Search results for: FTIR and chemometrics.

Authors: Raza Hussain, Claire Gaiani, Joël Scher

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Dispersions of casein micelles (CM) were studied at a constant protein concentration of 5 wt % in high NaCl environment ranging from 0% to 12% by Dynamic light scattering (DLS) and Fourier Transform Infrared (FTIR). The rehydration profiles obtained were interpreted in term of wetting, swelling and dispersion stages by using a turbidity method. Two behaviours were observed depending on the salt concentration. The first behaviour (low salt concentration) presents a typical rehydration profile with a significant change between 3 and 6% NaCl indicating quick wetting, swelling and long dispersion stage. On the opposite, the dispersion stage of the second behaviour (high salt concentration) was significantly shortened indicating a strong modification of the protein backbone. A salt increase result to a destabilization of the micelle and the formation of mini-micelles more or less aggregated indicating an average micelles size ranging from 100 to 200 nm. For the first time, the estimations of secondary structural elements (irregular, ß-sheet, α-helix and turn) by the Amide III assignments were correlated with results from Amide I.

Keywords: Casein, DLS, FTIR, Ionic environment.

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Authors: Gopalu Karunakaran, Matheswaran Jagathambal, Nguyen Van Minh, Evgeny Kolesnikov, Denis Kuznetsov

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This work investigated the use of Beijerinckia indica extracellular extract for the synthesis of silver nanoparticles using AgNO₃. The formation of nanoparticles was confirmed by different methods, such as UV-Vis absorption spectroscopy, XRD, FTIR, EDX, and TEM analysis. The formation of silver nanoparticles (AgNPs) was confirmed by the change in color from light yellow to dark brown. The absorbance peak obtained at 430 nm confirmed the presence of silver nanoparticles. The XRD analysis showed the cubic crystalline phase of the synthesized nanoparticles. FTIR revealed the presence of groups that acts as stabilizing and reducing agents for silver nanoparticles formation. The synthesized silver nanoparticles were generally found to be spherical in shape with size ranging from 5 to 20 nm, as evident by TEM analysis. These nanoparticles were found to inhibit pathogenic bacterial strains. This work proved that the bacterial extract is a potential eco-friendly candidate for the synthesis of silver nanoparticles with promising antibacterial and antioxidant properties. 

Keywords: Antioxidant activity, antimicrobial activity, Beijerinckia indica, characterisation, extracellular extracts, silver nanoparticles.

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Authors: N. P. Dhull, K. Gupta, R. Soni, D. K. Rahi, S. K. Soni

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The aim of the present work was to statistically design an autotrophic medium for maximum biomass production by Chlorella pyrenoidosa using response surface methodology. After evaluating one factor at a time approach, K2HPO4, KNO3, MgSO4.7H2O and NaHCO3 were preferred over the other components of the fog’s medium as most critical autotrophic medium components. The study showed that the maximum biomass yield was achieved while the concentrations of MgSO4.7H2O, K2HPO4, KNO3 and NaHCO3 were 0.409 g/L, 0.24 g/L, 1.033 g/L, and 3.265 g/L, respectively. The study reported that the biomass productivity of C. pyrenoidosa improved from 0.14 g/L in defined fog’s medium to 1.40 g/L in modified fog’s medium resulting 10 fold increase. The biochemical composition biosynthesis of C. pyrenoidosa was altered using nitrogen limiting stress bringing about 5.23 fold increase in lipid content than control (cell without stress), as analyzed by FTIR integration method.

Keywords: Autotrophic condition, Chlorella pyrenoidosa, FTIR, Response Surface Methodology, Optimization.

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Authors: Sucharat Limsitthichaikoon, Kedsarin Saodaeng, Aroonsri Priprem, Teerasak Damrongrungruang

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Complexation of anthocyanins to mimic natural copigmentation process was investigated. Cyanidin-rich extracts from Zea mays L. ceritina Kulesh. and delphinidin-rich extracts from Clitoria ternatea L. were used to form 4 anthocyanin complexes, AC1, AC2, AC3 and AC4, in the presence of several polyphenols and a trace metal. Characterizations of the ACs were conducted by UV, FTIR, DSC/TGA and morphological observations. Bathochromic shifts of the UV spectra of 4 formulas of ACs were observed at peak wavelengths of about 510-620 nm by 10 nm suggesting complex formation. FTIR spectra of the ACs indicate shifts of peaks from 1,733 cm-1 to 1,696 cm-1 indicating interactions and a decrease in the peak areas within the wavenumber of 3,400-3,500 cm-1 indicating changes in hydrogen bonding. Thermal analysis of all of the ACs suggests increases in melting temperature after complexation. AC with the highest melting temperature was morphologically observed by SEM and TEM to be crystal-like particles within a range of 50 to 200 nm. Particle size analysis of the AC by laser diffraction gave a range of 50-600 nm, indicating aggregation. This AC was shown to have no cytotoxic effect on cultured HGEPp0.5 and HGF (all p> 0.05) by MTT. Therefore, complexation of anthocyanins was simple and self-assembly process, potentially resulting in nanosized particles of anthocyanin complex.

Keywords: Anthocyanins, complexation, purple corn cops, butterfly pea, physicochemical characteristics, cytotoxicity.

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Authors: Seyed Mohammad Hosseini, Amirhossein Moghanian

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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: Christine O. Wangia, Jennifer A. Orwa, Francis W. Muregi, Patrick G. Kareru, Kipyegon Cheruiyot, Eric Guantai

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Ruellia (syn. Dipteracanthus) species are wild perennial creepers belonging to the Acanthaceae family. These species are reported to possess anti-inflammatory, analgesic, antioxidant, gastroprotective, anticancer, and immuno-stimulant properties. Phytochemical screening of both aqueous and methanolic extracts of Ruellia species revealed the presence of saponins. Saponins have been reported to possess anti-inflammatory, antioxidant, immuno-stimulant, antihepatotoxic, antibacterial, anticarcinogenic, and antiulcerogenic activities. The objective of this study was to quantify and analyze the Fourier transform infrared (FTIR) spectra of saponins in crude extracts of three Kenyan Ruellia species namely Ruellia prostrata (RPM), Ruellia lineari-bracteolata (RLB) and Ruellia bignoniiflora (RBK). Sequential organic extraction of the ground whole plant material was done using petroleum ether (PE), chloroform, ethyl acetate (EtOAc), and absolute methanol by cold maceration, while aqueous extraction was by hot maceration. The plant powders and extracts were mixed with spectroscopic grade KBr and compressed into a pellet. The infrared spectra were recorded using a Shimadzu FTIR spectrophotometer of 8000 series in the range of 3500 cm^-1 - 500 cm^-1. Quantitative determination of the saponins was done using standard procedures. Quantitative analysis of saponins showed that RPM had the highest quantity of crude saponins (2.05% ± 0.03), followed by RLB (1.4% ± 0.15) and RBK (1.25% ± 0.11), respectively. FTIR spectra revealed the spectral peaks characteristic for saponins in RPM, RLB, and RBK plant powders, aqueous and methanol extracts; O-H absorption (3265 - 3393 cm^-1), C-H absorption ranging from 2851 to 2924 cm^-1, C=C absorbance (1628 - 1655 cm^-1), oligosaccharide linkage (C-O-C) absorption due to sapogenins (1036 - 1042 cm^-1). The crude saponins from RPM, RLB and RBK showed similar peaks to their respective extracts. The presence of the saponins in extracts of RPM, RLB and RBK may be responsible for some of the biological activities reported in the Ruellia species.1

Keywords: Ruellia bignoniiflora, Ruellia lineari-bracteolata, Ruellia prostrata, Saponins.

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Authors: Caighley Logan, Suzzanne McColl

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The outcome of fire related fatalities, along with other research, has found fires can have a detrimental effect to the mineral and crystalline structures within bone. This study focused on the mineral and crystalline structures within porcine bone samples to analyse the changes caused, with the intent of effectively ‘reverse engineering’ the data collected from burned bone samples to discover what may have happened. Using Fourier Transform Infrared (FTIR), and X-Ray Fluorescence (XRF), the data were collected from a controlled source of intense heat (muffle furnace) and an open fire, based in a living room setting in a standard size shipping container (2.5 m x 2.4 m) of a similar temperature with a known ignition source, a gasoline lighter. This approach is to analyse the changes to the samples and how the changes differ depending on the heat source. Results have found significant differences in the levels of remaining minerals for each type of heat/burning (p =< 0.001), particularly Phosphorus and Calcium, this also includes notable additions of absorbed elements and minerals from the surrounding materials, i.e., Cerium (Ce), Bromine (Br) and Neodymium (Ne). The analysis techniques included provide validated results in conjunction with previous studies.

Keywords: Forensic anthropology, thermal alterations, porcine bone, FTIR, XRF.

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Authors: G.Vinitha, A.Ramalingam

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TiO2 nanoparticles were synthesized by hydrothermal method at 180°C from TiOSO4 aqueous solution with1m/l concentration. The obtained products were coated with silica by means of a seeded polymerization technique for a coating time of 1440 minutes to obtain well defined TiO2@SiO2 core-shell structure. The uncoated and coated nanoparticles were characterized by using X-Ray diffraction technique (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) to study their physico-chemical properties. Evidence from XRD and FTIR results show that SiO2 is homogenously coated on the surface of titania particles. FTIR spectra show that there exists an interaction between TiO2 and SiO2 and results in the formation of Ti-O-Si chemical bonds at the interface of TiO2 particles and SiO2 coating layer. The non linear optical limiting properties of TiO2 and TiO2@SiO2 nanoparticles dispersed in ethylene glycol were studied at 532nm using 5ns Nd:YAG laser pulses. Three-photon absorption is responsible for optical limiting characteristics in these nanoparticles and it is seen that the optical nonlinearity is enhanced in core-shell structures when compared with single counterparts. This effective three-photon type absorption at this wavelength, is of potential application in fabricating optical limiting devices.

Keywords: hydrothermal method, optical limiting devicesseeded polymerization technique, three-photon type absorption

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

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

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

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Authors: Marijana M. Ačanski, Kristian A. Pastor, Djura N. Vujić

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The identification of lipid and soluble sugar components in flour samples of different cultivars belonging to common oat species (Avena sativa L.) was performed: spring oat, winter oat and hulless oat. Fatty acids were extracted from flour samples with n-hexane, and derivatized into volatile methyl esters, using TMSH (trimethylsulfonium hydroxide in methanol). Soluble sugars were then extracted from defatted and dried samples of oat flour with 96% ethanol, and further derivatized into corresponding TMS-oximes, using hydroxylamine hydrochloride solution and BSTFA (N,O-bis-(trimethylsilyl)-trifluoroacetamide). The hexane and ethanol extracts of each oat cultivar were analyzed using GC-MS system. Lipid and simple sugar compositions are very similar in all samples of investigated cultivars. Chemometric tool was applied to numeric values of automatically integrated surface areas of detected lipid and simple sugar components in their corresponding derivatized forms. Hierarchical cluster analysis shows a very high similarity between the investigated flour samples of oat cultivars, according to the fatty acid content (0.9955). Moderate similarity was observed according to the content of soluble sugars (0.50). These preliminary results support the idea of establishing methods for oat flour authentication, and provide the means for distinguishing oat flour samples, regardless of the variety, from flour samples made of other cereal species, just by lipid and simple sugar profile analysis.

Keywords: Authentication, chemometrics, GC-MS, lipid and soluble sugar composition, oat cultivars.

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Authors: N. F .Hamedani, A.R. Mahjoub, A. A. khodadadi, Y. Mortazavi, F.Farzaneh

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ZnO nanostructure were synthesized via microwave method using zinc acetate as starting material, guanidinium as structure directing agents, and water as solvent.. This work investigates the photodegradation of azo dyes using the ZnO Flowerlike in aqueous solutions. As synthesized ZnO samples were characterized using X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), and FTIR spectroscopy.In this work photodecolorization of congored azo dye under UV irradiation by nano ZnO was studied.

Keywords: Photo catalyst, Nano crystals, Zinc Oxide

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Authors: M. Kumpugdee-Vollrath, T. Subongkot, T. Ngawhirunpat

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In this project we are interested in studying different kinds of shed snake skins in order to apply them as a model membrane for pharmaceutical purposes instead of human stratum corneum. Many types of shed snake skins as well as model drugs were studied by different techniques. The data will give deeper understanding about the interaction between drugs and model membranes and may allow us to choose the suitable model membrane for studying the effect of pharmaceutical products.

Keywords: DSC, FTIR, permeation, SAXS, shed snake skin.

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy, micro Raman spectroscopy, UV-Visible absorption spectroscopy, Photoluminescence spectroscopy, Field Effect Scanning Electron Microscopy.

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Authors: Liberty L Mguni, Reinout Meijboom, Kalala Jalama

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Nano-MgO was successfully deposited on titania using deposition-precipitation method. The catalyst produced was characterised using FTIR, XRD, BET and XRF and its activity was tested on the transesterification reaction of soybean oil to biodiesel. The catalyst activity improved when the reaction temperature was increasedfrom 150 and 225 OC. It was also observed that increasing the reaction time above 1h had no significant benefit on conversion. The stability fixed MgO on TiO2 was investigated using XRF and ICP-OES. It was observed that MgO loss during the reaction was between 0.5-2.3 percent and that there was no correlation between the reaction temperature and the MgO loss.

Keywords: Nano-MgO, TiO2, transesterification

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Authors: Thanaa Abdel Moghny, Mohamed Keshawy, Mahmoud Fathy, Abdul-Raheim M. Abdul-Raheim, Khalid I. Kabel, Ahmed F. El-Kafrawy, Mahmoud Ahmed Mousa, Ahmed E. Awadallah

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Ecological pollution is of great concern for human health and the environment. Numerous organic and inorganic pollutants usually discharged into the water caused carcinogenic or toxic effect for human and different life form. In this respect, this work aims to treat water contaminated by organic and inorganic waste using sorbent based on polystyrene. Therefore, two different series of adsorbent material were prepared; the first one included the preparation of polymeric sorbent from the reaction of styrene acrylate ester and alkyl acrylate. The second series involved syntheses of composite ion exchange resins of waste polystyrene and   amorphous carbon thin film (WPS/ACTF) by solvent evaporation using micro emulsion polymerization. The produced ACTF/WPS nanocomposite was sulfonated to produce cation exchange resins ACTF/WPSS nanocomposite. The sorbents of the first series were characterized using FTIR, ¹H NMR, and gel permeation chromatography. The thermal properties of the cross-linked sorbents were investigated using thermogravimetric analysis, and the morphology was characterized by scanning electron microscope (SEM). The removal of organic pollutant was determined through absorption tests in a various organic solvent. The chemical and crystalline structure of nanocomposite of second series has been proven by studies of FTIR spectrum, X-rays, thermal analysis, SEM and TEM analysis to study morphology of resins and ACTF that assembled with polystyrene chain. It is found that the composite resins ACTF/WPSS are thermally stable and show higher chemical stability than ion exchange WPSS resins. The composite resin was evaluated for calcium hardness removal. The result is evident that the ACTF/WPSS composite has more prominent inorganic pollutant removal than WPSS resin. So, we recommend the using of nanocomposite resin as new potential applications for water treatment process.

Keywords: Nanocomposite, sorbent materials, waste water, waste polystyrene.

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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: Senem Avaz, Alpay Taralp

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Chitosan has been an attractive biopolymer for decades, but its processability is lowered by its poor solubility, especially in physiological pH values. Freeze concentrated reactions of chitosan with several organic acids including acrylic, citraconic, itaconic, and maleic acid revealed improved solubility and morphological properties. Solubility traits were assessed with a modified ninhydrin test. Chitosan derivatives were characterized by ATR-FTIR and morphological characteristics were determined by SEM. This study is a unique approach to chemically modify chitosan to enhance water solubility.

Keywords: Chitosan, Freeze Concentration, Frozen Reactions, Ninhydrin Test, Water Soluble Chitosan.

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Authors: Abbas Teimouri, Leila Ghorbanian, Iren Dabirian

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This work focused on preparation and characterizations of silk fibroin (SF)/nanodiopside nanoceramic via electrospinning process. Nanofibrous scaffolds were characterized by combined techniques of scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD). The results confirmed that fabricated SF/diopside scaffolds improved cell attachment and proliferation. The results indicated that the electrospun of SF/nanodiopside nanofibrous scaffolds could be considered as ideal candidates for tissue engineering.

Keywords: Electrospinning, nanofibers, silk fibroin, diopside, composite scaffold.

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Authors: H. Assaedi, F. U. A. Shaikh, I. M. Low

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Geopolymer composites reinforced with flax fabrics and nanoclay are fabricated and studied for physical and mechanical properties using X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscope (SEM). Nanoclay platelets at a weight of 1.0%, 2.0%, and 3.0% were added to geopolymer pastes. Nanoclay at 2.0 wt.% was found to improve density and decrease porosity while improving flexural strength and post-peak toughness. A microstructural analysis indicated that nanoclay behaves as filler and as an activator supporting geopolymeric reaction while producing a higher content geopolymer gel improving the microstructure of binders. The process enhances adhesion between the geopolymer matrix and flax fibres.

Keywords: Flax fibres, geopolymer, mechanical properties, nanoclay.

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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: Seyed Abbas Tabatabaei

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One of the important factors of cracks on the asphalt pavements is bitumen aging that associated with the loss of volatile components and oxidation of asphalt binder. This paper is about effect of Styrene-Butadiene-Styrene (SBS) polymer on asphalt aging In order to decrease asphalt aging effects. For this purpose samples of base bitumen and SBS modified bitumen aged according to the rolling thin film oven test (RTFOT) and pressure aging vessel (PAV), respectively. Properties of each sample were evaluated using Fourier Transform Infrared (FTIR) spectroscopy, n-heptane precipitation, viscosity test, softening point test and penetration test. FT-IR Analysis, showed lower oxidation of SBS modified bitumen than base bitumen, after aging.

Keywords: SBS, Asphalt aging, modified bitumen.

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Authors: A.Doustgani, E.Vasheghani- Farahani, M. Soleimani, S. Hashemi-Najafabadi

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Aligned and random nanofibrous scaffolds of PVA/PCL/nHA were fabricated by electrospinning method. The composite nanofibrous scaffolds were subjected to detailed analysis. Morphological investigations revealed that the prepared nanofibers have uniform morphology and the average fiber diameters of aligned and random scaffolds were 135.5 and 290 nm, respectively. The obtained scaffolds have a porous structure with porosity of 88 and 76% for random and aligned nanofibers, respectively. Furthermore, FTIR analysis demonstrated that there were strong intramolecular interactions between the molecules of PVA/PCL/nHA. On the other hand, mechanical characterizations show that aligning the nanofibers, could significantly improve the rigidity of the resultant biocomposite nanofibrous scaffolds.

Keywords: Electrospinnig, nanofibrous scaffold, poly (vinyl alcohol), polycaprolactone.

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Authors: Bashar Mudhaffar Abdullah, Jumat Salimon

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Optimization study of the diesters biolubricant oleyl 9(12)-hydroxy-10(13)-oleioxy-12(9)-octadecanoate (OLHYOOT) was synthesized in the presence of sulfuric acid (SA) as catalyst has been done. Optimum conditions of the experiment to obtain high yield% of OLHYOOT were predicted at ratio of OL/HYOOA of 1:1 g/g, ratio of SA/HYOOA of 0.20:1 g/g, reaction temperature 110 °C and 4.5 h of reaction time. At this condition, the Yield% of OLHYOOT was 88.7. Disappearance of carboxylic acid (C=O) peak has observed by FTIR with appearance ester (C=O) at 1738 cm-1. 1H NMR spectra analyses confirmed the result of OLHYOOT with appearance ester (-CHOCOR) at 4.05ppm and also the 13C-NMR confirmed the result with appearance ester (C=O) peak at 173.93ppm.

Keywords: Esterification, Diesters, Biolubricant, D-optimaldesign.

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Authors: Merve Küçük, M. Lütfi Öveçoğlu

Abstract:

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: Amin Eisazadeh, Khairul Anuar Kassim, Hadi Nur

Abstract:

The expansive nature of soils containing high amounts of clay minerals can be altered through chemical stabilization, resulting in a material suitable for construction purposes. The primary objective of this investigation was to study the changes induced in the molecular structure of phosphoric acid stabilized bentonite and lateritic soil using Nuclear Magnetic Resonance (NMR) and Fourier Transform Infrared (FTIR) spectroscopy. Based on the obtained data, it was found that a surface alteration mechanism was the main reason responsible for the improvement of treated soils. Furthermore, the results indicated that the Al present in the octahedral layer of clay minerals were more amenable to chemical attacks and also partly responsible for the formation of new products.

Keywords: Bentonite, Laterite clay, Molecularcharacterization, Phosphoric acid, Stabilization

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

Abstract:

Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: Green chemistry, 1H-indole, NH-containing heteroaromatic, organic electrosynthesis.

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Authors: Velid Demir, Mesut Akgün

Abstract:

The lanthanum and zinc oxide were synthesized and then loaded with 6 wt% over γ-Al2O3 using the wet impregnation method. The samples were calcined at 900 °C to ensure a coherent structure with high catalytic performance. Characterization of the catalysts was verified by X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). The effect of catalysts on biodiesel content from jatropha oil was studied under supercritical conditions. The results showed that ZnO/γ-Al2O3 was the superior catalyst for jatropha oil with 98.05% biodiesel under reaction conditions of 7 min reaction time, 1:40 oil to methanol molar ratio, 6 wt% of catalyst loading, 90 bar of reaction pressure, and 300 °C of reaction temperature, compared to 95.50% with La2O3/γ-Al2O3 at the same parameters. For this study, ZnO/γ-Al2O3 was the most suitable catalyst due to performance and cost considerations.

Keywords: Biodiesel, heterogeneous catalyst, Jatropha oil, supercritical methanol, transesterification.

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Authors: Nesrin Köken, Esin A. Güvel, Nilgün Kızılcan

Abstract:

This work presents synthesis of α,ω-dithienyl terminated poly(ethylene glycol) (PEGTh) capable for further chain extension by either chemical or electrochemical polymeriztion. PEGTh was characterized by FTIR and 1H-NMR. Further copolymerization of PEGTh and pyrrole (Py) was performed by chemical oxidative polymerization using ceric (IV) salt as an oxidant (PPy-PEGTh). PEG without end group modification was used directly to prepare copolymers with Py by Ce (IV) salt (PPy-PEG). Block copolymers with mole ratio of pyrrole to PEGTh (PEG) 50:1 and 10:1 were synthesized. The electrical conductivities of copolymers PPy-PEGTh and PPy-PEG were determined by four point probe technique. Influence of the synthetic route and content of the insulating segment on conductivity and yield of the copolymers were investigated.

Keywords: Chemical oxidative polymerization, conducting copolymer, poly(ethylene glycol), polypyrrole.

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