Search results for: Dispersive liquid-liquid microextraction

Authors: Fariba Tadayon, Elmira Hassanlou, Hasan Bagheri, Mostafa Jafarian

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Heavy metals are released into water, plants, soil, and food by natural and human activities. Lead has toxic roles in the human body and may cause serious problems even in low concentrations, since it may have several adverse effects on human. Therefore, determination of lead in different samples is an important procedure in the studies of environmental pollution. In this work, an ultrasonic assisted-ionic liquid based-liquid-liquid microextraction (UA-IL-DLLME) procedure for the determination of lead in zucchini, pomegranate, and lettuce has been established and developed by using flame atomic absorption spectrometer (FAAS). For UA-IL-DLLME procedure, 10 mL of the sample solution containing Pb2+ was adjusted to pH=5 in a glass test tube with a conical bottom; then, 120 μL of 1-Hexyl-3-methylimidazolium hexafluoro phosphate (CMIM)(PF6) was rapidly injected into the sample solution with a microsyringe. After that, the resulting cloudy mixture was treated by ultrasonic for 5 min, then the separation of two phases was obtained by centrifugation for 5 min at 3000 rpm and IL-phase diluted with 1 cc ethanol, and the analytes were determined by FAAS. The effect of different experimental parameters in the extraction step including: ionic liquid volume, sonication time and pH was studied and optimized simultaneously by using Response Surface Methodology (RSM) employing a central composite design (CCD). The optimal conditions were determined to be an ionic liquid volume of 120 μL, sonication time of 5 min, and pH=5. The linear ranges of the calibration curve for the determination by FAAS of lead were 0.1-4 ppm with R2=0.992. Under optimized conditions, the limit of detection (LOD) for lead was 0.062 μg.mL-1, the enrichment factor (EF) was 93, and the relative standard deviation (RSD) for lead was calculated as 2.29%. The levels of lead for pomegranate, zucchini, and lettuce were calculated as 2.88 μg.g-1, 1.54 μg.g-1, 2.18 μg.g-1, respectively. Therefore, this method has been successfully applied for the analysis of the content of lead in different food samples by FAAS.

Keywords: Dispersive liquid-liquid microextraction, Central composite design, Food samples, Flame atomic absorption spectrometry.

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Authors: Najari Moghadam Sh., Qomi M., Raofie F., Khadiv J.

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In this study, a liquid phase microextraction by hollow fiber (HF-LPME) combined with high performance liquid chromatography-UV detector was applied to preconcentrate and determine trace levels of Cyproheptadine in human urine and plasma samples. Cyproheptadine was extracted from 10 mL alkaline aqueous solution (pH: 9.81) into an organic solvent (n-octnol) which was immobilized in the wall pores of a hollow fiber. Then was back-extracted into an acidified aqueous solution (pH: 2.59) located inside the lumen of the hollow fiber. This method is simple, efficient and cost-effective. It is based on pH gradient and differences between two aqueous phases. In order to optimize the HF-LPME some affecting parameters including the pH of donor and acceptor phases, the type of organic solvent, ionic strength, stirring rate, extraction time and temperature were studied and optimized. Under optimal conditions enrichment factor, limit of detection (LOD) and relative standard deviation (RSD(%), n=3) were up to 112, 15 μg.L⁻¹ and 2.7, respectively.

Keywords: Biological samples, Cyproheptadine, hollow fiber, liquid phase microextraction.

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Authors: Rui Qiu, Giles Hardy, Dong Qu, Robert Trengove, Manjree Agarwal, YongLin Ren

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Phytophthora cinnamomi (P. c) is a plant pathogenic oomycete that is capable of damaging plants in commercial production systems and natural ecosystems worldwide. The most common methods for the detection and diagnosis of P. c infection are expensive, elaborate and time consuming. This study was carried out to examine whether species specific and life cycle specific volatile organic compounds (VOCs) can be absorbed by solid-phase microextraction fibers and detected by gas chromatography that are produced by P. c and another oomycete Pythium dissotocum. A headspace solid-phase microextraction (HS-SPME) together with gas chromatography (GC) method was developed and optimized for the identification of the VOCs released by P. c. The optimized parameters included type of fiber, exposure time, desorption temperature and desorption time. Optimization was achieved with the analytes of P. c+V8A and V8A alone. To perform the HS-SPME, six types of fiber were assayed and compared: 7μm Polydimethylsiloxane (PDMS), 100μm Polydimethylsiloxane (PDMS), 50/30μm Divinylbenzene/CarboxenTM/Polydimethylsiloxane DVB/CAR/PDMS), 65μm Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), 85μm Polyacrylate (PA) fibre and 85μm CarboxenTM/ Polydimethylsiloxane (Carboxen™/PDMS). In a comparison of the efficacy of the fibers, the bipolar fiber DVB/CAR/PDMS had a higher extraction efficiency than the other fibers. An exposure time of 16h with DVB/CAR/PDMS fiber in the sample headspace was enough to reach the maximum extraction efficiency. A desorption time of 3min in the GC injector with the desorption temperature of 250°C was enough for the fiber to desorb the compounds of interest. The chromatograms and morphology study confirmed that the VOCs from P. c+V8A had distinct differences from V8A alone, as did different life cycle stages of P. c and different taxa such as Pythium dissotocum. The study proved that P. c has species and life cycle specific VOCs, which in turn demonstrated the feasibility of this method as means of

Keywords: Gas chromatography, headspace solid-phase microextraction, optimization, volatile compounds.

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Authors: K. Benhabib, X. Pierens, V-D Nguyen, G. Mimanne

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The main hypothesis of the dynamics of solid phase microextraction (SPME) is that steady-state mass transfer is respected throughout the SPME extraction process. It considers steady-state diffusion is established in the two phases and fast exchange of the analyte at the solid phase film/water interface. An improved model is proposed in this paper to handle with the situation when the analyte (atrazine) is in contact with colloid suspensions (carboxylate latex in aqueous solution). A mathematical solution is obtained by substituting the diffusion coefficient by the mean of diffusion coefficient between analyte and carboxylate latex, and also thickness layer by the mean thickness in aqueous solution. This solution provides an equation relating the extracted amount of the analyte to the extraction a little more complicated than previous models. It also gives a better description of experimental observations. Moreover, the rate constant of analyte obtained is in satisfactory agreement with that obtained from the initial curve fitting.

Keywords: Pesticide, SPME methods, polyacrylate, steady state.

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Authors: M. Trinidad Pérez-Palacios, Catarina Petisca, Olívia Pinho, Isabel M.P.L.V.O. Ferreira

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This work evaluated the effect of temperature on headspace solid-phase microextraction of volatile and furanic compounds in coated fish sticks. The major goal was the analysis of the samples as consumed, to reproduce volatile compounds people feel when consuming those products. Extraction at 37 ºC (the human body temperature) throughout the HS-SPME analysis of volatile and furanic compounds in coated fish was compared with higher extraction temperatures, which are frequently used for this kind of determinations. The profile of volatile compounds found in deepfried (F) and non-fried (NF) coated fish at 37 and 50 ºC was different from that obtained at 80 ºC. Concerning furan and its derivatives, an extra formation of these compounds was observed at higher extraction temperatures. The analysis of volatile and furanic compounds in fish coated sticks simulating the cooking and eating conditions can be reliably carried out setting the headspace absorption temperature at 37 ºC.

Keywords: Analysis of samples as consumed, fish coated sticks, furans, headspace extraction temperature, volatiles.

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Authors: Hanan Alenezi

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Membrane performance depends on the kind of solvent used in preparation. A membrane made by Polyetherimide (PEI) was evaluated for gas separation using X-Ray Diffraction (XRD), Scanning electron microscope (SEM), and Energy Dispersive X-Ray Spectroscopy (EDS). The purity and the thickness are detected to evaluate the membrane in order to optimize PEI membrane preparation.

Keywords: Energy Dispersive X-Ray Spectroscopy, EDS, membrane, Polyetherimide, PEI, Scanning electron microscope, SEM, Solvent, X-Ray Diffraction, XRD.

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Authors: Hamed Sadeghi, Pouya A. Panahi, Hamed Nasiri, Mohammad Sadeghi

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Collapsible soils like loess comprise an important category of problematic soils for construction purposes and sustainable development. As a result, research on both geological and geotechnical aspects of this type of soil have been in progress for decades. However, considerable natural variability in physical properties of in-situ loess strata even in a single block sample challenges the fundamental laboratory investigations. The reason behind this is that it is somehow impossible to remove the effect of a specific factor like void ratio from fair comparisons to come with a reliable conclusion. In order to cope with this limitation, two types of artificially made dispersive and calcareous loess are introduced which can be easily reproduced in any soil mechanics laboratory provided that all its compositions are known and controlled. The collapse potential is explored for a variety of soil water salinity and lime content and comparisons are made against the natural soil behavior. Trends are reported for the influence of pore water salinity on collapse potential under different osmotic flow conditions. The most important advantage of artificial loess is the ease of controlling cementing agent content like calcite or dispersive potential for studying their influence on mechanical soil behavior.

Keywords: Artificial loess, unsaturated soils, collapse potential, dispersive clays, laboratory tests.

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Authors: N. Outili, A-H. Meniai

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Modeling transfer phenomena in several chemical engineering operations leads to the resolution of partial differential equations systems. According to the complexity of the operations mechanisms, the equations present a nonlinear form and analytical solution became difficult, we have then to use numerical methods which are based on approximations in order to transform a differential system to an algebraic one.Finite element method is one of numerical methods which can be used to obtain an accurate solution in many complex cases of chemical engineering.The packed columns find a large application like contactor for liquid-liquid systems such solvent extraction. In the literature, the modeling of this type of equipment received less attention in comparison with the plate columns.A mathematical bidimensionnal model with radial and axial dispersion, simulating packed tower extraction behavior was developed and a partial differential equation was solved using the finite element method by adopting the Galerkine model. We developed a Mathcad program, which can be used for a similar equations and concentration profiles are obtained along the column. The influence of radial dispersion was prooved and it can-t be neglected, the results were compared with experimental concentration at the top of the column in the extraction system: acetone/toluene/water.

Keywords: finite element method, Galerkine method, liquidliquid extraction modelling, packed column simulation, two dimensional model

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Authors: Walid M. Saad

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techniques are examined to overcome the performance degradation caused by the channel dispersion using slow frequency hopping (SFH) with dynamic frequency hopping (DFH) pattern adaptation. In DFH systems, the frequency slots are selected by continuous quality monitoring of all frequencies available in a system and modification of hopping patterns for each individual link based on replacing slots which its signal to interference ratio (SIR) measurement is below a required threshold. Simulation results will show the improvements in BER obtained by DFH in comparison with matched frequency hopping (MFH), random frequency hopping (RFH) and multi-carrier code division multiple access (MC-CDMA) in multipath slowly fading dispersive channels using a generalized bandpass two-path transfer function model, and will show the improvement obtained according to the threshold selection.

Keywords: code division multiple access (CDMA), dynamic channel allocation (DCA), dynamic channel assignment, frequency hopping, matched frequency hopping (MFH).

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Authors: Faten. A. Khorshid, Gehan. A. Raouf, Salem. M. El-Hamidy, Gehan. S. Al-amri, Nourah. A. Alotaibi, Taha A. Kumosani

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Cancer becomes one of the leading cause of death in many countries over the world. Fourier-transform infrared (FTIR) spectra of human lung cancer cells (A549) treated with PMF (natural product extracted from PM 701) for different time intervals were examined. Second derivative and difference method were taken in comparison studies. Cesium (Cs) and Rubidium (Rb) nanoparticles in PMF were detected by Energy Dispersive X-ray attached to Scanning Electron Microscope SEM-EDX. Characteristic changes in protein secondary structure, lipid profile and changes in the intensities of DNA bands were identified in treated A549 cells spectra. A characteristic internucleosomal ladder of DNA fragmentation was also observed after 30 min of treatment. Moreover, the pH values were significantly increases upon treatment due to the presence of Cs and Rb nanoparticles in the PMF fraction. These results support the previous findings that PMF is selective anticancer agent and can produce apoptosis to A549 cells.

Keywords: Apoptosis, FTIR spectroscopy, pH therapy, Scanning Electron Microscope- Energy Dispersive X-ray (SEMEDX).

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Authors: Rita Riekstina-Dolge, Zanda Kruma, Daina Karklina

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Aroma forming volatiles are important components of fermented beverages. The aim of current research is to evaluate the volatile compounds and phenolic compounds of commercial ciders. Volatile aroma compounds and TPC of seven commercial ciders were determined. Extraction of aroma compounds was performed using solid phase microextraction (DVB/Car/PDMS fibre). Analysis of volatile aroma compounds was made using a Perkin Elmer Clarus 500 GC/MS. Total phenol content (TPC) was determined according to the Folin-Ciocalteu spectrophotometric method and results were expressed as gallic acid equivalents. The highest volatile compounds were in apple ciders with pear flavor. The highest TPC and lower content of volatile compounds were detected in French ciders.

Keywords: cider, TPC, volatile compounds

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Authors: Suttipong Phosuksirikul, Rawichar Chaipojjana, Arunsri Leejeerajumnean

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The aim of research was to define the relations between volatile compounds, some parameters (pH, titratable acidity (TA), total soluble solid (TSS), lactic acid bacteria count) and consumer preference of commercial fermented milks. These relations tend to be used for controlling and developing new fermented milk product. Three leading commercial brands of fermented milks in Thailand were evaluated by consumers (n=71) using hedonic scale for four attributes (sweetness, sourness, flavour, and overall liking), volatile compounds using headspace-solid phase microextraction (HS-SPME) GC-MS, pH, TA, TSS and LAB count. Then the relations were analyzed by principal component analysis (PCA). The PCA data showed that all of four attributes liking scores were related to each other. They were also related to TA, TSS and volatile compounds. The related volatile compounds were mainly on fermented produced compounds including acetic acid, furanmethanol, furfural, octanoic acid and the volatiles known as artificial fruit flavour (beta pinene, limonene, vanillin, and ethyl vanillin). These compounds were provided the information about flavour addition in commercial fermented milk in Thailand.

Keywords: Fermented milk, volatile compounds, preference, PCA.

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Authors: Y. Li, K. Buddharaju, X. P. Wang

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The mechanism of nickel (Ni) metallization in silicon-germanium (Si_0.5Ge_0.5) alloy nanowire (NW) was studied. Transmission electron microscope imaging with in-situ annealing was conducted at temperatures of 200^oC to 600°C. During rapid formation of Ni germanosilicide, loss of material from from the SiGe NW occurred which led to the formation of a thin Ni germanosilicide filament and eventual void. Energy dispersive X-ray spectroscopy analysis along the SiGe NW before and after annealing determined that Ge atoms tend to out-diffuse from the Ni germanosilicide towards the Ni source in the course of annealing. A model for the Ni germanosilicide formation in SiGe NW is proposed to explain this observation.

Keywords: SiGe, nanowires, germanosilicide.

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Authors: Maribel G. Guzmán, Jean Dille, Stephan Godet

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Silver nanoparticles were prepared by chemical reduction method. Silver nitrate was taken as the metal precursor and hydrazine hydrate as a reducing agent. The formation of the silver nanoparticles was monitored using UV-Vis absorption spectroscopy. The UV-Vis spectroscopy revealed the formation of silver nanopart├¡cles by exhibing the typical surface plasmon absorption maxima at 418-420 nm from the UV–Vis spectrum. Comparison of theoretical (Mie light scattering theory) and experimental results showed that diameter of silver nanoparticles in colloidal solution is about 60 nm. We have used energy-dispersive spectroscopy (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and, UV–Vis spectroscopy to characterize the nanoparticles obtained. The energy-dispersive spectroscopy (EDX) of the nanoparticles dispersion confirmed the presence of elemental silver signal no peaks of other impurity were detected. The average size and morphology of silver nanoparticles were determined by transmission electron microscopy (TEM). TEM photographs indicate that the nanopowders consist of well dispersed agglomerates of grains with a narrow size distribution (40 and 60 nm), whereas the radius of the individual particles are between 10 and 20 nm. The synthesized nanoparticles have been structurally characterized by X-ray diffraction and transmission high-energy electron diffraction (HEED). The peaks in the XRD pattern are in good agreement with the standard values of the face-centered-cubic form of metallic silver (ICCD-JCPDS card no. 4-0787) and no peaks of other impurity crystalline phases were detected. Additionally, the antibacterial activity of the nanopart├¡culas dispersion was measured by Kirby-Bauer method. The nanoparticles of silver showed high antimicrobial and bactericidal activity against gram positive bacteria such as Escherichia Coli, Pseudimonas aureginosa and staphylococcus aureus which is a highly methicillin resistant strain.

Keywords: Silver nanoparticles, surface plasmon, UV-Vis absorption spectrum, chemicals reduction.

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: Energy dispersive X-ray spectroscopy, high strength concrete, interfacial transition zone, mixing procedure, normal strength concrete, scanning electron microscopy.

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Authors: F. Kurtuluş, G. Çelik Gül

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Cesium molybdates with general formula CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich polymorphism, and crystallize in a layered structure. These properties cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differantial thermal analysis (TG/DTA).

Keywords: Cesium bismuth dimolybdate, microwave synthesis, powder x-ray diffraction, rare earth dimolybdates.

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Authors: Joon Ho Kim, Duck Su Kim, Tae Kwon Ha

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Aluminum/Copper clad sheet has been fabricated using asymmetric extrusion method, which caused severe shear deformation between Al and Cu plate to easily bond to each other. Interfacial microstructure and mechanical properties of Al/Cu clad were studied by scanning electron microscope equipped with energy dispersive X-ray detector, micro-hardness, and tension tests. The asymmetric extrusion bonding was very effective to provide a good interface for atoms diffusion during subsequent annealing. The strength of bonding was higher with the increasing extrusion ratio.

Keywords: Aluminum/Copper clad sheet, Asymmetric extrusion, Interfacial microstructure, Annealing, Tensile test.

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Authors: N. Bahiyah Baba, W. Waugh, A.M. Davidson

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The paper discusses optimising work on a method of processing ceramic / metal composite coatings for various applications and is based on preliminary work on processing anodes for solid oxide fuel cells (SOFCs). The composite coating is manufactured by the electroless co-deposition of nickel and yttria stabilised zirconia (YSZ) simultaneously on to a ceramic substrate. The effect on coating characteristics of substrate surface treatments and electroless nickel bath parameters such as pH and agitation methods are also investigated. Characterisation of the resulting deposit by scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDXA) is also discussed.

Keywords: Electroless deposition, nickel, YSZ, composite

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Authors: Kavita Burse, R.N. Yadav, S.C. Shrivastava, Vishnu Pratap Singh Kirar

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During signal transmission, the combined effect of the transmitter filter, the transmission medium, and additive white Gaussian noise (AWGN) are included in the channel which distort and add noise to the signal. This causes the well defined signal constellation to spread causing errors in bit detection. A compact pi neural network with minimum number of nodes is proposed. The replacement of summation at each node by multiplication results in more powerful mapping. The resultant pi network is tested on six different channels.

Keywords: Additive white Gaussian noise, digitalcommunication system, multiplicative neuron, Pi neural network.

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Authors: M. Sumida

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The flow of suspensions of wood pulp fibers in circular pipes has been investigated experimentally. The flow characteristics of pulp suspensions are discussed with regard to five flow regimes designated by the author. In particular, the effects of the shear stress at the pipe wall on the disruption and dispersion of networks of pulp fibers are examined. The values of the disruptive and dispersive shear stresses are formulated as simple expressions depending on only the fiber concentration. Furthermore, the flow properties of the suspensions are described using the yield shear stress.

Keywords: Fiber Concentration, Flow Properties, Pulp Suspension, Yield Shear Stress.

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Authors: G. Çelik Gül, F. Kurtuluş

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The first laboratory synthesis of hard materials such as diamond proceeded to attack of developing materials with high hardness to compete diamond. Boron rich solids are good candidates owing to their short interatomic bond lengths and strong covalent character. Boron containing hard material was synthesized by modifiedmicrowave method under nitrogen atmosphere by using a fuel (glycine or urea), amorphous boron and/or boric acid in appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differential thermal analysis (TG/DTA).

Keywords: Boron containing materials, hard materials, microwave synthesis, powder X-ray diffraction.

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Authors: B. Ghasemi, A. A. Najafzadeh Khoee

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In this study, the effect of mechanical activation on the synthesis of Fe3Al/Al2O3 nanocomposite has been investigated by using mechanochemical method. For this purpose, Aluminum powder and hematite as precursors, with stoichiometric ratio, have been utilized and other effective parameters in milling process were kept constant. Phase formation analysis, crystallite size measurement and lattice strain were studied by X-ray diffraction (XRD) by using Williamson-Hall method as well as microstructure and morphology were explored by Scanning electron microscopy (SEM). Also, Energy-dispersive X-ray spectroscopy (EDX) analysis was used in order to probe the particle distribution. The results showed that after 30-hour milling, the reaction was started, combustibly done and completed.

Keywords: hematite, mechanochemical, milling, nanocomposite

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Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: Lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS.

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Authors: K. B. Dermenci, B. Ebin, S.Gürmen

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Noble metal participation in nanostructured semiconductor catalysts has drawn much interest because of their improved properties. Recently, it has been discussed by many researchers that Ag participation in TiO2, CuO, ZnO semiconductors showed improved photocatalytic and optical properties. In this research, Ag/ZnO nanocomposite particles were prepared by Ultrasonic Spray Pyrolysis(USP) Method. 0.1M silver and zinc nitrate aqueous solutions were used as precursor solutions. The Ag:Zn atomic ratio of the solution was selected 1:1. Experiments were taken place under constant air flow of 400 mL/min at 800°C furnace temperature. Particles were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM) and Energy Dispersive Spectroscopy (EDS). The crystallite sizes of Ag and ZnO in composite particles are 24.6 nm, 19.7 nm respectively. Although, spherical nanocomposite particles are in a range of 300- 800 nm, these particles are formed by the aggregation of primary particles which are in a range of 20-60 nm.

Keywords: Ag/ZnO nanocatalysts, Nanotechnology, USP

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Authors: A. Karsenty, A. Chelly

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Ultrathin (UTD) and Nanoscale (NSD) SOI-MOSFET devices, sharing a similar W/L but with a channel thickness of 46nm and 1.6nm respectively, were fabricated using a selective “gate recessed” process on the same silicon wafer. The electrical transport characterization at room temperature has shown a large difference between the two kinds of devices and has been interpreted in terms of a huge unexpected series resistance. Electrical characteristics of the Nanoscale device, taken in the linear region, can be analytically derived from the ultrathin device ones. A comparison of the structure and composition of the layers, using advanced techniques such as Focused Ion Beam (FIB) and High Resolution TEM (HRTEM) coupled with Energy Dispersive X-ray Spectroscopy (EDS), contributes an explanation as to the difference of transport between the devices.

Keywords: Nanoscale Devices, SOI MOSFET, Analytical Model, Electron Transport.

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Authors: Rana Th. A. Al-Rubaye

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A novel chromium-free protective coating films based on a zeolite coating was growing onto a FeCrAlloy metal using in – situ hydrothermal method. The zeolite film was obtained using in-situ crystallization process that is capable of coating large surfaces with complex shape and in confined spaces has been developed. The zeolite coating offers an advantage of a high mechanical stability and thermal stability. The physicochemical properties were investigated using X-ray diffraction (XRD), Electron Microscopy (SEM), Energy Dispersive X–ray Analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550oC).

Keywords: FeCrAlloy, Zeolite ZSM-5. Zeolite coating.

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Authors: Merve Küçük, M. Lütfi Öveçoğlu

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Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.

Keywords: Dip coating, polyester fabrics, sol-gel, zinc oxide.

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Authors: Branko Skoric, Aleksandar Miletic, Pal Terek, Lazar Kovacevic, Milan Kukuruzovic

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In this paper, we present the results of a study of TiN thin films which are deposited by a Physical Vapour Deposition (PVD) and Ion Beam Assisted Deposition (IBAD). In the present investigation the subsequent ion implantation was provided with N⁵⁺ ions. The ion implantation was applied to enhance the mechanical properties of surface. The thin film deposition process exerts a number of effects such as crystallographic orientation, morphology, topography, densification of the films. A variety of analytic techniques were used for characterization, such as scratch test, calo test, Scanning electron microscopy (SEM), Atomic Force Microscope (AFM), X-ray diffraction (XRD) and Energy Dispersive X-ray analysis (EDAX).

Keywords: Steel, coating, super hard, ion implantation, nanohardness.

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Authors: Krasimir I. Ivanov, Penka S. Zapryanova, Stefan V. Krustev, Violina R. Angelova

Abstract:

Three commonly used digestion methods (dry ashing, acid digestion, and microwave digestion) in different variants were compared for digestion of tobacco leaves. Three main macroelements (K, Ca and Mg) were analysed using AAS Spectrometer Spectra АА 220, Varian, Australia. The accuracy and precision of the measurements were evaluated by using Polish reference material CTR-VTL-2 (Virginia tobacco leaves). To elucidate the problems with elemental recovery X-Ray and SEM–EDS analysis of all residues after digestion were performed. The X-ray investigation showed a formation of KClO₄ when HClO4 was used as a part of the acids mixture. The use of HF at Ca and Mg determination led to the formation of CaF₂ and MgF₂. The results were confirmed by energy dispersive X-ray microanalysis. SPSS program for Windows was used for statistical data processing.

Keywords: Digestion methods, determination of macroelements, plant tissue.

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Authors: Richard E. Miller

Abstract:

12.7-mm thick plates of 6061-T6511 aluminum alloy and high hardness steel (528 HV) were successfully joined by a friction stir bonding process using a tungsten-rhenium stir tool. Process parameter variation experiments, which included tool design geometry, plunge and traverse rates, tool offset, spindle tilt, and rotation speed, were conducted to develop a parameter set which yielded a defect free joint. Laboratory tensile tests exhibited yield stresses which exceed the strengths of comparable AA6061-to-AA6061 fusion and friction stir weld joints. Scanning electron microscopy and energy dispersive X-ray spectroscopy analysis also show atomic diffusion at the material interface region.

Keywords: Dissimilar materials, friction stir, welding.

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