary arteries, they suffer from inadequate quality and quantity. On the other hand, the major problems of the tissue engineered grafts are thrombosis and intimal hyperplasia. Provision of a suitable spatiotemporal release pattern of anticoagulant agents such as heparin and aspirin can be a step forward to overcome such issues . Herein, we fabricated electrospun scaffolds from FDA (Food and Drug Administration) approved poly-L-lactic acid (PLLA) with aspirin loaded into the nanofibers. Also, we surface coated the scaffolds with Amniotic Membrane lysate as a source for natural elastic polymers and a mimic of endothelial basement membrane. The scaffolds were characterized thoroughly structurally and mechanically for their morphology, fiber orientation, tensile strength, hydrophilicity, cytotoxicity, aspirin release and cell attachment support. According to the scanning electron microscopy (SEM) images, the size of fibers ranged from 250 to 500 nm. The scaffolds showed appropriate tensile strength expected for vascular grafts. Cellular attachment, growth, and infiltration were proved using SEM and MTT (3-(4,5-Dimethylthiazol-2-Yl)-2,5-Diphenyltetrazolium Bromide) assay. Drug-loaded scaffolds showed a sustained release profile of aspirin in 7 days. An enhanced cytocompatibility was observed in AM-coated electrospun PLLA fibers compared to uncoated scaffolds. Our results together indicated that AM lysate coated ASA releasing scaffolds have promising potentials for development of a biocompatible SDVG.

Keywords: vascular tissue engineering, vascular grafts, anticoagulant agent, aspirin, amniotic membrane

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

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

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

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

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481 Preliminary Study of the Hydrothermal Polymetallic Ore Deposit at the Karancs Mountain, North-East Hungary

Authors: Eszter Kulcsar, Agnes Takacs, Gabriella B. Kiss, Peter Prakfalvi

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The Karancs Mountain is part of the Miocene Inner Carpathian Volcanic Belt and is located in N-NE Hungary, along the Hungarian-Slovakian border. The 14 Ma old andesitic-dacitic units are surrounded by Oligocene sedimentary units (sandstone, siltstone). The host rocks of the mineralisation are siliceous and/or argillaceous volcanic units, quartz veins, hydrothermal breccia, and strongly silicified vuggy rocks, found in the various altered volcanic units. The hydrothermal breccia consists of highly silicified vuggy quartz clasts in quartz matrix. The hydrothermal alteration of the host units shows structural control at the deeper levels. The main ore minerals are galena, pyrite, marcasite, sphalerite, hematite, magnetite, arsenopyrite, anglesite and argentite The mineralisation was first mentioned in 1944 and the first exploration took place between 1961 and 1962 in the area. The first ore geological studies were performed between 1984-1985. The exploration programme was limited only to surface sampling; no drilling programme was performed. Petrographical and preliminary fluid inclusion studies were performed on calcite samples from a galena-bearing vein. Despite the early discovery of the mineralisation, no detailed description is available, thus its size, characteristics, and origin have remained unknown. The aim of this study is to examine the mineralisation, describe the characteristics in detail and to test the possible gold content of the various quartz veins and breccias. Finally, we also investigate the potential relation of the hydrothermal mineralisation to the surrounding similar mineralisations with similar ages (e.g. W-Mátra Mountains in Hungary, Banska Bystrica, Banska Stiavnica in Slovakia) in order to place the mineralisation within the volcanic-hydrothermal evolution of the Miocene Inner Carpathian Belt. As first steps, the study includes field mapping, traditional petrological and ore microscopy; X-ray diffraction analysis; SEM-EDS and EMPA studies on ore minerals, to obtain mineral chemical information. Fluid inclusion petrography and microthermometry and micro-Raman-spectroscopy studies are also planned on quartz-hosted inclusions to investigate the physical and chemical properties of the ore-forming fluid.

Keywords: epithermal, Karancs Mountain, Hungary, Miocene Inner Carpathian volcanic belt, polimetallic ore deposit

Procedia PDF Downloads 128