Search results for: Fourier Transform Infra-Red spectroscopy

Authors: Gülşah Çelik Gül, Figen Kurtuluş

Abstract:

Magnesium containing boron compounds with hexagonal structure have been drawn much attention due to their superconductive nature. The main target of this work is new modified microwave oven by on our own has an ability about passing through a gas in the oven medium for attainment of oxygen-free compounds such as c-BN.  Mg containing boride was synthesized by modified-microwave method under nitrogen atmosphere using amorphous boron and magnesium source in appropriate molar ratio. Microwave oven with oxygen free environment has been modified to aimed to obtain magnesium boride without oxygen. Characterizations were done by powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Mg containing boride, generally named magnesium boride, with amorphous character without oxygen is obtained via designed microwave oven system.

Keywords: Magnesium containing boron compounds, modified microwave synthesis, powder X-ray diffraction, FTIR.

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Authors: E. Moroydor Derun, N. Tugrul, F. T. Senberber, A. S. Kipcak, S. Piskin

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In this research, copper borates are synthesized by the reaction of copper sulfate pentahydrate (CuSO4.5H2O) and tincalconite (Na2O4B7.10H2O). The experimental parameters are selected as 80oC reaction temperature and 60 of reaction time. The effect of mole ratio of CuSO4.5H2O to Na2O4B7.5H2O is studied. For the identification analyses X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques are used. At the end of the experiments, synthesized copper borate is matched with the powder diffraction file of “00-001-0472” [Cu(BO2)2] and characteristic vibrations between B and O atoms are seen. The proper crystals are obtained at the mole ratio of 3:1. This study showed that simplified synthesis process is suitable for the production of copper borate minerals.

Keywords: Hydrothermal synthesis, copper borates, copper sulfate, tincalconite.

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Authors: R. Ridzuan, M. D. H. Beg, M. Y. Rosli, M. H. Rohaya, A. A. Astimar S. Samahani, I. Zawawi

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Alkali treated oil palm empty fruit bunch (EFB) fibres (TEFBF) and untreated EFBF fibers (UEFBF) were incorporated in polypropylene (PP) with and without malic anhydride grafted PP (MAPP) and magnesium hydroxide as flame retardant (FR) to produce TEFBF-PP and UEFBF-PP composites by the melt casting method. The composites were characterized by mechanical and burning tests along with a scanning electron microscope and Fourier transform infrared spectroscopy. The significant improvement in flexural modulus (133%) and flame retardant property (60%) of TEFBF-PP composite with MAPP and FR is observed. The improved mechanical property is discussed by the development of encapsulated textures.

Keywords: Empty fruit bunch fibers, polypropylene, mechanical property, flame retardant.

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Authors: Nattha Kaewnopparat, Sanae Kaewnopparat, Amaravadee Jangwang, Daungkhae Maneenaun, Thitima Chuchome, Pharkphoom Panichayupakaranant

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Solid dispersions (SD) of curcuminpolyvinylpyrrolidone in the ratio of 1:2, 1:4, 1:5, 1:6, and 1:8 were prepared in an attempt to increase the solubility and dissolution. Solubility, dissolution, powder X-ray diffraction (XRD), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR) of solid dispersions, physical mixtures (PM) and curcumin were evaluated. Both solubility and dissolution of curcumin solid dispersions were significantly greater than those observed for physical mixtures and intact curcumin. The powder X-ray diffractograms indicated that the amorphous curcumin was obtained from all solid dispersions. It was found that the optimum weight ratio for curcumin:PVP K-30 is 1:6. The 1:6 solid dispersion still in the amorphous from after storage at ambient temperature for 2 years and the dissolution profile did not significantly different from freshly prepared.

Keywords: Curcumin, polyvinylpyrrolidone K-30, solid dispersion, dissolution, physicochemical.

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Authors: Jinghui Peng, Shanyu Tang, Jia Li

Abstract:

Steganalysis seeks to detect the presence of secret data embedded in cover objects, and there is an imminent demand to detect hidden messages in streaming media. This paper shows how a steganalysis algorithm based on Fast Fourier Transform (FFT) can be used to detect the existence of secret data embedded in streaming media. The proposed algorithm uses machine parameter characteristics and a network sniffer to determine whether the Internet traffic contains streaming channels. The detected streaming data is then transferred from the time domain to the frequency domain through FFT. The distributions of power spectra in the frequency domain between original VoIP streams and stego VoIP streams are compared in turn using t-test, achieving the p-value of 7.5686E-176 which is below the threshold. The results indicate that the proposed FFT-based steganalysis algorithm is effective in detecting the secret data embedded in VoIP streaming media.

Keywords: Steganalysis, security, fast Fourier transform, streaming media.

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Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA). 

Keywords: Colemanite, conventional synthesis, powder x-ray diffraction, borates.

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Authors: M. Z. Norashikin, M. Z. Ibrahim

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The use of plastic materials in agriculture causes serious hazards to the environment. The introduction of biodegradable materials, which can be disposed directly into the soil can be one possible solution to this problem. In the present research results of experimental tests carried out on biodegradable film fabricated from natural waste (corn husk) are presented. The film was characterized by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimeter (DSC), thermal gravimetric analysis (TGA) and atomic force microscope (AFM) observation. The film is shown to be readily degraded within 7-9 months under controlled soil conditions, indicating a high biodegradability rate. The film fabricated was use to produce biodegradable pot (BioPot) for seedlings plantation. The introduction and the expanding use of biodegradable materials represent a really promising alternative for enhancing sustainable and environmentally friendly agricultural activities.

Keywords: Environment, waste, plastic, biodegradable.

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Authors: A. S. Kipcak, N. Baran Acarali, E. Moroydor Derun, N. Tugrul, S. Piskin

Abstract:

Zinc borates can be used as multi-functional synergistic additives with flame retardant additives in polymers. Zinc borate is white, non-hygroscopic and powder type product. The most important properties are low solubility in water and high dehydration temperature. Zinc borates dehydrate above 290°C and anhydrous zinc borate has thermal resistance about 400°C. Zinc borates can be synthesized using several methods such as hydrothermal and solidstate processes. In this study, the solid-state method was applied at low temperatures of 600oC and 700oC using the starting materials of ZnO and H3BO3 with several mole ratios. The reaction time was determined as 4 hours after some preliminary experiments. After the synthesis, the crystal structure and the morphology of the products were examined by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). As a result the forms of ZnB4O7, Zn3(BO3)2, ZnB2O4 were synthesized and obtained along with the unreacted ZnO.

Keywords: FT-IR, solid-state method, zinc borate, XRD.

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Authors: Zharama M. Llarena

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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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Authors: Marzieh Moosavi-Nasab, Ali R. Yousefi

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Bacterial cellulose, a biopolysaccharide, is produced by the bacterium, Gluconacetobacter xylinus. Static batch fermentation for bacterial cellulose production was studied in sucrose and date syrup solutions (Bx. 10%) at 28 °C using G. xylinus (PTCC, 1734). Results showed that the maximum yields of bacterial cellulose (BC) were 4.35 and 1.69 g/l00 ml for date syrup and sucrose medium after 336 hours fermentation period, respectively. Comparison of FTIR spectrum of cellulose with BC indicated appropriate coincidence which proved that the component produced by G. xylinus was cellulose. Determination of the area under X-ray diffractometry patterns demonstrated that the crystallinity amount of cellulose (83.61%) was more than that for the BC (60.73%). The scanning electron microscopy imaging of BC and cellulose were carried out in two magnifications of 1 and 6K. Results showed that the diameter ratio of BC to cellulose was approximately 1/30 which indicated more delicacy of BC fibers relative to cellulose.

Keywords: Gluconacetobacter xylinus, Fourier Transform Infrared spectroscopy, Scanning Electron Microscopy, X-ray diffractometry

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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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Authors: E. Moroydor Derun, A. S. Kipcak, A. Kaplan, S. Piskin

Abstract:

Waste problem is becoming a future problem all over the world. Magnesium wastes which can be used in recycling processes are produced by many industrial activities. Magnesium borates which have useful properties such as; high heat resistance, corrosion resistance, supermechanical strength, superinsulation, light weight, high coefficient of elasticity and so on. Addition, magnesium borates have great potential in the development of ceramic and detergents industry, whisker-reinforced composites, antiwear, and reducing friction additives.

In this study, using the starting materials of waste magnesium and H₃BO₃ the hydrothermal method was applied at a moderate temperature of 70^oC with different reaction times. Several reaction times of waste magnesium to H₃BO₃ were selected as; 30, 60, 120, 240 minutes. After the synthesis, X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques were applied to products. As a result, the forms of Admontite [MgO(B₂O₃)₃.7(H₂O)] and Mcallisterite [Mg₂(B₆O₇(OH)₆)₂.9(H₂O)] were synthesized.

Keywords: Hydrothermal synthesis, magnesium borates, waste magnesium.

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Authors: A. Ersan, A. S. Kipcak, M. Yildirim, A. M. Erayvaz, E. M. Derun, N. Tugrul, S. Piskin

Abstract:

Zinc borates are used as a multi-functional flame retardant additive for its high dehydration temperature. In this study, the method of ultrasonic mixing was used in the synthesis of zinc borates. The reactants of zinc oxide (ZnO) and boric acid (H3BO3) were used at the constant reaction parameters of 90°C reaction temperature and 55 min of reaction time. Several molar ratios of ZnO:H3BO3 (1:1, 1:2, 1:3, 1:4 and 1:5) were conducted for the determination of the optimum reaction ratio. Prior to synthesis the characterization of the synthesized zinc borates were made by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). From the results Zinc Oxide Borate Hydrate [Zn3B6O12.3.5H2O], were synthesized optimum at the molar ratio of 1:3, with a reaction efficiency of 95.2%.

Keywords: Zinc borates, ultrasonic mixing, XRD, FT-IR, reaction efficiency.

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Authors: J. M. de Luis Ruiz, P. M. Sierra García, R. P. García, R. P. Álvarez, F. P. García, E. C. López

Abstract:

Given the evolution of viaducts, structural health monitoring requires more complex techniques to define their state. two alternatives can be distinguished: experimental and operational modal analysis. Although accelerometers or Global Positioning System (GPS) have been applied for the monitoring of structures under exploitation, the dynamic monitoring during the stage of construction is not common. This research analyzes whether GPS data can be applied to certain dynamic geometric controls of evolving structures. The fundamentals of this work were applied to the New Bridge of Cádiz (Spain), a worldwide milestone in bridge building. GPS data were recorded with an interval of 1 second during the erection of segments and turned to the frequency domain with Fourier transform. The vibration period and amplitude were contrasted with those provided by the finite element model, with differences of less than 10%, which is admissible. This process provides a vibration record of the structure with GPS, avoiding specific equipment.

Keywords: Fourier transform, global position system, operational modal analysis, structural health monitoring.

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Authors: N. Tugrul, A. S. Kipcak, N. Baran Acarali, E. Moroydor Derun, S. Piskin

Abstract:

Magnesium borate(MB) istechnical ceramic for high heat-resisting, corrosion-resisting, super mechanical strength, superinsulation, light weight, high strength, and high coefficient of elasticity. Zinc borate (ZB) can be used as multi-functional synergistic additives with flame retardant additives in polymers. The most important properties are low solubility in water and high dehydration temperature. ZB dehydrates above 290°C and anhydrous ZB has thermal resistance about 400°C. In this study, the raw materials of ZnO, MgO and H₃BO₃ were used with mole ratio of 1:1:9. With the starting materials hydrothermal method was applied at a temperature of 100^oC. The reaction time was determined as 30, 60, 90 and 120 minutes after some preliminary experiments. After the synthesis, the crystal structure and the morphology of the products were examined by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). As a result, the forms of Zinc Oxide Borate Hydrate [Zn₃B₆O₁₂.3.5H₂O], Admontite [MgO(B₂O₃)₃.7(H₂O)] and Mcallisterite [Mg₂(B₆O₇(OH)₆)₂.9(H₂O)] were synthesized.

Keywords: Magnesium borate, zinc borate, XRD, FT-IR.

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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, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (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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Authors: Tao Liu, Qingliang Yu, H. J. H. Brouwers

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Among the reaction products in the alkali activated ground granulated blast furnace slag (AAS), the layered double hydroxides (LDHs) have a remarkable capacity of chloride and heavy metal ions absorption. The promotion of LDH phases in the AAS matrix can increase chloride resistance. The objective of this study is that using the different dosages of sodium aluminate to activate slag, consequently, promoting the formation of in-situ LDH. The hydration kinetics of the sodium aluminate activated slag (SAAS) was tested by the isothermal calorimetry. Meanwhile, the reaction products were determined by X-ray diffraction (XRD), thermogravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FTIR). The sodium hydroxide activated slag is selected as the reference. The results of XRD, TGA, and FTIR showed that the formation of LDH in SAAS is governed by the aluminate dosages.

Keywords: ground granulated blast furnace slag, sodium aluminate activated slag, in-situ LDH formation, chloride absorption

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Authors: Anjan Sil, Rajni Sharma, Subrata Ray

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The effect of carbon nanofibers (CNFs) on the electrical properties of Poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP)) based gel polymer electrolytes has been investigated in the present work. The length and diameter ranges of CNFs used in the present work are 5-50 μm and 200-600 nm respectively. The nanocomposite gel polymer electrolytes have been synthesized by solution casting technique with varying CNFs content in terms of weight percentage. Electrochemical impedance analysis demonstrates that the reinforcement of carbon nanofibers significantly enhances the ionic conductivity of the polymer electrolyte. The decrease of crystallinity of P(VdF-HFP) due the addition of CNFs has been confirmed by X-ray diffraction (XRD). The interaction of CNFs with various constituents of nanocomposite gel polymer electrolytes has been assessed by Fourier Transform Infrared (FTIR) spectroscopy. Moreover CNFs added gel polymer electrolytes offer superior thermal stability as compared to that of CNFs free electrolytes as confirmed by Thermogravimetric analysis (TGA).

Keywords: Polymer electrolytes, CNFs, Ionic conductivity, TGA.

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Authors: K. Kuntanoo, S. Promkotra, P. Kaewkannetra

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According to synthetic plastics obtained from petroleum cause some environmental problems. Therefore, degradable plastics become widely used and studied for replacing the synthetic plastic waste. A biopolymer of poly hydroxybutyrate-co-hydroxyvalerate (PHBV) is subgroups of a main kind of polyhydroxyalkanoates (PHAs). Naturally, PHBV is hard, brittle and low flexible while natural rubber (NR) is high elastic latex. Then, they are blended and the biodegradation of the blended PHBV and NR films were examined in soil environment. The results showed that the degradation occurs predominantly in the bulk of the samples. The order of biodegradability was shown as follows: PHBV> PHBV/NR> NR. After biodegradation, the blended films were characterized by appearance analysis such as Scanning Electron Microscope (SEM), Fourier transform infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). It was found that the biodegradation mainly occurred at the polymer surface.

Keywords: Biodegradation, polyhydroxyalkanoates (PHAs), Polyhydroxybutyrate-co-hydroxyvalerate (PHBV), natural rubber (NR).

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Authors: A. S. Kipcak, P. Gurses, E. Moroydor Derun, S. Piskin

Abstract:

Borate minerals have attracted considerable attention in the past years due to their structural chemistry and mechanical properties in several industries. Recently, increasing attention has been paid to the use of; synthetically produced magnesium borates as catalysts reinforcing material for plastics, the conversion of hydrocarbons, electro-conductive treating agent, anti-wear and anti-corrosion materials. Magnesium borates can be synthesized by several methods such as; hydrothermal and solid-state (thermal) processes. In this study the hydrothermal production method was applied at the modest temperature of 80C along with convenient crystal growth. Using MgCl2.6H2O, H3BO3, and NaOH as starting materials, 30, 60, 120, 240 minutes of reaction times were studied. After all, the crystal structure and the morphology of the products were examined by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). As a result the forms of Admontite and Mcallisterite minerals were synthesized.

Keywords: FT-IR, hydrothermal method, magnesium borates, XRD.

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Authors: Moulay A. Akhloufi, Abdelhakim Bendada

Abstract:

In this work we present an efficient approach for face recognition in the infrared spectrum. In the proposed approach physiological features are extracted from thermal images in order to build a unique thermal faceprint. Then, a distance transform is used to get an invariant representation for face recognition. The obtained physiological features are related to the distribution of blood vessels under the face skin. This blood network is unique to each individual and can be used in infrared face recognition. The obtained results are promising and show the effectiveness of the proposed scheme.

Keywords: Face recognition, biometrics, infrared imaging.

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Authors: N. Tugrul, F. T. Senberber, A. S. Kipcak E. Moroydor Derun, S. Piskin

Abstract:

In this research, it is aimed not only microwave synthesis of magnesium borates but also evaluation of magnesium wastes. Synthesis process can be described with the reaction of Mg wastes and boric acid using microwave energy. X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) were applied to synthesized minerals. According to XRD results, magnesium borate hydrate mixtures were obtained as mcallisterite (pdf# = 01-070-1902, Mg₂(B₆O₇(OH)₆)₂.9(H₂O)) at higher crystallinity properties was achieved at the mole ratio raw material 1:1. Also, other kinds of magnesium borate hydrates were obtained at lower crystallinity such as admontite (pdf # = 01-076-0540, MgO(B₂O₃)₃.7(H₂O)), inderite (pdf # = 01-072-2308, 2MgO.3B₂O₃.15(H₂O)) and magnesium borate hydrates (pdf # = 01-076-0539, MgO(B₂O₃)₃.6(H₂O)). FT-IR spectrums indicated that minor changes were seen at the band values of characteristic stretching in each experiment. At the end of experiments it is seen that using microwave energy may contribute positive effects to design of synthesis process such as reducing reaction time and products at higher crystallinity.

Keywords: Magnesium wastes, boric acid, magnesium borate, microwave energy.

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

Abstract:

The toxicity of bare zinc oxide nanoparticles used as drug carriers may be the result of releasing zinc ions. Thus, zinc oxide nanoparticles modified with galactose were obtained. The process of their formation was conducted in the microwave field. The physicochemical properties of the obtained products were studied. The size and electrokinetic potential were defined by using dynamic light scattering technique. The crystalline properties were assessed by X-ray diffractometry. In order to confirm the formation of the desired products, Fourier-transform infrared spectroscopy was used. Releasing of zinc ions from the prepared products when comparing to the bare oxide was analyzed. It was found out that modification of zinc oxide nanoparticles with galactose limits the releasing of zinc ions which are responsible for the toxic effect of the whole carrier-drug conjugate.

Keywords: Nanomaterials, zinc oxide, drug delivery system, toxicity.

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Authors: N. Tugrul, N. Baran Acarali, A. S. Kipcak, E. Moroydor Derun, S. Piskin

Abstract:

Turkey has 72 % of total world boron reserves on the basis of B2O3.Borates that is a refined form of boron minerals have a wide range of applications. Zinc borates can be used as multifunctional synergistic additives. The most important properties are low solubility in water and high dehydration temperature. Zinc borates dehydrate above 290°C and anhydrous zinc borate has thermal resistance about 400°C. Zinc borates can be synthesized using several methods such as hydrothermal and solid-state processes. In this study, the solid-state method was applied between 500 and 800°C using the starting materials of ZnO and H3BO3 with 1:4 mole ratio. The reaction time was determined as 4 hours after some preliminary experiments. After the synthesis, the crystal structure and the morphology of the products were examined by XRay Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman Spectrometer. As a result the form of ZnB4O7 was synthesized with the highest crystal score at 800°C.

Keywords: Raman, solid-state method, zinc borate, XRD.

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Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd₂Zr₃(MoO₄)₉ which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd2Zr3(MoO4)9, solid state synthesis, powder x-ray diffraction, zirconium molybdates.

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Authors: A. S. Kipcak, P. Gurses, K. Kunt, E. Moroydor Derun, S. Piskin

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There are many kinds of metal borates found not only in nature but also synthesized in the laboratory such as magnesium borates. Due to its excellent properties, as remarkable ceramic materials, they have also application areas in anti-wear and friction reducing additives as well as electro-conductive treating agents. The synthesis of magnesium borate powders can be fulfilled simply with two different methods, hydrothermal and thermal synthesis. Microwave assisted method, also another way of producing magnesium borate, can be classified into thermal synthesis because of using the principles of solid state synthesis. It also contributes producing particles with small size and high purity in nano-size material synthesize. In this study the production of magnesium borates, are aimed using MgCl2.6H2O and H3BO3. The identification of both starting materials and products were made by the equipments of, X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). After several synthesis steps magnesium borates were synthesized and characterized by XRD and FT-IR, as well.

Keywords: FT-IR, magnesium borates, microwave method, XRD.

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Authors: Jiri Plocek, Petr Holec, Simona Kubickova, Barbara Pacakova, Irena Matulkova, Alice Mantlikova, Ivan Nemec, Daniel Niznansky, Jana Vejpravova

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This article presents summary on preparation and characterization of zinc, copper, cadmium and cobalt chromite nanocrystals, embedded in an amorphous silica matrix. The ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2 nanocomposites were prepared by a conventional sol-gel method under acid catalysis. Final heat treatment of the samples was carried out at temperatures in the range of 900−1200 ◦C to adjust the phase composition and the crystallite size, respectively. The resulting samples were characterized by Powder X-ray diffraction (PXRD), High Resolution Transmission Electron Microscopy (HRTEM), Raman/FTIR spectroscopy and magnetic measurements. Formation of the spinel phase was confirmed in all samples. The average size of the nanocrystals was determined from the PXRD data and by direct particle size observation on HRTEM; both results were correlated. The mean particle size (reviewed by HRTEM) was in the range from ∼4 to 46 nm. The results showed that the sol-gel method can be effectively used for preparation of the spinel chromite nanoparticles embedded in the silica matrix and the particle size is driven by the type of the cation A2+ in the spinel structure and the temperature of the final heat treatment. Magnetic properties of the nanocrystals were found to be just moderately modified in comparison to the bulk phases.

Keywords: Chromite, Fourier transform infrared spectroscopy, agnetic properties, nanocomposites, Raman spectroscopy, Rietveld refinement, sol-gel method, spinel.

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Authors: Jyotsna Singh, Parul Garg, Alok Nath De

Abstract:

In this paper, we present a non-blind technique of adding the watermark to the Fourier spectral components of audio signal in a way such that the modified amplitude does not exceed the maximum amplitude spread (MAS). This MAS is due to individual Discrete fourier transform (DFT) coefficients in that particular frame, which is derived from the Energy Spreading function given by Schroeder. Using this technique one can store double the information within a given frame length i.e. overriding the watermark on the host of equal length with least perceptual distortion. The watermark is uniformly floating on the DFT components of original signal. This helps in detecting any intentional manipulations done on the watermarked audio. Also, the scheme is found robust to various signal processing attacks like presence of multiple watermarks, Additive white gaussian noise (AWGN) and mp3 compression.

Keywords: Discrete Fourier Transform, Spreading Function, Watermark, Pseudo Noise Sequence, Spectral Masking Effect

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

Abstract:

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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Authors: H K Lakshminarayana, J S Bhat, H M Mahesh

Abstract:

A new estimator for evolutionary spectrum (ES) based on short time Fourier transform (STFT) and modified group delay function (MGDF) by signal decomposition (SD) is proposed. The STFT due to its built-in averaging, suppresses the cross terms and the MGDF preserves the frequency resolution of the rectangular window with the reduction in the Gibbs ripple. The present work overcomes the magnitude distortion observed in multi-component non-stationary signals with STFT and MGDF estimation of ES using SD. The SD is achieved either through discrete cosine transform based harmonic wavelet transform (DCTHWT) or perfect reconstruction filter banks (PRFB). The MGDF also improves the signal to noise ratio by removing associated noise. The performance of the present method is illustrated for cross chirp and frequency shift keying (FSK) signals, which indicates that its performance is better than STFT-MGDF (STFT-GD) alone. Further its noise immunity is better than STFT. The SD based methods, however cannot bring out the frequency transition path from band to band clearly, as there will be gap in the contour plot at the transition. The PRFB based STFT-SD shows good performance than DCTHWT decomposition method for STFT-GD.

Keywords: Evolutionary Spectrum, Modified Group Delay, Discrete Cosine Transform, Harmonic Wavelet Transform, Perfect Reconstruction Filter Banks, Short Time Fourier Transform.

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