Search results for: X-ray photoelectron spectroscopy.
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 372

Search results for: X-ray photoelectron spectroscopy.

282 Structural Investigation of Na2O–B2O3–SiO2 Glasses Doped with NdF3

Authors: M. S. Gaafar, S. Y. Marzouk

Abstract:

Sodium borosilicate glasses doped with different content of NdF3 mol % have been prepared by rapid quenching method. Ultrasonic velocities (both longitudinal and shear) measurements have been carried out at room temperature and at ultrasonic frequency of 4 MHz. Elastic moduli, Debye temperature, softening temperature and Poisson's ratio have been obtained as a function of NdF3 modifier content. Results showed that the elastic moduli, Debye temperature, softening temperature and Poisson's ratio have very slight change with the change of NdF3 mol % content. Based on FTIR spectroscopy and theoretical (Bond compression) model, quantitative analysis has been carried out in order to obtain more information about the structure of these glasses. The study indicated that the structure of these glasses is mainly composed of SiO4 units with four bridging oxygens (Q4), and with three bridging and one nonbridging oxygens (Q3).

Keywords: Borosilicate glasses, ultrasonic velocity, elastic moduli, FTIR spectroscopy, bond compression model.

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281 A Computational Study of N–H…O Hydrogen Bonding to Investigate Cooperative Effects

Authors: Setareh Shekarsaraei, Marjan Moridi, Nasser L. Hadipour

Abstract:

In this study, nuclear magnetic resonance spectroscopy and nuclear quadrupole resonance spectroscopy parameters of 14N (Nitrogen in imidazole ring) in N–H…O hydrogen bonding for Histidine hydrochloride monohydrate were calculated via density functional theory. We considered a five-molecule model system of Histidine hydrochloride monohydrate. Also we examined the trends of environmental effect on hydrogen bonds as well as cooperativity. The functional used in this research is M06-2X which is a good functional and the obtained results has shown good agreement with experimental data. This functional was applied to calculate the NMR and NQR parameters. Some correlations among NBO parameters, NMR and NQR parameters have been studied which have shown the existence of strong correlations among them. Furthermore, the geometry optimization has been performed using M062X/6-31++G(d,p) method. In addition, in order to study cooperativity and changes in structural parameters, along with increase in cluster size, natural bond orbitals have been employed.

Keywords: Hydrogen bonding, Density Functional Theory (DFT), Natural bond Orbitals (NBO), cooperativity effects.

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280 In Vitro and Experimental Screening of Mangrove Herbal Extract against Vibrio Alginolyticus in Marine Ornamental Fish

Authors: N. B. Dhayanithi, T. T. Ajith Kumar, T. Balasubramanian

Abstract:

Present study summarizes the control of Vibrio alginolyticus infection in hatchery reared Clownfish, Amphiprion sebae with the extract of the mangrove plant, Avicennia marina. Fishes with visible symptoms of hemorrhagic spots were chosen and the genomic DNA of the causative bacterium was isolated and sequenced based on 16S rDNA gene. The in vitro assay revealed that a fraction of A. marina leaf extract elucidated with ethyl acetate: methanol (6:4) showed a high activity (28 mm) at 125 μg/ml concentrations. About 4 % of the fraction fed along with live V. alginolyticus was significantly decreased the cumulative mortality (P<0.05) in the experimental groups than the control group. The responsible fraction was investigated by gas chromatography - mass spectroscopy and found the presence of active compounds. This is the first research in India to control vibriosis infection in marine ornamental fish with mangrove leaf extract.

Keywords: Amphiprion seabe, Avicennia marina, Gas Chromatography - Mass Spectroscopy, Vibrio alginolyticus

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279 Nanostructured Pt/MnO2 Catalysts and Their Performance for Oxygen Reduction Reaction in Air Cathode Microbial Fuel Cell

Authors: Maksudur Rahman Khan, Kar Min Chan, Huei Ruey Ong, Chin Kui Cheng, Wasikur Rahman

Abstract:

Microbial fuel cells (MFCs) represent a promising technology for simultaneous bioelectricity generation and wastewater treatment. Catalysts are significant portions of the cost of microbial fuel cell cathodes. Many materials have been tested as aqueous cathodes, but air-cathodes are needed to avoid energy demands for water aeration. The sluggish oxygen reduction reaction (ORR) rate at air cathode necessitates efficient electrocatalyst such as carbon supported platinum catalyst (Pt/C) which is very costly. Manganese oxide (MnO2) was a representative metal oxide which has been studied as a promising alternative electrocatalyst for ORR and has been tested in air-cathode MFCs. However the single MnO2 has poor electric conductivity and low stability. In the present work, the MnO2 catalyst has been modified by doping Pt nanoparticle. The goal of the work was to improve the performance of the MFC with minimum Pt loading. MnO2 and Pt nanoparticles were prepared by hydrothermal and sol gel methods, respectively. Wet impregnation method was used to synthesize Pt/MnO2 catalyst. The catalysts were further used as cathode catalysts in air-cathode cubic MFCs, in which anaerobic sludge was inoculated as biocatalysts and palm oil mill effluent (POME) was used as the substrate in the anode chamber. The asprepared Pt/MnO2 was characterized comprehensively through field emission scanning electron microscope (FESEM), X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) where its surface morphology, crystallinity, oxidation state and electrochemical activity were examined, respectively. XPS revealed Mn (IV) oxidation state and Pt (0) nanoparticle metal, indicating the presence of MnO2 and Pt. Morphology of Pt/MnO2 observed from FESEM shows that the doping of Pt did not cause change in needle-like shape of MnO2 which provides large contacting surface area. The electrochemical active area of the Pt/MnO2 catalysts has been increased from 276 to 617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The CV results in O2 saturated neutral Na2SO4 solution showed that MnO2 and Pt/MnO2 catalysts could catalyze ORR with different catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode catalyst generates a maximum power density of 165 mW/m3, which is higher than that of MFC with MnO2 catalyst (95 mW/m3). The open circuit voltage (OCV) of the MFC operated with MnO2 cathode gradually decreased during 14 days of operation, whereas the MFC with Pt/MnO2 cathode remained almost constant throughout the operation suggesting the higher stability of the Pt/MnO2 catalyst. Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced performance.

Keywords: Microbial fuel cell, oxygen reduction reaction, Pt/MnO2, palm oil mill effluent, polarization curve.

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278 Influence of [Emim][OAc] and Water on Gelatinization Process and Interactions with Starch

Authors: Shajaratuldur Ismail, Nurlidia Mansor, Zakaria Man

Abstract:

Thermoplastic starch (TPS) plasticized by 1-ethyl-3-methylimidazolium acetate [Emim][OAc] were obtained through gelatinization process. The gelatinization process occurred in the presence of water and [Emim][OAc] as plasticizer at high temperature (90˚C). The influence of [Emim][OAc] and water on the gelatinization and interactions with starch have been studied over a range of compositions. The homogenous mass was obtained for the samples containing 35, 40 and 43.5 % of water contents which showed that water plays important role in gelatinization process. Detailed IR spectroscopy analysis showed decrease in hydrogen bonding intensity and strong interaction between acetate anion in [Emim][OAc] and starch hydroxyl groups in the presence of [Emim][OAc]. Starch-[Emim][OAc]-water mixture at 10-3-8.7 presented homogenous mass, less hydrogen bonding intensity and strong interaction between acetate anion in [Emim][OAc] and starch hydroxyl groups.

Keywords: Starch, ionic liquid, 1-ethyl-3-methylimidazolium acetate, plasticizer, gelatinization, IR spectroscopy.

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277 Fluorescence Spectroscopy of Lysozyme-Silver Nanoparticles Complex

Authors: S. Ashrafpour, T. Tohidi Moghadam, B. Ranjbar

Abstract:

Identifying the nature of protein-nanoparticle interactions and favored binding sites is an important issue in functional characterization of biomolecules and their physiological responses. Herein, interaction of silver nanoparticles with lysozyme as a model protein has been monitored via fluorescence spectroscopy. Formation of complex between the biomolecule and silver nanoparticles (AgNPs) induced a steady state reduction in the fluorescence intensity of protein at different concentrations of nanoparticles. Tryptophan fluorescence quenching spectra suggested that silver nanoparticles act as a foreign quencher, approaching the protein via this residue. Analysis of the Stern-Volmer plot showed quenching constant of 3.73 μM−1. Moreover, a single binding site in lysozyme is suggested to play role during interaction with AgNPs, having low affinity of binding compared to gold nanoparticles. Unfolding studies of lysozyme showed that complex of lysozyme- AgNPs has not undergone structural perturbations compared to the bare protein. Results of this effort will pave the way for utilization of sensitive spectroscopic techniques for rational design of nanobiomaterials in biomedical applications.

Keywords: Nanocarrier, Nanoparticles, Surface Plasmon Resonance, Quenching Fluorescence.

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276 Effect of Oxygen Annealing on the Surface Defects and Photoconductivity of Vertically Aligned ZnO Nanowire Array

Authors: Ajay Kushwaha, Hemen Kalita, M. Aslam

Abstract:

Post growth annealing of solution grown ZnO nanowire array is performed under controlled oxygen ambience. The role of annealing over surface defects and their consequence on dark/photo-conductivity and photosensitivity of nanowire array is investigated. Surface defect properties are explored using various measurement tools such as contact angle, photoluminescence, Raman spectroscopy and XPS measurements. The contact angle of the NW films reduces due to oxygen annealing and nanowire film surface changes from hydrophobic (96°) to hydrophilic (16°). Raman and XPS spectroscopy reveal that oxygen annealing improves the crystal quality of the nanowire films. The defect band emission intensity (relative to band edge emission, ID/IUV) reduces from 1.3 to 0.2 after annealing at 600 °C at 10 SCCM flow of oxygen. An order enhancement in dark conductivity is observed in O2 annealed samples, while photoconductivity is found to be slightly reduced due to lower concentration of surface related oxygen defects.

Keywords: Zinc Oxide, Surface defects, Photoluminescence, Photoconductivity, Photosensor and Nanowire thin film.

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275 Biomass and Pigment Production by Monascus during Miniaturized Submerged Culture on Adlay

Authors: Supavej Maniyom, Gerard H. Markx

Abstract:

Three reactor types were explored and successfully used for pigment production by Monascus: shake flasks, and shaken and stirred miniaturized reactors. Also, the use of dielectric spectroscopy for the on-line measurement of biomass levels was explored. Shake flasks gave good pigment yields, but scale up is difficult, and they cannot be automated. Shaken bioreactors were less successful with pigment production than stirred reactors. Experiments with different impeller speeds in different volumes of liquid in the reactor confirmed that this is most likely due oxygen availability. The availability of oxygen appeared to affect biomass levels less than pigment production; red pigment production in particular needed very high oxygen levels. Dielectric spectroscopy was effectively used to continuously measure biomass levels during the submerged fungal fermentation in the shaken and stirred miniaturized bioreactors, despite the presence of the solid substrate particles. Also, the capacitance signal gave useful information about the viability of the cells in the culture.

Keywords: Chinese pearl barley, miniature submerged culture, Monascus pigment, biomass, capacitance.

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274 Existence of Nano-Organic Carbon Particles below the Size Range of 10 nm in the Indoor Air Environment

Authors: Bireswar Paul, Amitava Datta

Abstract:

Indoor air environment is a big concern in the last few decades in the developing countries, with increased focus on monitoring the air quality. In this work, an experimental study has been conducted to establish the existence of carbon nanoparticles below the size range of 10 nm in the non-sooting zone of a LPG/air partially premixed flame. Mainly, four optical techniques, UV absorption spectroscopy, fluorescence spectroscopy, dynamic light scattering and TEM have been used to characterize and measure the size of carbon nanoparticles in the sampled materials collected from the inner surface of the flame front. The existence of the carbon nanoparticles in the sampled material has been confirmed with the typical nature of the absorption and fluorescence spectra already reported in the literature. The band gap energy shows that the particles are made up of three to six aromatic rings. The size measurement by DLS technique also shows that the particles below the size range of 10 nm. The results of DLS are also corroborated by the TEM image of the same material. 

Keywords: Indoor air, carbon nanoparticles, LPG, partially premixed flame, optical techniques.

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273 Pyrolysis of Rice Husk in a Fixed Bed Reactor

Authors: Natarajan. E, Ganapathy Sundaram. E

Abstract:

Fixed-bed slow pyrolysis experiments of rice husk have been conducted to determine the effect of pyrolysis temperature, heating rate, particle size and reactor length on the pyrolysis product yields. Pyrolysis experiments were performed at pyrolysis temperature between 400 and 600°C with a constant heating rate of 60°C/min and particle sizes of 0.60-1.18 mm. The optimum process conditions for maximum liquid yield from the rice husk pyrolysis in a fixed bed reactor were also identified. The highest liquid yield was obtained at a pyrolysis temperature of 500°C, particle size of 1.18-1.80 mm, with a heating rate of 60°C/min in a 300 mm length reactor. The obtained yield of, liquid, gas and solid were found be in the range of 22.57-31.78 %, 27.75-42.26 % and 34.17-42.52 % (all weight basics) respectively at different pyrolysis conditions. The results indicate that the effects of pyrolysis temperature and particle size on the pyrolysis yield are more significant than that of heating rate and reactor length. The functional groups and chemical compositions present in the liquid obtained at optimum conditions were identified by Fourier Transform-Infrared (FT-IR) spectroscopy and Gas Chromatography/ Mass Spectroscopy (GC/MS) analysis respectively.

Keywords: Slow pyrolysis, Rice husk, Recycling, Biomass.

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272 The Determination of the Potassium Nitrate, Sodium Hydroxide and Boric Acid Molar Ratio in the Synthesis of Potassium Borates via Hydrothermal Method

Authors: M. Yildirim, A. S. Kipcak, F. T. Senberber, M. O. Asensio, E. M. Derun, S. Piskin

Abstract:

Potassium borates, which are widely used in welding and metal refining industry, as a lubricating oil additive, cement additive, fiberglass additive and insulation compound, are one of the important groups of borate minerals. In this study the production of a potassium borate mineral via hydrothermal method is aimed. The potassium source of potassium nitrate (KNO3) was used along with a sodium source of sodium hydroxide (NaOH) and boron source of boric acid (H3BO3). The constant parameters of reaction temperature and reaction time were determined as 80°C and 1 h, respectively. The molar ratios of 1:1:3 (as KNO3:NaOH:H3BO3), 1:1:4, 1:1:5, 1:1:6 and 1:1:7 were used. Following the synthesis the identifications of the produced products were conducted by X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman Spectroscopy. The results of the experiments and analysis showed in the ratio of 1:1:6, the Santite mineral with powder diffraction file number (pdf no.) of 01-072-1688, which is known as potassium pentaborate (KB5O8·4H2O) was synthesized as best.

Keywords: Hydrothermal synthesis, potassium borate, potassium nitrate, santite.

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271 Study of Compost Maturity during Humification Process using UV-Spectroscopy

Authors: N. Sanmanee, K. Panishkan, K. Obsuwan, S. Dharmvanij

Abstract:

The increments of aromatic structures are widely used to monitor the degree of humification. Compost derived from mix manures mixed with agricultural wastes was studied. The compost collected at day 0, 7, 14, 21, 28, 35, 49, 77, 91, 105, and 119 was divided into 3 stages, initial stage at day 0, thermophilic stage during day 1-48, and mature stage during day 49-119. The change of highest absorptions at wavelength range between 210-235 nm during day 0- 49 implied that small molecules such as nitrates and carboxylic occurred faster than the aromatic molecules that were found at wavelength around 280 nm. The ratio of electron-transfer band at wavelength 253 nm by the benzonoid band at wavelength 230 nm (E253/E230) also gradually increased during the fermenting period indicating the presence of O-containing functional groups. This was in agreement with the shift change from aliphatic to aromatic structures as shown by the relationship with C/N and H/C ratios (r = - 0.631 and -0.717, p< 0.05) since both were decreasing. Although the amounts of humic acid (HA) were not different much during the humification process, the UV spectral deconvolution showed better qualitative characteristics to help in determining the compost quality. From this study, the compost should be used at day 49 and should not be kept longer than 3 months otherwise the quality of HA would decline regardless of the amounts of HA that might be rising. This implied that other processes, such as mineralization had an influence on the humification process changing HA-s structure and its qualities.

Keywords: Compost maturity, UV spectroscopy, humification, humic acid

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270 Photoimpedance Spectroscopy Analysis of Planar and Nano-Textured Thin-Film Silicon Solar Cells

Authors: P. Kumar, D. Eisenhauer, M. M. K. Yousef, Q. Shi, A. S. G. Khalil, M. R. Saber, C. Becker, T. Pullerits, K. J. Karki

Abstract:

In impedance spectroscopy (IS) the response of a photo-active device is analysed as a function of ac bias. It is widely applied in a broad class of material systems and devices. It gives access to fundamental mechanisms of operation of solar cells. We have implemented a method of IS where we modulate the light instead of the bias. This scheme allows us to analyze not only carrier dynamics but also impedance of device locally. Here, using this scheme, we have measured the frequency-dependent photocurrent response of the thin-film planar and nano-textured Si solar cells using this method. Photocurrent response is measured in range of 50 Hz to 50 kHz. Bode and Nyquist plots are used to determine characteristic lifetime of both the cells. Interestingly, the carrier lifetime of both planar and nano-textured solar cells depend on back and front contact positions. This is due to either heterogeneity of device or contacts are not optimized. The estimated average lifetime is found to be shorter for the nano-textured cell, which could be due to the influence of the textured interface on the carrier relaxation dynamics.

Keywords: Carrier lifetime, Impedance, nano-textured, and photocurrent.

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269 A Self Organized Map Method to Classify Auditory-Color Synesthesia from Frontal Lobe Brain Blood Volume

Authors: Takashi Kaburagi, Takamasa Komura, Yosuke Kurihara

Abstract:

Absolute pitch is the ability to identify a musical note without a reference tone. Training for absolute pitch often occurs in preschool education. It is necessary to clarify how well the trainee can make use of synesthesia in order to evaluate the effect of the training. To the best of our knowledge, there are no existing methods for objectively confirming whether the subject is using synesthesia. Therefore, in this study, we present a method to distinguish the use of color-auditory synesthesia from the separate use of color and audition during absolute pitch training. This method measures blood volume in the prefrontal cortex using functional Near-infrared spectroscopy (fNIRS) and assumes that the cognitive step has two parts, a non-linear step and a linear step. For the linear step, we assume a second order ordinary differential equation. For the non-linear part, it is extremely difficult, if not impossible, to create an inverse filter of such a complex system as the brain. Therefore, we apply a method based on a self-organizing map (SOM) and are guided by the available data. The presented method was tested using 15 subjects, and the estimation accuracy is reported.

Keywords: Absolute pitch, functional near-infrared spectroscopy, prefrontal cortex, synesthesia.

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268 Analysis of Bio-Oil Produced by Pyrolysis of Coconut Shell

Authors: D. S. Fardhyanti, A. Damayanti

Abstract:

The utilization of biomass as a source of new and renewable energy is being carried out. One of the technologies to convert biomass as an energy source is pyrolysis which is converting biomass into more valuable products, such as bio-oil. Bio-oil is a liquid which is produced by steam condensation process from the pyrolysis of coconut shells. The composition of a coconut shell e.g. hemicellulose, cellulose and lignin will be oxidized to phenolic compounds as the main component of the bio-oil. The phenolic compounds in bio-oil are corrosive; they cause various difficulties in the combustion system because of a high viscosity, low calorific value, corrosiveness, and instability. Phenolic compounds are very valuable components which phenol has used as the main component for the manufacture of antiseptic, disinfectant (known as Lysol) and deodorizer. The experiments typically occurred at the atmospheric pressure in a pyrolysis reactor at temperatures ranging from 300 oC to 350 oC with a heating rate of 10 oC/min and a holding time of 1 hour at the pyrolysis temperature. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the bio-oil components. The obtained bio-oil has the viscosity of 1.46 cP, the density of 1.50 g/cm3, the calorific value of 16.9 MJ/kg, and the molecular weight of 1996.64. By GC-MS, the analysis of bio-oil showed that it contained phenol (40.01%), ethyl ester (37.60%), 2-methoxy-phenol (7.02%), furfural (5.45%), formic acid (4.02%), 1-hydroxy-2-butanone (3.89%), and 3-methyl-1,2-cyclopentanedione (2.01%).

Keywords: Bio-oil, pyrolysis, coconut shell, phenol, gas chromatography-mass spectroscopy.

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267 Titanium Dioxide Modified with Glutathione as Potential Drug Carrier with Reduced Toxic Properties

Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

Abstract:

The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO2 nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO2 nanoparticles was characterized from 30 nm to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were: water, SBF and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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266 Effect of the Polymer Modification on the Cytocompatibility of Human and Rat Cells

Authors: N. Slepickova Kasalkova, P. Slepicka, L. Bacakova, V. Svorcik

Abstract:

Tissue engineering includes combination of materials and techniques used for the improvement, repair or replacement of the tissue. Scaffolds, permanent or temporally material, are used as support for the creation of the "new cell structures". For this important component (scaffold), a variety of materials can be used. The advantage of some polymeric materials is their cytocompatibility and possibility of biodegradation. Poly(L-lactic acid) (PLLA) is a biodegradable,  semi-crystalline thermoplastic polymer. PLLA can be fully degraded into H2O and CO2. In this experiment, the effect of the surface modification of biodegradable polymer (performed by plasma treatment) on the various cell types was studied. The surface parameters and changes of the physicochemical properties of modified PLLA substrates were studied by different methods. Surface wettability was determined by goniometry, surface morphology and roughness study were performed with atomic force microscopy and chemical composition was determined using photoelectron spectroscopy. The physicochemical properties were studied in relation to cytocompatibility of human osteoblast (MG 63 cells), rat vascular smooth muscle cells (VSMC), and human stem cells (ASC) of the adipose tissue in vitro. A fluorescence microscopy was chosen to study and compare cell-material interaction. Important parameters of the cytocompatibility like adhesion, proliferation, viability, shape, spreading of the cells were evaluated. It was found that the modification leads to the change of the surface wettability depending on the time of modification. Short time of exposition (10-120 s) can reduce the wettability of the aged samples, exposition longer than 150 s causes to increase of contact angle of the aged PLLA. The surface morphology is significantly influenced by duration of modification, too. The plasma treatment involves the formation of the crystallites, whose number increases with increasing time of modification. On the basis of physicochemical properties evaluation, the cells were cultivated on the selected samples. Cell-material interactions are strongly affected by material chemical structure and surface morphology. It was proved that the plasma treatment of PLLA has a positive effect on the adhesion, spreading, homogeneity of distribution and viability of all cultivated cells. This effect was even more apparent for the VSMCs and ASCs which homogeneously covered almost the whole surface of the substrate after 7 days of cultivation. The viability of these cells was high (more than 98% for VSMCs, 89-96% for ASCs). This experiment is one part of the basic research, which aims to easily create scaffolds for tissue engineering with subsequent use of stem cells and their subsequent "reorientation" towards the bone cells or smooth muscle cells.

Keywords: Poly(L-lactic acid), plasma treatment, surface characterization, cytocompatibility, human osteoblasts, rat vascular smooth muscle cells, human stem cells.

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265 Fe3O4 and Fe3O4@Au Nanoparticles: Synthesis and Functionalisation for Biomolecular Attachment

Authors: Hendriëtte van der Walt, Lesley Chown, Richard Harris, Ndabenhle Sosibo, Robert Tshikhudo

Abstract:

The use of magnetic and magnetic/gold core/shell nanoparticles in biotechnology or medicine has shown good promise due to their hybrid nature which possesses superior magnetic and optical properties. Some of these potential applications include hyperthermia treatment, bio-separations, diagnostics, drug delivery and toxin removal. Synthesis refinement to control geometric and magnetic/optical properties, and finding functional surfactants for biomolecular attachment, are requirements to meet application specifics. Various high-temperature preparative methods were used for the synthesis of iron oxide and gold-coated iron oxide nanoparticles. Different surface functionalities, such as 11-aminoundecanoic and 11-mercaptoundecanoic acid, were introduced on the surface of the particles to facilitate further attachment of biomolecular functionality and drug-like molecules. Nanoparticle thermal stability, composition, state of aggregation, size and morphology were investigated and the results from techniques such as Fourier Transform-Infra Red spectroscopy (FT-IR), Ultraviolet visible spectroscopy (UV-vis), Transmission Electron Microscopy (TEM) and thermal analysis are discussed.

Keywords: Core/shell, Iron oxide, Gold coating, Nanoparticles.

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264 Differentiation of Cancerous Prostate tissue from Non-Cancerous Prostate tissue by using Elastic Light Single-Scattering Spectroscopy: A Feasibility Study

Authors: T. Denkçeken, M. Canpolat, Đ. Bassorgun, S. Yücel, M.A. Çiftçioğlu, M. Baykara Murat Canpolat , Tuba Denkçeken , Đbrahim Bassorgun , Selçuk Yücel , M. Akif Çiftçioğlu , Mehmet Baykara

Abstract:

Elastic light single-scattering spectroscopy system with a single optical fiber probe was employed to differentiate cancerous prostate tissue from non-cancerous prostate tissue ex-vivo just after radical prostatectomy. First, ELSSS spectra were acquired from cancerous prostate tissue to define its spectral features. Then, spectra were acquired from normal prostate tissue to define difference in spectral features between the cancerous and normal prostate tissues. Of the total 66 tissue samples were evaluated from nine patients by ELSSS system. Comparing of histopathology results and ELSSS measurements revealed that sign of the spectral slopes of cancerous prostate tissue is negative and non-cancerous tissue is positive in the wavelength range from 450 to 750 nm. Based on the correlation between histopathology results and sign of the spectral slopes, ELSSS system differentiates cancerous prostate tissue from non- cancerous with a sensitivity of 0.95 and a specificity of 0.94.

Keywords: Diagnosis, prostatic neoplasm, prostatectomy, spectrum analysis

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263 The Data Processing Electronics of the METIS Coronagraph aboard the ESA Solar Orbiter Mission

Authors: M. Focardi, M. Pancrazzi, M. Uslenghi, G. Nicolini, E. Magli, F. Landini, M. Romoli, A. Bemporad, E. Antonucci, S. Fineschi, G. Naletto, P. Nicolosi, D. Spadaro, V. Andretta

Abstract:

METIS is the Multi Element Telescope for Imaging and Spectroscopy, a Coronagraph aboard the European Space Agency-s Solar Orbiter Mission aimed at the observation of the solar corona via both VIS and UV/EUV narrow-band imaging and spectroscopy. METIS, with its multi-wavelength capabilities, will study in detail the physical processes responsible for the corona heating and the origin and properties of the slow and fast solar wind. METIS electronics will collect and process scientific data thanks to its detectors proximity electronics, the digital front-end subsystem electronics and the MPPU, the Main Power and Processing Unit, hosting a space-qualified processor, memories and some rad-hard FPGAs acting as digital controllers.This paper reports on the overall METIS electronics architecture and data processing capabilities conceived to address all the scientific issues as a trade-off solution between requirements and allocated resources, just before the Preliminary Design Review as an ESA milestone in April 2012.

Keywords: Solar Coronagraph, Data Processing Electronics, VIS and UV/EUV Detectors, LEON Processor, Rad-hard FPGAs

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262 Spectroscopic Determination of Functionalized Active Principles from Coleus aromaticus Benth Leaf Extract Using Ionic Liquids

Authors: Zharama M. Llarena

Abstract:

Green chemistry for plant extraction of active principles is the main interest of many researchers concerned with climate change. While classical organic solvents are detrimental to our environment, greener alternatives to ionic liquids are very promising for sustainable organic chemistry. This study focused on the determination of functional groups observed in the main constituents from the ionic liquid extracts of Coleus aromaticus Benth leaves using FT-IR Spectroscopy. Moreover, this research aimed to determine the best ionic liquid that can separate functionalized plant constituents from the leaves Coleus aromaticus Benth using Fourier Transform Infrared Spectroscopy. Coleus aromaticus Benth leaf extract in different ionic liquids, elucidated pharmacologically important functional groups present in major constituents of the plant, namely, rosmarinic acid, caffeic acid and chlorogenic acid. In connection to distinctive appearance of functional groups in the spectrum and highest % transmittance, potassium chloride-glycerol is the best ionic liquid for green extraction.

Keywords: Coleus aromaticus, ionic liquid, rosmarinic acid, caffeic acid, chlorogenic acid.

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261 Synthesis and Fluorescence Spectroscopy of Sulphonic Acid-Doped Polyaniline When Exposed to Oxygen Gas

Authors: S.F.S. Draman, R. Daik, A. Musa

Abstract:

Three sulphonic acid-doped polyanilines were synthesized through chemical oxidation at low temperature (0-5 oC) and potential of these polymers as sensing agent for O2 gas detection in terms of fluorescence quenching was studied. Sulphuric acid, dodecylbenzene sulphonic acid (DBSA) and camphor sulphonic acid (CSA) were used as doping agents. All polymers obtained were dark green powder. Polymers obtained were characterized by Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, thermogravimetry analysis, elemental analysis, differential scanning calorimeter and gel permeation chromatography. Characterizations carried out showed that polymers were successfully synthesized with mass recovery for sulphuric aciddoped polyaniline (SPAN), DBSA-doped polyaniline (DBSA-doped PANI) and CSA-doped polyaniline (CSA-doped PANI) of 71.40%, 75.00% and 39.96%, respectively. Doping level of SPAN, DBSAdoped PANI and CSA-doped PANI were 32.86%, 33.13% and 53.96%, respectively as determined based on elemental analysis. Sensing test was carried out on polymer sample in the form of solution and film by using fluorescence spectrophotometer. Samples of polymer solution and polymer film showed positive response towards O2 exposure. All polymer solutions and films were fully regenerated by using N2 gas within 1 hour period. Photostability study showed that all samples of polymer solutions and films were stable towards light when continuously exposed to xenon lamp for 9 hours. The relative standard deviation (RSD) values for SPAN solution, DBSA-doped PANI solution and CSA-doped PANI solution for repeatability were 0.23%, 0.64% and 0.76%, respectively. Meanwhile RSD values for reproducibility were 2.36%, 6.98% and 1.27%, respectively. Results for SPAN film, DBSAdoped PANI film and CSA-doped PANI film showed the same pattern with RSD values for repeatability of 0.52%, 4.05% and 0.90%, respectively. Meanwhile RSD values for reproducibility were 2.91%, 10.05% and 7.42%, respectively. The study on effect of the flow rate on response time was carried out using 3 different rates which were 0.25 mL/s, 1.00 mL/s and 2.00 mL/s. Results obtained showed that the higher the flow rate, the shorter the response time.

Keywords: conjugated polymer, doping, fluorescence quenching, oxygen gas.

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260 Synthesis and Physicochemical Characterization of Biomimetic Scaffold of Gelatin/Zn-Incorporated 58S Bioactive Glass

Authors: Seyed Mohammad Hosseini, Amirhossein Moghanian

Abstract:

The main purpose of this research was to design a biomimetic system by freeze-drying method for evaluating the effect of adding 5 and 10 mol. % of zinc (Zn) in 58S bioactive glass and gelatin (5ZnBG/G and 10ZnBG/G) in terms of structural and biological changes. The structural analyses of samples were performed by X-Ray Diffraction (XRD), scanning electron microscopy (SEM) and Fourier-transform infrared (FTIR) spectroscopy. Also, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and alkaline phosphatase (ALP) activity tests were carried out for investigation of MC3T3-E1 cell behaviors. The SEM results demonstrated the spherical shape of the formed hydroxyapatite (HA) phases and also HA characteristic peaks were detected by XRD spectroscopy after 3 days of immersion in the simulated body fluid (SBF) solution. Meanwhile, FTIR spectra proved that the intensity of P–O peaks for 5ZnBG/G was more than 10ZnBG/G and control samples. Moreover, the results of ALP activity test illustrated that the optimal amount of Zn (5ZnBG/G) caused a considerable enhancement in bone cell growth. Taken together, the scaffold with 5 mol.% Zn was introduced as an optimal sample because of its higher biocompatibility, in vitro bioactivity and growth of MC3T3-E1 cells in comparison with other samples in bone tissue engineering.

Keywords: Scaffold, gelatin, modified bioactive glass, ALP, bone tissue engineering.

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259 Application of Voltammetry to Study Corrosion of Steel Buried in Unsaturated Soil in the Presence of Cathodic Protection

Authors: Mandlenkosi George Robert Mahlobo, Peter Apata Olubambi, Philippe Refait

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The aim of this study was to use voltammetry as a method to understand the behavior of steel in unsaturated soil in the presence of cathodic protection (CP). Three carbon steel coupons were buried in artificial soil wetted at 65-70% of saturation for 37 days. All three coupons were left at open circuit potential (OCP) for the first seven days in the unsaturated soil before CP which was only applied on two of the three coupons at the protection potential -0.8 V vs. Cu/CuSO4 for the remaining 30 days of the experiment. Voltammetry was performed weekly on the coupon without CP while electrochemical impedance spectroscopy (EIS) was performed daily to monitor and correct the applied CP potential from ohmic drop. Voltammetry was finally performed the last day on the coupons under CP. All the voltammograms were modeled with mathematical equations in order to compute the electrochemical parameters and subsequently deduce the corrosion rate of the steel coupons. For the coupon without CP, the corrosion rate was determined at 300 µm/y. For the coupons under CP, the residual corrosion rate under CP was estimated at 12 µm/y while the corrosion rate of the coupons, after interruption of CP, was estimated at 25 µm/y. This showed that CP was efficient due to two effects: a direct effect, from the decreased potential, and an induced effect, associated with the increased interfacial pH that promoted the formation of a protective layer on the steel surface.

Keywords: Carbon steel, cathodic protection, voltammetry, unsaturated soil, Raman spectroscopy.

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258 Preparation and Conductivity Measurements of LSM/YSZ Composite Solid Oxide Electrolysis Cell Anode Materials

Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO3 (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La0.8Sr0.2MnO3/Zr0.92Y0.08O2 (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10-1 S/cm at 600 oC with 0.22 eV activation energy.

Keywords: Ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy.

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257 Feasibility Investigation of Near Infrared Spectrometry for Particle Size Estimation of Nano Structures

Authors: A. Bagheri Garmarudi, M. Khanmohammadi, N. Khoddami, K. Shabani

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Determination of nano particle size is substantial since the nano particle size exerts a significant effect on various properties of nano materials. Accordingly, proposing non-destructive, accurate and rapid techniques for this aim is of high interest. There are some conventional techniques to investigate the morphology and grain size of nano particles such as scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffractometry (XRD). Vibrational spectroscopy is utilized to characterize different compounds and applied for evaluation of the average particle size based on relationship between particle size and near infrared spectra [1,4] , but it has never been applied in quantitative morphological analysis of nano materials. So far, the potential application of nearinfrared (NIR) spectroscopy with its ability in rapid analysis of powdered materials with minimal sample preparation, has been suggested for particle size determination of powdered pharmaceuticals. The relationship between particle size and diffuse reflectance (DR) spectra in near infrared region has been applied to introduce a method for estimation of particle size. Back propagation artificial neural network (BP-ANN) as a nonlinear model was applied to estimate average particle size based on near infrared diffuse reflectance spectra. Thirty five different nano TiO2 samples with different particle size were analyzed by DR-FTNIR spectrometry and the obtained data were processed by BP- ANN.

Keywords: near infrared, particle size, chemometrics, neuralnetwork, nano structure.

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256 Growth of Multi-Layered Graphene Using Organic Solvent-PMMA Film as the Carbon Source under Low Temperature Conditions

Authors: Alaa Y. Ali, Natalie P. Holmes, John Holdsworth, Warwick Belcher, Paul Dastoor, Xiaojing Zhou

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Multi-layered graphene has been produced under low temperature chemical vapour deposition (CVD) growth conditions by utilizing an organic solvent and polymer film source. Poly(methylmethacrylate) (PMMA) was dissolved in chlorobenzene solvent and used as a drop-cast film carbon source on a quartz slide. A source temperature (Tsource) of 180 °C provided sufficient carbon to grow graphene, as identified by Raman spectroscopy, on clean copper foil catalytic surfaces.  Systematic variation of hydrogen gas (H2) flow rate from 25 standard cubic centimeters per minute (sccm) to 100 sccm and CVD temperature (Tgrowth) from 400 to 800 °C, yielded graphene films of varying quality as characterized by Raman spectroscopy. The optimal graphene growth parameters were found to occur with a hydrogen flow rate of 75 sccm sweeping the 180 °C source carbon past the Cu foil at 600 °C for 1 min. The deposition at 600 °C with a H2 flow rate of 75 sccm yielded a 2D band peak with ~53.4 cm-1 FWHM and a relative intensity ratio of the G to 2D bands (IG/I2D) of 0.21. This recipe fabricated a few layers of good quality graphene.

Keywords: Graphene, chemical vapour deposition, carbon source, low temperature growth.

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255 Chaotic Properties of Hemodynamic Responsein Functional Near Infrared Spectroscopic Measurement of Brain Activity

Authors: Ni Ni Soe , Masahiro Nakagawa

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Functional near infrared spectroscopy (fNIRS) is a practical non-invasive optical technique to detect characteristic of hemoglobin density dynamics response during functional activation of the cerebral cortex. In this paper, fNIRS measurements were made in the area of motor cortex from C4 position according to international 10-20 system. Three subjects, aged 23 - 30 years, were participated in the experiment. The aim of this paper was to evaluate the effects of different motor activation tasks of the hemoglobin density dynamics of fNIRS signal. The chaotic concept based on deterministic dynamics is an important feature in biological signal analysis. This paper employs the chaotic properties which is a novel method of nonlinear analysis, to analyze and to quantify the chaotic property in the time series of the hemoglobin dynamics of the various motor imagery tasks of fNIRS signal. Usually, hemoglobin density in the human brain cortex is found to change slowly in time. An inevitable noise caused by various factors is to be included in a signal. So, principle component analysis method (PCA) is utilized to remove high frequency component. The phase pace is reconstructed and evaluated the Lyapunov spectrum, and Lyapunov dimensions. From the experimental results, it can be conclude that the signals measured by fNIRS are chaotic.

Keywords: Chaos, hemoglobin, Lyapunov spectrum, motorimagery, near infrared spectroscopy (NIRS), principal componentanalysis (PCA).

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254 The Effects and Interactions of Synthesis Parameters on Properties of Mg Substituted Hydroxyapatite

Authors: S. Sharma, U. Batra, S. Kapoor, A. Dua

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In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the assynthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p<0.0001, two way ANOVA), however, these were independent of TEA addition (p>0.15, two way ANOVA). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p<0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.

Keywords: Capping agent, hydroxyapatite, regression analysis, sol-gel, 2- sample t-test, two-way ANOVA.

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253 Application of Molecular Materials in the Manufacture of Flexible and Organic Devices for Photovoltaic Applications

Authors: M. Gómez-Gómez, M. E. Sánchez-Vergara

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Many sustainable approaches to generate electric energy have emerged in the last few decades; one of them is through solar cells. Yet, this also has the disadvantage of highly polluting inorganic semiconductor manufacturing processes. Therefore, the use of molecular semiconductors must be considered. In this work, allene compounds C24H26O4 and C24H26O5 were used as dopants to manufacture semiconductor films based on PbPc by high-vacuum evaporation technique. IR spectroscopy was carried out to determine the phase and any significant chemical changes which may occur during the thermal evaporation. According to UV-visible spectroscopy and Tauc’s model, the deposition process generated thin films with an activation energy range of 1.47 eV to 1.55 eV for direct transitions and 1.29 eV to 1.33 eV for indirect transitions. These values place the manufactured films within the range of low bandgap semiconductors. The flexible devices were manufactured: polyethylene terephthalate (PET), Indium tin oxide (ITO)/organic semiconductor/Cubic Close Packed (CCP). The characterization of the devices was carried out by evaluating electrical conductivity using the four-probe collinear method. I-V curves were obtained under different lighting conditions at room temperature. OS1 (PbPc/C24H26O4) showed an Ohmic behavior, while OS2 (PbPc/C24H26O5) reached higher current values at lower voltages. The results obtained show that the semiconductor devices doped with allene compounds can be used in the manufacture of optoelectronic devices.

Keywords: Electrical properties, optical gap, phthalocyanine, thin film.

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