Search results for: FT-IR spectroscopy

Authors: M. AlSawalha, F. Roessner, L. Novikova, L. Bel'chinskaya

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The acidity of different raw Jordanian clays containing zeolite, bentonite, red and white kaolinite and diatomite was characterized by means of temperature programmed desorption (TPD) of ammonia, conversion of 2-methyl-3-butyn-2-ol (MBOH), FTIR and BET-measurements. FTIR spectra proved presence of silanol and bridged hydroxyls on the clay surface. The number of acidic sites was calculated from experimental TPD-profiles. We observed the decrease of surface acidity correlates with the decrease of Si/Al ratio except for diatomite. On the TPD-plot for zeolite two maxima were registered due to different strength of surface acidic sites. Values of MBOH conversion, product yields and selectivity were calculated for the catalysis on Jordanian clays. We obtained that all clay samples are able to convert MBOH into a major product which is 3-methyl-3-buten-1-yne (MBYNE) catalyzed by acid surface sites with the selectivity close to 70%. There was found a correlation between MBOH conversion and acidity of clays determined by TPD-NH3, i.e. the higher the acidity the higher the conversion of MBOH. However, diatomite provided the lowest conversion of MBOH as result of poor polarization of silanol groups. Comparison of surface areas and conversions revealed the highest density of active sites for red kaolinite and the lowest for zeolite and diatomite.

Keywords: Acidity, Jordanian clay, Methylbutynol conversion, Temperature programmed desorption of ammonia

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Authors: A. Ould-Abbas, M. Bouchaour, , M. Madani, D. Trari, O. Zeggai, M. Boukais, N.-E.Chabane-Sari

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The porous silicon (PS), formed from the anodization of a p+ type substrate silicon, consists of a network organized in a pseudo-column as structure of multiple side ramifications. Structural micro-topology can be interpreted as the fraction of the interconnected solid phase contributing to thermal transport. The reduction of dimensions of silicon of each nanocristallite during the oxidation induced a reduction in thermal conductivity. Integration of thermal sensors in the Microsystems silicon requires an effective insulation of the sensor element. Indeed, the low thermal conductivity of PS consists in a very promising way in the fabrication of integrated thermal Microsystems.In this work we are interesting in the measurements of thermal conductivity (on the surface and in depth) of PS by the micro-Raman spectroscopy. The thermal conductivity is studied according to the parameters of anodization (initial doping and current density. We also, determine porosity of samples by spectroellipsometry.

Keywords: micro-Raman spectroscopy, mono-crysatl silicon, porous silicon, thermal conductivity

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Authors: S. Kassou, R. El Mrabet, A. Belaaraj, P. Guionneau, N. Hadi, T. Lamcharfi

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The organic–inorganic hybrid perovskite-like [C₆H₅C₂H₄NH₃]₂ZnCl₄ (PEA-ZnCl₄) was synthesized by saturated solutions method. X-ray powder diffraction, Raman spectroscopy, UV-visible transmittance, and capacitance meter measurements have been used to characterize the structure, the functional groups, the optical parameters, and the dielectric constants of the material. The material has a layered structure. The optical transmittance (T %) was recorded and applied to deduce the absorption coefficient (α) and optical band gap (Eg). The hybrid shows an insulator character with a direct band gap about 4.46 eV, and presents high dielectric constants up to a frequency of about 10⁵ Hz, which suggests a ferroelectric behavior. The reported optical and dielectric properties can help to understand the fundamental properties of perovskite materials and also to be used for optimizing or designing new devices.

Keywords: Dielectric constants, optical band gap (Eg), optical parameters, Raman spectroscopy, self-assembly organic inorganic hybrid.

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Authors: Aifa Afirah Rozlan, Mohamad Suhaimi Jaafar, Azhar Abdul Rahman

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Raman spectroscopy are used to characterize the chemical changes in normoxic polyhydroxyethylacrylate gel dosimeter (PHEA) induced by radiation. Irradiations in the low dose region are performed and the polymerizations of PHEA gels are monitored by the observing the changes of Raman shift intensity of the carbon covalent bond of PHEA originated from both monomer and the cross-linker. The variation in peak intensities with absorbed dose was observed. As the dose increase, the peak intensities of covalent bond of carbon in the polymer gels decrease. This point out that the amount of absorbed dose affect the polymerization of polymer gels. As the absorbed dose increase, the polymerizations also increase. Results verify that PHEA gel dosimeters are sensitive even in lower dose region.

Keywords: normoxic polymer gel, ascorbic acid, Ramanspectroscopy, radiation dosimetry.

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Authors: Marinos Xagoraris, Iliada K. Lappa, Charalambos Kanakis, Dimitra Daferera, Christina Papadopoulou, Georgios Sourounis, Charilaos Giotis, Pavlos Bouchagier, Christos S. Pappas, Petros A. Tarantilis, Efstathia Skotti

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The aim of this work was to recover phenolic compounds from grape skins produced in Greek varieties of the Ionian Islands in order to form the basis of calculations for their further utilization in the context of the circular economy. Isolation and further utilization of phenolic compounds is an important issue in winery by-products. For this purpose, 37 samples were collected, extracted, and analyzed in an attempt to provide the appropriate basis for their sustainable exploitation. Extraction of the bioactive compounds was held using an eco-friendly, non-toxic, and highly effective water-glycerol solvent system. Then, extracts were analyzed using UV-Vis, liquid chromatography-mass spectrometry (LC-MS), FTIR, and Raman spectroscopy. Also, total phenolic content and antioxidant activity were measured. LC-MS chromatography showed qualitative differences between different varieties. Peaks were attributed to monomeric 3-flavanols as well as monomeric, dimeric, and trimeric proanthocyanidins. The FT-IR and Raman spectra agreed with the chromatographic data and contributed to identifying phenolic compounds. Grape skins exhibited high total phenolic content (TPC), and it was proved that during vinification, a large number of polyphenols remained in the pomace. This study confirmed that grape skins from Ionian Islands are a promising source of bioactive compounds, suggesting their utilization under a bio-economic and environmental strategic framework.

Keywords: Antioxidant activity, grape skin, phenolic compounds, waste recovery.

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Authors: H. Ferfera-Harrar, N. Aiouaz, N. Dairi

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Superabsorbent polymers received much attention and are used in many fields because of their superior characters to traditional absorbents, e.g., sponge and cotton. So, it is very important but challenging to prepare highly and fast-swelling superabsorbents. A reliable, efficient and low-cost technique for removing heavy metal ions from wastewater is the adsorption using bio-adsorbents obtained from biological materials, such as polysaccharides-based hydrogels superabsorbents. In this study, novel multi-functional superabsorbent composites type semi-interpenetrating polymer networks (Semi-IPNs) were prepared via graft polymerization of acrylamide onto chitosan backbone in presence of gelatin, CTS-g-PAAm/Ge, using potassium persulfate and N,N’-methylene bisacrylamide as initiator and crosslinker, respectively. These hydrogels were also partially hydrolyzed to achieve superabsorbents with ampholytic properties and uppermost swelling capacity. The formation of the grafted network was evidenced by Fourier Transform Infrared Spectroscopy (ATR-FTIR) and Thermogravimetric Analysis (TGA). The porous structures were observed by Scanning Electron Microscope (SEM). From TGA analysis, it was concluded that the incorporation of the Ge in the CTS-g-PAAm network has marginally affected its thermal stability. The effect of gelatin content on the swelling capacities of these superabsorbent composites was examined in various media (distilled water, saline and pH-solutions). The water absorbency was enhanced by adding Ge in the network, where the optimum value was reached at 2 wt. % of Ge. Their hydrolysis has not only greatly optimized their absorption capacity but also improved the swelling kinetic.These materials have also showed reswelling ability. We believe that these super-absorbing materials would be very effective for the adsorption of harmful metal ions from wastewater.

Keywords: Chitosan, gelatin, superabsorbent, water absorbency.

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Authors: D. S. Fardhyanti, A. Damayanti

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Coal tar is a liquid by-product of coal pyrolysis processes. This liquid oil mixture contains various kinds of useful compounds such as benzoic aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. The coal tar was collected by pyrolysis process of coal obtained from PT Kaltim Prima Coal and Arutmin-Kalimantan. The experiments typically occurred at the atmospheric pressure in a laboratory furnace at temperatures ranging from 300 to 550oC with a heating rate of 10oC/min and a holding time of 1 hour at the pyrolysis temperature. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the coal tar components. The obtained coal tar has the viscosity of 3.12 cp, the density of 2.78 g/cm3, the calorific value of 11,048.44 cal/g, and the molecular weight of 222.67. The analysis result showed that the coal tar contained more than 78 chemical compounds such as benzene, cresol, phenol, xylene, naphtalene, etc. The total phenolic compounds contained in coal tar are 33.25% (PT KPC) and 17.58% (Arutmin-Kalimantan). The total naphtalene compounds contained in coal tar is 14.15% (PT KPC) and 17.13% (Arutmin-Kalimantan).

Keywords: Coal tar, pyrolysis, gas chromatography-mass spectroscopy.

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Authors: Morteza Elsa, Amirhossein Moghanian

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The major aim of this study was to evaluate the effect of CaO content on in vitro hydroxyapatite formation, MC3T3 cells cytotoxicity and proliferation as well as antibacterial efficiency of sol-gel derived SiO₂–CaO–P₂O₅ ternary system. For this purpose, first two grades of bioactive glass (BG); BG-58s (mol%: 60%SiO₂–36%CaO–4%P₂O₅) and BG-68s (mol%: 70%SiO₂–26%CaO–4%P₂O₅)) were synthesized by sol-gel method. Second, the effect of CaO content in their composition on in vitro bioactivity was investigated by soaking the BG-58s and BG-68s powders in simulated body fluid (SBF) for time periods up to 14 days and followed by characterization inductively coupled plasma atomic emission spectrometry (ICP-AES), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques. Additionally, live/dead staining, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), and alkaline phosphatase (ALP) activity assays were conducted respectively, as qualitatively and quantitatively assess for cell viability, proliferation and differentiations of MC3T3 cells in presence of 58s and 68s BGs. Results showed that BG-58s with higher CaO content showed higher in vitro bioactivity with respect to BG-68s. Moreover, the dissolution rate was inversely proportional to oxygen density of the BG. Live/dead assay revealed that both 58s and 68s increased the mean number live cells which were in good accordance with MTT assay. Furthermore, BG-58s showed more potential antibacterial activity against methicillin-resistant Staphylococcus aureus (MRSA) bacteria. Taken together, BG-58s with enhanced MC3T3 cells proliferation and ALP activity, acceptable bioactivity and significant high antibacterial effect against MRSA bacteria is suggested as a suitable candidate in order to further functionalizing for delivery of therapeutic ions and growth factors in bone tissue engineering.

Keywords: Antibacterial, bioactive glass, hydroxyapatite, proliferation, sol-gel processes.

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Authors: Dawid Stawski, Silviya Halacheva, Dorota Zielińska

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The surface properties of many materials can be readily and predictably modified by the controlled deposition of thin layers containing appropriate functional groups and this research area is now a subject of widespread interest. The layer-by-layer (lbl) method involves depositing oppositely charged layers of polyelectrolytes onto the substrate material which are stabilized due to strong electrostatic forces between adjacent layers. This type of modification affords products that combine the properties of the original material with the superficial parameters of the new external layers. Through an appropriate selection of the deposited layers, the surface properties can be precisely controlled and readily adjusted in order to meet the requirements of the intended application. In the presented paper a variety of anionic (poly(acrylic acid)) and cationic (linear poly(ethylene imine), polymers were successfully deposited onto the polypropylene nonwoven using the lbl technique. The chemical structure of the surface before and after modification was confirmed by reflectance FTIR spectroscopy, volumetric analysis and selective dyeing tests. As a direct result of this work, new materials with greatly improved properties have been produced. For example, following a modification process significant changes in the electrostatic activity of a range of novel nanocomposite materials were observed. The deposition of polyelectrolyte nanolayers was found to strongly accelerate the loss of electrostatically generated charges and to increase considerably the thermal resistance properties of the modified fabric (the difference in T50% is over 20oC). From our results, a clear relationship between the type of polyelectrolyte layer deposited onto the flat fabric surface and the properties of the modified fabric was identified.

Keywords: Layer-by-layer technique, polypropylene nonwoven, surface modification, surface properties.

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Authors: Yusuke Ayato, Takashi Itahashi, Akiko Takatsu, Kenji Kato, Naoki Matsuda

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In situ observation of absorption spectral change of heptil viologen cation radical (HV+.) was performed by slab optical waveguide (SOWG) spectroscopy utilizing indium-tin-oxide (ITO) electrodes. Synchronizing with electrochemical techniques, we observed the adsorption process of HV+.on the ITO electrode. In this study, we carried out the ITO-SOWG observations using KBr aqueous solution containing different concentration of HV to investigate the concentration dependent spectral change. A few specific absorption bands, which indicated HV+.existed as both monomer and dimer on ITO electrode surface with a monolayer or a few layers deposition, were observed in UV-visible region. The change in the peak position of the absorption spectra from adsorption species of HV+. were correlated with the concentration of HV as well as the electrode potential.

Keywords: absorption phenomena, heptil viologen, indium-tin-oxide (ITO) electrode, in situ, slab optical waveguide(SOWG) spectroscopy,

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Authors: Hisham M. Abourayana, Nuri A. Zreiba, Abdulkader M. Elamin

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Polymer-like organic thin films were deposited on both aluminum alloy type 6061 and glass substrates at room temperature by Plasma Enhanced Chemical Vapor Deposition (PECVD) methodusing benzene and hexamethyldisiloxane (HMDSO) as precursor materials. The surface and physical properties of plasma-polymerized organic thin films were investigated at different r.f. powers. The effects of benzene/argon ratio on the properties of plasma polymerized benzene films were also investigated. It is found that using benzene alone results in a non-coherent and non-adherent powdery deposited material. The chemical structure and surface properties of the asgrown plasma polymerized thin films were analyzed on glass substrates with FTIR and contact angle measurements. FTIR spectra of benzene deposited film indicated that the benzene rings are preserved when increasing benzene ratio and/or decreasing r.f. powers. FTIR spectra of HMDSO deposited films indicated an increase of the hydrogen concentration and a decrease of the oxygen concentration with the increase of r.f. power. The contact angle (θ) of the films prepared from benzene was found to increase by about 43% as benzene ratio increases from 10% to 20%. θ was then found to decrease to the original value (51°) when the benzene ratio increases to 100%. The contact angle, θ, for both benzene and HMDSO deposited films were found to increase with r.f. power. This signifies that the plasma polymerized organic films have substantially low surface energy as the r.f power increases. The corrosion resistance of aluminum alloy substrate both bare and covered with plasma polymerized thin films was carried out by potentiodynamic polarization measurements in standard 3.5 wt. % NaCl solution at room temperature. The results indicate that the benzene and HMDSO deposited films are suitable for protection of the aluminum substrate against corrosion. The changes in the processing parameters seem to have a strong influence on the film protective ability. Surface roughness of films deposited on aluminum alloy substrate was investigated using scanning electron microscopy (SEM). The SEM images indicate that the surface roughness of benzene deposited films increase with decreasing the benzene ratio. SEM images of benzene and HMDSO deposited films indicate that the surface roughness decreases with increasing r.f. power. Studying the above parameters indicate that the films produced are suitable for specific practical applications.

Keywords: Plasma polymerization, potentiodynamic test, Contact angle.

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Authors: O. I. H. Dimitry, N. A. Mansour, A. L. G. Saad

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Natural sodium montmorillonite (NaMMT), Cloisite Na⁺ and two organophilic montmorillonites (OMMTs), Cloisites 20A and 15A were used. Polycaprolactone (PCL)/MMT composites containing 1, 3, 5, and 10 wt% of Cloisite Na⁺ and PCL/OMMT nanocomposites containing 5 and 10 wt% of Cloisites 20A and 15A were prepared via solution intercalation technique to study the influence of organic modifier loading on particle dispersion of PCL/ NaMMT composites. Thermal stabilities of the obtained composites were characterized by thermal analysis using the thermogravimetric analyzer (TGA) which showed that in the presence of nitrogen flow the incorporation of 5 and 10 wt% of filler brings some decrease in PCL thermal stability in the sequence: Cloisite Na+>Cloisite 15A > Cloisite 20A, while in the presence of air flow these fillers scarcely influenced the thermoxidative stability of PCL by slightly accelerating the process. The interaction between PCL and silicate layers was studied by Fourier transform infrared (FTIR) spectroscopy which confirmed moderate interactions between nanometric silicate layers and PCL segments. The electrical conductivity (σ) which describes the ionic mobility of the systems was studied as a function of temperature and showed that σ of PCL was enhanced on increasing the modifier loading at filler content of 5 wt%, especially at higher temperatures in the sequence: Cloisite Na⁺<Cloisite 20A<Cloisite 15A, and was then decreased to some extent with a further increase to 10 wt%. The activation energy E_σ obtained from the dependency of σ on temperature using Arrhenius equation was found to be lowest for the nanocomposite containing 5 wt% of Cloisite 15A. The dispersed behavior of clay in PCL matrix was evaluated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses which revealed partial intercalated structures in PCL/NaMMT composites and semi-intercalated/semi-exfoliated structures in PCL/OMMT nanocomposites containing 5 wt% of Cloisite 20A or Cloisite 15A.

Keywords: Polycaprolactone, organoclay, nanocomposite, montmorillonite, electrical conductivity, activation energy, exfoliation, intercalation.

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

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

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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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Authors: Kamyar Shameli, Mansor Bin Ahmad, Wan Md Zin Wan Yunus, Nor Azowa Ibrahim, Maryam Jokar, Majid Darroudi

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Silver/polylactide nanocomposites (Ag/PLA-NCs) were synthesized via chemical reduction method in diphase solvent. Silver nitrate and sodium borohydride were used as a silver precursor and reducing agent in the polylactide (PLA). The properties of Ag/PLA-NCs were studied as a function of the weight percentages of silver nanoparticles (8, 16 and 32 wt% of Ag-NPs) relative to the weight of PLA. The Ag/PLA-NCs were characterized by Xray diffraction (XRD), transmission electron microscopy (TEM), electro-optical microscopy (EOM), UV-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FT-IR). XRD patterns confirmed that Ag-NPs crystallographic planes were face centered cubic (fcc) type. TEM images showed that mean diameters of Ag-NPs were 3.30, 3.80 and 4.80 nm. Electro-optical microscopy revealed excellent dispersion and interaction between Ag-NPs and PLA films. The generation of silver nanoparticles was confirmed from the UVvisible spectra. FT-IR spectra showed that there were no significant differences between PLA and Ag/PLA-NCs films. The synthesized Ag/PLA-NCs were stable in organic solution over a long period of time without sign of precipitation.

Keywords: Nanocomposites, Polylactide, Silver Nanoparticles, Sodium Borohydride, Transmission Electron Microscopy.

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Authors: Shajaratuldur Ismail, Nurlidia Mansor, Zakaria Man

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

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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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Authors: Ajay Kushwaha, Hemen Kalita, M. Aslam

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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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Authors: Supavej Maniyom, Gerard H. Markx

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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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Authors: Bireswar Paul, Amitava Datta

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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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Authors: Natarajan. E, Ganapathy Sundaram. E

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

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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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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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Authors: Mohammad Beyki, Justus Pawlak, Robert Patzke, Franz Renz

Abstract:

In the context of planetary exploration, the MIMOS II (miniaturized M¨ossbauer spectrometer) serves as a proven and reliable measuring instrument. The transmission behaviour of the electronics in the M¨ossbauer spectroscopy is further developed and optimized. For this purpose, the overall electronics is split into three parts. This elaboration deals exclusively with the first part of the signal chain for the evaluation of photons in experiments with gamma radiation. Parallel to the analysis of the electronics, an additional method for analysing the stability of linear and non-linear systems is presented: The extended method of Lyapunov’s stability criteria. The design helps to weigh advantages and disadvantages against other simulated circuits in order to optimize the MIMOS II for the terestric and extraterestric measurment. Finally, after stability analysis, the controller design according to Ackermann is performed, achieving the best possible optimization of the output variable through a skillful pole assignment.

Keywords: Controller design for MIMOS II, stability analysis, M¨ossbauer spectroscopy, electronic signal amplifier, light processing technology, photocurrent, transimpedance amplifier, extended Lyapunov method.

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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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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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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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Authors: A. Morelos-Gómez, S. M. Vega-Díaz, V. J. González, F. Tristán-López, R. Cruz-Silva , K. Fujisawa, H. Muramatsu , T. Hayashi , Xi Mi , Yunfeng Shi , H. Sakamoto , F. Khoerunnisa , K. Kaneko , B. G. Sumpter , Y.A. Kim , V. Meunier, M. Endo , E. Muñoz-Sandoval, M. Terrones

Abstract:

A novel physico-chemical route to produce few layer graphene nanoribbons with atomically smooth edges is reported, via acid treatment (H2SO4:HNO3) followed by characteristic thermal shock processes involving extremely cold substances. Samples were studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy. This method demonstrates the importance of having the nanotubes open ended for an efficient uniform unzipping along the nanotube axis. The average dimensions of these nanoribbons are approximately ca. 210 nm wide and consist of few layers, as observed by transmission electron microscopy. The produced nanoribbons exhibit different chiralities, as observed by high resolution transmission electron microscopy. This method is able to provide graphene nanoribbons with atomically smooth edges which could be used in various applications including sensors, gas adsorption materials, composite fillers, among others.

Keywords: Carbon nanoribbons, carbon nanotubes, unzipping.

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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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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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