Search results for: impedance spectroscopy
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 535

Search results for: impedance spectroscopy

145 Cr, Fe and Se Contents of the Turkish Black and Green Teas and the Effect of Lemon Addition

Authors: E. Moroydor Derun, A. S. Kipcak, O. Dere Ozdemir, M. B. Piskin

Abstract:

Tea is consumed by a big part of the world-s population. It has an enormous importance for the Turkish culture. Nearly it is brewed every morning and evening at the all houses. Also it is consumed with lemon wedge. Habitual drinking of tea infusions may significantly contribute to daily dietary requirements of elements. Different instrumental techniques are used for determination of these elements. But atomic and mass spectroscopic methods are preferred most. In these study chromium, iron and selenium contents after the hot water brewing of black and green tea were determined by Optical Emission Spectroscopy (ICP-OES). Furthermore, effect of lemon addition on chromium, iron and selenium concentration tea infusions is investigated. Results of the investigation showed that concentration of chromium, iron and selenium increased in black tea with lemon addition. On the other hand only selenium is increased with lemon addition in green tea. And iron concentration is not detected in green tea but its concentration is determined as 1.420 ppm after lemon addition.

Keywords: Black tea, green tea, ICP-OES, lemon

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144 Synthesis of Magnesium Borates from the Slurries of Magnesium Wastes by Microwave Energy

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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143 Metal-Based Anticancer Agents: In vitro DNA Binding, Cleavage and Cytotoxicity

Authors: Mala Nath, Nagamani Kompelli, Partha Roy, Snehasish Das

Abstract:

Two new metal-based anticancer chemotherapeutic agents, [(Ph2Sn)2(HGuO)2(phen)Cl2] 1 and [(Ph3Sn)(HGuO)(phen)]- Cl.CH3OH.H2O 2, were designed, prepared and characterized by analytical and spectral (IR, ESI-Mass, 1H, 13C and 119Sn NMR) techniques. The proposed geometry of Sn(IV) in 1 and 2 is distorted octahedral and distorted trigonal-bipyramidal, respectively. Both 1 and 2 exhibit potential cytotoxicity in vitro against MCF-7, HepG-2 and DU-145 cell lines. The intrinsic binding constant (Kb) values of 1 (2.33 × 105 M-1) and 2 (2.46 × 105 M-1) evaluated from UV-Visible absorption studies suggest non-classical electrostatic mode of interaction via phosphate backbone of DNA double helix. The Stern- Volmer quenching constant (Ksv) of 1 (9.74 × 105 M-1) and 2 (2.9 × 106 M-1) determined by fluorescence studies suggests the groove binding and intercalation mode for 1 and 2, respectively. Effective cleavage of pBR322 DNA is induced by 1.Their interaction with DNA of cancer cells may account for potency.

Keywords: Anticancer agents, DNA binding studies, NMR spectroscopy, organotin.

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142 The Influence of Surface Potential on the Kinetics of Bovine Serum Albumin Adsorption on a Biomedical Grade 316LVM Stainless Steel Surface

Authors: Khawtar Hasan Ahmed, Sasha Omanovic

Abstract:

Polarization modulation infrared reflection absorption spectroscopy (PM-IRRAS) in combination with electrochemistry, was employed to study the influence of surface charge (potential) on the kinetics of bovine serum albumin (BSA) adsorption on a biomedical-grade 316LVM stainless steel surface is discussed. The BSA adsorption kinetics was found to greatly depend on the surface potential. With an increase in surface potential towards more negative values, both the BSA initial adsorption rate and the equilibrium (saturated) surface concentration also increased. Both effects were explained on the basis of replacement of well-ordered water molecules at the 316LVM / solution interface, i.e. by the increase in entropy of the system.

Keywords: adsorption, biomedical grade stainless steel, bovine serum albumin (BSA), electrode surface potential / charge, kinetics, PM-IRRAS, protein/surface interactions

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141 Zinc Oxide Nanoparticles Modified with Galactose as Potential Drug Carrier with Reduced Releasing of Zinc Ions

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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140 Electrochemical Performance of Al-Mn2O3 Based Electrode Materials

Authors: Noor Ul Ain Bhatti, M. Junaid Khan, Javed Ahmad, Murtaza Saleem, Shahid M. Ramay, Saadat A. Siddiqi

Abstract:

Manganese oxide is being recently used as electrode material for rechargeable batteries. In this study, Al incorporated Mn2O3 compositions were synthesized to study the effect of Al doping on electrochemical performance of host material. Structural studies were carried out using X-ray diffraction analysis to confirm the phase stability and explore the lattice parameters, crystallite size, lattice strain, density and cell volume. Morphology and composition were analyzed using field emission scanning electron microscope and energy dispersive X-ray spectroscopy, respectively. Dynamic light scattering analysis was performed to observe the average particle size of the compositions. FTIR measurements exhibit the O-Al-O and O-Mn-O and Al-O bonding and with increasing the concentration of Al, the vibrational peaks of Mn-O become sharper. An enhanced electrochemical performance was observed in compositions with higher Al content.

Keywords: Mn2O3, electrode materials, energy storage and conversion, electrochemical performance.

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139 Temperature Effect on the Solid-State Synthesis of Dehydrated Zinc Borates

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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138 Conventional Synthesis and Characterization of Zirconium Molybdate, Nd2Zr3(MoO4)9

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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137 Magnesium Borate Synthesis by Microwave Method Using MgCl2.6H2O and H3BO3

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

Abstract:

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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136 Strengthening and Toughening of Dental Porcelain by the Inclusion of an Yttria-Stabilized Zirconia Reinforcing Phase

Authors: Bruno Henriques, Rafaela Santos, Mihaela Buciumeanu, Júlio Matias de Souza, Filipe Silva, Rubens Nascimento, Márcio Fredel

Abstract:

Dental porcelain composites reinforced and toughened by 20 wt.% tetragonal zirconia (3Y-TZP) were processed by hot pressing at 1000°C. Two types of particles were tested: yttriastabilized zirconia (ZrO2–3%Y2O3) agglomerates and pre-sintered yttria-stabilized zirconia (ZrO2–3%Y2O3) particles. The composites as well as the reinforcing particles were analyzed by the means of optical and Scanning Electron Microscopy (SEM), Energy Dispersion Spectroscopy (EDS) and X-Ray Diffraction (XRD). The mechanical properties were obtained by the transverse rupture strength test. Wear tests were also performed on the composites and monolithic porcelain. The best mechanical results were displayed by the porcelain reinforced with the pre-sintered ZrO2–3%Y2O3 agglomerates.

Keywords: Composite, dental restoration, porcelain, strengthening, toughening, wear, zirconia.

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135 Microbial Production of Levan using Date Syrup and Investigation of Its Properties

Authors: Marzieh Moosavi-Nasab, Behnaz Layegh , Ladan Aminlari, Mohammad B. Hashemi

Abstract:

Levan, an exopolysaccharide, was produced by Microbacterium laevaniformans and its yield was characterized as a function of concentrations of date syrup, sucrose and the fermentation time. The optimum condition for levan production from sucrose was at concentration of 20% sucrose for 48 h and for date syrup was 25% for 48 h. The results show that an increase in fermentation time caused a decrease in the levan production at all concentrations of date syrup tested. Under these conditions after 48 h in sucrose medium, levan production reached 48.9 g/L and for date syrup reached 10.48 g/L . The effect of pH on the yield of the purified levan was examined and the optimum pH for levan production was determined to be 6.0. Levan was composed mainly of fructose residues when analyzed by TLC and FT-IR spectroscopy. Date syrup is a cheap substrate widely available in Iran and has potential for levan production. The thermal stability of levan was assessed by Thermo Gravimetric Analysis (TGA) that revealed the onset of decomposition near to 49°C for the levan produced from sucrose and 51°C for the levan from date syrup. DSC results showed a single Tg at 98°C for levan produced from sucrose and 206 °C for levan from date syrup.

Keywords: Date syrup, Fermentation, Levan, Microbacteriumlaevaniformans

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134 pH-Responsiveness Properties of a Biodigradable Hydrogels Based on Carrageenan-g-poly(NaAA-co-NIPAM)

Authors: Mohammad Sadeghi, Behrouz Heidari, Korush Montazeri

Abstract:

A novel thermo-sensitive superabsorbent hydrogel with salt- and pH-responsiveness properties was obtained by grafting of mixtures of acrylic acid (AA) and N-isopropylacrylamide (NIPAM) monomers onto kappa-carrageenan, kC, using ammonium persulfate (APS) as a free radical initiator in the presence of methylene bisacrylamide (MBA) as a crosslinker. Infrared spectroscopy was carried out to confirm the chemical structure of the hydrogel. Moreover, morphology of the samples was examined by scanning electron microscopy (SEM). The effect of MBA concentration and AA/NIPAM weight ratio on the water absorbency capacity has been investigated. The swelling variations of hydrogels were explained according to swelling theory based on the hydrogel chemical structure. The hydrogels exhibited salt-sensitivity and cation exchange properties. The temperature- and pH-reversibility properties of the hydrogels make the intelligent polymers as good candidates for considering as potential carriers for bioactive agents, e.g. drugs.

Keywords: superabsorbent, carrageenan, acrylic acid, Nisopropylacrylamide, hydrogel, swelling

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133 Nanomechanical Characterization of Titanium Alloy Modified by Nitrogen Ion Implantation

Authors: Josef Sepitka, Petr Vlcak, Tomas Horazdovsky, Vratislav Perina

Abstract:

An ion implantation technique was used for designing the surface area of a titanium alloy and for irradiation-enhanced hardening of the surface. The Ti6Al4V alloy was treated by nitrogen ion implantation at fluences of 2·1017 and 4·1017 cm-2 and at ion energy 90 keV. The depth distribution of the nitrogen was investigated by Rutherford Backscattering Spectroscopy. The gradient of mechanical properties was investigated by nanoindentation. The continuous measurement mode was used to obtain depth profiles of the indentation hardness and the reduced storage modulus of the modified surface area. The reduced storage modulus and the hardness increase with increasing fluence. Increased fluence shifts the peak of the mechanical properties as well as the peak of nitrogen concentration towards to the surface. This effect suggests a direct relationship between mechanical properties and nitrogen distribution.

Keywords: Nitrogen ion implantation, titanium-based nanolayer, storage modulus, hardness, microstructure.

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132 Micromachining with ECDM: Research Potentials and Experimental Investigations

Authors: C.S. Jawalkar, Apurbba Kumar Sharma, Pradeep Kumar

Abstract:

Electro Chemical Discharge Machining (ECDM) is an emerging hybrid machining process used in precision machining of hard and brittle non-conducting materials. The present paper gives a critical review on materials machined by ECDM under the prevailing machining conditions; capability indicators of the process are reported. Some results obtained while performing experiments in micro-channeling on soda lime glass using ECDM are also presented. In these experiments, Tool Wear (TW) and Material Removal (MR) were studied using design of experiments and L–4 orthogonal array. Experimental results showed that the applied voltage was the most influencing parameter in both MR and TW studies. Field emission scanning electron microscopy (FESEM) results obtained on the microchannels confirmed the presence of micro-cracks, primarily responsible for MR. Chemical etching was also seen along the edges. The Energy dispersive spectroscopy (EDS) results were used to detect the elements present in the debris and specimens.

Keywords: ECDM, applied-voltage, FESEM, EDS.

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131 Effect of pH and Ionic Exchange on the Reactivity of Bioglass/Chitosan Composites Used as a Bone Graft Substitute

Authors: Samira Jebahi, Hassane Oudadesse, Eric Wers, Jiheun Elleuch, Hafedh Elfekih, Hassib Keskes, Xuan Vuong Bui, Abdelfatteh Elfeki

Abstract:

Chitosan (CH) material reinforced by bioactive glass (46S6) was fabricated. 46S6 containing 17% wt% CH was studied in vitro and in vivo. Physicochemical techniques, such as Fourier transform infrared spectroscopy (FT-IR), coupled plasma optical emission spectrometry (ICP-OES) analysis were used. The behavior of 46S6CH17 was studied by measuring the in situ pH in a SBF solution. The 46S6CH17 was implanted in the rat femoral condyl. In vitro 46S6CH17 gave an FTIR - spectrum in which three absorption bands with the maxima at 565, 603 and 1039cm-1 after 3 days of soaking in physiological solution. They are assigned to stretching vibrations of PO4^3- group in phosphate crystalline. Moreover, the pH measurement was decreased in the SBF solution. The stability of the calcium phosphate precipitation depended on the pH value. In vivo, a rise in the Ca and phosphate P ions concentrations in the implanted microenvironment was determined.

Keywords: Bioglass, Chitosan, pH measurement, Hydroxyapatite Carbonateted Layer.

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130 Zinc Borate Synthesis Using Hydrozincite and Boric Acid with Ultrasonic Method

Authors: D. S. Vardar, A. S. Kipcak, F. T. Senberber, E. M. Derun, N. Tugrul, S. Piskin

Abstract:

Zinc borate is an important inorganic hydrate borate material, which can be used as a flame retardant agent and corrosion resistance material. This compound can loss its structural water content at higher than 290°C. Due to thermal stability; Zinc Borate can be used as flame retardant at high temperature process of plastic and gum. In this study, the ultrasonic reaction of zinc borates were studied using hydrozincite (Zn5(CO3)2·(OH)6) and boric acid (H3BO3) raw materials. Before the synthesis raw materials were characterized by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). Ultrasonic method is a new application on the zinc borate synthesis. The synthesis parameters were set to 90°C reaction temperature and 55 minutes of reaction time, with 1:1, 1:2, 1:3, 1:4 and 1:5 molar ratio of starting materials (Zn5(CO3)2·(OH)6 : H3BO3). After the zinc borate synthesis, the products were analyzed by XRD and FT-IR. As a result, optimum molar ratio of 1:5 is determined for the synthesis of zinc borates with ultrasonic method.

Keywords: Borate, ultrasonic method, zinc borate, zinc borate synthesis.

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129 Decolorization of Reactive Black 5 and Reactive Red 198 using Nanoscale Zerovalent Iron

Authors: C. Chompuchan, T. Satapanajaru, P. Suntornchot, P. Pengthamkeerati

Abstract:

Residual dye contents in textile dyeing wastewater have complex aromatic structures that are resistant to degrade in biological wastewater treatment. The objectives of this study were to determine the effectiveness of nanoscale zerovalent iron (NZVI) to decolorize Reactive Black 5 (RB5) and Reactive Red 198 (RR198) in synthesized wastewater and to investigate the effects of the iron particle size, iron dosage and solution pHs on the destruction of RB5 and RR198. Synthesized NZVI was confirmed by transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The removal kinetic rates (kobs) of RB5 (0.0109 min-1) and RR198 (0.0111 min-1) by 0.5% NZVI were many times higher than those of microscale zerovalent iron (ZVI) (0.0007 min-1 and 0.0008 min-1, respectively). The iron dosage increment exponentially increased the removal efficiencies of both RB5 and RR198. Additionally, lowering pH from 9 to 5 increased the decolorization kinetic rates of both RB5 and RR198 by NZVI. The destruction of azo bond (N=N) in the chromophore of both reactive dyes led to decolorization of dye solutions.

Keywords: decolorization, nanoscale zerovalent iron, Reactive Black 5, Reactive Red 198.

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128 Green-Reduction of Covalently Functionalized Graphene Oxide with Varying Stoichiometry

Authors: A. Pruna, D. Pullini, D. Busquets

Abstract:

Graphene-based materials were prepared by chemical reduction of covalently functionalized graphene oxide with environmentally friendly agents. Two varying stoichiometry of graphene oxide (GO) induced by using different chemical preparation conditions, further covalent functionalization of the GO materials with 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride / N-hydroxysuccinimide and ascorbic acid and sodium bisulfite as reducing agents were exploited in order to obtain controllable properties of the final solution-based graphene materials. The obtained materials were characterized by thermo-gravimetric analysis, Fourier transform infrared and Raman spectroscopy and X-ray diffraction. The results showed successful functionalization of the GO materials, while a comparison of the deoxygenation efficiency of the two-type functionalized graphene oxide suspensions by the different reducing agents has been made, revealing the strong dependence of their properties on the GO structure and reducing agents.

Keywords: Graphene oxide, covalent functionalization, reduction, ascorbic acid, sodium bisulfate.

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127 Phenolic-Based Chemical Production from Catalytic Depolymerization of Alkaline Lignin over Fumed Silica Catalyst

Authors: S. Totong, P. Daorattanachai, N. Laosiripojana

Abstract:

Lignin depolymerization into phenolic-based chemicals is an interesting process for utilizing and upgrading a benefit and value of lignin. In this study, the depolymerization reaction was performed to convert alkaline lignin into smaller molecule compounds. Fumed SiO₂ was used as a catalyst to improve catalytic activity in lignin decomposition. The important parameters in depolymerization process (i.e., reaction temperature, reaction time, etc.) were also investigated. In addition, gas chromatography with mass spectrometry (GC-MS), flame-ironized detector (GC-FID), and Fourier transform infrared spectroscopy (FT-IR) were used to analyze and characterize the lignin products. It was found that fumed SiO₂ catalyst led the good catalytic activity in lignin depolymerization. The main products from catalytic depolymerization were guaiacol, syringol, vanillin, and phenols. Additionally, metal supported on fumed SiO₂ such as Cu/SiO₂ and Ni/SiO₂ increased the catalyst activity in terms of phenolic products yield.

Keywords: Alkaline lignin, catalytic, depolymerization, fumed SiO2, phenolic-based chemicals.

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126 Heavy Metals and Polycyclic Aromatic Hydrocarbons in Roadside Soil Samples: A Review

Authors: R. Kaur, J. K. Katnoria

Abstract:

Diverse contaminants released into the environment through progress of urbanization and industrialization adversely affect human health. Among various sources of contaminants, especially, in big cities, automobiles play a significant role in aggravating the pollution. Various pollutants viz., heavy metals (Pb, Mn, Ni, Zn, As, Hg, Cd) and Polyaromatic hydrocarbons (Benzo-a-pyrene, fluoranthene, pyrene, benzo-b-anthracene, benzo-b-fluoranthene, acenaphthylene, fluorine, phenantherene, anthracene, chrysene, benzo-k-fluoranthene, benzo-e-pyrene, indenol-1,2,3-cd-pyrene, dibenzo-a,h-anthracene, benzo-ghi-perylene) are released by vehicles. Further, these pollutants are expected to cause severe mutagenic, genotoxic and carcinogenic effects. Considering this, many authors monitored the levels of pollution in roadside soil, water and plants. The present review focuses upon the analysis and effects of heavy metals and polycyclic aromatic hydrocarbons from the roadside samples.

Keywords: Automobiles, Carcinogenicity, Atomic Absorption Spectrophotometer, Gas Chromatography – Mass Spectroscopy, Soil pollution.

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125 Structural and Electronic Characterization of Supported Ni and Au Catalysts used in Environment Protection Determined by XRD,XAS and XPS methods

Authors: N. Aldea, V. Rednic, F. Matei, Tiandou Hu, M. Neumann

Abstract:

The nickel and gold nanoclusters as supported catalysts were analyzed by XAS, XRD and XPS in order to determine their local, global and electronic structure. The present study has pointed out a strong deformation of the local structure of the metal, due to its interaction with oxide supports. The average particle size, the mean squares of the microstrain, the particle size distribution and microstrain functions of the supported Ni and Au catalysts were determined by XRD method using Generalized Fermi Function for the X-ray line profiles approximation. Based on EXAFS analysis we consider that the local structure of the investigated systems is strongly distorted concerning the atomic number pairs. Metal-support interaction is confirmed by the shape changes of the probability densities of electron transitions: Ni K edge (1s → continuum and 2p), Au LIII-edge (2p3/2 → continuum, 6s, 6d5/2 and 6d3/2). XPS investigations confirm the metal-support interaction at their interface.

Keywords: local and global structure, metal-support interaction, supported metal catalysts, synchrotron radiation, X-ray absorptionspectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy.

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124 Functionalization of Carbon Nanotubes Using Nitric Acid Oxidation and DBD Plasma

Authors: M. Vesali Naseh, A. A. Khodadadi, Y. Mortazavi, O. Alizadeh Sahraei, F. Pourfayaz, S. Mosadegh Sedghi

Abstract:

In this study, multiwall carbon nanotubes (MWNTs) were modified with nitric acid chemically and by dielectric barrier discharge (DBD) plasma in an oxygen-based atmosphere. Used carbon nanotubes (CNTs) were prepared by chemical vapour deposition (CVD) floating catalyst method. For removing amorphous carbon and metal catalyst, MWNTs were exposed to dry air and washed with hydrochloric acid. Heating purified CNTs under helium atmosphere caused elimination of acidic functional groups. Fourier transformed infrared spectroscopy (FTIR) shows formation of oxygen containing groups such as C=O and COOH. Brunauer, Emmett, Teller (BET) analysis revealed that functionalization causes generation of defects on the sidewalls and opening of the ends of CNTs. Results of temperature-programmed desorption (TPD) and gas chromatography(GC) indicate that nitric acid treatment create more acidic groups than plasma treatment.

Keywords: Carbon nanotubes (CNTs), chemical treatment, functionalization, plasma.

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123 Density Functional Calculations of N-14 andB-11 NQR Parameters in the H-capped (5, 5)Single-Wall BN Nanotube

Authors: Ahmad Seif, Karim Zare, Asadallah Boshra, Mehran Aghaie

Abstract:

Density functional theory (DFT) calculations were performed to compute nitrogen-14 and boron-11 nuclear quadrupole resonance (NQR) spectroscopy parameters in the representative model of armchair boron nitride nanotube (BNNT) for the first time. The considered model consisting of 1 nm length of H-capped (5, 5) single-wall BNNT were first allowed to fully relax and then the NQR calculations were carried out on the geometrically optimized model. The evaluated nuclear quadrupole coupling constants and asymmetry parameters for the mentioned nuclei reveal that the model can be divided into seven layers of nuclei with an equivalent electrostatic environment where those nuclei at the ends of tubes have a very strong electrostatic environment compared to the other nuclei along the length of tubes. The calculations were performed via Gaussian 98 package of program.

Keywords: Armchair Nanotube, Density Functional Theory, Nuclear Quadrupole Resonance.

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122 Synthesis, Characterization and Antibacterial Screening of 3-Hydroxy-2-[3-(2/3/4-Methoxybenzoyl)Thioureido]Butyric Acid

Authors: M. S. M. Yusof, R. Ramli, S. K. C. Soh, N. Ismail, N. Ngah

Abstract:

This study presents the synthesis of a series of methoxybenzoylthiourea amino acid derivatives. The compounds were obtained from the reactions between 2/3/4-methoxybenzoyl isothiocyanate with threonine. All of the compounds were characterized via mass spectrometry, 1H and 13C NMR spectrometry, UV-Vis spectrophotometer and FT-IR spectroscopy. Mass spectra for all of the compounds showed the presence of molecular ion [M]+ peaks at m/z 312, which are in agreement to the calculated molecular weight. For 1H NMR spectra, the presence of OCH3, C=S-NH and C=O-NH protons were observed within range of δH 3.8-4.0 ppm, 11.1-11.5 ppm and 10.0-11.5 ppm, respectively. 13C NMR spectra in all compounds displayed the presence of OCH3, C=O-NH, C=O-OH and C=S carbon resonances within range of δC 55.0-57.0 ppm, 165.0-168.0 ppm, 170.0-171.0 ppm and 180.0-182.0 ppm, respectively. In UV spectra, two absorption bands have been observed and both were assigned to the n-π* and π-π* transitions. Six vibrational modes of v(N-H), v(O-H), v(C=O-OH), v(C=O-NH), v(C=C) aromatic and v(C=S) appeared in the FT-IR spectra within the range of 3241-3467 cm-1, 2976-3302 cm-1, 1720-1768 cm-1, 1655-1672 cm-1, 1519-1525 cm-1 and 754-763 cm-1, respectively. The antibacterial activity for all of the compounds was screened against Staphylococcus aureus, Staphylococcus epidermidis, Salmonella typhimurium and Escherichia coli. However, no activity was observed.

Keywords: Methoxybenzoyl isothiocyanate, amino acid, threonine, antibacterial.

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121 Effect of Different Types of Nano/Micro Fillers on the Interfacial Shear Properties of Polyamide 6 with De-Sized Carbon Fiber

Authors: Mohamed H. Gabr, Kiyoshi Uzawa

Abstract:

The current study aims to investigate the effect of fillers with different geometries and sizes on the interfacial shear properties of PA6 composites with de-sized carbon fiber. The fillers which have been investigated are namely; nano-layer silicates (nanoclay), sub-micro aluminum titanium (ALTi) particles, and multiwall carbon nanotube (MWCNT). By means of X-ray photoelectron spectroscopy (XPS), epoxide group which defined as a sizing agent, has been removed. Sizing removal can reduce the acid parameter of carbon fibers surface promoting bonding strength at the fiber/matrix interface which is a desirable property for the carbon fiber composites. Microdroplet test showed that the interfacial shear strength (IFSS) has been enhanced with the addition of 10wt% ALTi by about 23% comparing with neat PA6. However, with including other types of fillers into PA6, the results did not show enhancement of IFSS.

Keywords: Sub-micro-filler, nano-composites, interfacial shear strength, polyamide.

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120 Extraction of Polystyrene from Styrofoam Waste: Synthesis of Novel Chelating Resin for the Enrichment and Speciation of Cr(III)/Cr(VI) Ions in Industrial Effluents

Authors: Ali N. Siyal, Saima Q. Memon, Latif Elçi, Aydan Elçi

Abstract:

Polystyrene (PS) was extracted from Styrofoam (expanded polystyrene foam) waste, so called white pollutant. The PS was functionalized with N,N- Bis(2-aminobenzylidene)benzene-1,2-diamine (ABA) ligand through an azo spacer. The resin was characterized by FT-IR spectroscopy and elemental analysis. The PS-N=N-ABA resin was used for the enrichment and speciation of Cr(III)/Cr(VI) ions and total Cr determination in aqueous samples by flame atomic absorption spectrometry (FAAS). The separation of Cr(III)/Cr(VI) ions was achieved at pH 2. The recovery of Cr(VI) ions was achieved ≥ 95.0% at optimum parameters: pH 2; resin amount 300mg; flow rates 2.0mL min-1 of solution and 2.0mL min-1 of eluent (2.0mol L-1 HNO3). Total Cr was determined by oxidation of Cr(III) to Cr(VI) ions using H2O2. The limit of detection (LOD) and quantification (LOQ) of Cr(VI) were found to be 0.40 and 1.20μg L-1, respectively with preconcentration factor of 250. Total saturation and breakthrough capacitates of the resin for Cr(IV) ions were found to be 0.181 and 0.531mmol g-1, respectively. The proposed method was successfully applied for the preconcentration/speciation of Cr(III)/Cr(VI) ions and determination of total Cr in industrial effluents.

Keywords: Styrofoam waste, Polymeric resin, Preconcentration, Speciation, Cr(III)/Cr(VI) ions, FAAS.

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119 Binding Ability of Carbazolylphenyl Dendrimers with Zinc (II) Tetraphenylporphyrin Core towards Cryptands

Authors: Galina Mamardashvili, Nugzar Mamardashvili, Win Dehaen

Abstract:

The processes of complexation of the Zn-tetraarylporphyrins with eight 4-(4-(3,6-bis(t-butyl)carbazol-9-yl-phenyl)-1,2,3-triazole (ZnP1) and eight 4-(4-(3,6-di-tert-butyl-9-H-carbazol-9-yl)phenoxy)methyl)-2,4,6-trimethylphenyl (ZnP2)with the 1,10-diaza-4,7,13,18tetraoxabicyclo[8.5.5]eicosane (L1),1,10-diaza-4,7,13,16,21,24-hexaoxabicyclo[8.8.8]hexacosane (L2)and 1,10-diaza-5,6,14,15-dibenzo-4,7,13,16,21,24 hexaoxabicyclo[8.8.8] hexacosane (L3) were investigated by the method of spectrophotometric titration and 1H NMR-spectroscopy. We determined the structures of the host-guest complexes, and their stability constants in toluene were calculated. It was found out that the ZnP1 interacts with the guest molecules L1, L2 with the formation of stable "nest" type complexes and does not form similar complexes with the L3 (presumably due to the fact that the L3 does not match the size of the porphyrin ZnP(1) cavity). On the other hand, the porphyrin ZnP2 binds all of the ligands L1-L3, however complexes thus formed are less stable than complexes ZnP1-L1, ZnP1-L2. In the report, we will also discuss the influence of the alkali cations additives on the stability of the complexes between the porphyrin ZnP1, ZnP2 hosts and guest molecules of the ligands L1-L3.

Keywords: Porphyrin, cryptand, cation, complex guest-host.

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118 Electrochemical Performance of Carbon Nanotube Based Supercapacitor

Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

Abstract:

Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750oC analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: Carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry.

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117 A Study for Carbonation Degree on Concrete using a Phenolphthalein Indicator and Fourier-Transform Infrared Spectroscopy

Authors: Ho Jae Lee, Do Gyeum Kim, Jang Hwa Lee, Myoung Suk Cho

Abstract:

A concrete structure is designed and constructed for its purpose of use, and is expected to maintain its function for the target durable years from when it was planned. Nevertheless, as time elapses the structure gradually deteriorates and then eventually degrades to the point where the structure cannot exert the function for which it was planned. The performance of concrete that is able to maintain the level of the performance required over the designed period of use as it has less deterioration caused by the elapse of time under the designed condition is referred to as Durability. There are a number of causes of durability degradation, but especially chloride damage, carbonation, freeze-thaw, etc are the main causes. In this study, carbonation, one of the main causes of deterioration of the durability of a concrete structure, was investigated via a microstructure analysis technique. The method for the measurement of carbonation was studied using the existing indicator method, and the method of measuring the progress of carbonation in a quantitative manner was simultaneously studied using a FT-IR (Fourier-Transform Infrared) Spectrometer along with the microstructure analysis technique.

Keywords: Concrete, Carbonation, Microsturcture, FT-IR

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116 Effect of Laser Input Energy on the Laser Joining of Polyethylene Terephthalate to Titanium

Authors: Y. J. Chen, T. M. Yue, Z. N. Guo

Abstract:

This paper reports the effects of laser energy on the characteristics of bubbles generated in the weld zone and the formation of new chemical bonds at the Polyethylene Terephthalate (PET)/Ti joint interface in laser joining of PET to Ti. The samples were produced by using different laser energies ranging from 1.5 J – 6 J in steps of 1.5 J, while all other joining parameters remained unchanged. The types of chemical bonding at the joint interface were analysed by the x-ray photoelectron spectroscopy (XPS) depth-profiling method. The results show that the characteristics of the bubbles and the thickness of the chemically bonded interface, which contains the laser generated bonds of Ti–C and Ti–O, increase markedly with increasing laser energy input. The tensile failure load of the joint depends on the combined effect of the amount and distribution of the bubbles formed and the chemical bonding intensity of the joint interface.

Keywords: Laser direct joining, Ti/PET interface, laser energy, XPS depth profiling, chemical bond, tensile failure load.

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